PATENT ABSTRACT
Disclosed are methods of purifying (20R) and (20S) analogs of 2-methylene-19-nor-22-dimethyl-1α,25-dihydroxyvitamin D 3  to obtain the (20R) and (20S) analogs in crystalline form. The method includes the steps of preparing a solvent of either diethyl ether or a mixture of 2-propanol and hexane, dissolving a product containing the (20R) and (20S) analog to be purified in the solvent, cooling the solvent and dissolved product below ambient temperature for a sufficient amount of time to form a precipitate of crystals, and recovering the crystals.

PATENT DESCRIPTION
CROSS-REFERENCE TO RELATED PATENT APPLICATIONS 
       [0001]    The present application claims the benefit under 35 U.S.C. §119(e) to U.S. Provisional Patent Application No. 61/652,965, filed on May 30, 2012, the content of which is incorporated herein by reference in its entirety. 
     
    
     STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT 
       [0002]    This invention was made with government support under DK047814 awarded by the National Institutes of Health. The government has certain rights in the invention. 
     
    
     BACKGROUND 
       [0003]    The field of the present invention relates to purification of organic compounds, and more particularly to the purification of (20S) and (20R) analogs of 2-Methylene-19-nor-22-dimethyl-1α,25-dihydroxyvitamin D 3  (referred to herein as “MET-1” and “MET-2” respectively) by preparing them in crystalline form. 
         [0004]    Purification of organic compounds, especially those designated for pharmaceutical use, is of considerable importance for chemists synthesizing such compounds. Preparation of the compound usually requires many synthetic steps and, therefore, the final product can be contaminated not only with side-products derived from the last synthetic step of the procedure but also with compounds that were formed in previous steps. Even chromatographic purification, which is a very efficient but relatively time-consuming process, does not usually provide compounds which are sufficiently pure to be used as drugs. 
         [0005]    Depending on the method used to synthesize 1α-hydroxyvitamin D compounds, different minor undesirable compounds can accompany the final product. Thus, for example, if direct C-1 hydroxylation of the 5,6-trans geometric isomer of vitamin D is performed, followed by SeO 2 /NMO oxidation and photochemical irradiation, (see Andrews et al.,  J. Org. Chem.  51, 1635 (1986); Calverley et al.,  Tetrahedron  43, 4609 (1987); Choudry et al.,  J. Org. Chem.  58, 1496 (1993)), the final 1α-hydroxyvitamin D product can be contaminated with 1β-hydroxy- as well as 5,6-trans isomers. If the method consists of C-1 allylic oxidation of the 4-phenyl-1,2,4-triazoline-3,5-dione adduct of the pre-vitamin D compound, followed by cycloreversion of the modified adduct under basic conditions, (see Nevinckx et al.,  Tetrahedron  47, 9419 (1991); Vanmaele et al.,  Tetrahedron  41, 141 (1985) and 40, 1179 (1994); Vanmaele et al.,  Tetrahedron Lett.  23. 995 (1982)), one can expect that the desired 1α-hydroxyvitamin can be contaminated with the pre-vitamin 5(10), 6,8-triene and 1β-hydroxy isomer. One of the most useful C-1 hydroxylation methods, of very broad scope and numerous applications, is the experimentally simple procedure elaborated by Paaren et al.,  J. Org. Chem.  45, 3253 (1980) and  Proc. Natl. Acad. Sci. U.S.A.  75, 2080 (1978). This method consists of allylic oxidation of 3,5-cyclovitamin D derivatives, readily obtained from the buffered solvolysis of vitamin D tosylates, with SeO 2 /t-BuOOH and subsequent acid-catalyzed cycloreversion to the desired 1α-hydroxy compounds. Taking into account this synthetic path, it is reasonable to assume that the final product can be contaminated with 1α-hydroxy epimer, 5,6-trans isomer and the previtamin D form. 1α-hydroxyvitamin D 4  is another undesirable contaminant found in 1α-hydroxyvitamin D compounds synthesized from vitamin D 2  or from ergosterol. 1α-hydroxyvitamin D 4  results from C-1 oxidation of vitamin D 4 , which in turn is derived from contamination of the commercial ergosterol material. Typically, the final product may contain up to about 1.5% by weight 1α-hydroxyvitamin D 4 . Thus, a purification technique that would eliminate or substantially reduce the amount of 1α-hydroxyvitamin D 4  in the final product to less than about 0.1-0.2% would be highly desirable. 
         [0006]    The vitamin D conjugated triene system is not only heat- and light-sensitive but it is also prone to oxidation, leading to the complex mixture of very polar compounds. Oxidation usually happens when a vitamin D compound has been stored for a prolonged time. Other types of processes that can lead to a partial decomposition of vitamin D compounds consist of some water-elimination reactions. The driving force for these reactions is the allylic (1α-) and homoallylic (3β-) position of the hydroxy groups. The presence of such above-mentioned oxidation and elimination products can be easily detected by thin-layer chromatography. 
         [0007]    Usually, all 1α-hydroxylatation procedures require at least one chromatographic purification. However, even chromatographically purified 1α-hydroxyvitamin D compounds, although showing consistent spectroscopic data that suggests homogeneity, do not meet the purity criteria required for therapeutic agents that can be orally, parenterally or transdermally administered. Therefore, it is evident that a suitable method of purification of the 1α-hydroxylated vitamin D compounds MET-1 and MET-2 is required. 
       SUMMARY 
       [0008]    Disclosed are methods of purifying MET-1 and MET-2 by means of crystallization to obtain MET-1 and MET-2 in crystalline form. The solvent plays an important role in the crystallization process, and is typically an individual liquid substance or a suitable mixture of different liquids. For crystallizing MET-1 and MET-2, the most appropriate solvent and/or solvent system is characterized by the following factors:
       (1) low toxicity;   (2) low boiling point;   (3) significant dependence of solubility properties with regard to temperature (condition necessary for providing satisfactory crystallization yield); and   (4) relatively low cost.       
 
         [0013]    Interestingly, hexane, so frequently used for crystallization purposes, was found less suitable as the sole solvent for crystallization of MET-1 and MET-2. However, it was found that diethyl ether (Et 2 O) was most useful for the crystallization of MET-1, and a mixture of 2-propanol and hexane, was most useful for the crystallization of MET-2. In particular, it was determined that a mixture of about 10% to about 20% 2-propanol with about 90% to about 80% hexane by volume, (preferably 15% 2-propanol with about 85% hexane by volume) performed well. The diethyl ether solvent and the 2-propanol/hexane solvent mixture both were easy to remove by evaporation or other well-known methods. In all cases the crystallization process occurred easily and efficiently. The precipitated crystals were sufficiently large to assure their recovery by filtration or other means, and thus were suitable for x-ray analysis. 
         [0014]    Accordingly, disclosed is a compound having the formula: 
         [0000]    
       
                 
         
             
             
         
       
     
         [0000]    in crystalline form, where the wavy line at carbon 20 indicates the methyl group attached to carbon 20 may be in its R or S orientation. More specifically, disclosed are (20S)-2-methylene-19-nor-22-dimethyl-1α,25-dihydroxyvitamin D 3  in crystalline form (otherwise referred to as “MET-1”), and (20R)-2-methylene-19-nor-22-dimethyl-1α,25-dihydroxyvitamin D 3  in crystalline form, (otherwise referred to as “MET-2”). 
     
    
     
       BRIEF DESCRIPTION OF THE DRAWINGS 
         [0015]      FIG. 1  is an illustration of the three dimensional molecular structure for MET-1 as defined by the atomic positional parameters discovered and set forth herein. 
           [0016]      FIG. 2  is an illustration of the three dimensional molecular structure for MET-2 as defined by the atomic positional parameters discovered and set forth herein. 
       
    
    
     DETAILED DESCRIPTION 
       [0017]    Disclosed herein is (20S)-2-methylene-19-nor-22-dimethyl-1α,25-dihydroxyvitamin D3 (MET-1) in crystalline form, which is a pharmacologically important compound characterized by the formula I shown below: 
         [0000]    
       
                 
         
             
             
         
       
     
         [0018]    Also disclosed herein is (20R)-2-methylene-19-nor-22-dimethyl-1α,25-dihydroxyvitamin D3 (MET-2) in crystalline form, which also is a pharmacologically important compound characterized by the formula II shown below: 
         [0000]    
       
                 
         
             
             
         
       
     
         [0019]    Also disclosed herein are methods of purifying MET-1 and MET-2. The purification technique typically involves obtaining the MET-1 and MET-2 products in crystalline form by utilizing a crystallization procedure wherein the material to be purified is dissolved using as the solvent either diethyl ether (Et 2 O) as the sole solvent to obtain MET-1, or a mixture comprised of 2-propanol and hexane to obtain MET-2. In particular, it was determined that a mixture of about 10% to about 20% 2-propanol (v/v) with about 90% to about 80% hexane (v/v) performed well. Preferably the mixture comprises about 15% 2-propanol (v/v) and about 85% hexane (v/v). Thereafter, the solvent can be removed by evaporation, with or without vacuum, or other means as is well-known in the art. Alternatively, the resultant crystals may be filtered from the mother liquor. The technique can be used to purify a wide range of final products containing MET-1 and MET-2 obtained from any known synthesis thereof, and in varying concentrations, which may range from microgram amounts to kilogram amounts. As is well known to those skilled in this art, the amount of solvent utilized should be modulated according to the amount of MET-1 and MET-2 to be purified. 
       EXAMPLES 
       [0020]    The following examples are illustrative and should not be interpreted as limiting the claimed subject matter. 
         [0021]    The usefulness and advantages of the present crystallization procedure is shown in the following specific Examples. After crystallization, the precipitated material was observed under a microscope to confirm its crystalline form. Yields of crystals were relatively high and the obtained crystals showed a relatively sharp melting point of 99° C. (MET-1) and 154° C. (MET-2). 
         [0022]    The described crystallization process of the synthetic MET-1 and MET-2 products represents a valuable purification method, which can remove most side products derived from the synthetic path. Such impurity may result from contamination of starting raw materials. The crystallization process occurred easily and efficiently. The precipitated crystals were sufficiently large to assure their recovery by filtration, or other means, and thus were suitable for x-ray analysis. 
       Example 1 
     Crystallization of (20S)-2-methylene-19-nor-22-dimethyl-1α,25 dihydroxyvitamin D 3  (MET-1) 
       [0023]    Crystallization from Diethyl Ether. 
         [0024]    (20 S2-methylene-19-nor-22-dimethyl-1α,25-dihydroxyvitamin D 3  (MET-1) (14.3 mg), was dissolved in boiling diethyl ether (3 mL) and left at room temperature for about 1 hour, then it was kept in a refrigerator for about 48 hours. The precipitated crystals were filtered off, washed with a small volume of a cold (0° C.) diethyl ether, and dried to give crystalline material. 
         [0025]    Experimental. 
         [0026]    A colorless prism-shaped crystal of dimensions 0.25×0.34×0.55 mm was selected for structural analysis. Intensity data were collected using a Bruker AXS Platinum 135 CCD detector controlled with the PROTEUM software suite (Bruker AXS Inc., Madison, Wis.). The x-ray source was CuK radiation (1.54178 Å) from a Rigaku RU200 x-ray generator equipped with Montel optics, operated at 50 kV and 90 mA. The x-ray data were processed with SAINT version 7.06 A (Broker AXS Inc.) and internally scaled with SADABS version 2005/1 (Broker AXS Inc.). The sample was mounted on a glass fiber using vacuum grease and cooled to 100 K. The intensity data were measured as a series of phi and omega oscillation frames each of 1 o  for 10-25 sec/frame. The detector was operated in 1024×1024 mode and was positioned 4.5 cm from the sample. Cell parameters were determined from a non-linear least squares fit of 3265 peaks in the range of 4.0&lt;theta&lt;55°. The data were merged to form a set of 4624 independent data with R(int)=0.0287. 
         [0027]    The monoclinic space group P2(1) was determined by systematic absences and statistical tests and verified by subsequent refinement. The structure was solved by direct methods and refined by full-matrix least-squares methods on F 2 , (a) G. M. Sheldrick (1994), SHELXTL Version 5 Reference Manual, Broker AXS Inc.; (b)  International Tables for Crystallography, Vol . C, Kluwer: Boston (1995). Hydrogen atom positions were determined from difference peaks and ultimately refined by a riding model with idealized geometry. Non-hydrogen atoms were refined with anisotropic displacement parameters. In addition to the molecule of MET-1, one molecule of diethyl ether was present in the asymmetric unit of the crystalline lattice. A total of 334 parameters were refined against 1 restraint and 4624 data to give wR2=0.0995 and S=1.040 for weights of w=1/[s 2 (F 2 ) (0.0675P) 2 ], where P=[F o   2 +2F c   2 ]/3. The final R(F) was 0.0332 for the 4624 observed data. The largest shift/s.u. was 0.001 in the final refinement cycle and the final difference map had maxima and minima of 0.238 and −0.201 e/Å 3 , respectively. The absolute structure was determined by refinement of the Flack parameter, H. D. Flack,  Acta Cryst. A, vol.  39, 876-881 (1983). 
         [0028]    The three dimensional structure of MET-1 as defined by the following physical data and atomic positional parameters described and calculated herein (Tables 1-8) is illustrated in  FIG. 1 . 
       Example 2 
     Crystallization of (20R)-2-methylene-19-nor-22-dimethyl-1α,25-dihydroxyvitamin D 3  (MET-2) 
       [0029]    Crystallization from 2-propanol/hexane. 
         [0030]    (20R)-2-methylene-19-nor-22-dimethyl-1α,25-dihydroxyvitamin D 3  (22.7 mg), was suspended in hexane (4 mL) and then 2-propanol was added dropwise to the suspension. The mixture was heated in a water bath to dissolve the vitamin, then was left at room temperature for about 1 hour, and finally was kept in a refrigerator for about 48 hours. The precipitated crystals were filtered off, washed with a small volume of a cold (0° C.) 2-propanol/hexane (3:1) mixture, and dried to give crystalline material. It should be noted that an excess of 2-propanol should be avoided to get the point of saturation, i.e. only about 1 mole or less of 2-propanol should be added. 
         [0031]    Experimental. 
         [0032]    A colorless prism-shaped crystal of dimensions 0.36×0.17 x 0.03 mm was selected for structural analysis. Intensity data were collected using a Bruker AXS Platinum 135 CCD detector controlled with the PROTEUM software suite (Bruker AXS Inc., Madison, Wis.). The x-ray source was CuK radiation (1.54178 Å) from a Rigaku RU200 x-ray generator equipped with Montel optics, operated at 50 kV and 90 mA.The x-ray data were processed with SAINT version 7.06 A (Bruker AXS Inc.) and internally scaled with SADABS version 2005/1 (Bruker AXS Inc.). The sample was mounted in a quartz capillary tube and data collected at 298 K. The intensity data were measured as a series of phi and omega oscillation frames each of 1 o  for 20-40 sec/frame. The detector was operated in 1024×1024 mode and was positioned 4.5 cm from the sample. Cell parameters were determined from a non-linear least squares fit of 9999 peaks in the range of 2.51&lt;theta&lt;58.69 o . The data were merged to form a set of 3985 independent data with R(int)=0.0473. 
         [0033]    The monoclinic space group C2 was determined by systematic absences and statistical tests and verified by subsequent refinement. The structure was solved by direct methods and refined by full-matrix least-squares methods on F 2 , (a) G. M. Sheldrick (1994), SHELXTL Version 5 Reference Manual, Bruker AXS Inc.; (b)  International Tables for Crystallography, Vol . C, Kluwer: Boston (1995). Hydrogen atom positions were determined from difference peaks and ultimately refined by a riding model with idealized geometry. Non-hydrogen atoms were refined with anisotropic displacement parameters. In addition to the molecule of MET-2, one molecule of isopropanol was present in the asymmetric unit of the crystalline lattice. A total of 325 parameters were refined against 1 restraint and 3985 data to give wR2=0.1600 and S=1.073 for weights of w=1/[s 2 (F 2 )+(0.1033P) 2 ], where P=[F o   2 +2F c   2 ]/3. The final R(F) was 0.0844 for the 3985 observed data. The largest shift/s.u. was 0.001 in the final refinement cycle and the final difference map had maxima and minima of 0.140 and −0.190 e/Å 3 , respectively. The absolute structure was determined by refinement of the Flack parameter, H. D. Flack,  Acta Cryst. A , vol. 39, 876-881 (1983). 
         [0034]    The three dimensional structure of MET-2 as defined by the following physical data and atomic positional parameters described and calculated herein (Tables 9-16) is illustrated in  FIG. 2 . 
         [0000]    
       
         
               
             
               
               
               
             
               
               
             
           
               
                 TABLE 1 
               
               
                   
               
               
                 Crystal data and structure refinement for MET-1. 
               
               
                   
               
             
             
               
                   
               
             
          
           
               
                 Empirical formula 
                 C33H58O4 
                   
               
               
                 Formula weight 
                 518.79 
               
               
                 Temperature 
                 100(1) K 
               
               
                 Wavelength 
                 1.54178 Å 
               
               
                 Crystal system, space group 
                 Monoclinic, P2(1) 
               
               
                 Unit cell dimensions 
                 a = 7.5780(15)Å 
                 α = 90° 
               
               
                   
                 b = 14.792(3) Å 
                 β = 102.22(3)° 
               
               
                   
                 c = 14.481(3) Å 
                 γ = 9° 
               
             
          
           
               
                 Volume 
                 1586.5(6) Å 3   
               
               
                 Z 
                  2 
               
               
                 Calculated density 
                 1.086 Mg/m 3   
               
               
                 Absorption coefficient 
                 0.532 mm −1   
               
               
                 F(000) 
                 576 
               
               
                 Crystal size 
                 0.25 × 0.34 × 0.55 mm 
               
               
                 Theta range for data collection 
                 3.12 to 63.06° 
               
               
                 Limiting indices 
                 −8 &lt;= h &lt;= 8, −17 &lt;= k &lt;= 16, 
               
               
                   
                 0 &lt;= l &lt;= 16 
               
               
                 Reflections collected/unique 
                 7564/4624 [R(int) = 0.0287] 
               
               
                 Data/restraints/parameters 
                 4624/1/334 
               
               
                 Goodness-of-fit on F 2   
                  1.040 
               
               
                 Final R indices [I &gt; 2□(I)] 
                 R1 = 0.0330, wR2 = 0.0955 
               
               
                 R indices (all data) 
                 R1 = 0.0332, wR2 = 0.0959 
               
               
                 Absolute structure parameter 
                  −0.01(15) 
               
               
                 Largest diff. peak and hole 
                 0.238 and −0.201 e/Å 3   
               
               
                   
               
             
          
         
       
     
         [0000]    
       
         
               
             
               
               
               
               
               
             
               
               
               
               
               
               
             
           
               
                 TABLE 2 
               
             
             
               
                   
               
               
                 Atomic coordinates (Å 2  × 10 4 ) and equivalent isotropic 
               
               
                 displacement parameters (Å 2  × 10 3 ) for MET-1 U(eq) 
               
               
                 is defined as one third of the trace of the orthogonalized Uij tensor. 
               
             
          
           
               
                   
                 x 
                 y 
                 z 
                 U(eq) 
               
               
                   
                   
               
             
          
           
               
                   
                 O(3) 
                 −1435(2) 
                 3847(1) 
                 11389(1) 
                 26(1) 
               
               
                   
                 O(100) 
                 −1576(2) 
                 5643(1) 
                 10959(1) 
                 32(1) 
               
               
                   
                 O(25) 
                 −4404(2) 
                 −6333(1) 
                 12194(1) 
                 27(1) 
               
               
                   
                 O(1) 
                 3382(2) 
                 2361(1) 
                 11284(1) 
                 28(1) 
               
               
                   
                 C(5) 
                 −1471(2) 
                 1831(1) 
                 11117(1) 
                 22(1) 
               
               
                   
                 C(13) 
                 −3621(2) 
                 −1411(1) 
                 13186(1) 
                 22(1) 
               
               
                   
                 C(6) 
                 −2465(2) 
                 1391(1) 
                 11638(1) 
                 23(1) 
               
               
                   
                 C(20) 
                 −3217(2) 
                 −3144(1) 
                 13759(1) 
                 23(1) 
               
               
                   
                 C(14) 
                 −2234(2) 
                 −617(1) 
                 13380(1) 
                 23(1) 
               
               
                   
                 C(2) 
                 716(2) 
                 3237(1) 
                 10539(1) 
                 24(1) 
               
               
                   
                 C(22) 
                 −2071(2) 
                 −3839(1) 
                 14466(1) 
                 27(1) 
               
               
                   
                 C(7) 
                 −1882(2) 
                 618(1) 
                 12255(1) 
                 23(1) 
               
               
                   
                 C(4) 
                 −2313(2) 
                 2542(1) 
                 10414(1) 
                 24(1) 
               
               
                   
                 C(8) 
                 −2850(2) 
                 217(1) 
                 12818(1) 
                 24(1) 
               
               
                   
                 C(23) 
                 −2980(2) 
                 −4791(1) 
                 14332(1) 
                 28(1) 
               
               
                   
                 C(3) 
                 −1246(2) 
                 3423(1) 
                 10520(1) 
                 25(1) 
               
               
                   
                 C(21) 
                 −5206(2) 
                 −3181(1) 
                 13826(1) 
                 30(1) 
               
               
                   
                 C(24) 
                 −3359(2) 
                 −5161(1) 
                 13320(1) 
                 27(1) 
               
               
                   
                 C(1) 
                 1560(2) 
                 2561(1) 
                 11290(1) 
                 23(1) 
               
               
                   
                 C(10) 
                 502(2) 
                 1670(1) 
                 11152(1) 
                 22(1) 
               
               
                   
                 C(15) 
                 −456(2) 
                 −1058(1) 
                 13319(1) 
                 26(1) 
               
               
                   
                 C(12) 
                 −5392(2) 
                 −1054(1) 
                 13413(1) 
                 28(1) 
               
               
                   
                 C(9) 
                 −4631(2) 
                 555(1) 
                 12982(1) 
                 29(1) 
               
               
                   
                 C(17) 
                 −2546(2) 
                 −2145(1) 
                 13863(1) 
                 22(1) 
               
               
                   
                 C(101) 
                 −280(3) 
                 6264(1) 
                 11455(1) 
                 40(1) 
               
               
                   
                 C(29) 
                 1591(3) 
                 3619(1) 
                 9940(1) 
                 31(1) 
               
               
                   
                 C(30) 
                 −125(2) 
                 −3978(1) 
                 14326(1) 
                 31(1) 
               
               
                   
                 C(16) 
                 −580(2) 
                 −2012(1) 
                 13723(1) 
                 25(1) 
               
               
                   
                 C(18) 
                 −3930(2) 
                 −1723(1) 
                 12152(1) 
                 24(1) 
               
               
                   
                 C(11) 
                 −6056(2) 
                 −197(1) 
                 12851(1) 
                 29(1) 
               
               
                   
                 C(25) 
                 −3972(3) 
                 −6149(1) 
                 13189(1) 
                 31(1) 
               
               
                   
                 C(201) 
                 −3380(3) 
                 6000(1) 
                 10736(1) 
                 38(1) 
               
               
                   
                 C(27) 
                 −2516(4) 
                 −6804(2) 
                 13656(2) 
                 65(1) 
               
               
                   
                 C(28) 
                 −1941(3) 
                 −3553(1) 
                 15498(1) 
                 35(1) 
               
               
                   
                 C(202) 
                 −4591(3) 
                 5306(2) 
                 10178(2) 
                 48(1) 
               
               
                   
                 C(26) 
                 −5726(3) 
                 −6301(2) 
                 13518(1) 
                 50(1) 
               
               
                   
                 C(102) 
                 1535(3) 
                 5832(2) 
                 11596(2) 
                 54(1) 
               
               
                   
                   
               
             
          
         
       
     
         [0000]    
       
         
               
             
               
               
               
               
             
           
               
                 TABLE 3 
               
               
                   
               
               
                 Bond lengths [Å] for MET-1. 
               
               
                   
               
             
             
               
                   
               
             
          
           
               
                 O(3)—C(3) 
                 1.440(2) 
                 O(100)—C(101) 
                 1.423(2) 
               
               
                 O(100)—C(201) 
                 1.437(2) 
                 O(25)—C(25) 
                 1.435(2) 
               
               
                 O(1)—C(1) 
                 1.4140(19) 
                 C(5)—C(6) 
                 1.342(2) 
               
               
                 C(5)—C(10) 
                 1.504(2) 
                 C(5)—C(4) 
                 1.508(2) 
               
               
                 C(13)—C(18) 
                 1.537(2) 
                 C(13)—C(12) 
                 1.542(2) 
               
               
                 C(13)—C(14) 
                 1.561(2) 
                 C(13)—C(17) 
                 1.570(2) 
               
               
                 C(6)—C(7) 
                 1.461(2) 
                 C(20)—C(21) 
                 1.532(2) 
               
               
                 C(20)—C(17) 
                 1.559(2) 
                 C(20)—C(22) 
                 1.575(2) 
               
               
                 C(14)—C(8) 
                 1.497(2) 
                 C(14)—C(15) 
                 1.516(2) 
               
               
                 C(2)—C(29) 
                 1.325(2) 
                 C(2)—C(3) 
                 1.506(2) 
               
               
                 C(2)—C(1) 
                 1.516(2) 
                 C(22)—C(28) 
                 1.536(2) 
               
               
                 C(22)—C(30) 
                 1.544(2) 
                 C(22)—C(23) 
                 1.562(2) 
               
               
                 C(7)—C(8) 
                 1.345(2) 
                 C(4)—C(3) 
                 1.524(2) 
               
               
                 C(8)—C(9) 
                 1.505(2) 
                 C(23)—C(24) 
                 1.533(2) 
               
               
                 C(24)—C(25) 
                 1.532(2) 
                 C(1)—C(10) 
                 1.533(2) 
               
               
                 C(15)—C(16) 
                 1.539(2) 
                 C(12)—C(11) 
                 1.532(2) 
               
               
                 C(9)—C(11) 
                 1.534(2) 
                 C(17)—C(16) 
                 1.558(2) 
               
               
                 C(101)—C(102) 
                 1.491(3) 
                 C(25)—C(27) 
                 1.516(3) 
               
               
                 C(25)—C(26) 
                 1.521(3) 
                 C(201)—C(202) 
                 1.495(3) 
               
               
                   
               
             
          
         
       
     
         [0000]    
       
         
               
             
               
               
               
             
           
               
                 TABLE 4 
               
               
                   
               
               
                 Bond angles [°] for MET-1. 
               
               
                   
               
             
             
               
                   
               
             
          
           
               
                   
                 C(101)—O(100)—C(201) 
                 113.47(15) 
               
               
                   
                 C(6)—C(5)—C(10) 
                 125.17(14) 
               
               
                   
                 C(6)—C(5)—C(4) 
                 120.68(15) 
               
               
                   
                 C(10)—C(5)—C(4) 
                 114.14(13) 
               
               
                   
                 C(18)—C(13)—C(12) 
                 110.52(13) 
               
               
                   
                 C(18)—C(13)—C(14) 
                 111.04(12) 
               
               
                   
                 C(12)—C(13)—C(14) 
                 106.64(13) 
               
               
                   
                 C(18)—C(13)—C(17) 
                 110.70(13) 
               
               
                   
                 C(12)—C(13)—C(17) 
                 117.67(13) 
               
               
                   
                 C(14)—C(13)—C(17) 
                 99.63(12) 
               
               
                   
                 C(5)—C(6)—C(7) 
                 126.18(15) 
               
               
                   
                 C(21)—C(20)—C(17) 
                 109.44(13) 
               
               
                   
                 C(21)—C(20)—C(22) 
                 110.45(13) 
               
               
                   
                 C(17)—C(20)—C(22) 
                 115.60(13) 
               
               
                   
                 C(8)—C(14)—C(15) 
                 120.05(14) 
               
               
                   
                 C(8)—C(14)—C(13) 
                 113.68(13) 
               
               
                   
                 C(15)—C(14)—C(13) 
                 103.82(13) 
               
               
                   
                 C(29)—C(2)—C(3) 
                 122.61(16) 
               
               
                   
                 C(29)—C(2)—C(1) 
                 123.89(16) 
               
               
                   
                 C(3)—C(2)—C(1) 
                 113.49(13) 
               
               
                   
                 C(28)—C(22)—C(30) 
                 107.31(14) 
               
               
                   
                 C(28)—C(22)—C(23) 
                 107.77(13) 
               
               
                   
                 C(30)—C(22)—C(23) 
                 105.76(14) 
               
               
                   
                 C(28)—C(22)—C(20) 
                 111.43(14) 
               
               
                   
                 C(30)—C(22)—C(20) 
                 114.34(13) 
               
               
                   
                 C(23)—C(22)—C(20) 
                 109.89(13) 
               
               
                   
                 C(8)—C(7)—C(6) 
                 125.67(15) 
               
               
                   
                 C(5)—C(4)—C(3) 
                 112.89(14) 
               
               
                   
                 C(7)—C(8)—C(14) 
                 123.11(15) 
               
               
                   
                 C(7)—C(8)—C(9) 
                 124.84(15) 
               
               
                   
                 C(14)—C(8)—C(9) 
                 112.04(14) 
               
               
                   
                 C(24)—C(23)—C(22) 
                 115.43(13) 
               
               
                   
                 O(3)—C(3)—C(2) 
                 110.16(13) 
               
               
                   
                 O(3)—C(3)—C(4) 
                 108.15(12) 
               
               
                   
                 C(2)—C(3)—C(4) 
                 110.21(13) 
               
               
                   
                 C(25)—C(24)—C(23) 
                 116.71(14) 
               
               
                   
                 O(1)—C(1)—C(2) 
                 113.40(13) 
               
               
                   
                 O(1)—C(1)—C(10) 
                 107.71(12) 
               
               
                   
                 C(2)—C(1)—C(10) 
                 110.12(13) 
               
               
                   
                 C(5)—C(10)—C(1) 
                 110.88(13) 
               
               
                   
                 C(14)—C(15)—C(16) 
                 104.17(13) 
               
               
                   
                 C(11)—C(12)—C(13) 
                 111.93(13) 
               
               
                   
                 C(8)—C(9)—C(11) 
                 111.72(14) 
               
               
                   
                 C(20)—C(17)—C(16) 
                 114.06(13) 
               
               
                   
                 C(20)—C(17)—C(13) 
                 118.64(13) 
               
               
                   
                 C(16)—C(17)—C(13) 
                 102.46(12) 
               
               
                   
                 O(100)—C(101)—C(102) 
                 108.10(16) 
               
               
                   
                 C(15)—C(16)—C(17) 
                 107.60(13) 
               
               
                   
                 C(12)—C(11)—C(9) 
                 113.01(14) 
               
               
                   
                 O(25)—C(25)—C(27) 
                 108.39(16) 
               
               
                   
                 O(25)—C(25)—C(26) 
                 104.95(14) 
               
               
                   
                 C(27)—C(25)—C(26) 
                 111.5(2) 
               
               
                   
                 O(25)—C(25)—C(24) 
                 107.75(13) 
               
               
                   
                 C(27)—C(25)—C(24) 
                 112.43(16) 
               
               
                   
                 C(26)—C(25)—C(24) 
                 111.40(16) 
               
               
                   
                 O(100)—C(201)—C(202) 
                 108.38(16) 
               
               
                   
                   
               
             
          
         
       
     
         [0000]    
       
         
               
             
               
               
               
               
               
               
               
             
               
               
               
               
               
               
               
             
           
               
                 TABLE 5 
               
             
             
               
                   
               
               
                 Anisotropic displacement parameters (Å 2  × 10 3 ) for MET-1. 
               
               
                 The anisotropic displacement factor exponent takes the form: 
               
               
                 −2π 2 [h 2 a* 2 U 11  + . . . + 2hka * b * U 12 . 
               
             
          
           
               
                   
                 U 11   
                 U 22   
                 U 33   
                 U 23   
                 U 13   
                 U 12   
               
               
                   
                   
               
             
          
           
               
                 O(3) 
                 26(1) 
                 17(1) 
                 37(1) 
                 0(1) 
                 10(1) 
                 1(1) 
               
               
                 O(100) 
                 40(1) 
                 19(1) 
                 37(1) 
                 2(1) 
                 9(1) 
                 3(1) 
               
               
                 O(25) 
                 28(1) 
                 28(1) 
                 26(1) 
                 −2(1) 
                 6(1) 
                 −7(1) 
               
               
                 O(1) 
                 17(1) 
                 23(1) 
                 44(1) 
                 −6(1) 
                 8(1) 
                 −2(1) 
               
               
                 C(5) 
                 21(1) 
                 16(1) 
                 27(1) 
                 −4(1) 
                 4(1) 
                 −2(1) 
               
               
                 C(13) 
                 23(1) 
                 21(1) 
                 24(1) 
                 0(1) 
                 8(1) 
                 −2(1) 
               
               
                 C(6) 
                 19(1) 
                 18(1) 
                 32(1) 
                 −2(1) 
                 6(1) 
                 0(1) 
               
               
                 C(20) 
                 28(1) 
                 20(1) 
                 23(1) 
                 1(1) 
                 8(1) 
                 −5(1) 
               
               
                 C(14) 
                 25(1) 
                 20(1) 
                 25(1) 
                 −2(1) 
                 6(1) 
                 −3(1) 
               
               
                 C(2) 
                 27(1) 
                 17(1) 
                 29(1) 
                 −5(1) 
                 7(1) 
                 −4(1) 
               
               
                 C(22) 
                 33(1) 
                 22(1) 
                 24(1) 
                 3(1) 
                 4(1) 
                 −6(1) 
               
               
                 C(7) 
                 19(1) 
                 18(1) 
                 30(1) 
                 −2(1) 
                 6(1) 
                 −1(1) 
               
               
                 C(4) 
                 21(1) 
                 21(1) 
                 30(1) 
                 1(1) 
                 3(1) 
                 1(1) 
               
               
                 C(8) 
                 25(1) 
                 18(1) 
                 29(1) 
                 −3(1) 
                 6(1) 
                 −1(1) 
               
               
                 C(23) 
                 38(1) 
                 21(1) 
                 25(1) 
                 3(1) 
                 6(1) 
                 −5(1) 
               
               
                 C(3) 
                 29(1) 
                 20(1) 
                 28(1) 
                 4(1) 
                 7(1) 
                 2(1) 
               
               
                 C(21) 
                 29(1) 
                 23(1) 
                 39(1) 
                 2(1) 
                 11(1) 
                 −6(1) 
               
               
                 C(24) 
                 34(1) 
                 22(1) 
                 24(1) 
                 2(1) 
                 6(1) 
                 −4(1) 
               
               
                 C(1) 
                 20(1) 
                 22(1) 
                 29(1) 
                 −2(1) 
                 8(1) 
                 0(1) 
               
               
                 C(10) 
                 21(1) 
                 20(1) 
                 27(1) 
                 2(1) 
                 7(1) 
                 2(1) 
               
               
                 C(15) 
                 20(1) 
                 23(1) 
                 33(1) 
                 3(1) 
                 4(1) 
                 −3(1) 
               
               
                 C(12) 
                 29(1) 
                 24(1) 
                 34(1) 
                 1(1) 
                 14(1) 
                 −2(1) 
               
               
                 C(9) 
                 30(1) 
                 24(1) 
                 38(1) 
                 2(1) 
                 16(1) 
                 4(1) 
               
               
                 C(17) 
                 25(1) 
                 20(1) 
                 20(1) 
                 0(1) 
                 6(1) 
                 −4(1) 
               
               
                 C(101) 
                 65(1) 
                 25(1) 
                 29(1) 
                 −1(1) 
                 10(1) 
                 −9(1) 
               
               
                 C(29) 
                 33(1) 
                 24(1) 
                 39(1) 
                 3(1) 
                 13(1) 
                 −2(1) 
               
               
                 C(30) 
                 33(1) 
                 23(1) 
                 36(1) 
                 9(1) 
                 1(1) 
                 −1(1) 
               
               
                 C(16) 
                 22(1) 
                 21(1) 
                 29(1) 
                 2(1) 
                 1(1) 
                 −2(1) 
               
               
                 C(18) 
                 25(1) 
                 20(1) 
                 26(1) 
                 0(1) 
                 4(1) 
                 −1(1) 
               
               
                 C(11) 
                 25(1) 
                 28(1) 
                 39(1) 
                 3(1) 
                 16(1) 
                 3(1) 
               
               
                 C(25) 
                 42(1) 
                 23(1) 
                 25(1) 
                 2(1) 
                 1(1) 
                 −6(1) 
               
               
                 C(201) 
                 48(1) 
                 28(1) 
                 44(1) 
                 11(1) 
                 22(1) 
                 15(1) 
               
               
                 C(27) 
                 93(2) 
                 25(1) 
                 55(1) 
                 0(1) 
                 −32(1) 
                 8(1) 
               
               
                 C(28) 
                 49(1) 
                 29(1) 
                 26(1) 
                 2(1) 
                 4(1) 
                 −12(1) 
               
               
                 C(202) 
                 35(1) 
                 46(1) 
                 58(1) 
                 14(1) 
                 2(1) 
                 13(1) 
               
               
                 C(26) 
                 75(2) 
                 50(1) 
                 31(1) 
                 −7(1) 
                 23(1) 
                 −34(1) 
               
               
                 C(102) 
                 54(1) 
                 41(1) 
                 57(1) 
                 2(1) 
                 −10(1) 
                 −14(1) 
               
               
                   
               
             
          
         
       
     
         [0000]    
       
         
               
             
               
               
               
               
               
               
             
           
               
                 TABLE 6 
               
               
                   
               
               
                 Hydrogen coordinates (Å 2  × 10 4 ) and isotropic 
               
               
                 displacement parameters (Å 2  × 10 3 ) for MET-1. 
               
               
                   
               
             
             
               
                   
               
             
          
           
               
                   
                 H(3A) 
                 −1246 
                 4391 
                 11360 
                 40 
               
               
                   
                 H(25A) 
                 −3854 
                 −5981 
                 11920 
                 41 
               
               
                   
                 H(1A) 
                 4033 
                 2763 
                 11559 
                 41 
               
               
                   
                 H(6A) 
                 −3636 
                 1598 
                 11604 
                 27 
               
               
                   
                 H(20F) 
                 −3157 
                 −3339 
                 13120 
                 28 
               
               
                   
                 H(14A) 
                 −2129 
                 −451 
                 14045 
                 28 
               
               
                   
                 H(7A) 
                 −743 
                 383 
                 12258 
                 27 
               
               
                   
                 H(4A) 
                 −3529 
                 2665 
                 10495 
                 29 
               
               
                   
                 H(4B) 
                 −2398 
                 2310 
                 9780 
                 29 
               
               
                   
                 H(23A) 
                 −2206 
                 −5217 
                 14739 
                 34 
               
               
                   
                 H(23B) 
                 −4112 
                 −4761 
                 14542 
                 34 
               
               
                   
                 H(3B) 
                 −1735 
                 3823 
                 9988 
                 30 
               
               
                   
                 H(21A) 
                 −5886 
                 −2755 
                 13392 
                 45 
               
               
                   
                 H(21B) 
                 −5311 
                 −3033 
                 14458 
                 45 
               
               
                   
                 H(21C) 
                 −5668 
                 −3779 
                 13671 
                 45 
               
               
                   
                 H(24A) 
                 −4282 
                 −4787 
                 12936 
                 40 
               
               
                   
                 H(24B) 
                 −2270 
                 −5094 
                 13075 
                 40 
               
               
                   
                 H(1B) 
                 1502 
                 2809 
                 11910 
                 28 
               
               
                   
                 H(10F) 
                 646 
                 1386 
                 10569 
                 27 
               
               
                   
                 H(10G) 
                 983 
                 1262 
                 11669 
                 27 
               
               
                   
                 H(15A) 
                 554 
                 −727 
                 13690 
                 31 
               
               
                   
                 H(15B) 
                 −316 
                 −1087 
                 12669 
                 31 
               
               
                   
                 H(12A) 
                 −6313 
                 −1518 
                 13267 
                 33 
               
               
                   
                 H(12B) 
                 −5200 
                 −923 
                 14084 
                 33 
               
               
                   
                 H(9A) 
                 −5058 
                 1043 
                 12544 
                 35 
               
               
                   
                 H(9B) 
                 −4464 
                 795 
                 13618 
                 35 
               
               
                   
                 H(17A) 
                 −2559 
                 −1957 
                 14511 
                 26 
               
               
                   
                 H(10A) 
                 −557 
                 6412 
                 12061 
                 48 
               
               
                   
                 H(10B) 
                 −298 
                 6817 
                 11094 
                 48 
               
               
                   
                 H(29A) 
                 994 
                 4020 
                 9485 
                 37 
               
               
                   
                 H(29B) 
                 2803 
                 3486 
                 9975 
                 37 
               
               
                   
                 H(30A) 
                 485 
                 −4408 
                 14780 
                 47 
               
               
                   
                 H(30B) 
                 509 
                 −3412 
                 14411 
                 47 
               
               
                   
                 H(30C) 
                 −160 
                 −4201 
                 13700 
                 47 
               
               
                   
                 H(16A) 
                 271 
                 −2075 
                 14322 
                 30 
               
               
                   
                 H(16B) 
                 −299 
                 −2463 
                 13290 
                 30 
               
               
                   
                 H(18A) 
                 −4591 
                 −1267 
                 11750 
                 35 
               
               
                   
                 H(18B) 
                 −4607 
                 −2276 
                 12077 
                 35 
               
               
                   
                 H(18C) 
                 −2787 
                 −1820 
                 11983 
                 35 
               
               
                   
                 H(11A) 
                 −7122 
                 26 
                 13048 
                 35 
               
               
                   
                 H(11B) 
                 −6400 
                 −349 
                 12186 
                 35 
               
               
                   
                 H(20A) 
                 −3409 
                 6551 
                 10371 
                 46 
               
               
                   
                 H(20B) 
                 −3782 
                 6139 
                 11313 
                 46 
               
               
                   
                 H(27A) 
                 −1429 
                 −6689 
                 13435 
                 97 
               
               
                   
                 H(27B) 
                 −2910 
                 −7412 
                 13498 
                 97 
               
               
                   
                 H(27C) 
                 −2288 
                 −6726 
                 14328 
                 97 
               
               
                   
                 H(28A) 
                 −1234 
                 −3988 
                 15910 
                 53 
               
               
                   
                 H(28B) 
                 −3130 
                 −3522 
                 15627 
                 53 
               
               
                   
                 H(28C) 
                 −1377 
                 −2970 
                 15600 
                 53 
               
               
                   
                 H(20C) 
                 −5804 
                 5534 
                 10022 
                 71 
               
               
                   
                 H(20D) 
                 −4560 
                 4764 
                 10546 
                 71 
               
               
                   
                 H(20E) 
                 −4187 
                 5175 
                 9607 
                 71 
               
               
                   
                 H(26A) 
                 −6077 
                 −6924 
                 13425 
                 75 
               
               
                   
                 H(26B) 
                 −6654 
                 −5923 
                 13161 
                 75 
               
               
                   
                 H(26C) 
                 −5554 
                 −6154 
                 14177 
                 75 
               
               
                   
                 H(10C) 
                 2433 
                 6241 
                 11927 
                 81 
               
               
                   
                 H(10D) 
                 1798 
                 5688 
                 10993 
                 81 
               
               
                   
                 H(10E) 
                 1544 
                 5288 
                 11958 
               
               
                   
                   
               
             
          
         
       
     
         [0000]    
       
         
               
             
               
               
               
             
           
               
                 TABLE 7 
               
               
                   
               
               
                 Torsion angles [deg] for MET-1. 
               
               
                   
               
             
             
               
                   
               
             
          
           
               
                   
                 C(10)—C(5)—C(6)—C(7) 
                 −6.9(3) 
               
               
                   
                 C(4)—C(5)—C(6)—C(7) 
                 172.04(14) 
               
               
                   
                 C(18)—C(13)—C(14)—C(8) 
                 62.64(17) 
               
               
                   
                 C(12)—C(13)—C(14)—C(8) 
                 −57.81(17) 
               
               
                   
                 C(17)—C(13)—C(14)—C(8) 
                 179.34(12) 
               
               
                   
                 C(18)—C(13)—C(14)—C(15) 
                 −69.49(16) 
               
               
                   
                 C(12)—C(13)—C(14)—C(15) 
                 170.05(13) 
               
               
                   
                 C(17)—C(13)—C(14)—C(15) 
                 47.21(14) 
               
               
                   
                 C(21)—C(20)—C(22)—C(28) 
                 −68.60(17) 
               
               
                   
                 C(17)—C(20)—C(22)—C(28) 
                 56.32(18) 
               
               
                   
                 C(21)—C(20)—C(22)—C(30) 
                 169.50(14) 
               
               
                   
                 C(17)—C(20)—C(22)—C(30) 
                 −65.58(18) 
               
               
                   
                 C(21)—C(20)—C(22)—C(23) 
                 50.77(17) 
               
               
                   
                 C(17)—C(20)—C(22)—C(23) 
                 175.69(13) 
               
               
                   
                 C(5)—C(6)—C(7)—C(8) 
                 175.69(16) 
               
               
                   
                 C(6)—C(5)—C(4)—C(3) 
                 129.93(16) 
               
               
                   
                 C(10)—C(5)—C(4)—C(3) 
                 −50.98(18) 
               
               
                   
                 C(6)—C(7)—C(8)—C(14) 
                 175.28(14) 
               
               
                   
                 C(6)—C(7)—C(8)—C(9) 
                 −6.4(3) 
               
               
                   
                 C(15)—C(14)—C(8)—C(7) 
                 −0.9(2) 
               
               
                   
                 C(13)—C(14)—C(8)—C(7) 
                 −124.65(17) 
               
               
                   
                 C(15)—C(14)—C(8)—C(9) 
                 −179.41(15) 
               
               
                   
                 C(13)—C(14)—C(8)—C(9) 
                 56.87(17) 
               
               
                   
                 C(28)—C(22)—C(23)—C(24) 
                 175.53(15) 
               
               
                   
                 C(30)—C(22)—C(23)—C(24) 
                 −69.94(18) 
               
               
                   
                 C(20)—C(22)—C(23)—C(24) 
                 53.94(19) 
               
               
                   
                 C(29)—C(2)—C(3)—O(3) 
                 −116.79(17) 
               
               
                   
                 C(1)—C(2)—C(3)—O(3) 
                 64.38(16) 
               
               
                   
                 C(29)—C(2)—C(3)—C(4) 
                 123.95(17) 
               
               
                   
                 C(1)—C(2)—C(3)—C(4) 
                 −54.88(17) 
               
               
                   
                 C(5)—C(4)—C(3)—O(3) 
                 −69.91(16) 
               
               
                   
                 C(5)—C(4)—C(3)—C(2) 
                 50.56(17) 
               
               
                   
                 C(22)—C(23)—C(24)—C(25) 
                 170.72(15) 
               
               
                   
                 C(29)—C(2)—C(1)—O(1) 
                 −1.0(2) 
               
               
                   
                 C(3)—C(2)—C(1)—O(1) 
                 177.82(12) 
               
               
                   
                 C(29)—C(2)—C(1)—C(10) 
                 −121.76(17) 
               
               
                   
                 C(3)—C(2)—C(1)—C(10) 
                 57.05(16) 
               
               
                   
                 C(6)—C(5)—C(10)—C(1) 
                 −128.78(16) 
               
               
                   
                 C(4)—C(5)—C(10)—C(1) 
                 52.18(17) 
               
               
                   
                 O(1)—C(1)—C(10)—C(5) 
                 −178.02(11) 
               
               
                   
                 C(2)—C(1)—C(10)—C(5) 
                 −53.90(16) 
               
               
                   
                 C(8)—C(14)—C(15)—C(16) 
                 −163.10(13) 
               
               
                   
                 C(13)—C(14)—C(15)—C(16) 
                 −34.78(16) 
               
               
                   
                 C(18)—C(13)—C(12)—C(11) 
                 −65.07(17) 
               
               
                   
                 C(14)—C(13)—C(12)—C(11) 
                 55.72(17) 
               
               
                   
                 C(17)—C(13)—C(12)—C(11) 
                 166.45(14) 
               
               
                   
                 C(7)—C(8)—C(9)—C(11) 
                 130.33(18) 
               
               
                   
                 C(14)—C(8)—C(9)—C(11) 
                 −51.22(17) 
               
               
                   
                 C(21)—C(20)—C(17)—C(16) 
                 −175.23(13) 
               
               
                   
                 C(22)—C(20)—C(17)—C(16) 
                 59.33(17) 
               
               
                   
                 C(21)—C(20)—C(17)—C(13) 
                 −54.36(17) 
               
               
                   
                 C(22)—C(20)—C(17)—C(13) 
                 −179.80(12) 
               
               
                   
                 C(18)—C(13)—C(17)—C(20) 
                 −50.06(18) 
               
               
                   
                 C(12)—C(13)—C(17)—C(20) 
                 78.34(18) 
               
               
                   
                 C(14)—C(13)—C(17)—C(20) 
                 −167.02(12) 
               
               
                   
                 C(18)—C(13)—C(17)—C(16) 
                 76.56(15) 
               
               
                   
                 C(12)—C(13)—C(17)—C(16) 
                 −155.04(14) 
               
               
                   
                 C(14)—C(13)—C(17)—C(16) 
                 −40.40(14) 
               
               
                   
                 C(201)—O(100)—C(101)—C(102) 
                 −177.01(16) 
               
               
                   
                 C(14)—C(15)—C(16)—C(17) 
                 8.55(16) 
               
               
                   
                 C(20)—C(17)—C(16)—C(15) 
                 150.05(13) 
               
               
                   
                 C(13)—C(17)—C(16)—C(15) 
                 20.53(16) 
               
               
                   
                 C(13)—C(12)—C(11)—C(9) 
                 −54.82(19) 
               
               
                   
                 C(8)—C(9)—C(11)—C(12) 
                 50.78(18) 
               
               
                   
                 C(23)—C(24)—C(25)—O(25) 
                 175.01(14) 
               
               
                   
                 C(23)—C(24)—C(25)—C(27) 
                 −65.6(2) 
               
               
                   
                 C(23)—C(24)—C(25)—C(26) 
                 60.4(2) 
               
               
                   
                 C(101)—O(100)—C(201)—C(202) 
                 177.20(15) 
               
               
                   
                   
               
             
          
         
       
     
         [0000]    
       
         
               
             
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
             
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
             
           
               
                 TABLE 8 
               
             
             
               
                   
               
               
                 Observed and calculated structure factors for MET-1. 
               
             
          
           
               
                 h 
                 k 
                 l 
                 10Fo 
                 10Fc 
                 10s 
                 h 
                 k 
                 l 
                 10Fo 
                 10Fc 
                 10s 
                 h 
                 k 
                 l 
                 10Fo 
                 10Fc 
                 10s 
                 h 
                 k 
                 l 
                 10Fo 
                 10Fc 
                 10s 
                 h 
                 k 
                 l 
                 10Fo 
                 10Fc 
                 10s 
               
               
                   
               
             
          
           
               
                 0 
                 −16 
                 0 
                 150 
                 149 
                 2 
                 1 
                 2 
                 0 
                 479 
                 489 
                 5 
                 2 
                 15 
                 0 
                 41 
                 44 
                 1 
                 3 
                 −9 
                 1 
                 37 
                 37 
                 1 
                 4 
                 1 
                 1 
                 139 
                 136 
                 2 
               
               
                 1 
                 −16 
                 0 
                 52 
                 52 
                 1 
                 2 
                 2 
                 0 
                 217 
                 210 
                 2 
                 3 
                 15 
                 0 
                 34 
                 36 
                 1 
                 4 
                 −9 
                 1 
                 188 
                 187 
                 3 
                 5 
                 1 
                 1 
                 75 
                 72 
                 1 
               
               
                 2 
                 −16 
                 0 
                 77 
                 74 
                 1 
                 3 
                 2 
                 0 
                 118 
                 120 
                 1 
                 4 
                 15 
                 0 
                 95 
                 95 
                 1 
                 5 
                 −9 
                 1 
                 192 
                 181 
                 3 
                 6 
                 1 
                 1 
                 131 
                 124 
                 2 
               
               
                 3 
                 −16 
                 0 
                 134 
                 137 
                 2 
                 4 
                 2 
                 0 
                 253 
                 245 
                 3 
                 2 
                 16 
                 0 
                 76 
                 74 
                 1 
                 6 
                 −9 
                 1 
                 3 
                 6 
                 3 
                 7 
                 1 
                 1 
                 154 
                 157 
                 2 
               
               
                 1 
                 −15 
                 0 
                 106 
                 109 
                 1 
                 5 
                 2 
                 0 
                 56 
                 51 
                 1 
                 0 
                 −17 
                 1 
                 74 
                 72 
                 1 
                 −6 
                 −8 
                 1 
                 25 
                 23 
                 1 
                 8 
                 1 
                 1 
                 21 
                 20 
                 1 
               
               
                 2 
                 −15 
                 0 
                 44 
                 45 
                 1 
                 6 
                 2 
                 0 
                 195 
                 199 
                 3 
                 −3 
                 −16 
                 1 
                 41 
                 39 
                 1 
                 −5 
                 −8 
                 1 
                 142 
                 141 
                 2 
                 −8 
                 2 
                 1 
                 47 
                 49 
                 1 
               
               
                 3 
                 −15 
                 0 
                 34 
                 36 
                 1 
                 7 
                 2 
                 0 
                 79 
                 74 
                 1 
                 −2 
                 −16 
                 1 
                 75 
                 77 
                 1 
                 −4 
                 −8 
                 1 
                 24 
                 21 
                 1 
                 −7 
                 2 
                 1 
                 143 
                 145 
                 2 
               
               
                 4 
                 −15 
                 0 
                 91 
                 94 
                 1 
                 8 
                 2 
                 0 
                 50 
                 49 
                 1 
                 −1 
                 −16 
                 1 
                 5 
                 5 
                 4 
                 −3 
                 −8 
                 1 
                 44 
                 43 
                 1 
                 −6 
                 2 
                 1 
                 40 
                 38 
                 1 
               
               
                 0 
                 −14 
                 0 
                 137 
                 148 
                 1 
                 1 
                 3 
                 0 
                 141 
                 142 
                 1 
                 0 
                 −16 
                 1 
                 51 
                 50 
                 1 
                 −2 
                 −8 
                 1 
                 66 
                 64 
                 1 
                 −5 
                 2 
                 1 
                 46 
                 49 
                 1 
               
               
                 1 
                 −14 
                 0 
                 18 
                 16 
                 1 
                 2 
                 3 
                 0 
                 272 
                 281 
                 3 
                 1 
                 −16 
                 1 
                 167 
                 170 
                 1 
                 −1 
                 −8 
                 1 
                 103 
                 98 
                 1 
                 −4 
                 2 
                 1 
                 59 
                 51 
                 1 
               
               
                 2 
                 −14 
                 0 
                 98 
                 96 
                 1 
                 3 
                 3 
                 0 
                 252 
                 247 
                 3 
                 2 
                 −16 
                 1 
                 4 
                 6 
                 4 
                 0 
                 −8 
                 1 
                 149 
                 161 
                 3 
                 −3 
                 2 
                 1 
                 448 
                 429 
                 5 
               
               
                 3 
                 −14 
                 0 
                 110 
                 106 
                 1 
                 4 
                 3 
                 0 
                 55 
                 60 
                 1 
                 −4 
                 −15 
                 1 
                 112 
                 113 
                 2 
                 1 
                 −8 
                 1 
                 187 
                 189 
                 2 
                 −2 
                 2 
                 1 
                 146 
                 146 
                 1 
               
               
                 4 
                 −14 
                 0 
                 22 
                 21 
                 1 
                 5 
                 3 
                 0 
                 70 
                 68 
                 1 
                 −3 
                 −15 
                 1 
                 114 
                 109 
                 1 
                 2 
                 −8 
                 1 
                 160 
                 151 
                 1 
                 −1 
                 2 
                 1 
                 328 
                 333 
                 3 
               
               
                 1 
                 −13 
                 0 
                 104 
                 107 
                 1 
                 6 
                 3 
                 0 
                 151 
                 145 
                 2 
                 −2 
                 −15 
                 1 
                 105 
                 99 
                 1 
                 3 
                 −8 
                 1 
                 88 
                 80 
                 1 
                 0 
                 2 
                 1 
                 275 
                 279 
                 4 
               
               
                 2 
                 −13 
                 0 
                 74 
                 72 
                 1 
                 7 
                 3 
                 0 
                 72 
                 70 
                 1 
                 −1 
                 −15 
                 1 
                 63 
                 66 
                 1 
                 4 
                 −8 
                 1 
                 203 
                 198 
                 3 
                 1 
                 2 
                 1 
                 372 
                 371 
                 4 
               
               
                 3 
                 −13 
                 0 
                 102 
                 95 
                 1 
                 8 
                 3 
                 0 
                 30 
                 33 
                 1 
                 0 
                 −15 
                 1 
                 57 
                 53 
                 1 
                 5 
                 −8 
                 1 
                 115 
                 116 
                 2 
                 2 
                 2 
                 1 
                 189 
                 195 
                 2 
               
               
                 4 
                 −13 
                 0 
                 123 
                 117 
                 2 
                 0 
                 4 
                 0 
                 924 
                 916 
                 22 
                 1 
                 −15 
                 1 
                 39 
                 39 
                 1 
                 6 
                 −8 
                 1 
                 27 
                 27 
                 1 
                 3 
                 2 
                 1 
                 167 
                 170 
                 2 
               
               
                 5 
                 −13 
                 0 
                 41 
                 42 
                 1 
                 1 
                 4 
                 0 
                 319 
                 318 
                 4 
                 2 
                 −15 
                 1 
                 72 
                 73 
                 1 
                 −4 
                 −7 
                 1 
                 268 
                 270 
                 5 
                 4 
                 2 
                 1 
                 66 
                 71 
                 1 
               
               
                 0 
                 −12 
                 0 
                 43 
                 42 
                 1 
                 2 
                 4 
                 0 
                 399 
                 410 
                 4 
                 3 
                 −15 
                 1 
                 48 
                 46 
                 1 
                 −3 
                 −7 
                 1 
                 110 
                 109 
                 1 
                 5 
                 2 
                 1 
                 63 
                 65 
                 1 
               
               
                 1 
                 −12 
                 0 
                 76 
                 72 
                 1 
                 3 
                 4 
                 0 
                 250 
                 245 
                 3 
                 −5 
                 −14 
                 1 
                 57 
                 62 
                 1 
                 −2 
                 −7 
                 1 
                 153 
                 142 
                 1 
                 6 
                 2 
                 1 
                 123 
                 120 
                 2 
               
               
                 2 
                 −12 
                 0 
                 67 
                 63 
                 1 
                 4 
                 4 
                 0 
                 87 
                 81 
                 1 
                 −4 
                 −14 
                 1 
                 66 
                 72 
                 1 
                 −1 
                 −7 
                 1 
                 391 
                 378 
                 5 
                 7 
                 2 
                 1 
                 130 
                 133 
                 2 
               
               
                 3 
                 −12 
                 0 
                 44 
                 40 
                 1 
                 5 
                 4 
                 0 
                 153 
                 154 
                 1 
                 −3 
                 −14 
                 1 
                 7 
                 10 
                 3 
                 0 
                 −7 
                 1 
                 185 
                 171 
                 2 
                 8 
                 2 
                 1 
                 56 
                 50 
                 1 
               
               
                 4 
                 −12 
                 0 
                 75 
                 86 
                 1 
                 6 
                 4 
                 0 
                 31 
                 38 
                 1 
                 −2 
                 −14 
                 1 
                 49 
                 45 
                 1 
                 1 
                 −7 
                 1 
                 354 
                 336 
                 4 
                 −8 
                 3 
                 1 
                 22 
                 20 
                 1 
               
               
                 5 
                 −12 
                 0 
                 79 
                 74 
                 1 
                 7 
                 4 
                 0 
                 69 
                 74 
                 1 
                 −1 
                 −14 
                 1 
                 63 
                 65 
                 1 
                 2 
                 −7 
                 1 
                 236 
                 227 
                 2 
                 −7 
                 3 
                 1 
                 101 
                 95 
                 1 
               
               
                 6 
                 −12 
                 0 
                 66 
                 61 
                 1 
                 8 
                 4 
                 0 
                 12 
                 18 
                 1 
                 0 
                 −14 
                 1 
                 34 
                 35 
                 1 
                 3 
                 −7 
                 1 
                 211 
                 209 
                 3 
                 −6 
                 3 
                 1 
                 74 
                 74 
                 1 
               
               
                 1 
                 −11 
                 0 
                 88 
                 88 
                 1 
                 1 
                 5 
                 0 
                 48 
                 55 
                 1 
                 1 
                 −14 
                 1 
                 83 
                 88 
                 1 
                 −3 
                 −6 
                 1 
                 480 
                 451 
                 5 
                 −5 
                 3 
                 1 
                 117 
                 119 
                 1 
               
               
                 2 
                 −11 
                 0 
                 105 
                 103 
                 1 
                 2 
                 5 
                 0 
                 241 
                 222 
                 3 
                 2 
                 −14 
                 1 
                 31 
                 30 
                 1 
                 −2 
                 −6 
                 1 
                 598 
                 575 
                 6 
                 −4 
                 3 
                 1 
                 251 
                 235 
                 3 
               
               
                 3 
                 −11 
                 0 
                 158 
                 162 
                 1 
                 3 
                 5 
                 0 
                 163 
                 165 
                 2 
                 3 
                 −14 
                 1 
                 10 
                 8 
                 2 
                 −1 
                 −6 
                 1 
                 152 
                 146 
                 1 
                 −3 
                 3 
                 1 
                 143 
                 128 
                 1 
               
               
                 4 
                 −11 
                 0 
                 50 
                 52 
                 1 
                 4 
                 5 
                 0 
                 158 
                 167 
                 1 
                 4 
                 −14 
                 1 
                 26 
                 28 
                 1 
                 0 
                 −6 
                 1 
                 303 
                 302 
                 4 
                 −2 
                 3 
                 1 
                 191 
                 189 
                 2 
               
               
                 5 
                 −11 
                 0 
                 133 
                 130 
                 2 
                 5 
                 5 
                 0 
                 89 
                 87 
                 1 
                 −5 
                 −13 
                 1 
                 125 
                 128 
                 2 
                 1 
                 −6 
                 1 
                 562 
                 533 
                 6 
                 −1 
                 3 
                 1 
                 406 
                 413 
                 6 
               
               
                 6 
                 −11 
                 0 
                 18 
                 22 
                 1 
                 6 
                 5 
                 0 
                 192 
                 193 
                 3 
                 −4 
                 −13 
                 1 
                 41 
                 41 
                 1 
                 2 
                 −6 
                 1 
                 254 
                 234 
                 2 
                 0 
                 3 
                 1 
                 293 
                 280 
                 5 
               
               
                 0 
                 −10 
                 0 
                 186 
                 194 
                 1 
                 7 
                 5 
                 0 
                 43 
                 42 
                 1 
                 −3 
                 −13 
                 1 
                 76 
                 76 
                 1 
                 −3 
                 −5 
                 1 
                 126 
                 122 
                 3 
                 1 
                 3 
                 1 
                 364 
                 373 
                 4 
               
               
                 1 
                 −10 
                 0 
                 65 
                 57 
                 1 
                 8 
                 5 
                 0 
                 35 
                 37 
                 1 
                 −2 
                 −13 
                 1 
                 57 
                 52 
                 1 
                 −2 
                 −5 
                 1 
                 54 
                 55 
                 1 
                 2 
                 3 
                 1 
                 242 
                 241 
                 2 
               
               
                 2 
                 −10 
                 0 
                 167 
                 171 
                 1 
                 0 
                 6 
                 0 
                 382 
                 366 
                 8 
                 −1 
                 −13 
                 1 
                 137 
                 144 
                 1 
                 −1 
                 −5 
                 1 
                 358 
                 351 
                 3 
                 3 
                 3 
                 1 
                 275 
                 287 
                 5 
               
               
                 3 
                 −10 
                 0 
                 238 
                 244 
                 1 
                 1 
                 6 
                 0 
                 453 
                 436 
                 8 
                 0 
                 −13 
                 1 
                 91 
                 97 
                 1 
                 0 
                 −5 
                 1 
                 275 
                 275 
                 2 
                 4 
                 3 
                 1 
                 137 
                 135 
                 1 
               
               
                 4 
                 −10 
                 0 
                 158 
                 152 
                 2 
                 3 
                 6 
                 0 
                 312 
                 309 
                 4 
                 1 
                 −13 
                 1 
                 193 
                 196 
                 1 
                 1 
                 −5 
                 1 
                 58 
                 66 
                 1 
                 5 
                 3 
                 1 
                 36 
                 39 
                 1 
               
               
                 5 
                 −10 
                 0 
                 96 
                 90 
                 1 
                 4 
                 6 
                 0 
                 232 
                 222 
                 1 
                 2 
                 −13 
                 1 
                 199 
                 205 
                 1 
                 2 
                 −5 
                 1 
                 37 
                 36 
                 1 
                 6 
                 3 
                 1 
                 134 
                 135 
                 2 
               
               
                 6 
                 −10 
                 0 
                 92 
                 92 
                 1 
                 5 
                 6 
                 0 
                 158 
                 155 
                 1 
                 3 
                 −13 
                 1 
                 82 
                 85 
                 1 
                 −3 
                 −4 
                 1 
                 406 
                 386 
                 10 
                 7 
                 3 
                 1 
                 84 
                 81 
                 1 
               
               
                 1 
                 −9 
                 0 
                 185 
                 185 
                 1 
                 6 
                 6 
                 0 
                 170 
                 175 
                 2 
                 4 
                 −13 
                 1 
                 29 
                 27 
                 1 
                 −2 
                 −4 
                 1 
                 198 
                 185 
                 2 
                 8 
                 3 
                 1 
                 45 
                 44 
                 1 
               
               
                 2 
                 −9 
                 0 
                 171 
                 177 
                 1 
                 7 
                 6 
                 0 
                 138 
                 133 
                 2 
                 5 
                 −13 
                 1 
                 23 
                 21 
                 1 
                 −1 
                 −4 
                 1 
                 367 
                 368 
                 3 
                 −8 
                 4 
                 1 
                 37 
                 38 
                 1 
               
               
                 3 
                 −9 
                 0 
                 86 
                 87 
                 1 
                 8 
                 6 
                 0 
                 57 
                 61 
                 1 
                 −6 
                 −12 
                 1 
                 40 
                 39 
                 1 
                 0 
                 −4 
                 1 
                 229 
                 233 
                 1 
                 −7 
                 4 
                 1 
                 113 
                 118 
                 2 
               
               
                 4 
                 −9 
                 0 
                 185 
                 178 
                 3 
                 1 
                 7 
                 0 
                 256 
                 225 
                 4 
                 −5 
                 −12 
                 1 
                 80 
                 74 
                 1 
                 1 
                 −4 
                 1 
                 508 
                 500 
                 5 
                 −6 
                 4 
                 1 
                 116 
                 116 
                 2 
               
               
                 5 
                 −9 
                 0 
                 128 
                 130 
                 2 
                 2 
                 7 
                 0 
                 113 
                 122 
                 3 
                 −4 
                 −12 
                 1 
                 88 
                 92 
                 1 
                 2 
                 −4 
                 1 
                 242 
                 228 
                 2 
                 −5 
                 4 
                 1 
                 108 
                 109 
                 1 
               
               
                 6 
                 −9 
                 0 
                 53 
                 55 
                 1 
                 3 
                 7 
                 0 
                 87 
                 95 
                 1 
                 −3 
                 −12 
                 1 
                 64 
                 66 
                 1 
                 −3 
                 −3 
                 1 
                 146 
                 127 
                 3 
                 −4 
                 4 
                 1 
                 69 
                 60 
                 1 
               
               
                 0 
                 −8 
                 0 
                 262 
                 252 
                 6 
                 4 
                 7 
                 0 
                 119 
                 119 
                 1 
                 −2 
                 −12 
                 1 
                 170 
                 176 
                 1 
                 −2 
                 −3 
                 1 
                 189 
                 189 
                 2 
                 −3 
                 4 
                 1 
                 402 
                 384 
                 6 
               
               
                 1 
                 −8 
                 0 
                 168 
                 164 
                 2 
                 5 
                 7 
                 0 
                 180 
                 184 
                 1 
                 −1 
                 −12 
                 1 
                 151 
                 147 
                 1 
                 −1 
                 −3 
                 1 
                 403 
                 412 
                 4 
                 −2 
                 4 
                 1 
                 191 
                 185 
                 2 
               
               
                 2 
                 −8 
                 0 
                 44 
                 41 
                 1 
                 6 
                 7 
                 0 
                 25 
                 23 
                 1 
                 0 
                 −12 
                 1 
                 147 
                 146 
                 1 
                 0 
                 −3 
                 1 
                 289 
                 281 
                 2 
                 −1 
                 4 
                 1 
                 365 
                 367 
                 4 
               
               
                 3 
                 −8 
                 0 
                 155 
                 149 
                 1 
                 7 
                 7 
                 0 
                 73 
                 73 
                 1 
                 1 
                 −12 
                 1 
                 39 
                 40 
                 1 
                 1 
                 −3 
                 1 
                 377 
                 373 
                 3 
                 0 
                 4 
                 1 
                 227 
                 233 
                 4 
               
               
                 4 
                 −8 
                 0 
                 232 
                 231 
                 4 
                 0 
                 8 
                 0 
                 267 
                 253 
                 6 
                 2 
                 −12 
                 1 
                 125 
                 128 
                 1 
                 2 
                 −3 
                 1 
                 240 
                 242 
                 2 
                 1 
                 4 
                 1 
                 504 
                 501 
                 8 
               
               
                 5 
                 −8 
                 0 
                 120 
                 115 
                 2 
                 1 
                 8 
                 0 
                 170 
                 164 
                 4 
                 3 
                 −12 
                 1 
                 93 
                 94 
                 1 
                 −2 
                 −2 
                 1 
                 142 
                 145 
                 1 
                 2 
                 4 
                 1 
                 236 
                 228 
                 2 
               
               
                 6 
                 −8 
                 0 
                 88 
                 85 
                 1 
                 2 
                 8 
                 0 
                 41 
                 41 
                 1 
                 4 
                 −12 
                 1 
                 30 
                 34 
                 1 
                 −1 
                 −2 
                 1 
                 330 
                 333 
                 3 
                 3 
                 4 
                 1 
                 315 
                 294 
                 4 
               
               
                 1 
                 −7 
                 0 
                 254 
                 225 
                 3 
                 3 
                 8 
                 0 
                 154 
                 150 
                 1 
                 5 
                 −12 
                 1 
                 40 
                 35 
                 1 
                 0 
                 −2 
                 1 
                 274 
                 279 
                 2 
                 4 
                 4 
                 1 
                 235 
                 230 
                 2 
               
               
                 2 
                 −7 
                 0 
                 120 
                 123 
                 1 
                 4 
                 8 
                 0 
                 231 
                 231 
                 2 
                 −6 
                 −11 
                 1 
                 81 
                 84 
                 1 
                 1 
                 −2 
                 1 
                 375 
                 372 
                 3 
                 5 
                 4 
                 1 
                 243 
                 242 
                 1 
               
               
                 3 
                 −7 
                 0 
                 89 
                 96 
                 1 
                 5 
                 8 
                 0 
                 118 
                 115 
                 1 
                 −5 
                 −11 
                 1 
                 66 
                 65 
                 1 
                 2 
                 −2 
                 1 
                 186 
                 196 
                 4 
                 6 
                 4 
                 1 
                 79 
                 80 
                 1 
               
               
                 0 
                 −6 
                 0 
                 346 
                 368 
                 9 
                 6 
                 8 
                 0 
                 87 
                 85 
                 1 
                 −4 
                 −11 
                 1 
                 36 
                 33 
                 1 
                 −8 
                 −1 
                 1 
                 23 
                 27 
                 1 
                 7 
                 4 
                 1 
                 48 
                 50 
                 1 
               
               
                 1 
                 −6 
                 0 
                 458 
                 436 
                 4 
                 7 
                 8 
                 0 
                 56 
                 57 
                 1 
                 −3 
                 −11 
                 1 
                 10 
                 12 
                 1 
                 −7 
                 −1 
                 1 
                 107 
                 107 
                 1 
                 8 
                 4 
                 1 
                 53 
                 57 
                 1 
               
               
                 2 
                 −6 
                 0 
                 246 
                 233 
                 2 
                 1 
                 9 
                 0 
                 180 
                 185 
                 3 
                 −2 
                 −11 
                 1 
                 113 
                 112 
                 1 
                 −2 
                 −1 
                 1 
                 44 
                 48 
                 1 
                 −8 
                 5 
                 1 
                 75 
                 75 
                 1 
               
               
                 3 
                 −6 
                 0 
                 318 
                 309 
                 7 
                 2 
                 9 
                 0 
                 171 
                 176 
                 2 
                 −1 
                 −11 
                 1 
                 122 
                 122 
                 1 
                 −1 
                 −1 
                 1 
                 228 
                 240 
                 2 
                 −7 
                 5 
                 1 
                 131 
                 135 
                 2 
               
               
                 1 
                 −5 
                 0 
                 47 
                 53 
                 1 
                 3 
                 9 
                 0 
                 87 
                 88 
                 1 
                 0 
                 −11 
                 1 
                 120 
                 110 
                 1 
                 0 
                 −1 
                 1 
                 99 
                 95 
                 1 
                 −6 
                 5 
                 1 
                 218 
                 238 
                 2 
               
               
                 2 
                 −5 
                 0 
                 247 
                 222 
                 2 
                 4 
                 9 
                 0 
                 186 
                 178 
                 2 
                 1 
                 −11 
                 1 
                 138 
                 138 
                 1 
                 1 
                 −1 
                 1 
                 339 
                 344 
                 3 
                 −5 
                 5 
                 1 
                 131 
                 120 
                 1 
               
               
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                 1 
                 −1 
                 7 
                 15 
                 14 
                 11 
                 2 
               
               
                 −1 
                 9 
                 13 
                 36 
                 35 
                 1 
                 −4 
                 −1 
                 14 
                 117 
                 117 
                 1 
                 1 
                 5 
                 14 
                 70 
                 70 
                 1 
                 −4 
                 −1 
                 15 
                 85 
                 86 
                 1 
                 −3 
                 −4 
                 16 
                 43 
                 42 
                 1 
               
               
                 0 
                 9 
                 13 
                 75 
                 71 
                 1 
                 −3 
                 −1 
                 14 
                 47 
                 44 
                 1 
                 2 
                 5 
                 14 
                 49 
                 47 
                 1 
                 −3 
                 −1 
                 15 
                 56 
                 57 
                 1 
                 −2 
                 −4 
                 16 
                 49 
                 51 
                 1 
               
               
                 1 
                 9 
                 13 
                 35 
                 32 
                 1 
                 −2 
                 −1 
                 14 
                 26 
                 26 
                 1 
                 −5 
                 6 
                 14 
                 62 
                 62 
                 1 
                 −2 
                 −1 
                 15 
                 31 
                 34 
                 1 
                 −1 
                 −4 
                 16 
                 30 
                 29 
                 1 
               
               
                 −3 
                 10 
                 13 
                 24 
                 23 
                 1 
                 −1 
                 −1 
                 14 
                 78 
                 76 
                 1 
                 −4 
                 6 
                 14 
                 125 
                 120 
                 1 
                 −1 
                 −1 
                 15 
                 149 
                 147 
                 1 
                 −3 
                 −3 
                 16 
                 12 
                 10 
                 1 
               
               
                 −1 
                 10 
                 13 
                 125 
                 125 
                 1 
                 0 
                 −1 
                 14 
                 149 
                 148 
                 1 
                 −3 
                 6 
                 14 
                 105 
                 102 
                 1 
                 0 
                 −1 
                 15 
                 40 
                 40 
                 1 
                 −2 
                 −3 
                 16 
                 24 
                 25 
                 1 
               
               
                 0 
                 10 
                 13 
                 45 
                 43 
                 1 
                 1 
                 −1 
                 14 
                 48 
                 51 
                 1 
                 −2 
                 6 
                 14 
                 28 
                 27 
                 1 
                 1 
                 −1 
                 15 
                 37 
                 36 
                 1 
                 −1 
                 −3 
                 16 
                 49 
                 50 
                 1 
               
               
                 −2 
                 −9 
                 14 
                 64 
                 69 
                 1 
                 2 
                 −1 
                 14 
                 17 
                 15 
                 1 
                 −1 
                 6 
                 14 
                 64 
                 62 
                 1 
                 2 
                 −1 
                 15 
                 55 
                 54 
                 1 
                 0 
                 −3 
                 16 
                 45 
                 43 
                 1 
               
               
                 −1 
                 −9 
                 14 
                 52 
                 49 
                 1 
                 −5 
                 0 
                 14 
                 38 
                 37 
                 1 
                 0 
                 6 
                 14 
                 28 
                 22 
                 1 
                 −5 
                 0 
                 15 
                 45 
                 45 
                 1 
                 −4 
                 −2 
                 16 
                 40 
                 41 
                 1 
               
               
                 −3 
                 −8 
                 14 
                 26 
                 25 
                 1 
                 −4 
                 0 
                 14 
                 17 
                 19 
                 2 
                 1 
                 6 
                 14 
                 55 
                 53 
                 1 
                 −4 
                 0 
                 15 
                 80 
                 82 
                 1 
                 −3 
                 −2 
                 16 
                 34 
                 30 
                 1 
               
               
                 −2 
                 −8 
                 14 
                 66 
                 64 
                 1 
                 −3 
                 0 
                 14 
                 43 
                 42 
                 1 
                 2 
                 6 
                 14 
                 126 
                 129 
                 2 
                 −3 
                 0 
                 15 
                 14 
                 9 
                 1 
                 −2 
                 −2 
                 16 
                 54 
                 57 
                 1 
               
               
                 −1 
                 −8 
                 14 
                 34 
                 33 
                 1 
                 −2 
                 0 
                 14 
                 95 
                 97 
                 1 
                 −4 
                 7 
                 14 
                 29 
                 30 
                 1 
                 −2 
                 0 
                 15 
                 42 
                 48 
                 1 
                 −1 
                 −2 
                 16 
                 60 
                 57 
                 1 
               
               
                 0 
                 −8 
                 14 
                 85 
                 83 
                 1 
                 −1 
                 0 
                 14 
                 132 
                 132 
                 1 
                 −3 
                 7 
                 14 
                 90 
                 83 
                 1 
                 −1 
                 0 
                 15 
                 5 
                 4 
                 5 
                 0 
                 −2 
                 16 
                 117 
                 118 
                 1 
               
               
                 −4 
                 −7 
                 14 
                 30 
                 30 
                 1 
                 0 
                 0 
                 14 
                 81 
                 76 
                 1 
                 −2 
                 7 
                 14 
                 129 
                 129 
                 2 
                 0 
                 0 
                 15 
                 10 
                 12 
                 3 
                 −4 
                 −1 
                 16 
                 89 
                 86 
                 1 
               
               
                 −3 
                 −7 
                 14 
                 89 
                 83 
                 1 
                 1 
                 0 
                 14 
                 62 
                 60 
                 1 
                 −1 
                 7 
                 14 
                 33 
                 36 
                 1 
                 1 
                 0 
                 15 
                 12 
                 14 
                 1 
                 −3 
                 −1 
                 16 
                 78 
                 78 
                 1 
               
               
                 −2 
                 −7 
                 14 
                 130 
                 129 
                 1 
                 2 
                 0 
                 14 
                 4 
                 2 
                 4 
                 0 
                 7 
                 14 
                 66 
                 64 
                 1 
                 2 
                 0 
                 15 
                 54 
                 48 
                 1 
                 −2 
                 −1 
                 16 
                 12 
                 13 
                 1 
               
               
                 −1 
                 −7 
                 14 
                 32 
                 36 
                 1 
                 −6 
                 1 
                 14 
                 59 
                 60 
                 1 
                 1 
                 7 
                 14 
                 15 
                 15 
                 1 
                 −5 
                 1 
                 15 
                 26 
                 30 
                 1 
                 −1 
                 −1 
                 16 
                 104 
                 100 
                 1 
               
               
                 0 
                 −7 
                 14 
                 67 
                 64 
                 1 
                 −5 
                 1 
                 14 
                 83 
                 85 
                 1 
                 −3 
                 8 
                 14 
                 27 
                 26 
                 1 
                 −4 
                 1 
                 15 
                 86 
                 86 
                 1 
                 0 
                 −1 
                 16 
                 129 
                 129 
                 1 
               
               
                 1 
                 −7 
                 14 
                 15 
                 16 
                 1 
                 −4 
                 1 
                 14 
                 117 
                 117 
                 1 
                 −2 
                 8 
                 14 
                 66 
                 64 
                 1 
                 −3 
                 1 
                 15 
                 57 
                 57 
                 1 
                 −4 
                 0 
                 16 
                 106 
                 108 
                 1 
               
               
                 −4 
                 −6 
                 14 
                 120 
                 120 
                 1 
                 −3 
                 1 
                 14 
                 47 
                 44 
                 1 
                 −1 
                 8 
                 14 
                 34 
                 32 
                 1 
                 −2 
                 1 
                 15 
                 34 
                 34 
                 1 
                 −3 
                 0 
                 16 
                 4 
                 6 
                 4 
               
               
                 −3 
                 −6 
                 14 
                 103 
                 102 
                 1 
                 −2 
                 1 
                 14 
                 25 
                 26 
                 1 
                 0 
                 8 
                 14 
                 85 
                 82 
                 1 
                 −1 
                 1 
                 15 
                 150 
                 147 
                 1 
                 −2 
                 0 
                 16 
                 40 
                 35 
                 1 
               
               
                 −2 
                 −6 
                 14 
                 28 
                 27 
                 1 
                 −1 
                 1 
                 14 
                 79 
                 76 
                 1 
                 −1 
                 9 
                 14 
                 53 
                 49 
                 1 
                 0 
                 1 
                 15 
                 41 
                 40 
                 1 
                 −1 
                 0 
                 16 
                 32 
                 33 
                 1 
               
               
                 −1 
                 −6 
                 14 
                 66 
                 63 
                 1 
                 0 
                 1 
                 14 
                 150 
                 148 
                 2 
                 −3 
                 −7 
                 15 
                 50 
                 47 
                 1 
                 1 
                 1 
                 15 
                 35 
                 36 
                 1 
                 0 
                 0 
                 16 
                 30 
                 30 
                 1 
               
               
                 0 
                 −6 
                 14 
                 27 
                 22 
                 1 
                 1 
                 1 
                 14 
                 47 
                 51 
                 1 
                 −2 
                 −7 
                 15 
                 77 
                 80 
                 1 
                 2 
                 1 
                 15 
                 53 
                 53 
                 1 
                 −4 
                 1 
                 16 
                 86 
                 86 
                 1 
               
               
                 1 
                 −6 
                 14 
                 59 
                 53 
                 1 
                 2 
                 1 
                 14 
                 15 
                 16 
                 1 
                 −1 
                 −7 
                 15 
                 10 
                 11 
                 1 
                 −5 
                 2 
                 15 
                 50 
                 51 
                 1 
                 −3 
                 1 
                 16 
                 79 
                 79 
                 1 
               
               
                 −5 
                 −5 
                 14 
                 36 
                 34 
                 1 
                 −6 
                 2 
                 14 
                 21 
                 23 
                 1 
                 −3 
                 −6 
                 15 
                 55 
                 60 
                 1 
                 −4 
                 2 
                 15 
                 27 
                 29 
                 1 
                 −2 
                 1 
                 16 
                 13 
                 13 
                 1 
               
               
                 −4 
                 −5 
                 14 
                 96 
                 95 
                 1 
                 −5 
                 2 
                 14 
                 42 
                 40 
                 1 
                 −2 
                 −6 
                 15 
                 26 
                 24 
                 1 
                 −3 
                 2 
                 15 
                 118 
                 119 
                 1 
                 −1 
                 1 
                 16 
                 103 
                 100 
                 1 
               
               
                 −3 
                 −5 
                 14 
                 25 
                 22 
                 1 
                 −4 
                 2 
                 14 
                 164 
                 160 
                 1 
                 −1 
                 −6 
                 15 
                 35 
                 35 
                 1 
                 −2 
                 2 
                 15 
                 72 
                 68 
                 1 
                 0 
                 1 
                 16 
                 128 
                 129 
                 1 
               
               
                 −2 
                 −5 
                 14 
                 86 
                 82 
                 1 
                 −3 
                 2 
                 14 
                 209 
                 202 
                 2 
                 0 
                 −6 
                 15 
                 36 
                 36 
                 1 
                 −1 
                 2 
                 15 
                 83 
                 87 
                 1 
                 −4 
                 2 
                 16 
                 42 
                 41 
                 1 
               
               
                 −1 
                 −5 
                 14 
                 76 
                 69 
                 1 
                 −2 
                 2 
                 14 
                 75 
                 76 
                 1 
                 −4 
                 −5 
                 15 
                 75 
                 73 
                 1 
                 0 
                 2 
                 15 
                 156 
                 149 
                 2 
                 −3 
                 2 
                 16 
                 36 
                 30 
                 1 
               
               
                 0 
                 −5 
                 14 
                 54 
                 57 
                 1 
                 −1 
                 2 
                 14 
                 66 
                 66 
                 1 
                 −3 
                 −5 
                 15 
                 30 
                 26 
                 1 
                 1 
                 2 
                 15 
                 47 
                 47 
                 1 
                 −2 
                 2 
                 16 
                 54 
                 57 
                 1 
               
               
                 1 
                 −5 
                 14 
                 71 
                 71 
                 1 
                 0 
                 2 
                 14 
                 87 
                 87 
                 1 
                 −2 
                 −5 
                 15 
                 9 
                 5 
                 1 
                 −4 
                 3 
                 15 
                 41 
                 37 
                 1 
                 −1 
                 2 
                 16 
                 60 
                 56 
                 1 
               
               
                 −5 
                 −4 
                 14 
                 64 
                 65 
                 1 
                 1 
                 2 
                 14 
                 83 
                 83 
                 1 
                 −1 
                 −5 
                 15 
                 77 
                 77 
                 1 
                 −3 
                 3 
                 15 
                 35 
                 36 
                 1 
                 0 
                 2 
                 16 
                 117 
                 118 
                 1 
               
               
                 −4 
                 −4 
                 14 
                 94 
                 92 
                 1 
                 2 
                 2 
                 14 
                 33 
                 37 
                 1 
                 0 
                 −5 
                 15 
                 39 
                 35 
                 1 
                 −2 
                 3 
                 15 
                 19 
                 19 
                 1 
                 −3 
                 3 
                 16 
                 13 
                 11 
                 4 
               
               
                 −3 
                 −4 
                 14 
                 35 
                 33 
                 1 
                 −5 
                 3 
                 14 
                 27 
                 22 
                 1 
                 1 
                 −5 
                 15 
                 110 
                 110 
                 2 
                 −1 
                 3 
                 15 
                 38 
                 35 
                 1 
                 −2 
                 3 
                 16 
                 25 
                 25 
                 1 
               
               
                 −2 
                 −4 
                 14 
                 98 
                 97 
                 1 
                 −4 
                 3 
                 14 
                 34 
                 32 
                 1 
                 −4 
                 −4 
                 15 
                 21 
                 21 
                 1 
                 0 
                 3 
                 15 
                 56 
                 53 
                 1 
                 −1 
                 3 
                 16 
                 49 
                 49 
                 1 
               
               
                 −1 
                 −4 
                 14 
                 86 
                 80 
                 1 
                 −3 
                 3 
                 14 
                 20 
                 20 
                 1 
                 −3 
                 −4 
                 15 
                 8 
                 9 
                 3 
                 1 
                 3 
                 15 
                 35 
                 30 
                 1 
                 0 
                 3 
                 16 
                 45 
                 43 
                 1 
               
               
                 0 
                 −4 
                 14 
                 118 
                 111 
                 1 
                 −2 
                 3 
                 14 
                 85 
                 83 
                 1 
                 −2 
                 −4 
                 15 
                 35 
                 32 
                 1 
                 −4 
                 4 
                 15 
                 22 
                 21 
                 1 
                 −3 
                 4 
                 16 
                 42 
                 42 
                 1 
               
               
                 1 
                 −4 
                 14 
                 72 
                 75 
                 1 
                 −1 
                 3 
                 14 
                 34 
                 34 
                 1 
                 −1 
                 −4 
                 15 
                 38 
                 37 
                 1 
                 −3 
                 4 
                 15 
                 10 
                 9 
                 1 
                 −2 
                 4 
                 16 
                 49 
                 51 
                 1 
               
               
                 −5 
                 −3 
                 14 
                 21 
                 22 
                 1 
                 0 
                 3 
                 14 
                 91 
                 90 
                 1 
                 0 
                 −4 
                 15 
                 86 
                 84 
                 1 
                 −2 
                 4 
                 15 
                 34 
                 32 
                 1 
                 −1 
                 4 
                 16 
                 29 
                 29 
                 1 
               
               
                 −4 
                 −3 
                 14 
                 32 
                 32 
                 1 
                 1 
                 3 
                 14 
                 113 
                 107 
                 1 
                 1 
                 −4 
                 15 
                 14 
                 15 
                 2 
                 −1 
                 4 
                 15 
                 39 
                 37 
                 1 
               
               
                   
               
             
          
         
       
     
         [0000]    
       
         
               
             
               
               
             
               
               
               
             
               
               
             
           
               
                 TABLE 9 
               
               
                   
               
               
                 Crystal data and structure refinement for MET-2. 
               
               
                   
               
             
             
               
                   
               
             
          
           
               
                 Empirical formula 
                 C32H56O4 
               
               
                 Formula weight 
                  504.77 
               
               
                 Temperature 
                 298(1) K 
               
               
                 Wavelength 
                 1.54178 Å 
               
               
                 Crystal system, 
                 space group Monoclinic, C2 
               
             
          
           
               
                 Unit cell dimensions 
                 a = 27.3382(16) Å 
                 α = 90° 
               
               
                   
                 b = 6.6860(13) Å 
                 β = 113.57(3)° 
               
               
                   
                 c = 19.221(10) A 
                 γ = 90° 
               
             
          
           
               
                 Volume 
                 3320.3(11) Å 3   
               
               
                 Z 
                   4 
               
               
                 Calculated density 
                 1.041 Mg/m 3   
               
               
                 Absorption coefficient 
                 0.513 mm −1   
               
               
                 F(000) 
                 1120 
               
               
                 Crystal size 
                 0.36 × 0.17 × 0.03 mm 
               
               
                 Theta range for data collection 
                 2.51 to 58.69° 
               
               
                 Limiting indices 
                 −29 &lt;= h &lt;= 28, −6 &lt;= k &lt;= 6, 
               
               
                   
                 −21 &lt;= l &lt;= 21 
               
               
                 Reflections collected/unique 
                 10383/3985 [R(int) = 0.0473] 
               
               
                 Data/restraints/parameters 
                 3985/1/325 
               
               
                 Goodness-of-fit on F 2   
                   1.073 
               
               
                 Final R indices [I &gt; 2σ(I)] 
                 R1 = 0.0618, wR2 = 0.1600 
               
               
                 R indices (all data) 
                 R1 = 0.0844, wR2 = 0.1778 
               
               
                 Absolute structure parameter 
                   0.2(4) 
               
               
                 Largest diff. peak and hole 
                 0.140 and −0.190 e/Å −3   
               
               
                   
               
             
          
         
       
     
         [0000]    
       
         
               
             
               
               
               
               
               
             
               
               
               
               
               
               
             
           
               
                 TABLE 10 
               
             
             
               
                   
               
               
                 Atomic coordinates (Å 2  × 10 4 ) and equivalent isotropic 
               
               
                 displacement parameters (Å 2  × 10 3 ) for MET-2 U(eq) 
               
               
                 is defined as one third of the trace of the orthogonalized Uij tensor. 
               
             
          
           
               
                   
                 x 
                 y 
                 z 
                 U(eq) 
               
               
                   
                   
               
             
          
           
               
                   
                 O(3) 
                 9651(1) 
                 8018(5) 
                 3345(2) 
                 80(1) 
               
               
                   
                 C(20) 
                 7634(1) 
                 8343(6) 
                 −2763(2) 
                 67(1) 
               
               
                   
                 O(25) 
                 9328(1) 
                 7952(6) 
                 −3391(2) 
                 102(1) 
               
               
                   
                 C(13) 
                 7985(1) 
                 7574(6) 
                 −1301(2) 
                 59(1) 
               
               
                   
                 C(1) 
                 9449(2) 
                 12075(6)  
                 2708(2) 
                 66(1) 
               
               
                   
                 C(17) 
                 8118(1) 
                 8204(6) 
                 −1982(2) 
                 59(1) 
               
               
                   
                 O(1) 
                 9565(1) 
                 14167(5)  
                 2735(2) 
                 88(1) 
               
               
                   
                 C(10) 
                 8922(2) 
                 11685(7)  
                 2036(2) 
                 73(1) 
               
               
                   
                 C(23) 
                 8253(2) 
                 8546(7) 
                 −3469(2) 
                 70(1) 
               
               
                   
                 C(2) 
                 9409(2) 
                 11384(7)  
                 3438(2) 
                 67(1) 
               
               
                   
                 C(12) 
                 7838(2) 
                 5387(7) 
                 −1291(2) 
                 74(1) 
               
               
                   
                 C(14) 
                 8539(1) 
                 7926(6) 
                 −637(2) 
                 64(1) 
               
               
                   
                 C(22) 
                 7766(2) 
                 7484(7) 
                 −3431(2) 
                 69(1) 
               
               
                   
                 C(18) 
                 7564(2) 
                 8908(7) 
                 −1201(3) 
                 79(1) 
               
               
                   
                 C(5) 
                 8739(2) 
                 9568(7) 
                 2011(2) 
                 68(1) 
               
               
                   
                 C(3) 
                 9242(2) 
                 9248(7) 
                 3413(2) 
                 68(1) 
               
               
                   
                 C(15) 
                 8704(2) 
                 9975(8) 
                 −812(2) 
                 77(1) 
               
               
                   
                 C(9) 
                 8370(2) 
                 5285(7) 
                 139(2) 
                 83(1) 
               
               
                   
                 C(16) 
                 8471(2) 
                 10076(7)  
                 −1687(2) 
                 76(1) 
               
               
                   
                 C(25) 
                 8924(2) 
                  8719(10) 
                 −4091(2) 
                 93(2) 
               
               
                   
                 C(8) 
                 8525(2) 
                 7441(7) 
                 118(2) 
                 69(1) 
               
               
                   
                 C(30) 
                 7870(2) 
                 5245(7) 
                 −3306(3) 
                 98(2) 
               
               
                   
                 C(28) 
                 7279(2) 
                  7779(10) 
                 −4185(2) 
                 103(2) 
               
               
                   
                 C(24) 
                 8394(2) 
                  7945(10) 
                 −4124(2) 
                 91(2) 
               
               
                   
                 C(11) 
                 7843(2) 
                 4765(8) 
                 −517(2) 
                 83(1) 
               
               
                   
                 C(4) 
                 8712(2) 
                 8882(8) 
                 2740(2) 
                 74(1) 
               
               
                   
                 C(27) 
                 8974(2) 
                 10999(12) 
                 −4028(4) 
                 134(3) 
               
               
                   
                 C(6) 
                 8624(1) 
                 8330(8) 
                 1421(2) 
                 72(1) 
               
               
                   
                 C(21) 
                 7379(2) 
                 10414(8)  
                 −2945(3) 
                 98(2) 
               
               
                   
                 C(26) 
                 9029(2) 
                  7983(18) 
                 −4745(3) 
                 177(4) 
               
               
                   
                 C(7) 
                 8639(2) 
                 8753(7) 
                 686(2) 
                 72(1) 
               
               
                   
                 C(29) 
                 9490(2) 
                 12565(9)  
                 4016(2) 
                 97(2) 
               
               
                   
                 O(201) 
                 10425(1) 
                 14824(6)  
                 2396(2) 
                 112(1) 
               
               
                   
                 C(202) 
                 10381(3) 
                 15282(14) 
                 1660(3) 
                 128(2) 
               
               
                   
                 C(201) 
                 10109(4) 
                 17151(16) 
                 1381(5) 
                 185(4) 
               
               
                   
                 C(203) 
                 10130(5) 
                 13539(17) 
                 1161(5) 
                 223(5) 
               
               
                   
                   
               
             
          
         
       
     
         [0000]    
       
         
               
             
               
               
               
             
           
               
                 TABLE 11 
               
               
                   
               
               
                 Bond lengths [Å] for MET-2. 
               
               
                   
               
             
             
               
                   
               
             
          
           
               
                   
                 O(3)—C(3) 
                 1.434(5) 
               
               
                   
                 C(20)—C(21) 
                 1.527(6) 
               
               
                   
                 C(20)—C(17) 
                 1.558(5) 
               
               
                   
                 C(20)—C(22) 
                 1.573(5) 
               
               
                   
                 O(25)—C(25) 
                 1.451(5) 
               
               
                   
                 C(13)—C(12) 
                 1.518(6) 
               
               
                   
                 C(13)—C(18) 
                 1.527(6) 
               
               
                   
                 C(13)—C(17) 
                 1.549(5) 
               
               
                   
                 C(13)—C(14) 
                 1.560(5) 
               
               
                   
                 C(1)—O(1) 
                 1.431(5) 
               
               
                   
                 C(1)—C(2) 
                 1.521(5) 
               
               
                   
                 C(1)—C(10) 
                 1.524(6) 
               
               
                   
                 C(17)—C(16) 
                 1.543(6) 
               
               
                   
                 C(10)—C(5) 
                 1.495(6) 
               
               
                   
                 C(23)—C(24) 
                 1.511(5) 
               
               
                   
                 C(23)—C(22) 
                 1.535(6) 
               
               
                   
                 C(2)—C(29) 
                 1.308(6) 
               
               
                   
                 C(2)—C(3) 
                 1.495(6) 
               
               
                   
                 C(12)—C(11) 
                 1.541(5) 
               
               
                   
                 C(14)—C(8) 
                 1.501(5) 
               
               
                   
                 C(14)—C(15) 
                 1.522(6) 
               
               
                   
                 C(22)—C(30) 
                 1.524(7) 
               
               
                   
                 C(22)—C(28) 
                 1.541(6) 
               
               
                   
                 C(5)—C(6) 
                 1.336(6) 
               
               
                   
                 C(5)—C(4) 
                 1.505(5) 
               
               
                   
                 C(3)—C(4) 
                 1.527(5) 
               
               
                   
                 C(15)—C(16) 
                 1.543(5) 
               
               
                   
                 C(9)—C(8) 
                 1.508(7) 
               
               
                   
                 C(9)—C(11) 
                 1.527(6) 
               
               
                   
                 C(25)—C(26) 
                 1.483(8) 
               
               
                   
                 C(25)—C(24) 
                 1.516(7) 
               
               
                   
                 C(25)—C(27) 
                 1.532(9) 
               
               
                   
                 C(8)—C(7) 
                 1.336(6) 
               
               
                   
                 C(6)—C(7) 
                 1.458(5) 
               
               
                   
                 O(201)—C(202) 
                 1.405(7) 
               
               
                   
                 C(202)—C(201) 
                 1.443(11) 
               
               
                   
                 C(202)—C(203) 
                 1.490(11) 
               
               
                   
                   
               
             
          
         
       
     
         [0000]    
       
         
               
             
               
               
               
             
           
               
                 TABLE 12 
               
               
                   
               
               
                 bond angles [°] for MET-2. 
               
               
                   
               
             
             
               
                   
               
             
          
           
               
                   
                 C(21)—C(20)—C(17) 
                 114.1(3) 
               
               
                   
                 C(21)—C(20)—C(22) 
                 112.2(4) 
               
               
                   
                 C(17)—C(20)—C(22) 
                 112.4(3) 
               
               
                   
                 C(12)—C(13)—C(18) 
                 110.1(3) 
               
               
                   
                 C(12)—C(13)—C(17) 
                 115.2(3) 
               
               
                   
                 C(18)—C(13)—C(17) 
                 113.0(3) 
               
               
                   
                 C(12)—C(13)—C(14) 
                 108.1(3) 
               
               
                   
                 C(18)—C(13)—C(14) 
                 110.0(3) 
               
               
                   
                 C(17)—C(13)—C(14) 
                 99.8(3) 
               
               
                   
                 O(1)—C(1)—C(2) 
                 111.1(3) 
               
               
                   
                 O(1)—C(1)—C(10) 
                 108.7(4) 
               
               
                   
                 C(2)—C(1)—C(10) 
                 109.7(3) 
               
               
                   
                 C(16)—C(17)—C(13) 
                 103.5(3) 
               
               
                   
                 C(16)—C(17)—C(20) 
                 118.1(3) 
               
               
                   
                 C(13)—C(17)—C(20) 
                 115.7(3) 
               
               
                   
                 C(5)—C(10)—C(1) 
                 112.3(3) 
               
               
                   
                 C(24)—C(23)—C(22) 
                 115.5(4) 
               
               
                   
                 C(29)—C(2)—C(3) 
                 123.4(4) 
               
               
                   
                 C(29)—C(2)—C(1) 
                 123.4(4) 
               
               
                   
                 C(3)—C(2)—C(1) 
                 113.2(3) 
               
               
                   
                 C(13)—C(12)—C(11) 
                 111.8(3) 
               
               
                   
                 C(8)—C(14)—C(15) 
                 122.2(3) 
               
               
                   
                 C(8)—C(14)—C(13) 
                 111.5(3) 
               
               
                   
                 C(15)—C(14)—C(13) 
                 103.4(3) 
               
               
                   
                 C(30)—C(22)—C(23) 
                 110.6(4) 
               
               
                   
                 C(30)—C(22)—C(28) 
                 108.1(4) 
               
               
                   
                 C(23)—C(22)—C(28) 
                 109.6(3) 
               
               
                   
                 C(30)—C(22)—C(20) 
                 108.7(3) 
               
               
                   
                 C(23)—C(22)—C(20) 
                 110.8(3) 
               
               
                   
                 C(28)—C(22)—C(20) 
                 109.1(3) 
               
               
                   
                 C(6)—C(5)—C(10) 
                 125.2(4) 
               
               
                   
                 C(6)—C(5)—C(4) 
                 121.3(4) 
               
               
                   
                 C(10)—C(5)—C(4) 
                 113.5(4) 
               
               
                   
                 O(3)—C(3)—C(2) 
                 108.1(3) 
               
               
                   
                 O(3)—C(3)—C(4) 
                 109.9(3) 
               
               
                   
                 C(2)—C(3)—C(4) 
                 110.8(4) 
               
               
                   
                 C(14)—C(15)—C(16) 
                 104.5(3) 
               
               
                   
                 C(8)—C(9)—C(11) 
                 112.2(4) 
               
               
                   
                 C(17)—C(16)—C(15) 
                 106.9(3) 
               
               
                   
                 O(25)—C(25)—C(26) 
                 109.6(5) 
               
               
                   
                 O(25)—C(25)—C(24) 
                 106.2(4) 
               
               
                   
                 C(26)—C(25)—C(24) 
                 111.0(5) 
               
               
                   
                 O(25)—C(25)—C(27) 
                 105.5(5) 
               
               
                   
                 C(26)—C(25)—C(27) 
                 110.8(6) 
               
               
                   
                 C(24)—C(25)—C(27) 
                 113.4(5) 
               
               
                   
                 C(7)—C(8)—C(14) 
                 124.1(4) 
               
               
                   
                 C(7)—C(8)—C(9) 
                 125.5(4) 
               
               
                   
                 C(14)—C(8)—C(9) 
                 110.4(3) 
               
               
                   
                 C(23)—C(24)—C(25) 
                 115.6(4) 
               
               
                   
                 C(9)—C(11)—C(12) 
                 112.2(3) 
               
               
                   
                 C(5)—C(4)—C(3) 
                 110.9(3) 
               
               
                   
                 C(5)—C(6)—C(7) 
                 127.9(4) 
               
               
                   
                 C(8)—C(7)—C(6) 
                 125.2(4) 
               
               
                   
                 O(201)—C(202)—C(201) 
                 112.8(6) 
               
               
                   
                 O(201)—C(202)—C(203) 
                 108.1(7) 
               
               
                   
                 C(201)—C(202)—C(203) 
                 113.8(7) 
               
               
                   
                   
               
             
          
         
       
     
         [0000]    
       
         
               
             
               
               
               
               
               
               
               
             
               
               
               
               
               
               
               
             
           
               
                 TABLE 13 
               
             
             
               
                   
               
               
                 Anisotropic displacement parameters (Å 2  × 10 3 ) for MET-2. The 
               
               
                 anisotropic displacement factor exponent takes the form 
               
               
                 “−2π 2 [h 2 a * 2U 11  + + 2hka * b * U 12 ] 
               
             
          
           
               
                   
                 U 11   
                 U 22   
                 U 33   
                 U 23   
                 U 13   
                 U 12   
               
               
                   
                   
               
             
          
           
               
                 O(3) 
                 67(2) 
                 71(2) 
                 93(2) 
                  −5(2) 
                 22(1) 
                  −7(2) 
               
               
                 C(20) 
                 58(2) 
                 70(3) 
                 67(2) 
                  −4(2) 
                 20(2) 
                  −6(2) 
               
               
                 O(25) 
                 79(2) 
                 144(3)  
                 86(2) 
                  43(2) 
                 36(2) 
                  34(2) 
               
               
                 C(13) 
                 63(2) 
                 53(3) 
                 67(2) 
                 −10(2) 
                 31(2) 
                  −4(2) 
               
               
                 C(1) 
                 73(3) 
                 52(3) 
                 75(3) 
                  −5(2) 
                 31(2) 
                  −8(2) 
               
               
                 C(17) 
                 53(2) 
                 65(3) 
                 60(2) 
                 −10(2) 
                 23(2) 
                 −12(2) 
               
               
                 O(1) 
                 102(2)  
                 67(2) 
                 87(2) 
                 −11(2) 
                 31(2) 
                 −14(2) 
               
               
                 C(10) 
                 76(3) 
                 76(3) 
                 60(2) 
                  −6(2) 
                 18(2) 
                  −3(2) 
               
               
                 C(23) 
                 65(2) 
                 79(3) 
                 65(2) 
                  −1(2) 
                 25(2) 
                  −7(2) 
               
               
                 C(2) 
                 62(2) 
                 73(3) 
                 63(2) 
                  −7(2) 
                 21(2) 
                  −5(2) 
               
               
                 C(12) 
                 88(3) 
                 74(3) 
                 65(2) 
                 −12(2) 
                 37(2) 
                 −23(2) 
               
               
                 C(14) 
                 65(2) 
                 65(3) 
                 63(2) 
                  −9(2) 
                 27(2) 
                 −11(2) 
               
               
                 C(22) 
                 61(2) 
                 79(3) 
                 64(2) 
                  −9(2) 
                 21(2) 
                 −16(2) 
               
               
                 C(18) 
                 68(2) 
                 86(3) 
                 91(3) 
                 −20(2) 
                 38(2) 
                  −8(2) 
               
               
                 C(5) 
                 54(2) 
                 82(3) 
                 58(2) 
                  −6(2) 
                 14(2) 
                 −13(2) 
               
               
                 C(3) 
                 68(2) 
                 76(3) 
                 59(2) 
                  −4(2) 
                 24(2) 
                  −9(2) 
               
               
                 C(15) 
                 78(3) 
                 82(3) 
                 71(2) 
                 −11(2) 
                 30(2) 
                 −23(3) 
               
               
                 C(9) 
                 106(3)  
                 76(3) 
                 68(2) 
                  −4(2) 
                 38(2) 
                 −11(3) 
               
               
                 C(16) 
                 73(3) 
                 80(3) 
                 73(2) 
                  −7(2) 
                 26(2) 
                 −26(2) 
               
               
                 C(25) 
                 68(3) 
                 146(6)  
                 64(3) 
                  17(3) 
                 24(2) 
                  3(3) 
               
               
                 C(8) 
                 66(2) 
                 72(3) 
                 65(2) 
                  −4(2) 
                 22(2) 
                  −6(2) 
               
               
                 C(30) 
                 152(5)  
                 58(3) 
                 103(3)  
                 −15(3) 
                 70(3) 
                 −17(3) 
               
               
                 C(28) 
                 76(3) 
                 148(5)  
                 71(3) 
                  −6(3) 
                 16(2) 
                 −18(3) 
               
               
                 C(24) 
                 81(3) 
                 129(5)  
                 65(2) 
                  −4(3) 
                 31(2) 
                 −11(3) 
               
               
                 C(11) 
                 108(3)  
                 78(3) 
                 76(3) 
                 −16(2) 
                 49(3) 
                 −37(3) 
               
               
                 C(4) 
                 60(2) 
                 97(4) 
                 67(2) 
                  −2(2) 
                 28(2) 
                 −14(2) 
               
               
                 C(27) 
                 75(4) 
                 156(7)  
                 150(5)  
                  72(5) 
                 22(3) 
                 −12(4) 
               
               
                 C(6) 
                 60(2) 
                 84(3) 
                 67(2) 
                  −7(2) 
                 20(2) 
                 −19(2) 
               
               
                 C(21) 
                 88(3) 
                 94(4) 
                 103(3)  
                  10(3) 
                 26(3) 
                  32(3) 
               
               
                 C(26) 
                 137(5)  
                 337(12) 
                 83(3) 
                  −5(6) 
                 72(4) 
                 −23(7) 
               
               
                 C(7) 
                 65(2) 
                 81(3) 
                 60(2) 
                  −4(2) 
                 15(2) 
                 −17(2) 
               
               
                 C(29) 
                 125(4)  
                 92(4) 
                 69(3) 
                 −10(3) 
                 35(3) 
                  −8(3) 
               
               
                 O(201) 
                 123(3)  
                 122(3)  
                 96(2) 
                 −17(2) 
                 51(2) 
                 −23(2) 
               
               
                 C(202) 
                 113(4)  
                 180(8)  
                 101(4)  
                  −8(5) 
                 54(4) 
                 −21(5) 
               
               
                 C(201) 
                 192(8)  
                 180(9)  
                 152(7)  
                  42(6) 
                 36(6) 
                  15(8) 
               
               
                 C(203) 
                 305(13) 
                 227(11) 
                 134(6)  
                 −84(7) 
                 85(7) 
                  −25(10) 
               
               
                   
               
             
          
         
       
     
         [0000]    
       
         
               
             
               
               
               
               
               
             
               
               
               
               
               
               
             
           
               
                 TABLE 14 
               
             
             
               
                   
               
               
                 Hydrogen coordinates (Å 2  × 10 4 ) and isotropic 
               
               
                 displacement parameters (Å 2  × 10 3 ) for MET-2. 
               
             
          
           
               
                   
                 x 
                 y 
                 z 
                 U(eq) 
               
               
                   
                   
               
             
          
           
               
                   
                 H(3A) 
                 9521 
                 6950 
                 3147 
                 120 
               
               
                   
                 H(20I) 
                 7360 
                 7457 
                 −2725 
                 80 
               
               
                   
                 H(25A) 
                 9621 
                 8007 
                 −3413 
                 153 
               
               
                   
                 H(1A) 
                 9733 
                 11326 
                 2636 
                 79 
               
               
                   
                 H(17A) 
                 8352 
                 7159 
                 −2035 
                 71 
               
               
                   
                 H(1B) 
                 9853 
                 14390 
                 3088 
                 131 
               
               
                   
                 H(10A) 
                 8651 
                 12572 
                 2069 
                 88 
               
               
                   
                 H(10B) 
                 8963 
                 11988 
                 1569 
                 88 
               
               
                   
                 H(23A) 
                 8187 
                 9976 
                 −3499 
                 84 
               
               
                   
                 H(23B) 
                 8559 
                 8290 
                 −2999 
                 84 
               
               
                   
                 H(12A) 
                 8088 
                 4563 
                 −1405 
                 88 
               
               
                   
                 H(12B) 
                 7484 
                 5157 
                 −1683 
                 88 
               
               
                   
                 H(14A) 
                 8784 
                 6962 
                 −710 
                 77 
               
               
                   
                 H(18A) 
                 7495 
                 8444 
                 −777 
                 119 
               
               
                   
                 H(18B) 
                 7241 
                 8859 
                 −1653 
                 119 
               
               
                   
                 H(18C) 
                 7693 
                 10260 
                 −1111 
                 119 
               
               
                   
                 H(3B) 
                 9203 
                 8917 
                 3885 
                 82 
               
               
                   
                 H(15A) 
                 9090 
                 10101 
                 −603 
                 92 
               
               
                   
                 H(15B) 
                 8558 
                 11029 
                 −605 
                 92 
               
               
                   
                 H(9A) 
                 8338 
                 5027 
                 616 
                 99 
               
               
                   
                 H(9B) 
                 8649 
                 4428 
                 116 
                 99 
               
               
                   
                 H(16A) 
                 8260 
                 11280 
                 −1864 
                 92 
               
               
                   
                 H(16B) 
                 8756 
                 10086 
                 −1867 
                 92 
               
               
                   
                 H(30A) 
                 7954 
                 4704 
                 −3709 
                 147 
               
               
                   
                 H(30B) 
                 7558 
                 4597 
                 −3304 
                 147 
               
               
                   
                 H(30C) 
                 8165 
                 5024 
                 −2829 
                 147 
               
               
                   
                 H(28A) 
                 7358 
                 7266 
                 −4595 
                 154 
               
               
                   
                 H(28B) 
                 7197 
                 9178 
                 −4264 
                 154 
               
               
                   
                 H(28C) 
                 6978 
                 7076 
                 −4166 
                 154 
               
               
                   
                 H(24A) 
                 8114 
                 8414 
                 −4591 
                 109 
               
               
                   
                 H(24B) 
                 8398 
                 6496 
                 −4147 
                 109 
               
               
                   
                 H(11A) 
                 7553 
                 5434 
                 −441 
                 100 
               
               
                   
                 H(11B) 
                 7783 
                 3335 
                 −517 
                 100 
               
               
                   
                 H(4A) 
                 8627 
                 7467 
                 2706 
                 89 
               
               
                   
                 H(4B) 
                 8430 
                 9599 
                 2818 
                 89 
               
               
                   
                 H(27A) 
                 9317 
                 11395 
                 −4006 
                 201 
               
               
                   
                 H(27B) 
                 8937 
                 11432 
                 −3575 
                 201 
               
               
                   
                 H(27C) 
                 8699 
                 11600 
                 −4462 
                 201 
               
               
                   
                 H(6A) 
                 8522 
                 7041 
                 1487 
                 87 
               
               
                   
                 H(21A) 
                 7302 
                 10877 
                 −2527 
                 148 
               
               
                   
                 H(21B) 
                 7054 
                 10341 
                 −3393 
                 148 
               
               
                   
                 H(21C) 
                 7620 
                 11328 
                 −3030 
                 148 
               
               
                   
                 H(26A) 
                 8994 
                 6554 
                 −4776 
                 265 
               
               
                   
                 H(26B) 
                 9385 
                 8347 
                 −4679 
                 265 
               
               
                   
                 H(26C) 
                 8778 
                 8571 
                 −5205 
                 265 
               
               
                   
                 H(7A) 
                 8736 
                 10038 
                 606 
                 86 
               
               
                   
                 H(29A) 
                 9444 
                 12086 
                 4440 
                 116 
               
               
                   
                 H(29B) 
                 9594 
                 13885 
                 4003 
                 116 
               
               
                   
                 H(20A) 
                 10540 
                 15801 
                 2672 
                 167 
               
               
                   
                 H(20B) 
                 10744 
                 15418 
                 1682 
                 154 
               
               
                   
                 H(20C) 
                 10300 
                 18216 
                 1714 
                 278 
               
               
                   
                 H(20D) 
                 9753 
                 17079 
                 1362 
                 278 
               
               
                   
                 H(20E) 
                 10094 
                 17402 
                 881 
                 278 
               
               
                   
                 H(20F) 
                 10095 
                 13823 
                 653 
                 334 
               
               
                   
                 H(20G) 
                 9784 
                 13292 
                 1161 
                 334 
               
               
                   
                 H(20H) 
                 10351 
                 12378 
                 1348 
                 334 
               
               
                   
                   
               
             
          
         
       
     
         [0000]    
       
         
               
             
               
               
               
             
           
               
                 TABLE 15 
               
               
                   
               
               
                 Torsion angles [deg] for MET-2. 
               
               
                   
               
             
             
               
                   
               
             
          
           
               
                   
                 C(12)—C(13)—C(17)—C(16) 
                 −156.5(4) 
               
               
                   
                 C(18)—C(13)—C(17)—C(16) 
                 75.8(4) 
               
               
                   
                 C(14)—C(13)—C(17)—C(16) 
                 −41.0(4) 
               
               
                   
                 C(12)—C(13)—C(17)—C(20) 
                 72.7(5) 
               
               
                   
                 C(18)—C(13)—C(17)—C(20) 
                 −55.1(4) 
               
               
                   
                 C(14)—C(13)—C(17)—C(20) 
                 −171.9(3) 
               
               
                   
                 C(21)—C(20)—C(17)—C(16) 
                 −32.0(5) 
               
               
                   
                 C(22)—C(20)—C(17)—C(16) 
                 97.2(4) 
               
               
                   
                 C(21)—C(20)—C(17)—C(13) 
                 91.5(5) 
               
               
                   
                 C(22)—C(20)—C(17)—C(13) 
                 −139.3(4) 
               
               
                   
                 O(1)—C(1)—C(10)—C(5) 
                 −174.1(4) 
               
               
                   
                 C(2)—C(1)—C(10)—C(5) 
                 −52.4(5) 
               
               
                   
                 O(1)—C(1)—C(2)—C(29) 
                 −2.0(6) 
               
               
                   
                 C(10)—C(1)—C(2)—C(29) 
                 −122.2(5) 
               
               
                   
                 O(1)—C(1)—C(2)—C(3) 
                 175.1(4) 
               
               
                   
                 C(10)—C(1)—C(2)—C(3) 
                 54.9(5) 
               
               
                   
                 C(18)—C(13)—C(12)—C(11) 
                 −64.5(5) 
               
               
                   
                 C(17)—C(13)—C(12)—C(11) 
                 166.3(3) 
               
               
                   
                 C(14)—C(13)—C(12)—C(11) 
                 55.7(4) 
               
               
                   
                 C(12)—C(13)—C(14)—C(8) 
                 −59.9(4) 
               
               
                   
                 C(18)—C(13)—C(14)—C(8) 
                 60.3(5) 
               
               
                   
                 C(17)—C(13)—C(14)—C(8) 
                 179.4(3) 
               
               
                   
                 C(12)—C(13)—C(14)—C(15) 
                 167.1(3) 
               
               
                   
                 C(18)—C(13)—C(14)—C(15) 
                 −72.7(4) 
               
               
                   
                 C(17)—C(13)—C(14)—C(15) 
                 46.3(4) 
               
               
                   
                 C(24)—C(23)—C(22)—C(30) 
                 63.6(5) 
               
               
                   
                 C(24)—C(23)—C(22)—C(28) 
                 −55.4(5) 
               
               
                   
                 C(24)—C(23)—C(22)—C(20) 
                 −175.9(4) 
               
               
                   
                 C(21)—C(20)—C(22)—C(30) 
                 −164.4(4) 
               
               
                   
                 C(17)—C(20)—C(22)—C(30) 
                 65.4(4) 
               
               
                   
                 C(21)—C(20)—C(22)—C(23) 
                 73.9(4) 
               
               
                   
                 C(17)—C(20)—C(22)—C(23) 
                 −56.3(5) 
               
               
                   
                 C(21)—C(20)—C(22)—C(28) 
                 −46.8(5) 
               
               
                   
                 C(17)—C(20)—C(22)—C(28) 
                 −177.0(4) 
               
               
                   
                 C(1)—C(10)—C(5)—C(6) 
                 −124.5(4) 
               
               
                   
                 C(1)—C(10)—C(5)—C(4) 
                 53.4(5) 
               
               
                   
                 C(29)—C(2)—C(3)—O(3) 
                 −118.5(5) 
               
               
                   
                 C(1)—C(2)—C(3)—O(3) 
                 64.5(4) 
               
               
                   
                 C(29)—C(2)—C(3)—C(4) 
                 121.0(5) 
               
               
                   
                 C(1)—C(2)—C(3)—C(4) 
                 −56.1(4) 
               
               
                   
                 C(8)—C(14)—C(15)—C(16) 
                 −159.9(4) 
               
               
                   
                 C(13)—C(14)—C(15)—C(16) 
                 −33.4(4) 
               
               
                   
                 C(13)—C(17)—C(16)—C(15) 
                 21.6(4) 
               
               
                   
                 C(20)—C(17)—C(16)—C(15) 
                 151.0(3) 
               
               
                   
                 C(14)—C(15)—C(16)—C(17) 
                 7.3(5) 
               
               
                   
                 C(15)—C(14)—C(8)—C(7) 
                 2.0(6) 
               
               
                   
                 C(13)—C(14)—C(8)—C(7) 
                 −120.8(4) 
               
               
                   
                 C(15)—C(14)—C(8)—C(9) 
                 −177.6(4) 
               
               
                   
                 C(13)—C(14)—C(8)—C(9) 
                 59.6(5) 
               
               
                   
                 C(11)—C(9)—C(8)—C(7) 
                 125.6(4) 
               
               
                   
                 C(11)—C(9)—C(8)—C(14) 
                 −54.8(5) 
               
               
                   
                 C(22)—C(23)—C(24)—C(25) 
                 −170.1(4) 
               
               
                   
                 O(25)—C(25)—C(24)—C(23) 
                 59.0(6) 
               
               
                   
                 C(26)—C(25)—C(24)—C(23) 
                 178.1(6) 
               
               
                   
                 C(27)—C(25)—C(24)—C(23) 
                 −56.4(6) 
               
               
                   
                 C(8)—C(9)—C(11)—C(12) 
                 51.6(6) 
               
               
                   
                 C(13)—C(12)—C(11)—C(9) 
                 −53.0(5) 
               
               
                   
                 C(6)—C(5)—C(4)—C(3) 
                 124.7(4) 
               
               
                   
                 C(10)—C(5)—C(4)—C(3) 
                 −53.3(5) 
               
               
                   
                 O(3)—C(3)—C(4)—C(5) 
                 −65.7(5) 
               
               
                   
                 C(2)—C(3)—C(4)—C(5) 
                 53.8(5) 
               
               
                   
                 C(10)—C(5)—C(6)—C(7) 
                 −1.2(7) 
               
               
                   
                 C(4)—C(5)—C(6)—C(7) 
                 −179.0(4) 
               
               
                   
                 C(14)—C(8)—C(7)—C(6) 
                 179.4(4) 
               
               
                   
                 C(9)—C(8)—C(7)—C(6) 
                 −1.1(7) 
               
               
                   
                 C(5)—C(6)—C(7)—C(8) 
                 179.2(4) 
               
               
                   
                   
               
             
          
         
       
     
         [0000]    
       
         
               
             
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
             
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
             
           
               
                 TABLE 16 
               
             
             
               
                   
               
               
                 Observed and calculated structure factors for MET-2. 
               
             
          
           
               
                 h 
                 k 
                 l 
                 10Fo 
                 10Fc 
                 10s 
                 h 
                 k 
                 l 
                 10Fo 
                 10Fc 
                 10s 
                 h 
                 k 
                 l 
                 10Fo 
                 10Fc 
                 10s 
                 h 
                 k 
                 l 
                 10Fo 
                 10Fc 
                 10s 
                 h 
                 k 
                 l 
                 10Fo 
                 10Fc 
                 10s 
               
               
                   
               
             
          
           
               
                 16 
                 −6 
                 0 
                 23 
                 6 
                 23 
                 8 
                 2 
                 0 
                 224 
                 220 
                 8 
                 −15 
                 −3 
                 1 
                 173 
                 173 
                 6 
                 0 
                 0 
                 1 
                 381 
                 388 
                 6 
                 −12 
                 4 
                 1 
                 124 
                 117 
                 4 
               
               
                 9 
                 −5 
                 0 
                 179 
                 178 
                 8 
                 10 
                 2 
                 0 
                 276 
                 310 
                 10 
                 −13 
                 −3 
                 1 
                 172 
                 175 
                 6 
                 2 
                 0 
                 1 
                 833 
                 936 
                 12 
                 −10 
                 4 
                 1 
                 197 
                 179 
                 4 
               
               
                 11 
                 −5 
                 0 
                 59 
                 52 
                 13 
                 12 
                 2 
                 0 
                 175 
                 180 
                 7 
                 −11 
                 −3 
                 1 
                 115 
                 118 
                 5 
                 4 
                 0 
                 1 
                 1025 
                 1083 
                 15 
                 −8 
                 4 
                 1 
                 91 
                 99 
                 4 
               
               
                 13 
                 −5 
                 0 
                 99 
                 92 
                 9 
                 14 
                 2 
                 0 
                 56 
                 63 
                 14 
                 −9 
                 −3 
                 1 
                 240 
                 217 
                 8 
                 6 
                 0 
                 1 
                 570 
                 567 
                 9 
                 −6 
                 4 
                 1 
                 295 
                 284 
                 5 
               
               
                 15 
                 −5 
                 0 
                 0 
                 21 
                 1 
                 18 
                 2 
                 0 
                 194 
                 198 
                 6 
                 −7 
                 −3 
                 1 
                 205 
                 199 
                 8 
                 8 
                 0 
                 1 
                 1171 
                 1214 
                 18 
                 −4 
                 4 
                 1 
                 213 
                 211 
                 4 
               
               
                 17 
                 −5 
                 0 
                 60 
                 46 
                 13 
                 20 
                 2 
                 0 
                 86 
                 102 
                 12 
                 −5 
                 −3 
                 1 
                 348 
                 327 
                 10 
                 10 
                 0 
                 1 
                 73 
                 67 
                 4 
                 −2 
                 4 
                 1 
                 387 
                 390 
                 4 
               
               
                 19 
                 −5 
                 0 
                 23 
                 27 
                 23 
                 22 
                 2 
                 0 
                 76 
                 77 
                 13 
                 −3 
                 −3 
                 1 
                 592 
                 563 
                 18 
                 12 
                 0 
                 1 
                 331 
                 349 
                 8 
                 0 
                 4 
                 1 
                 224 
                 227 
                 3 
               
               
                 4 
                 −4 
                 0 
                 167 
                 167 
                 8 
                 24 
                 2 
                 0 
                 110 
                 145 
                 10 
                 −1 
                 −3 
                 1 
                 463 
                 464 
                 10 
                 14 
                 0 
                 1 
                 13 
                 30 
                 13 
                 2 
                 4 
                 1 
                 452 
                 446 
                 5 
               
               
                 6 
                 −4 
                 0 
                 204 
                 189 
                 5 
                 26 
                 2 
                 0 
                 23 
                 38 
                 22 
                 1 
                 −3 
                 1 
                 614 
                 614 
                 12 
                 16 
                 0 
                 1 
                 59 
                 53 
                 7 
                 4 
                 4 
                 1 
                 237 
                 239 
                 4 
               
               
                 8 
                 −4 
                 0 
                 112 
                 93 
                 8 
                 1 
                 3 
                 0 
                 862 
                 875 
                 14 
                 3 
                 −3 
                 1 
                 295 
                 286 
                 9 
                 18 
                 0 
                 1 
                 215 
                 210 
                 8 
                 6 
                 4 
                 1 
                 54 
                 49 
                 5 
               
               
                 10 
                 −4 
                 0 
                 72 
                 88 
                 8 
                 3 
                 3 
                 0 
                 361 
                 364 
                 7 
                 5 
                 −3 
                 1 
                 244 
                 265 
                 9 
                 20 
                 0 
                 1 
                 0 
                 10 
                 1 
                 8 
                 4 
                 1 
                 68 
                 55 
                 5 
               
               
                 12 
                 −4 
                 0 
                 183 
                 165 
                 6 
                 7 
                 3 
                 0 
                 457 
                 449 
                 16 
                 7 
                 −3 
                 1 
                 236 
                 224 
                 9 
                 22 
                 0 
                 1 
                 58 
                 50 
                 20 
                 10 
                 4 
                 1 
                 69 
                 74 
                 5 
               
               
                 14 
                 −4 
                 0 
                 196 
                 198 
                 9 
                 9 
                 3 
                 0 
                 222 
                 220 
                 9 
                 9 
                 −3 
                 1 
                 245 
                 235 
                 6 
                 24 
                 0 
                 1 
                 91 
                 86 
                 5 
                 12 
                 4 
                 1 
                 97 
                 91 
                 5 
               
               
                 16 
                 −4 
                 0 
                 175 
                 189 
                 8 
                 15 
                 3 
                 0 
                 145 
                 135 
                 11 
                 11 
                 −3 
                 1 
                 122 
                 109 
                 7 
                 −23 
                 1 
                 1 
                 65 
                 87 
                 16 
                 14 
                 4 
                 1 
                 169 
                 156 
                 9 
               
               
                 18 
                 −4 
                 0 
                 40 
                 45 
                 24 
                 17 
                 3 
                 0 
                 220 
                 212 
                 8 
                 13 
                 −3 
                 1 
                 157 
                 144 
                 6 
                 −21 
                 1 
                 1 
                 352 
                 352 
                 5 
                 16 
                 4 
                 1 
                 112 
                 138 
                 9 
               
               
                 20 
                 −4 
                 0 
                 30 
                 28 
                 30 
                 19 
                 3 
                 0 
                 126 
                 122 
                 9 
                 15 
                 −3 
                 1 
                 72 
                 59 
                 9 
                 −19 
                 1 
                 1 
                 221 
                 213 
                 3 
                 18 
                 4 
                 1 
                 109 
                 114 
                 9 
               
               
                 22 
                 −4 
                 0 
                 0 
                 22 
                 1 
                 21 
                 3 
                 0 
                 67 
                 69 
                 15 
                 17 
                 −3 
                 1 
                 171 
                 169 
                 9 
                 −17 
                 1 
                 1 
                 202 
                 194 
                 3 
                 20 
                 4 
                 1 
                 32 
                 31 
                 32 
               
               
                 1 
                 −3 
                 0 
                 869 
                 873 
                 18 
                 23 
                 3 
                 0 
                 59 
                 59 
                 16 
                 19 
                 −3 
                 1 
                 52 
                 50 
                 17 
                 −15 
                 1 
                 1 
                 147 
                 143 
                 3 
                 22 
                 4 
                 1 
                 0 
                 11 
                 1 
               
               
                 3 
                 −3 
                 0 
                 364 
                 365 
                 11 
                 25 
                 3 
                 0 
                 0 
                 32 
                 1 
                 21 
                 −3 
                 1 
                 72 
                 59 
                 14 
                 −13 
                 1 
                 1 
                 416 
                 412 
                 16 
                 −21 
                 5 
                 1 
                 33 
                 19 
                 33 
               
               
                 5 
                 −3 
                 0 
                 400 
                 372 
                 12 
                 0 
                 4 
                 0 
                 429 
                 436 
                 6 
                 23 
                 −3 
                 1 
                 46 
                 46 
                 13 
                 −11 
                 1 
                 1 
                 902 
                 941 
                 20 
                 −19 
                 5 
                 1 
                 0 
                 34 
                 1 
               
               
                 7 
                 −3 
                 0 
                 476 
                 447 
                 14 
                 2 
                 4 
                 0 
                 403 
                 390 
                 5 
                 −26 
                 −2 
                 1 
                 61 
                 57 
                 9 
                 −9 
                 1 
                 1 
                 403 
                 389 
                 6 
                 −17 
                 5 
                 1 
                 92 
                 86 
                 10 
               
               
                 9 
                 −3 
                 0 
                 232 
                 220 
                 5 
                 4 
                 4 
                 0 
                 170 
                 167 
                 5 
                 −24 
                 −2 
                 1 
                 97 
                 102 
                 16 
                 −7 
                 1 
                 1 
                 587 
                 602 
                 9 
                 −15 
                 5 
                 1 
                 143 
                 128 
                 6 
               
               
                 11 
                 −3 
                 0 
                 252 
                 248 
                 6 
                 6 
                 4 
                 0 
                 208 
                 189 
                 4 
                 −22 
                 −2 
                 1 
                 212 
                 217 
                 6 
                 −5 
                 1 
                 1 
                 1112 
                 1157 
                 19 
                 −13 
                 5 
                 1 
                 157 
                 146 
                 5 
               
               
                 13 
                 −3 
                 0 
                 126 
                 117 
                 7 
                 8 
                 4 
                 0 
                 111 
                 93 
                 4 
                 −20 
                 −2 
                 1 
                 199 
                 190 
                 5 
                 −3 
                 1 
                 1 
                 965 
                 1044 
                 30 
                 −11 
                 5 
                 1 
                 133 
                 125 
                 5 
               
               
                 15 
                 −3 
                 0 
                 138 
                 135 
                 6 
                 10 
                 4 
                 0 
                 77 
                 89 
                 5 
                 −18 
                 −2 
                 1 
                 47 
                 54 
                 10 
                 −1 
                 1 
                 1 
                 1304 
                 1398 
                 16 
                 −9 
                 5 
                 1 
                 41 
                 24 
                 11 
               
               
                 17 
                 −3 
                 0 
                 214 
                 212 
                 6 
                 12 
                 4 
                 0 
                 169 
                 165 
                 4 
                 −16 
                 −2 
                 1 
                 214 
                 194 
                 5 
                 1 
                 1 
                 1 
                 1131 
                 1213 
                 15 
                 −7 
                 5 
                 1 
                 110 
                 106 
                 6 
               
               
                 19 
                 −3 
                 0 
                 110 
                 122 
                 9 
                 14 
                 4 
                 0 
                 190 
                 198 
                 6 
                 −14 
                 −2 
                 1 
                 274 
                 254 
                 5 
                 3 
                 1 
                 1 
                 395 
                 453 
                 5 
                 −5 
                 5 
                 1 
                 309 
                 295 
                 6 
               
               
                 21 
                 −3 
                 0 
                 71 
                 69 
                 13 
                 16 
                 4 
                 0 
                 184 
                 189 
                 8 
                 −12 
                 −2 
                 1 
                 87 
                 85 
                 6 
                 5 
                 1 
                 1 
                 501 
                 544 
                 7 
                 −3 
                 5 
                 1 
                 147 
                 145 
                 3 
               
               
                 23 
                 −3 
                 0 
                 41 
                 59 
                 24 
                 18 
                 4 
                 0 
                 52 
                 45 
                 18 
                 −10 
                 −2 
                 1 
                 433 
                 429 
                 14 
                 7 
                 1 
                 1 
                 556 
                 601 
                 7 
                 −1 
                 5 
                 1 
                 28 
                 32 
                 9 
               
               
                 25 
                 −3 
                 0 
                 16 
                 32 
                 16 
                 20 
                 4 
                 0 
                 0 
                 28 
                 1 
                 −8 
                 −2 
                 1 
                 134 
                 160 
                 6 
                 9 
                 1 
                 1 
                 322 
                 313 
                 6 
                 1 
                 5 
                 1 
                 90 
                 83 
                 3 
               
               
                 0 
                 −2 
                 0 
                 1263 
                 1370 
                 38 
                 22 
                 4 
                 0 
                 41 
                 22 
                 34 
                 −6 
                 −2 
                 1 
                 255 
                 251 
                 6 
                 11 
                 1 
                 1 
                 175 
                 185 
                 13 
                 3 
                 5 
                 1 
                 26 
                 29 
                 13 
               
               
                 2 
                 −2 
                 0 
                 379 
                 408 
                 10 
                 1 
                 5 
                 0 
                 130 
                 130 
                 3 
                 −4 
                 −2 
                 1 
                 474 
                 505 
                 10 
                 13 
                 1 
                 1 
                 363 
                 359 
                 8 
                 5 
                 5 
                 1 
                 119 
                 122 
                 5 
               
               
                 4 
                 −2 
                 0 
                 107 
                 94 
                 4 
                 3 
                 5 
                 0 
                 66 
                 73 
                 4 
                 −2 
                 −2 
                 1 
                 245 
                 257 
                 5 
                 15 
                 1 
                 1 
                 412 
                 413 
                 5 
                 7 
                 5 
                 1 
                 97 
                 91 
                 6 
               
               
                 6 
                 −2 
                 0 
                 224 
                 223 
                 6 
                 5 
                 5 
                 0 
                 35 
                 25 
                 12 
                 0 
                 −2 
                 1 
                 731 
                 763 
                 15 
                 17 
                 1 
                 1 
                 46 
                 47 
                 7 
                 9 
                 5 
                 1 
                 110 
                 108 
                 5 
               
               
                 8 
                 −2 
                 0 
                 202 
                 222 
                 13 
                 7 
                 5 
                 0 
                 98 
                 95 
                 6 
                 2 
                 −2 
                 1 
                 266 
                 299 
                 5 
                 19 
                 1 
                 1 
                 162 
                 160 
                 3 
                 11 
                 5 
                 1 
                 130 
                 133 
                 5 
               
               
                 10 
                 −2 
                 0 
                 270 
                 310 
                 22 
                 9 
                 5 
                 0 
                 185 
                 178 
                 4 
                 4 
                 −2 
                 1 
                 303 
                 318 
                 5 
                 21 
                 1 
                 1 
                 29 
                 21 
                 14 
                 13 
                 5 
                 1 
                 80 
                 73 
                 7 
               
               
                 12 
                 −2 
                 0 
                 175 
                 180 
                 4 
                 11 
                 5 
                 0 
                 11 
                 51 
                 10 
                 6 
                 −2 
                 1 
                 476 
                 490 
                 11 
                 −26 
                 2 
                 1 
                 48 
                 58 
                 21 
                 15 
                 5 
                 1 
                 113 
                 110 
                 8 
               
               
                 14 
                 −2 
                 0 
                 64 
                 62 
                 6 
                 13 
                 5 
                 0 
                 111 
                 93 
                 6 
                 8 
                 −2 
                 1 
                 529 
                 557 
                 37 
                 −24 
                 2 
                 1 
                 100 
                 102 
                 10 
                 17 
                 5 
                 1 
                 60 
                 81 
                 10 
               
               
                 16 
                 −2 
                 0 
                 136 
                 130 
                 10 
                 15 
                 5 
                 0 
                 27 
                 21 
                 27 
                 10 
                 −2 
                 1 
                 459 
                 504 
                 30 
                 −22 
                 2 
                 1 
                 219 
                 218 
                 9 
                 19 
                 5 
                 1 
                 34 
                 60 
                 21 
               
               
                 18 
                 −2 
                 0 
                 192 
                 198 
                 5 
                 17 
                 5 
                 0 
                 28 
                 45 
                 28 
                 12 
                 −2 
                 1 
                 124 
                 130 
                 4 
                 −20 
                 2 
                 1 
                 199 
                 190 
                 7 
                 −16 
                 6 
                 1 
                 10 
                 23 
                 10 
               
               
                 20 
                 −2 
                 0 
                 112 
                 102 
                 6 
                 19 
                 5 
                 0 
                 22 
                 27 
                 21 
                 14 
                 −2 
                 1 
                 104 
                 89 
                 6 
                 −18 
                 2 
                 1 
                 63 
                 52 
                 11 
                 −14 
                 6 
                 1 
                 0 
                 20 
                 1 
               
               
                 22 
                 −2 
                 0 
                 62 
                 77 
                 17 
                 4 
                 6 
                 0 
                 47 
                 57 
                 11 
                 16 
                 −2 
                 1 
                 290 
                 278 
                 7 
                 −16 
                 2 
                 1 
                 215 
                 194 
                 6 
                 −12 
                 6 
                 1 
                 61 
                 61 
                 10 
               
               
                 24 
                 −2 
                 0 
                 119 
                 145 
                 6 
                 6 
                 6 
                 0 
                 57 
                 56 
                 6 
                 18 
                 −2 
                 1 
                 393 
                 384 
                 7 
                 −10 
                 2 
                 1 
                 436 
                 431 
                 14 
                 −10 
                 6 
                 1 
                 28 
                 39 
                 24 
               
               
                 26 
                 −2 
                 0 
                 0 
                 38 
                 1 
                 8 
                 6 
                 0 
                 47 
                 52 
                 8 
                 20 
                 −2 
                 1 
                 106 
                 120 
                 21 
                 −8 
                 2 
                 1 
                 134 
                 159 
                 7 
                 −8 
                 6 
                 1 
                 71 
                 79 
                 6 
               
               
                 1 
                 −1 
                 0 
                 1074 
                 1170 
                 22 
                 10 
                 6 
                 0 
                 22 
                 12 
                 22 
                 22 
                 −2 
                 1 
                 167 
                 142 
                 11 
                 −6 
                 2 
                 1 
                 252 
                 250 
                 9 
                 −6 
                 6 
                 1 
                 34 
                 39 
                 10 
               
               
                 3 
                 −1 
                 0 
                 1769 
                 1951 
                 39 
                 12 
                 6 
                 0 
                 45 
                 37 
                 14 
                 24 
                 −2 
                 1 
                 34 
                 23 
                 20 
                 −2 
                 2 
                 1 
                 249 
                 257 
                 4 
                 −4 
                 6 
                 1 
                 25 
                 26 
                 25 
               
               
                 5 
                 −1 
                 0 
                 1600 
                 1755 
                 36 
                 14 
                 6 
                 0 
                 0 
                 24 
                 1 
                 26 
                 −2 
                 1 
                 40 
                 37 
                 23 
                 0 
                 2 
                 1 
                 730 
                 762 
                 10 
                 4 
                 6 
                 1 
                 36 
                 35 
                 9 
               
               
                 7 
                 −1 
                 0 
                 967 
                 1006 
                 20 
                 16 
                 6 
                 0 
                 16 
                 6 
                 16 
                 −27 
                 −1 
                 1 
                 0 
                 7 
                 1 
                 2 
                 2 
                 1 
                 259 
                 300 
                 3 
                 6 
                 6 
                 1 
                 89 
                 86 
                 4 
               
               
                 9 
                 −1 
                 0 
                 38 
                 38 
                 12 
                 −16 
                 −6 
                 1 
                 27 
                 23 
                 26 
                 −25 
                 −1 
                 1 
                 105 
                 98 
                 8 
                 4 
                 2 
                 1 
                 304 
                 317 
                 4 
                 8 
                 6 
                 1 
                 18 
                 31 
                 18 
               
               
                 11 
                 −1 
                 0 
                 201 
                 210 
                 5 
                 −21 
                 −5 
                 1 
                 0 
                 18 
                 1 
                 −23 
                 −1 
                 1 
                 97 
                 87 
                 9 
                 6 
                 2 
                 1 
                 485 
                 489 
                 15 
                 10 
                 6 
                 1 
                 59 
                 78 
                 8 
               
               
                 13 
                 −1 
                 0 
                 262 
                 261 
                 6 
                 −19 
                 −5 
                 1 
                 18 
                 35 
                 18 
                 −21 
                 −1 
                 1 
                 349 
                 352 
                 6 
                 8 
                 2 
                 1 
                 556 
                 557 
                 17 
                 12 
                 6 
                 1 
                 24 
                 10 
                 23 
               
               
                 15 
                 −1 
                 0 
                 273 
                 271 
                 4 
                 −17 
                 −5 
                 1 
                 95 
                 86 
                 9 
                 −19 
                 −1 
                 1 
                 221 
                 214 
                 4 
                 10 
                 2 
                 1 
                 488 
                 503 
                 15 
                 14 
                 6 
                 1 
                 11 
                 30 
                 10 
               
               
                 17 
                 −1 
                 0 
                 232 
                 224 
                 4 
                 −15 
                 −5 
                 1 
                 135 
                 128 
                 8 
                 −17 
                 −1 
                 1 
                 204 
                 193 
                 4 
                 12 
                 2 
                 1 
                 134 
                 129 
                 7 
                 −16 
                 −6 
                 2 
                 14 
                 13 
                 14 
               
               
                 19 
                 −1 
                 0 
                 311 
                 304 
                 5 
                 −13 
                 −5 
                 1 
                 142 
                 146 
                 8 
                 −15 
                 −1 
                 1 
                 141 
                 143 
                 4 
                 14 
                 2 
                 1 
                 103 
                 90 
                 10 
                 −21 
                 −5 
                 2 
                 75 
                 53 
                 10 
               
               
                 21 
                 −1 
                 0 
                 44 
                 41 
                 14 
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                 20 
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                 21 
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                 20 
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                 28 
                 34 
                 28 
                 −6 
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                 30 
                 23 
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                 −12 
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                 20 
                 29 
                 37 
                 29 
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                 −11 
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                 21 
                 41 
                 21 
                 15 
               
               
                   
               
             
          
         
       
     
       REFERENCES 
       [0000]    
       
         1. CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28 cycle2 beta (release 25-10-2005 CrysAlis171.NET) (compiled Oct. 25 2005, 08:50:05). Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. 
         2. CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.28 cycle2 beta; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28 cycle2 beta. 
         3. G. M. Sheldrick, Acta Crystallogr. 1990, A46, 467-473. 
         4. G. M. Sheldrick, SHELXL93 . Program for the Reminement of Crystal Structures ., Univ. of Göttingen, Germany. 
         5 . International Tables for Crystallography , Ed. A. J. C. Wilson, Kluwer:Dordrecth, 1992, Vol.C. 
       
     
       Example 3 
     Synthesis of MET-1 and MET-2 
       [0040]    The preparation of MET-1 and MET-2 having the basic structures I and II can be accomplished by a common general method otherwise referred to as the condensation of a bicyclic Windaus-Grundmann type ketone IIIa or IIIb with the allylic phosphine oxide IV to the corresponding 2-methylene-19-nor-vitamin D analog Va or Vb followed by deprotection at C-1 and C-3 in the latter compound Va or Vb to obtain compound I (MET-1) or compound II (MET-2). 
         [0000]    
       
                 
         
             
             
         
       
     
         [0041]    In phosphine oxide IV, Y 1  and Y 2  are preferably hydroxy-protecting groups such as silyl protecting groups. The t-butyldimethylsilyl (TMDMS) group is an example of a particularly useful hydroxy-protecting group. The process described above represents an application of the convergent synthesis concept, which has been applied effectively to the preparation of numerous vitamin D compounds. (See Lythgoe et al.,  J. Chem. Soc. Perkin Trans. I,  590 (1978); Lythgoe,  Chem. Soc. Rev.  9, 449 (1983); Toh et al.,  J. Org. Chem.  48, 1414 (1983); Baggiolini et al.,  J. Org. Chem.  51, 3098 (1986); Sardina et al.,  J. Org. Chem.  51, 1264 (1986);  J. Org. Chem.  51, 1269 (1986); DeLuca et al., U.S. Pat. No. 5,086,191; DeLuca et al., U.S. Pat. No. 5,536,713; and DeLuca et al., U.S. Pat. No. 5,843,928 all of which are hereby incorporated by reference in their entirety and for all purposes as if fully set forth herein). 
         [0042]    Phosphine oxide IV is a convenient reagent that can be used to prepare a large number of 19-nor-vitamin D compounds and is prepared according to the procedures described by Sicinski et al.,  J. Med. Chem.,  41, 4662 (1998); DeLuca et al., U.S. Pat. No. 5,843,928; Perlman et al.,  Tetrahedron Lett.  32, 7663 (1991); and DeLuca et al., U.S. Pat. No. 5,086,191; which are hereby incorporated by reference in their entirety as if fully set forth herein. 
         [0043]    An overall process for the synthesis of compounds I and II is illustrated and described more completely in U.S. Pat. No. 5,843,928 entitled “2-Alkylidene-19-Nor-Vitamin D Compounds” and in U.S. patent application Ser. No. 13/053,844 filed Mar. 22, 2011, entitled “(20S)-2-Methylene-19-Nor-22-Dimethyl-1α,25-Dihydroxyvitamin D 3  and (20R)-2-Methylene-19-Nor-22-Dimethyl-1α,25-Hydroxyvitamin D 3 ” published as U.S. Publication No. US 2011/0237556A1 the specification of which is specifically incorporated herein by reference.