Abstract:
A method of purifying (20R,25S)-2-methylene-19,26-dinor-1α,25-dihydroxyvitamin D 3  to obtain (20R,25S)-2-methylene-19,26-dinor-1α,25-dihydroxyvitamin D 3  in crystalline form. The method includes the steps of preparing a solvent of methanol and water, dissolving a product containing (20R,25S)-2-methylene-19,26-dinor-1α,25-dihydroxyvitamin D 3  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 (20R,25S)-2-methylene-19,26-dinor-1α,25-dihydroxyvitamin D 3  crystals, and recovering the (20R,25S)-2-methylene-19,26-dinor-1α,25-dihydroxyvitamin D 3  crystals.

Description:
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT 
     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 OF THE INVENTION 
     The present invention relates to purification of organic compounds, and more particularly to the purification of (20R,25S)-2-Methylene-19,26-Dinor-1α,25-Dihydroxyvitamin D 3  (referred to herein as “NEL”) by preparing it in crystalline form. 
     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. 
     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 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 previtamin D compound, followed by cycloreversion of the modified adduct under basic conditions [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 previtamin 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. [see  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 1αhydroxy 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. 
     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; their driving force is 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. 
     Usually, all 1α-hydroxylatation procedures require at least one chromatographic purification. However, even chromatographically purified 1αhydroxyvitamin D compounds, although showing consistent spectroscopic data, suggesting homogeneity, do not meet the purity criteria required for therapeutic agents that can be orally, parenterally or transdermally administered. Therefore, it was evident that a suitable method of purification of the 1αhydroxylated vitamin D compound NEL is required. 
     SUMMARY OF THE INVENTION 
     The present invention relates to a method of purifying NEL by means of crystallization to obtain NEL in crystalline form. The solvent plays a crucial role in the crystallization process, and is typically an individual liquid substance or a suitable mixture of different liquids. For crystallizing NEL, 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. 
     Interestingly, hexane, so frequently used for crystallization purposes, was found less suitable for crystallization of NEL. However, it was found that a mixture of two liquids, namely water and methanol, in amounts of from about 10% water with about 90% methanol to about 30% water with about 70% methanol, was most useful for the crystallization of NEL. In particular, it, was determined that a mixture of 20% water with 80% methanol (by volume) performed well. The water/methanol solvent mixture was also easy to remove by evaporation or other well known methods. In all cases the crystallization process occurred easily and efficiently; and the precipitated crystals were sufficiently large to assure their recovery by filtration or other means. 
    
    
     
       BRIEF DESCRIPTION OF THE DRAWINGS 
         FIG. 1A  is an illustration of the three dimensional structure of a first asymmetric molecular structure for NEL as defined by the atomic positional parameters discovered and set forth herein; 
         FIG. 1B  is, an illustration of the three dimensional structure of a second asymmetric molecular structure for NEL as defined by the atomic positional parameters discovered and set forth herein; 
         FIG. 2  is an HPLC (9.4 mm×25 cm Zorbax-Sil column, 15% 2-propanol in hexane; 6 mL/min; R t =5.8 min.) profile of the solid material of NEL compound obtained after chemical synthesis; purity of the NEL compound before further HPLC purification was found to be 88.9%, checked by straight-phase HPLC; 
         FIG. 3  is an HPLC (9.4 mm×25 cm Zorbax RX-C18 column, 15% water in methanol; 3 mL/min; R t =9.9 min.) profile of the NEL compound obtained after a first, straight-phase HPLC purification of the solid NEL material; purity of the NEL compound after this first HPLC purification was found to be 95.3%, checked by reversed-phase HPLC; and 
         FIG. 4  is an HPLC (9.4 mm×25 cm Zorbax RX-C18 column, 15% water in methanol; 3 ml/min; R t =9.9 min.) profile of the NEL compound obtained after a second reversed-phase HPLC purification of the NEL compound obtained from the first HPLC purification; purity of the NEL compound after this second HPLC purification was found to be 99.5%, checked by reversed-phase HPLC. Crystals of the NEL compound were obtained after reversed-phase HPLC purification by single crystallization using a 20% water/80% methanol solvent system. 
     
    
    
     DETAILED DESCRIPTION OF THE INVENTION 
     The present invention provides (20R,25S)-2-methylene-19,26-dinor-1α,25-dihydroxyvitamin D 3  (NEL) in crystalline form, a pharmacologically important compound, characterized by the formula I shown below: 
     
       
                 
         
             
             
         
      
     
     The present invention also provides a valuable method of purification of NEL. The purification technique involves obtaining the NEL product in crystalline form by utilizing a crystallization procedure wherein the NEL material to be purified is dissolved using as the solvent a mixture comprised of methanol and water in amounts of from about 10% water with about 90% methanol to about 30% water with about 70% methanol, by volume. Preferably the mixture comprises 80% methanol and 20% water (by volume). The solvent and dissolved product containing (20R,25S)-2-methylene-19,26-dinor-1α,25-dihydroxyvitamin D3 (NEL) to be purified may then be cooled to about −20° C., or may in a first step be maintained at ambient temperature for a period of time (1 hour to 1 week) and then cooled in a second step to about −20° C. In either case, the solution is then maintained at about −20° C. for up to 7 weeks. Thereafter, the solvent can be removed by evaporation, with or without vacuum, or other means as is well known, or the resultant crystals may be filtered from the mother liquor. The technique can be used to purify a wide range of final products containing NEL obtained from any known synthesis thereof, and in varying concentrations, i.e. from microgram amounts to kilogram amounts. As is well known to those skilled in this art, the amount of solvent utilized should be minimized and/or adjusted according to the amount of NEL to be purified. 
     The usefulness and advantages of the present crystallization procedure is shown in the following specific Examples 1 and 2. After crystallization, the precipitated material was observed under a microscope to confirm its crystalline form. Additionally, the crystals were then analyzed to determine their initial purity (88.9%;  FIG. 2 ), and their significantly improved purity was confirmed after a first, straight-phase HPLC (95.3%,  FIG. 3 ), as well as a second, reversed-phase HPLC (99.5%;  FIG. 4 ). Yields of crystals were high and the obtained crystals showed a relatively sharp melting point of 154-155° C. 
     The described crystallization process of the synthetic NEL product represents a valuable purification method, which can remove most side products derived from the synthetic path. Such impurity is the result of the contamination of starting raw materials. The crystallization process occurred easily and efficiently; and the precipitated crystals were sufficiently large to assure their recovery by filtration, or other means. 
     EXAMPLE 1 
     Crystallization of (20R,25S)-2-methylene-19,26-dinor-1α,25-dihydroxyvitamin D 3  (NEL) 
     Crystals of the NEL analog were obtained from a solution of the compound in 20% water and 80% methanol (20% H 2 O/80% MeOH) as follows:
         14 mg of pure NEL compound was dissolved in 8 mL of water/methanol solvent mixture (water/methanol=2/8). The solution was kept at −20 degrees Celsius for 7 weeks. The precipitated crystals (M.p. 154-155° C.) were analyzed by straight phase HPLC (crystals:  FIG. 2 ) and found to be 99.5% pure.       

     EXAMPLE 2 
     Experimental 
     A colorless prism-shaped crystal of dimensions 0.47×0.12×0.18 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 CuKα radiation (1.54178 Å) from a Rigaku RU200 x-ray generator equipped with Montel optics, operated at 50 kV and 80 mA. The x-ray data were processed with SAINT version 7.06A (Bruker AXS Inc) and, internally scaled with SADABS version 2005/1 (Bruker 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° for 10-15 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 3.0&lt;theta&lt;64.8°. The data were merged to form a set of 6791 independent data with R(int)=0.0326. 
     The triclinic space group P1 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). The asymmetric unit was comprised of two molecules of NEL, designated with A and B. 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. A total of 523 parameters were refined against 3 restraints and 6781 data to give wR2=0.0943 and S=1.066 for weights of w=1/[s 2 (F 2 )+(0.0613P) 2 ], where P=[F 2 +2F c   2 ]/3. The final R(F) was 0.0342 for the 6781 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 0.217 and −0.177 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). 
     The three dimensional structure of NEL as defined by the following physical data and atomic positional parameters described and calculated herein is illustrated in  FIG. 1A  and  FIG. 1B . 
     
       
         
               
             
               
               
             
               
               
               
             
               
               
             
           
               
                 TABLE 1 
               
               
                   
               
               
                 Crystal data and structure refinement for NEL. 
               
               
                   
               
             
             
               
                   
               
             
          
           
               
                 Identification code 
                 NEL 
               
               
                 Empirical formula 
                 C26H42O3 
               
               
                 Formula weight 
                 402.60 
               
               
                 Temperature 
                 100(1) K 
               
               
                 Wavelength 
                 1.54178 Å 
               
               
                 Crystal system, space group 
                 P1, 
               
             
          
           
               
                 Unit cell dimensions 
                 a = 6.3820(11) Å 
                 α = 110.920(5)° 
               
               
                   
                 b = 12.594(2) Å 
                 β = 95.256(5)° 
               
               
                   
                 c = 15.996(3)° Å 
                 γ = 90.609(5)° 
               
               
                 Volume 
                 1194.6(4) Å 3   
               
             
          
           
               
                 Z, Calculated density 
                 2, 1.119 Mg/m 3   
               
               
                 Absorption coefficient 
                 0.549 mm −1   
               
               
                 F(000) 
                 444 
               
               
                 Crystal size 
                 0.47 × 0.12 × 0.18 mm 
               
               
                 Theta range for data collection 
                 2.97 to 64.82° 
               
               
                 Limiting indices 
                 −7 &lt;= h &lt;= 7, −14 &lt;= k &lt;= 14, 
               
               
                   
                 −18 &lt;= l &lt;= 18 
               
               
                 Reflections collected/unique 
                 18206/6781 [R(int) = 0.0326] 
               
               
                 Completeness to theta = 64.82 
                 96.0% 
               
               
                 Refinement method 
                 Full-matrix least-squares on F 2   
               
               
                 Data/restraints/parameters 
                 6781/3/523 
               
               
                 Goodness-of-fit on F 2   
                 1.066 
               
               
                 Final R indices [I &gt; 2σ(I)] 
                 R1 = 0.0336, wR2 = 0.0943 
               
               
                 R indices (all data) 
                 R1 = 0.0342, wR2 = 0.0948 
               
               
                 Absolute structure parameter 
                 −0.04(13) 
               
               
                 Largest diff. peak and hole 
                 0.217 and −0.177 e/A 3   
               
               
                   
               
             
          
         
       
     
     
       
         
               
             
               
               
               
               
               
               
             
               
               
               
               
               
               
             
           
               
                 TABLE 2 
               
             
             
               
                   
               
               
                 Atomic coordinates (×10 4 ) and equivalent isotropic 
               
               
                 displacement parameters (A 2  × 10 3 ) for NEL. 
               
               
                 U(eq) is defined as one third of the trace of 
               
               
                 the orthogonalized Uij tensor. 
               
             
          
           
               
                   
                   
                 x 
                 y 
                 z 
                 U(eq) 
               
               
                   
                   
               
             
          
           
               
                   
                 O(1B) 
                 20004(2) 
                 17550(1) 
                 1623(1) 
                 24(1) 
               
               
                   
                 O(25A) 
                 17814(2) 
                 15531(1) 
                 1308(1) 
                 22(1) 
               
               
                   
                 O(1A) 
                 17343(2) 
                 13368(1) 
                 9956(1) 
                 25(1) 
               
               
                   
                 O(2B) 
                 26264(2) 
                 18348(1) 
                 1150(1) 
                 24(1) 
               
               
                   
                 O(25B) 
                 24669(2) 
                 16177(1) 
                 10298(1) 
                 25(1) 
               
               
                   
                 O(2A) 
                 23666(2) 
                 12775(1) 
                 10464(1) 
                 30(1) 
               
               
                   
                 C(12B) 
                 29763(3) 
                 18997(2) 
                 6571(1) 
                 21(1) 
               
               
                   
                 C(3B) 
                 24736(3) 
                 19211(2) 
                 1351(1) 
                 21(1) 
               
               
                   
                 C(14A) 
                 22676(3) 
                 13599(2) 
                 6215(1) 
                 20(1) 
               
               
                   
                 C(1A) 
                 19399(3) 
                 12961(2) 
                 9789(1) 
                 22(1) 
               
               
                   
                 C(1B) 
                 22059(3) 
                 18070(2) 
                 1796(1) 
                 20(1) 
               
               
                   
                 C(7B) 
                 26024(3) 
                 18595(2) 
                 4148(1) 
                 23(1) 
               
               
                   
                 C(9B) 
                 29674(3) 
                 19090(2) 
                 4995(1) 
                 21(1) 
               
               
                   
                 C(7A) 
                 22104(3) 
                 12709(2) 
                 7363(1) 
                 22(1) 
               
               
                   
                 C(8A) 
                 23258(3) 
                 12850(2) 
                 6750(1) 
                 20(1) 
               
               
                   
                 C(18B) 
                 25854(3) 
                 19292(2) 
                 6615(1) 
                 23(1) 
               
               
                   
                 C(8B) 
                 27529(3) 
                 18497(2) 
                 4760(1) 
                 20(1) 
               
               
                   
                 C(4A) 
                 22392(3) 
                 11177(2) 
                 9084(1) 
                 22(1) 
               
               
                   
                 C(10B) 
                 22526(3) 
                 18874(2) 
                 2783(1) 
                 24(1) 
               
               
                   
                 C(13A) 
                 22519(3) 
                 12966(2) 
                 5181(1) 
                 21(1) 
               
               
                   
                 C(5A) 
                 21554(3) 
                 11878(2) 
                 8545(1) 
                 21(1) 
               
               
                   
                 C(13B) 
                 27557(3) 
                 18418(1) 
                 6337(1) 
                 18(1) 
               
               
                   
                 C(12A) 
                 24663(3) 
                 12455(2) 
                 4951(1) 
                 24(1) 
               
               
                   
                 C(4B) 
                 25235(3) 
                 19984(2) 
                 2339(1) 
                 23(1) 
               
               
                   
                 C(6B) 
                 26236(3) 
                 19238(2) 
                 3562(1) 
                 21(1) 
               
               
                   
                 C(5B) 
                 24742(3) 
                 19367(2) 
                 2960(1) 
                 22(1) 
               
               
                   
                 C(14B) 
                 27268(3) 
                 17751(2) 
                 5300(1) 
                 21(1) 
               
               
                   
                 C(10A) 
                 19424(3) 
                 12345(2) 
                 8773(1) 
                 24(1) 
               
               
                   
                 C(2B) 
                 22531(3) 
                 18696(2) 
                 1180(1) 
                 20(1) 
               
               
                   
                 C(11B) 
                 30116(3) 
                 19743(2) 
                 6014(1) 
                 22(1) 
               
               
                   
                 C(25A) 
                 16921(3) 
                 15954(2) 
                 2170(1) 
                 21(1) 
               
               
                   
                 C(11A) 
                 25307(3) 
                 11695(2) 
                 5489(1) 
                 26(1) 
               
               
                   
                 C(9A) 
                 25341(3) 
                 12322(2) 
                 6512(1) 
                 23(1) 
               
               
                   
                 C(2A) 
                 20095(3) 
                 12173(2) 
                 10275(1) 
                 22(1) 
               
               
                   
                 C(15B) 
                 25289(4) 
                 17009(2) 
                 5155(1) 
                 29(1) 
               
               
                   
                 C(19B) 
                 21153(3) 
                 18805(2) 
                 546(1) 
                 26(1) 
               
               
                   
                 C(22B) 
                 26528(3) 
                 16572(2) 
                 7829(1) 
                 24(1) 
               
               
                   
                 C(16A) 
                 20397(3) 
                 14647(2) 
                 5542(1) 
                 24(1) 
               
               
                   
                 C(19A) 
                 18923(3) 
                 11833(2) 
                 10779(1) 
                 29(1) 
               
               
                   
                 C(3A) 
                 22290(3) 
                 11784(2) 
                 10098(1) 
                 23(1) 
               
               
                   
                 C(6A) 
                 22665(3) 
                 12056(2) 
                 7932(1) 
                 22(1) 
               
               
                   
                 C(24A) 
                 18538(3) 
                 15914(2) 
                 2914(1) 
                 24(1) 
               
               
                   
                 C(15A) 
                 20687(3) 
                 14277(2) 
                 6365(1) 
                 28(1) 
               
               
                   
                 C(18A) 
                 20768(3) 
                 12036(2) 
                 4871(1) 
                 27(1) 
               
               
                   
                 C(20B) 
                 26644(3) 
                 17688(2) 
                 7646(1) 
                 22(1) 
               
               
                   
                 C(26B) 
                 21533(3) 
                 15634(2) 
                 9292(1) 
                 27(1) 
               
               
                   
                 C(25B) 
                 23829(3) 
                 15374(2) 
                 9433(1) 
                 21(1) 
               
               
                   
                 C(23B) 
                 25282(3) 
                 16605(2) 
                 8603(1) 
                 26(1) 
               
               
                   
                 C(16B) 
                 25461(3) 
                 16641(2) 
                 5984(1) 
                 26(1) 
               
               
                   
                 C(24B) 
                 25149(3) 
                 15444(2) 
                 8706(1) 
                 23(1) 
               
               
                   
                 C(23A) 
                 19136(3) 
                 14732(2) 
                 2894(1) 
                 26(1) 
               
               
                   
                 C(20A) 
                 21004(3) 
                 13700(2) 
                 3878(1) 
                 24(1) 
               
               
                   
                 C(17B) 
                 27207(3) 
                 17428(2) 
                 6678(1) 
                 20(1) 
               
               
                   
                 C(17A) 
                 21928(3) 
                 13962(1) 
                 4855(1) 
                 20(1) 
               
               
                   
                 C(22A) 
                 20565(3) 
                 14826(2) 
                 3734(1) 
                 24(1) 
               
               
                   
                 C(26A) 
                 14899(3) 
                 15287(2) 
                 2077(1) 
                 28(1) 
               
               
                   
                 C(21B) 
                 28182(4) 
                 18550(2) 
                 8366(1) 
                 33(1) 
               
               
                   
                 C(21A) 
                 22416(4) 
                 12988(2) 
                 3186(1) 
                 40(1) 
               
               
                   
                   
               
             
          
         
       
     
     
       
         
               
             
               
               
               
             
           
               
                 TABLE 3 
               
               
                   
               
               
                 Bond lengths [Å] for NEL. 
               
               
                   
               
             
             
               
                   
               
             
          
           
               
                   
                 O(1B)—C(1B) 
                 1.419(2) 
               
               
                   
                 O(1B)—H(1BA) 
                 0.8200 
               
               
                   
                 O(25A)—C(25A) 
                 1.461(2) 
               
               
                   
                 O(25A)—H(25A) 
                 0.8200 
               
               
                   
                 O(1A)—C(1A) 
                 1.427(2) 
               
               
                   
                 O(1A)—H(1AA) 
                 0.8200 
               
               
                   
                 O(2B)—C(3B) 
                 1.438(2) 
               
               
                   
                 O(2B)—H(2BA) 
                 0.8200 
               
               
                   
                 O(25B)—C(25B) 
                 1.441(2) 
               
               
                   
                 O(25B)—H(25B) 
                 0.8200 
               
               
                   
                 O(2A)—C(3A) 
                 1.426(2) 
               
               
                   
                 O(2A)—H(2AA) 
                 0.8200 
               
               
                   
                 C(12B)—C(13B) 
                 1.529(3) 
               
               
                   
                 C(12B)—C(11B) 
                 1.536(3) 
               
               
                   
                 C(12B)—H(12A) 
                 0.9700 
               
               
                   
                 C(12B)—H(12B) 
                 0.9700 
               
               
                   
                 C(3B)—C(2B) 
                 1.503(3) 
               
               
                   
                 C(3B)—C(4B) 
                 1.533(2) 
               
               
                   
                 C(3B)—H(3BA) 
                 0.9800 
               
               
                   
                 C(14A)—C(8A) 
                 1.511(3) 
               
               
                   
                 C(14A)—C(15A) 
                 1.527(3) 
               
               
                   
                 C(14A)—C(13A) 
                 1.552(2) 
               
               
                   
                 C(14A)—H(14A) 
                 0.9800 
               
               
                   
                 C(1A)—C(2A) 
                 1.511(3) 
               
               
                   
                 C(1A)—C(10A) 
                 1.532(3) 
               
               
                   
                 C(1A)—H(1AB) 
                 0.9800 
               
               
                   
                 C(1B)—C(2B) 
                 1.513(3) 
               
               
                   
                 C(1B)—C(10B) 
                 1.540(3) 
               
               
                   
                 C(1B)—H(1BB) 
                 0.9800 
               
               
                   
                 C(7B)—C(8B) 
                 1.346(3) 
               
               
                   
                 C(7B)—C(6B) 
                 1.454(3) 
               
               
                   
                 C(7B)—H(7BA) 
                 0.9300 
               
               
                   
                 C(9B)—C(8B) 
                 1.502(3) 
               
               
                   
                 C(9B)—C(11B) 
                 1.538(3) 
               
               
                   
                 C(9B)—H(9BA) 
                 0.9700 
               
               
                   
                 C(9B)—H(9BB) 
                 0.9700 
               
               
                   
                 C(7A)—C(8A) 
                 1.338(3) 
               
               
                   
                 C(7A)—C(6A) 
                 1.453(3) 
               
               
                   
                 C(7A)—H(7AA) 
                 0.9300 
               
               
                   
                 C(8A)—C(9A) 
                 1.512(3) 
               
               
                   
                 C(18B)—C(13B) 
                 1.535(2) 
               
               
                   
                 C(18B)—H(18A) 
                 0.9600 
               
               
                   
                 C(18B)—H(18B) 
                 0.9600 
               
               
                   
                 C(18B)—H(18C) 
                 0.9600 
               
               
                   
                 C(8B)—C(14B) 
                 1.504(2) 
               
               
                   
                 C(4A)—C(5A) 
                 1.508(3) 
               
               
                   
                 C(4A)—C(3A) 
                 1.535(3) 
               
               
                   
                 C(4A)—H(4AA) 
                 0.9700 
               
               
                   
                 C(4A)—H(4AB) 
                 0.9700 
               
               
                   
                 C(10B)—C(5B) 
                 1.499(3) 
               
               
                   
                 C(10B)—H(10A) 
                 0.9700 
               
               
                   
                 C(10B)—H(10B) 
                 0.9700 
               
               
                   
                 C(13A)—C(18A) 
                 1.524(3) 
               
               
                   
                 C(13A)—C(12A) 
                 1.538(2) 
               
               
                   
                 C(13A)—C(17A) 
                 1.558(2) 
               
               
                   
                 C(5A)—C(6A) 
                 1.342(3) 
               
               
                   
                 C(5A)—C(10A) 
                 1.510(3) 
               
               
                   
                 C(13B)—C(17B) 
                 1.551(2) 
               
               
                   
                 C(13B)—C(14B) 
                 1.560(2) 
               
               
                   
                 C(12A)—C(11A) 
                 1.536(3) 
               
               
                   
                 C(12A)—H(12C) 
                 0.9700 
               
               
                   
                 C(12A)—H(12D) 
                 0.9700 
               
               
                   
                 C(4B)—C(5B) 
                 1.515(3) 
               
               
                   
                 C(4B)—H(4BA) 
                 0.9700 
               
               
                   
                 C(4B)—H(4BB) 
                 0.9700 
               
               
                   
                 C(6B)—C(5B) 
                 1.345(3) 
               
               
                   
                 C(6B)—H(6BA) 
                 0.9300 
               
               
                   
                 C(14B)—C(15B) 
                 1.513(3) 
               
               
                   
                 C(14B)—H(14B) 
                 0.9800 
               
               
                   
                 C(10A)—H(10C) 
                 0.9700 
               
               
                   
                 C(10A)—H(10D) 
                 0.9700 
               
               
                   
                 C(2B)—C(19B) 
                 1.326(3) 
               
               
                   
                 C(11B)—H(11A) 
                 0.9700 
               
               
                   
                 C(11B)—H(11B) 
                 0.9700 
               
               
                   
                 C(25A)—C(26A) 
                 1.499(3) 
               
               
                   
                 C(25A)—C(24A) 
                 1.518(3) 
               
               
                   
                 C(25A)—H(25C) 
                 0.9800 
               
               
                   
                 C(11A)—C(9A) 
                 1.539(3) 
               
               
                   
                 C(11A)—H(11C) 
                 0.9700 
               
               
                   
                 C(11A)—H(11D) 
                 0.9700 
               
               
                   
                 C(9A)—H(9AA) 
                 0.9700 
               
               
                   
                 C(9A)—H(9AB) 
                 0.9700 
               
               
                   
                 C(2A)—C(19A) 
                 1.320(3) 
               
               
                   
                 C(2A)—C(3A) 
                 1.507(3) 
               
               
                   
                 C(15B)—C(16B) 
                 1.548(3) 
               
               
                   
                 C(15B)—H(15A) 
                 0.9700 
               
               
                   
                 C(15B)—H(15B) 
                 0.9700 
               
               
                   
                 C(19B)—H(19A) 
                 0.9300 
               
               
                   
                 C(19B)—H(19B) 
                 0.9300 
               
               
                   
                 C(22B)—C(23B) 
                 1.520(3) 
               
               
                   
                 C(22B)—C(20B) 
                 1.537(2) 
               
               
                   
                 C(22B)—H(22A) 
                 0.9700 
               
               
                   
                 C(22B)—H(22B) 
                 0.9700 
               
               
                   
                 C(16A)—C(15A) 
                 1.542(3) 
               
               
                   
                 C(16A)—C(17A) 
                 1.563(2) 
               
               
                   
                 C(16A)—H(16A) 
                 0.9700 
               
               
                   
                 C(16A)—H(16B) 
                 0.9700 
               
               
                   
                 C(19A)—H(19C) 
                 0.9300 
               
               
                   
                 C(19A)—H(19D) 
                 0.9300 
               
               
                   
                 C(3A)—H(3AA) 
                 0.9800 
               
               
                   
                 C(6A)—H(6AA) 
                 0.9300 
               
               
                   
                 C(24A)—C(23A) 
                 1.531(3) 
               
               
                   
                 C(24A)—H(24A) 
                 0.9700 
               
               
                   
                 C(24A)—H(24B) 
                 0.9700 
               
               
                   
                 C(15A)—H(15C) 
                 0.9700 
               
               
                   
                 C(15A)—H(15D) 
                 0.9700 
               
               
                   
                 C(18A)—H(18D) 
                 0.9600 
               
               
                   
                 C(18A)—H(18E) 
                 0.9600 
               
               
                   
                 C(18A)—H(18F) 
                 0.9600 
               
               
                   
                 C(20B)—C(21B) 
                 1.532(3) 
               
               
                   
                 C(20B)—C(17B) 
                 1.541(2) 
               
               
                   
                 C(20B)—H(20A) 
                 0.9800 
               
               
                   
                 C(26B)—C(25B) 
                 1.519(3) 
               
               
                   
                 C(26B)—H(26A) 
                 0.9600 
               
               
                   
                 C(26B)—H(26B) 
                 0.9600 
               
               
                   
                 C(26B)—H(26C) 
                 0.9600 
               
               
                   
                 C(25B)—C(24B) 
                 1.523(3) 
               
               
                   
                 C(25B)—H(25D) 
                 0.9800 
               
               
                   
                 C(23B)—C(24B) 
                 1.531(2) 
               
               
                   
                 C(23B)—H(23A) 
                 0.9700 
               
               
                   
                 C(23B)—H(23B) 
                 0.9700 
               
               
                   
                 C(16B)—C(17B) 
                 1.556(3) 
               
               
                   
                 C(16B)—H(16C) 
                 0.9700 
               
               
                   
                 C(16B)—H(16D) 
                 0.9700 
               
               
                   
                 C(24B)—H(24B) 
                 0.9700 
               
               
                   
                 C(24B)—H(24C) 
                 0.9700 
               
               
                   
                 C(23A)—C(22A) 
                 1.519(3) 
               
               
                   
                 C(23A)—H(23C) 
                 0.9700 
               
               
                   
                 C(23A)—H(23D) 
                 0.9700 
               
               
                   
                 C(20A)—C(21A) 
                 1.527(3) 
               
               
                   
                 C(20A)—C(17A) 
                 1.536(3) 
               
               
                   
                 C(20A)—C(22A) 
                 1.541(2) 
               
               
                   
                 C(20A)—H(20B) 
                 0.9800 
               
               
                   
                 C(17B)—H(17A) 
                 0.9800 
               
               
                   
                 C(17A)—H(17B) 
                 0.9800 
               
               
                   
                 C(22A)—H(22C) 
                 0.9700 
               
               
                   
                 C(22A)—H(22D) 
                 0.9700 
               
               
                   
                 C(26A)—H(26D) 
                 0.9600 
               
               
                   
                 C(26A)—H(26E) 
                 0.9600 
               
               
                   
                 C(26A)—H(26F) 
                 0.9600 
               
               
                   
                 C(21B)—H(21A) 
                 0.9600 
               
               
                   
                 C(21B)—H(21B) 
                 0.9600 
               
               
                   
                 C(21B)—H(21C) 
                 0.9600 
               
               
                   
                 C(21A)—H(21D) 
                 0.9600 
               
               
                   
                 C(21A)—H(21E) 
                 0.9600 
               
               
                   
                 C(21A)—H(21F) 
                 0.9600 
               
               
                   
                   
               
             
          
         
       
     
     
       
         
               
             
               
               
               
             
           
               
                 TABLE 4 
               
               
                   
               
               
                 Bond angles [°] for NEL. 
               
               
                   
               
             
             
               
                   
               
             
          
           
               
                   
                 C(1B)—O(1B)—H(1BA) 
                 109.5 
               
               
                   
                 C(25A)—O(25A)—H(25A) 
                 109.5 
               
               
                   
                 C(1A)—O(1A)—H(1AA) 
                 109.5 
               
               
                   
                 C(3B)—O(2B)—H(2BA) 
                 109.5 
               
               
                   
                 C(25B)—O(25B)—H(25B) 
                 109.5 
               
               
                   
                 C(3A)—O(2A)—H(2AA) 
                 109.5 
               
               
                   
                 C(13B)—C(12B)—C(11B) 
                 111.64(14) 
               
               
                   
                 C(13B)—C(12B)—H(12A) 
                 109.3 
               
               
                   
                 C(11B)—C(12B)—H(12A) 
                 109.3 
               
               
                   
                 C(13B)—C(12B)—H(12B) 
                 109.3 
               
               
                   
                 C(11B)—C(12B)—H(12B) 
                 109.3 
               
               
                   
                 H(12A)—C(12B)—H(12B) 
                 108.0 
               
               
                   
                 O(2B)—C(3B)—C(2B) 
                 111.37(14) 
               
               
                   
                 O(2B)—C(3B)—C(4B) 
                 107.64(14) 
               
               
                   
                 C(2B)—C(3B)—C(4B) 
                 110.89(15) 
               
               
                   
                 O(2B)—C(3B)—H(3BA) 
                 109.0 
               
               
                   
                 C(2B)—C(3B)—H(3BA) 
                 109.0 
               
               
                   
                 C(4B)—C(3B)—H(3BA) 
                 109.0 
               
               
                   
                 C(8A)—C(14A)—C(15A) 
                 120.67(16) 
               
               
                   
                 C(8A)—C(14A)—C(13A) 
                 113.85(14) 
               
               
                   
                 C(15A)—C(14A)—C(13A) 
                 104.06(14) 
               
               
                   
                 C(8A)—C(14A)—H(14A) 
                 105.7 
               
               
                   
                 C(15A)—C(14A)—H(14A) 
                 105.7 
               
               
                   
                 C(13A)—C(14A)—H(14A) 
                 105.7 
               
               
                   
                 O(1A)—C(1A)—C(2A) 
                 113.69(15) 
               
               
                   
                 O(1A)—C(1A)—C(10A) 
                 108.29(14) 
               
               
                   
                 C(2A)—C(1A)—C(10A) 
                 109.59(14) 
               
               
                   
                 O(1A)—C(1A)—H(1AB) 
                 108.4 
               
               
                   
                 C(2A)—C(1A)—H(1AB) 
                 108.4 
               
               
                   
                 C(10A)—C(1A)—H(1AB) 
                 108.4 
               
               
                   
                 O(1B)—C(1B)—C(2B) 
                 114.49(15) 
               
               
                   
                 O(1B)—C(1B)—C(10B) 
                 111.74(15) 
               
               
                   
                 C(2B)—C(1B)—C(10B) 
                 109.51(15) 
               
               
                   
                 O(1B)—C(1B)—H(1BB) 
                 106.9 
               
               
                   
                 C(2B)—C(1B)—H(1BB) 
                 106.9 
               
               
                   
                 C(10B)—C(1B)—H(1BB) 
                 106.9 
               
               
                   
                 C(8B)—C(7B)—C(6B) 
                 125.92(18) 
               
               
                   
                 C(8B)—C(7B)—H(7BA) 
                 117.0 
               
               
                   
                 C(6B)—C(7B)—H(7BA) 
                 117.0 
               
               
                   
                 C(8B)—C(9B)—C(11B) 
                 111.32(15) 
               
               
                   
                 C(8B)—C(9B)—H(9BA) 
                 109.4 
               
               
                   
                 C(11B)—C(9B)—H(9BA) 
                 109.4 
               
               
                   
                 C(8B)—C(9B)—H(9BB) 
                 109.4 
               
               
                   
                 C(11B)—C(9B)—H(9BB) 
                 109.4 
               
               
                   
                 H(9BA)—C(9B)—H(9BB) 
                 108.0 
               
               
                   
                 C(8A)—C(7A)—C(6A) 
                 126.04(17) 
               
               
                   
                 C(8A)—C(7A)—H(7AA) 
                 117.0 
               
               
                   
                 C(6A)—C(7A)—H(7AA) 
                 117.0 
               
               
                   
                 C(7A)—C(8A)—C(14A) 
                 124.19(17) 
               
               
                   
                 C(7A)—C(8A)—C(9A) 
                 125.42(16) 
               
               
                   
                 C(14A)—C(8A)—C(9A) 
                 110.37(15) 
               
               
                   
                 C(13B)—C(18B)—H(18A) 
                 109.5 
               
               
                   
                 C(13B)—C(18B)—H(18B) 
                 109.5 
               
               
                   
                 H(18A)—C(18B)—H(18B) 
                 109.5 
               
               
                   
                 C(13B)—C(18B)—H(18C) 
                 109.5 
               
               
                   
                 H(18A)—C(18B)—H(18C) 
                 109.5 
               
               
                   
                 H(18B)—C(18B)—H(18C) 
                 109.5 
               
               
                   
                 C(7B)—C(8B)—C(9B) 
                 125.88(17) 
               
               
                   
                 C(7B)—C(8B)—C(14B) 
                 123.46(18) 
               
               
                   
                 C(9B)—C(8B)—C(14B) 
                 110.66(15) 
               
               
                   
                 C(5A)—C(4A)—C(3A) 
                 112.48(14) 
               
               
                   
                 C(5A)—C(4A)—H(4AA) 
                 109.1 
               
               
                   
                 C(3A)—C(4A)—H(4AA) 
                 109.1 
               
               
                   
                 C(5A)—C(4A)—H(4AB) 
                 109.1 
               
               
                   
                 C(3A)—C(4A)—H(4AB) 
                 109.1 
               
               
                   
                 H(4AA)—C(4A)—H(4AB) 
                 107.8 
               
               
                   
                 C(5B)—C(10B)—C(1B) 
                 110.68(15) 
               
               
                   
                 C(5B)—C(10B)—H(10A) 
                 109.5 
               
               
                   
                 C(1B)—C(10B)—H(10A) 
                 109.5 
               
               
                   
                 C(5B)—C(10B)—H(10B) 
                 109.5 
               
               
                   
                 C(1B)—C(10B)—H(10B) 
                 109.5 
               
               
                   
                 H(10A)—C(10B)—H(10B) 
                 108.1 
               
               
                   
                 C(18A)—C(13A)—C(12A) 
                 110.65(15) 
               
               
                   
                 C(18A)—C(13A)—C(14A) 
                 111.01(15) 
               
               
                   
                 C(12A)—C(13A)—C(14A) 
                 107.41(15) 
               
               
                   
                 C(18A)—C(13A)—C(17A) 
                 110.89(15) 
               
               
                   
                 C(12A)—C(13A)—C(17A) 
                 116.13(15) 
               
               
                   
                 C(14A)—C(13A)—C(17A) 
                 100.21(13) 
               
               
                   
                 C(6A)—C(5A)—C(4A) 
                 121.11(17) 
               
               
                   
                 C(6A)—C(5A)—C(10A) 
                 124.93(17) 
               
               
                   
                 C(4A)—C(5A)—C(10A) 
                 113.96(16) 
               
               
                   
                 C(12B)—C(13B)—C(18B) 
                 111.30(15) 
               
               
                   
                 C(12B)—C(13B)—C(17B) 
                 115.91(14) 
               
               
                   
                 C(18B)—C(13B)—C(17B) 
                 110.94(15) 
               
               
                   
                 C(12B)—C(13B)—C(14B) 
                 107.44(15) 
               
               
                   
                 C(18B)—C(13B)—C(14B) 
                 110.58(14) 
               
               
                   
                 C(17B)—C(13B)—C(14B) 
                 100.00(13) 
               
               
                   
                 C(11A)—C(12A)—C(13A) 
                 111.24(15) 
               
               
                   
                 C(11A)—C(12A)—H(12C) 
                 109.4 
               
               
                   
                 C(13A)—C(12A)—H(12C) 
                 109.4 
               
               
                   
                 C(11A)—C(12A)—H(12D) 
                 109.4 
               
               
                   
                 C(13A)—C(12A)—H(12D) 
                 109.4 
               
               
                   
                 H(12C)—C(12A)—H(12D) 
                 108.0 
               
               
                   
                 C(5B)—C(4B)—C(3B) 
                 110.96(15) 
               
               
                   
                 C(5B)—C(4B)—H(4BA) 
                 109.4 
               
               
                   
                 C(3B)—C(4B)—H(4BA) 
                 109.4 
               
               
                   
                 C(5B)—C(4B)—H(4BB) 
                 109.4 
               
               
                   
                 C(3B)—C(4B)—H(4BB) 
                 109.4 
               
               
                   
                 H(4BA)—C(4B)—H(4BB) 
                 108.0 
               
               
                   
                 C(5B)—C(6B)—C(7B) 
                 126.94(18) 
               
               
                   
                 C(5B)—C(6B)—H(6BA) 
                 116.5 
               
               
                   
                 C(7B)—C(6B)—H(6BA) 
                 116.5 
               
               
                   
                 C(6B)—C(5B)—C(10B) 
                 125.49(17) 
               
               
                   
                 C(6B)—C(5B)—C(4B) 
                 121.22(18) 
               
               
                   
                 C(10B)—C(5B)—C(4B) 
                 113.17(15) 
               
               
                   
                 C(8B)—C(14B)—C(15B) 
                 121.27(16) 
               
               
                   
                 C(8B)—C(14B)—C(13B) 
                 113.18(14) 
               
               
                   
                 C(15B)—C(14B)—C(13B) 
                 104.01(15) 
               
               
                   
                 C(8B)—C(14B)—H(14B) 
                 105.7 
               
               
                   
                 C(15B)—C(14B)—H(14B) 
                 105.7 
               
               
                   
                 C(13B)—C(14B)—H(14B) 
                 105.7 
               
               
                   
                 C(5A)—C(10A)—C(1A) 
                 111.36(15) 
               
               
                   
                 C(5A)—C(10A)—H(10C) 
                 109.4 
               
               
                   
                 C(1A)—C(10A)—H(10C) 
                 109.4 
               
               
                   
                 C(5A)—C(10A)—H(10D) 
                 109.4 
               
               
                   
                 C(1A)—C(10A)—H(10D) 
                 109.4 
               
               
                   
                 H(10C)—C(10A)—H(10D) 
                 108.0 
               
               
                   
                 C(19B)—C(2B)—C(3B) 
                 121.69(17) 
               
               
                   
                 C(19B)—C(2B)—C(1B) 
                 124.35(18) 
               
               
                   
                 C(3B)—C(2B)—C(1B) 
                 113.96(15) 
               
               
                   
                 C(12B)—C(11B)—C(9B) 
                 112.84(15) 
               
               
                   
                 C(12B)—C(11B)—H(11A) 
                 109.0 
               
               
                   
                 C(9B)—C(11B)—H(11A) 
                 109.0 
               
               
                   
                 C(12B)—C(11B)—H(11B) 
                 109.0 
               
               
                   
                 C(9B)—C(11B)—H(11B) 
                 109.0 
               
               
                   
                 H(11A)—C(11B)—H(11B) 
                 107.8 
               
               
                   
                 O(25A)—C(25A)—C(26A) 
                 108.17(15) 
               
               
                   
                 O(25A)—C(25A)—C(24A) 
                 109.76(15) 
               
               
                   
                 C(26A)—C(25A)—C(24A) 
                 114.61(16) 
               
               
                   
                 O(25A)—C(25A)—H(25C) 
                 108.0 
               
               
                   
                 C(26A)—C(25A)—H(25C) 
                 108.0 
               
               
                   
                 C(24A)—C(25A)—H(25C) 
                 108.0 
               
               
                   
                 C(12A)—C(11A)—C(9A) 
                 112.71(15) 
               
               
                   
                 C(12A)—C(11A)—H(11C) 
                 109.0 
               
               
                   
                 C(9A)—C(11A)—H(11C) 
                 109.0 
               
               
                   
                 C(12A)—C(11A)—H(11D) 
                 109.0 
               
               
                   
                 C(9A)—C(11A)—H(11D) 
                 109.0 
               
               
                   
                 H(11C)—C(11A)—H(11D) 
                 107.8 
               
               
                   
                 C(8A)—C(9A)—C(11A) 
                 110.93(15) 
               
               
                   
                 C(8A)—C(9A)—H(9AA) 
                 109.5 
               
               
                   
                 C(11A)—C(9A)—H(9AA) 
                 109.5 
               
               
                   
                 C(8A)—C(9A)—H(9AB) 
                 109.5 
               
               
                   
                 C(11A)—C(9A)—H(9AB) 
                 109.5 
               
               
                   
                 H(9AA)—C(9A)—H(9AB) 
                 108.0 
               
               
                   
                 C(19A)—C(2A)—C(3A) 
                 123.23(17) 
               
               
                   
                 C(19A)—C(2A)—C(1A) 
                 124.78(18) 
               
               
                   
                 C(3A)—C(2A)—C(1A) 
                 111.96(16) 
               
               
                   
                 C(14B)—C(15B)—C(16B) 
                 103.37(15) 
               
               
                   
                 C(14B)—C(15B)—H(15A) 
                 111.1 
               
               
                   
                 C(16B)—C(15B)—H(15A) 
                 111.1 
               
               
                   
                 C(14B)—C(15B)—H(15B) 
                 111.1 
               
               
                   
                 C(16B)—C(15B)—H(15B) 
                 111.1 
               
               
                   
                 H(15A)—C(15B)—H(15B) 
                 109.1 
               
               
                   
                 C(2B)—C(19B)—H(19A) 
                 120.0 
               
               
                   
                 C(2B)—C(19B)—H(19B) 
                 120.0 
               
               
                   
                 H(19A)—C(19B)—H(19B) 
                 120.0 
               
               
                   
                 C(23B)—C(22B)—C(20B) 
                 115.28(16) 
               
               
                   
                 C(23B)—C(22B)—H(22A) 
                 108.5 
               
               
                   
                 C(20B)—C(22B)—H(22A) 
                 108.5 
               
               
                   
                 C(23B)—C(22B)—H(22B) 
                 108.5 
               
               
                   
                 C(20B)—C(22B)—H(22B) 
                 108.5 
               
               
                   
                 H(22A)—C(22B)—H(22B) 
                 107.5 
               
               
                   
                 C(15A)—C(16A)—C(17A) 
                 107.70(14) 
               
               
                   
                 C(15A)—C(16A)—H(16A) 
                 110.2 
               
               
                   
                 C(17A)—C(16A)—H(16A) 
                 110.2 
               
               
                   
                 C(15A)—C(16A)—H(16B) 
                 110.2 
               
               
                   
                 C(17A)—C(16A)—H(16B) 
                 110.2 
               
               
                   
                 H(16A)—C(16A)—H(16B) 
                 108.5 
               
               
                   
                 C(2A)—C(19A)—H(19C) 
                 120.0 
               
               
                   
                 C(2A)—C(19A)—H(19D) 
                 120.0 
               
               
                   
                 H(19C)—C(19A)—H(19D) 
                 120.0 
               
               
                   
                 O(2A)—C(3A)—C(2A) 
                 106.68(15) 
               
               
                   
                 O(2A)—C(3A)—C(4A) 
                 112.30(15) 
               
               
                   
                 C(2A)—C(3A)—C(4A) 
                 109.87(15) 
               
               
                   
                 O(2A)—C(3A)—H(3AA) 
                 109.3 
               
               
                   
                 C(2A)—C(3A)—H(3AA) 
                 109.3 
               
               
                   
                 C(4A)—C(3A)—H(3AA) 
                 109.3 
               
               
                   
                 C(5A)—C(6A)—C(7A) 
                 128.24(17) 
               
               
                   
                 C(5A)—C(6A)—H(6AA) 
                 115.9 
               
               
                   
                 C(7A)—C(6A)—H(6AA) 
                 115.9 
               
               
                   
                 C(25A)—C(24A)—C(23A) 
                 116.64(15) 
               
               
                   
                 C(25A)—C(24A)—H(24A) 
                 108.1 
               
               
                   
                 C(23A)—C(24A)—H(24A) 
                 108.1 
               
               
                   
                 C(25A)—C(24A)—H(24B) 
                 108.1 
               
               
                   
                 C(23A)—C(24A)—H(24B) 
                 108.1 
               
               
                   
                 H(24A)—C(24A)—H(24B) 
                 107.3 
               
               
                   
                 C(14A)—C(15A)—C(16A) 
                 103.22(15) 
               
               
                   
                 C(14A)—C(15A)—H(15C) 
                 111.1 
               
               
                   
                 C(16A)—C(15A)—H(15C) 
                 111.1 
               
               
                   
                 C(14A)—C(15A)—H(15D) 
                 111.1 
               
               
                   
                 C(16A)—C(15A)—H(15D) 
                 111.1 
               
               
                   
                 H(15C)—C(15A)—H(15D) 
                 109.1 
               
               
                   
                 C(13A)—C(18A)—H(18D) 
                 109.5 
               
               
                   
                 C(13A)—C(18A)—H(18E) 
                 109.5 
               
               
                   
                 H(18D)—C(18A)—H(18E) 
                 109.5 
               
               
                   
                 C(13A)—C(18A)—H(18F) 
                 109.5 
               
               
                   
                 H(18D)—C(18A)—H(18F) 
                 109.5 
               
               
                   
                 H(18E)—C(18A)—H(18F) 
                 109.5 
               
               
                   
                 C(21B)—C(20B)—C(22B) 
                 109.89(15) 
               
               
                   
                 C(21B)—C(20B)—C(17B) 
                 113.74(16) 
               
               
                   
                 C(22B)—C(20B)—C(17B) 
                 109.14(14) 
               
               
                   
                 C(21B)—C(20B)—H(20A) 
                 108.0 
               
               
                   
                 C(22B)—C(20B)—H(20A) 
                 108.0 
               
               
                   
                 C(17B)—C(20B)—H(20A) 
                 108.0 
               
               
                   
                 C(25B)—C(26B)—H(26A) 
                 109.5 
               
               
                   
                 C(25B)—C(26B)—H(26B) 
                 109.5 
               
               
                   
                 H(26A)—C(26B)—H(26B) 
                 109.5 
               
               
                   
                 C(25B)—C(26B)—H(26C) 
                 109.5 
               
               
                   
                 H(26A)—C(26B)—H(26C) 
                 109.5 
               
               
                   
                 H(26B)—C(26B)—H(26C) 
                 109.5 
               
               
                   
                 O(25B)—C(25B)—C(26B) 
                 106.88(15) 
               
               
                   
                 O(25B)—C(25B)—C(24B) 
                 109.97(15) 
               
               
                   
                 C(26B)—C(25B)—C(24B) 
                 113.97(15) 
               
               
                   
                 O(25B)—C(25B)—H(25D) 
                 108.6 
               
               
                   
                 C(26B)—C(25B)—H(25D) 
                 108.6 
               
               
                   
                 C(24B)—C(25B)—H(25D) 
                 108.6 
               
               
                   
                 C(22B)—C(23B)—C(24B) 
                 111.82(15) 
               
               
                   
                 C(22B)—C(23B)—H(23A) 
                 109.3 
               
               
                   
                 C(24B)—C(23B)—H(23A) 
                 109.3 
               
               
                   
                 C(22B)—C(23B)—H(23B) 
                 109.3 
               
               
                   
                 C(24B)—C(23B)—H(23B) 
                 109.3 
               
               
                   
                 H(23A)—C(23B)—H(23B) 
                 107.9 
               
               
                   
                 C(15B)—C(16B)—C(17B) 
                 107.10(15) 
               
               
                   
                 C(15B)—C(16B)—H(16C) 
                 110.3 
               
               
                   
                 C(17B)—C(16B)—H(16C) 
                 110.3 
               
               
                   
                 C(15B)—C(16B)—H(16D) 
                 110.3 
               
               
                   
                 C(17B)—C(16B)—H(16D) 
                 110.3 
               
               
                   
                 H(16C)—C(16B)—H(16D) 
                 108.6 
               
               
                   
                 C(25B)—C(24B)—C(23B) 
                 115.78(15) 
               
               
                   
                 C(25B)—C(24B)—H(24B) 
                 108.3 
               
               
                   
                 C(23B)—C(24B)—H(24B) 
                 108.3 
               
               
                   
                 C(25B)—C(24B)—H(24C) 
                 108.3 
               
               
                   
                 C(23B)—C(24B)—H(24C) 
                 108.3 
               
               
                   
                 H(24B)—C(24B)—H(24C) 
                 107.4 
               
               
                   
                 C(22A)—C(23A)—C(24A) 
                 110.47(15) 
               
               
                   
                 C(22A)—C(23A)—H(23C) 
                 109.6 
               
               
                   
                 C(24A)—C(23A)—H(23C) 
                 109.6 
               
               
                   
                 C(22A)—C(23A)—H(23D) 
                 109.6 
               
               
                   
                 C(24A)—C(23A)—H(23D) 
                 109.6 
               
               
                   
                 H(23C)—C(23A)—H(23D) 
                 108.1 
               
               
                   
                 C(21A)—C(20A)—C(17A) 
                 113.40(17) 
               
               
                   
                 C(21A)—C(20A)—C(22A) 
                 110.07(17) 
               
               
                   
                 C(17A)—C(20A)—C(22A) 
                 109.15(14) 
               
               
                   
                 C(21A)—C(20A)—H(20B) 
                 108.0 
               
               
                   
                 C(17A)—C(20A)—H(20B) 
                 108.0 
               
               
                   
                 C(22A)—C(20A)—H(20B) 
                 108.0 
               
               
                   
                 C(20B)—C(17B)—C(13B) 
                 119.83(14) 
               
               
                   
                 C(20B)—C(17B)—C(16B) 
                 110.64(15) 
               
               
                   
                 C(13B)—C(17B)—C(16B) 
                 104.20(14) 
               
               
                   
                 C(20B)—C(17B)—H(17A) 
                 107.2 
               
               
                   
                 C(13B)—C(17B)—H(17A) 
                 107.2 
               
               
                   
                 C(16B)—C(17B)—H(17A) 
                 107.2 
               
               
                   
                 C(20A)—C(17A)—C(13A) 
                 119.67(14) 
               
               
                   
                 C(20A)—C(17A)—C(16A) 
                 111.84(15) 
               
               
                   
                 C(13A)—C(17A)—C(16A) 
                 103.18(14) 
               
               
                   
                 C(20A)—C(17A)—H(17B) 
                 107.2 
               
               
                   
                 C(13A)—C(17A)—H(17B) 
                 107.2 
               
               
                   
                 C(16A)—C(17A)—H(17B) 
                 107.2 
               
               
                   
                 C(23A)—C(22A)—C(20A) 
                 116.00(16) 
               
               
                   
                 C(23A)—C(22A)—H(22C) 
                 108.3 
               
               
                   
                 C(20A)—C(22A)—H(22C) 
                 108.3 
               
               
                   
                 C(23A)—C(22A)—H(22D) 
                 108.3 
               
               
                   
                 C(20A)—C(22A)—H(22D) 
                 108.3 
               
               
                   
                 H(22C)—C(22A)—H(22D) 
                 107.4 
               
               
                   
                 C(25A)—C(26A)—H(26D) 
                 109.5 
               
               
                   
                 C(25A)—C(26A)—H(26E) 
                 109.5 
               
               
                   
                 H(26D)—C(26A)—H(26E) 
                 109.5 
               
               
                   
                 C(25A)—C(26A)—H(26F) 
                 109.5 
               
               
                   
                 H(26D)—C(26A)—B(26F) 
                 109.5 
               
               
                   
                 H(26E)—C(26A)—H(26F) 
                 109.5 
               
               
                   
                 C(20B)—C(21B)—H(21A) 
                 109.5 
               
               
                   
                 C(20B)—C(21B)—H(21B) 
                 109.5 
               
               
                   
                 H(21A)—C(21B)—H(21B) 
                 109.5 
               
               
                   
                 C(20B)—C(21B)—H(21C) 
                 109.5 
               
               
                   
                 H(21A)—C(21B)—H(21C) 
                 109.5 
               
               
                   
                 H(21B)—C(21B)—H(21C) 
                 109.5 
               
               
                   
                 C(20A)—C(21A)—H(21D) 
                 109.5 
               
               
                   
                 C(20A)—C(21A)—H(21E) 
                 109.5 
               
               
                   
                 H(21D)—C(21A)—H(21E) 
                 109.5 
               
               
                   
                 C(20A)—C(21A)—H(21F) 
                 109.5 
               
               
                   
                 H(21D)—C(21A)—H(21F) 
                 109.5 
               
               
                   
                 H(21E)—C(21A)—H(21F) 
                 109.5 
               
               
                   
                   
               
             
          
         
       
     
     
       
         
               
             
               
               
               
               
               
               
               
             
               
               
               
               
               
               
               
             
           
               
                 TABLE 5 
               
             
             
               
                   
               
               
                 Anisotropic displacement parameters (Å 2  × 10 3 ) for NEL. 
               
               
                 The anisotropic displacement factor exponent takes the form: 
               
               
                 −2π 2  [h 2 a *  2 U 11  + . . . + 2hka * b * U 12 ] 
               
             
          
           
               
                   
                 U11 
                 U22 
                 U33 
                 U23 
                 U13 
                 U12 
               
               
                   
                   
               
             
          
           
               
                 O(1B) 
                 17(1) 
                 27(1) 
                 31(1) 
                 16(1) 
                 0(1) 
                 −2(1) 
               
               
                 O(25A) 
                 26(1) 
                 23(1) 
                 20(1) 
                  9(1) 
                 4(1) 
                  1(1) 
               
               
                 O(1A) 
                 20(1) 
                 26(1) 
                 28(1) 
                  8(1) 
                 5(1) 
                  3(1) 
               
               
                 O(2B) 
                 19(1) 
                 24(1) 
                 26(1) 
                  6(1) 
                 2(1) 
                  2(1) 
               
               
                 O(25B) 
                 30(1) 
                 24(1) 
                 20(1) 
                  9(1) 
                 −2(1)  
                  4(1) 
               
               
                 O(2A) 
                 21(1) 
                 34(1) 
                 29(1) 
                  4(1) 
                 2(1) 
                 −6(1) 
               
               
                 C(12B) 
                 18(1) 
                 24(1) 
                 22(1) 
                 11(1) 
                 −3(1)  
                 −4(1) 
               
               
                 C(3B) 
                 22(1) 
                 22(1) 
                 23(1) 
                 13(1) 
                 2(1) 
                  4(1) 
               
               
                 C(14A) 
                 21(1) 
                 19(1) 
                 20(1) 
                  7(1) 
                 3(1) 
                  1(1) 
               
               
                 C(1A) 
                 20(1) 
                 20(1) 
                 25(1) 
                  7(1) 
                 2(1) 
                 −2(1) 
               
               
                 C(1B) 
                 18(1) 
                 21(1) 
                 24(1) 
                 11(1) 
                 3(1) 
                  2(1) 
               
               
                 C(7B) 
                 23(1) 
                 22(1) 
                 20(1) 
                  5(1) 
                 1(1) 
                 −5(1) 
               
               
                 C(9B) 
                 20(1) 
                 22(1) 
                 23(1) 
                 11(1) 
                 2(1) 
                  0(1) 
               
               
                 C(7A) 
                 23(1) 
                 20(1) 
                 20(1) 
                  5(1) 
                 2(1) 
                  3(1) 
               
               
                 C(8A) 
                 21(1) 
                 18(1) 
                 19(1) 
                  5(1) 
                 −1(1)  
                  1(1) 
               
               
                 C(18B) 
                 24(1) 
                 26(1) 
                 24(1) 
                 13(1) 
                 3(1) 
                  4(1) 
               
               
                 C(8B) 
                 25(1) 
                 18(1) 
                 15(1) 
                  3(1) 
                 2(1) 
                 −1(1) 
               
               
                 C(4A) 
                 24(1) 
                 21(1) 
                 23(1) 
                 10(1) 
                 3(1) 
                  2(1) 
               
               
                 C(10B) 
                 26(1) 
                 27(1) 
                 22(1) 
                 13(1) 
                 5(1) 
                  3(1) 
               
               
                 C(13A) 
                 23(1) 
                 19(1) 
                 22(1) 
                  9(1) 
                 2(1) 
                  1(1) 
               
               
                 C(5A) 
                 24(1) 
                 17(1) 
                 18(1) 
                  4(1) 
                 0(1) 
                 −1(1) 
               
               
                 C(13B) 
                 20(1) 
                 19(1) 
                 17(1) 
                  7(1) 
                 0(1) 
                 −1(1) 
               
               
                 C(12A) 
                 26(1) 
                 26(1) 
                 24(1) 
                 12(1) 
                 9(1) 
                  7(1) 
               
               
                 C(4B) 
                 24(1) 
                 20(1) 
                 25(1) 
                  9(1) 
                 2(1) 
                  1(1) 
               
               
                 C(6B) 
                 25(1) 
                 19(1) 
                 17(1) 
                  4(1) 
                 1(1) 
                 −2(1) 
               
               
                 C(5B) 
                 27(1) 
                 20(1) 
                 18(1) 
                  6(1) 
                 5(1) 
                  3(1) 
               
               
                 C(14B) 
                 24(1) 
                 19(1) 
                 18(1) 
                  7(1) 
                 1(1) 
                 −2(1) 
               
               
                 C(10A) 
                 25(1) 
                 25(1) 
                 24(1) 
                 13(1) 
                 1(1) 
                  1(1) 
               
               
                 C(2B) 
                 20(1) 
                 19(1) 
                 20(1) 
                  6(1) 
                 2(1) 
                  3(1) 
               
               
                 C(11B) 
                 17(1) 
                 24(1) 
                 25(1) 
                 12(1) 
                 −2(1)  
                 −4(1) 
               
               
                 C(25A) 
                 27(1) 
                 21(1) 
                 17(1) 
                  8(1) 
                 4(1) 
                  5(1) 
               
               
                 C(11A) 
                 24(1) 
                 29(1) 
                 31(1) 
                 17(1) 
                 11(1)  
                 11(1) 
               
               
                 C(9A) 
                 21(1) 
                 26(1) 
                 27(1) 
                 14(1) 
                 2(1) 
                  2(1) 
               
               
                 C(2A) 
                 24(1) 
                 23(1) 
                 17(1) 
                  6(1) 
                 0(1) 
                 −3(1) 
               
               
                 C(15B) 
                 35(1) 
                 28(1) 
                 22(1) 
                  9(1) 
                 −4(1)  
                 −13(1)  
               
               
                 C(19B) 
                 22(1) 
                 31(1) 
                 29(1) 
                 17(1) 
                 2(1) 
                  1(1) 
               
               
                 C(22B) 
                 26(1) 
                 24(1) 
                 22(1) 
                  9(1) 
                 0(1) 
                 −2(1) 
               
               
                 C(16A) 
                 26(1) 
                 23(1) 
                 25(1) 
                 10(1) 
                 4(1) 
                  5(1) 
               
               
                 C(19A) 
                 26(1) 
                 37(1) 
                 29(1) 
                 17(1) 
                 5(1) 
                  2(1) 
               
               
                 C(3A) 
                 23(1) 
                 24(1) 
                 21(1) 
                 11(1) 
                 −2(1)  
                 −1(1) 
               
               
                 C(6A) 
                 24(1) 
                 18(1) 
                 22(1) 
                  6(1) 
                 1(1) 
                  2(1) 
               
               
                 C(24A) 
                 33(1) 
                 19(1) 
                 20(1) 
                  6(1) 
                 1(1) 
                  3(1) 
               
               
                 C(15A) 
                 34(1) 
                 27(1) 
                 27(1) 
                 13(1) 
                 10(1)  
                 12(1) 
               
               
                 C(18A) 
                 29(1) 
                 22(1) 
                 32(1) 
                 13(1) 
                 −4(1)  
                 −3(1) 
               
               
                 C(20B) 
                 22(1) 
                 24(1) 
                 19(1) 
                  9(1) 
                 1(1) 
                 −1(1) 
               
               
                 C(26B) 
                 26(1) 
                 29(1) 
                 26(1) 
                 10(1) 
                 1(1) 
                 −4(1) 
               
               
                 C(25B) 
                 24(1) 
                 19(1) 
                 21(1) 
                  8(1) 
                 −1(1)  
                 −1(1) 
               
               
                 C(23B) 
                 36(1) 
                 23(1) 
                 23(1) 
                 11(1) 
                 6(1) 
                  1(1) 
               
               
                 C(16B) 
                 30(1) 
                 26(1) 
                 21(1) 
                 10(1) 
                 −1(1)  
                 −7(1) 
               
               
                 C(24B) 
                 27(1) 
                 20(1) 
                 22(1) 
                  8(1) 
                 0(1) 
                 −1(1) 
               
               
                 C(23A) 
                 35(1) 
                 21(1) 
                 21(1) 
                  8(1) 
                 −2(1)  
                  2(1) 
               
               
                 C(20A) 
                 29(1) 
                 19(1) 
                 24(1) 
                  6(1) 
                 0(1) 
                  3(1) 
               
               
                 C(17B) 
                 20(1) 
                 20(1) 
                 20(1) 
                  8(1) 
                 1(1) 
                  0(1) 
               
               
                 C(17A) 
                 20(1) 
                 17(1) 
                 22(1) 
                  7(1) 
                 0(1) 
                  0(1) 
               
               
                 C(22A) 
                 30(1) 
                 21(1) 
                 22(1) 
                  9(1) 
                 −1(1)  
                  1(1) 
               
               
                 C(26A) 
                 30(1) 
                 34(1) 
                 25(1) 
                 15(1) 
                 3(1) 
                  3(1) 
               
               
                 C(21B) 
                 43(1) 
                 33(1) 
                 22(1) 
                 14(1) 
                 −6(1)  
                 −10(1)  
               
               
                 C(21A) 
                 59(2) 
                 42(1) 
                 23(1) 
                 13(1) 
                 8(1) 
                 25(1) 
               
               
                   
               
             
          
         
       
     
     
       
         
               
             
               
               
               
               
               
             
               
               
               
               
               
               
             
           
               
                 TABLE 6 
               
             
             
               
                   
               
               
                 Hydrogen coordinates (×10 4 ) and isotropic 
               
               
                 displacement parameters (Å 2  × 10 3 ) for NEL. 
               
             
          
           
               
                   
                 x 
                 y 
                 z 
                 U(eq) 
               
               
                   
                   
               
             
          
           
               
                   
                 H(1BA) 
                 19161 
                 17964 
                 1490 
                 35 
               
               
                   
                 H(25A) 
                 18570 
                 16034 
                 1263 
                 33 
               
               
                   
                 H(1AA) 
                 17440 
                 14003 
                 10350 
                 38 
               
               
                   
                 H(2BA) 
                 25660 
                 17721 
                 897 
                 36 
               
               
                   
                 H(25B) 
                 25582 
                 15881 
                 10525 
                 37 
               
               
                   
                 H(2AA) 
                 24659 
                 12701 
                 10160 
                 45 
               
               
                   
                 H(12A) 
                 30805 
                 18420 
                 6459 
                 25 
               
               
                   
                 H(12B) 
                 29951 
                 19463 
                 7205 
                 25 
               
               
                   
                 H(3BA) 
                 24872 
                 19664 
                 970 
                 25 
               
               
                   
                 H(14A) 
                 23849 
                 14164 
                 6358 
                 24 
               
               
                   
                 N(1AB) 
                 20405 
                 13618 
                 9985 
                 26 
               
               
                   
                 H(1BB) 
                 23051 
                 17459 
                 1699 
                 24 
               
               
                   
                 H(7BA) 
                 24730 
                 18218 
                 4096 
                 27 
               
               
                   
                 H(9BA) 
                 29766 
                 19618 
                 4680 
                 25 
               
               
                   
                 H(9BB) 
                 30734 
                 18533 
                 4798 
                 25 
               
               
                   
                 H(7AA) 
                 20824 
                 13061 
                 7432 
                 26 
               
               
                   
                 H(18A) 
                 26102 
                 19896 
                 6397 
                 35 
               
               
                   
                 H(18B) 
                 25900 
                 19599 
                 7259 
                 35 
               
               
                   
                 H(18C) 
                 24494 
                 18928 
                 6363 
                 35 
               
               
                   
                 H(4AA) 
                 23843 
                 11012 
                 8972 
                 27 
               
               
                   
                 H(4AB) 
                 21582 
                 10459 
                 8883 
                 27 
               
               
                   
                 H(10A) 
                 21552 
                 19485 
                 2912 
                 29 
               
               
                   
                 H(10B) 
                 22323 
                 18458 
                 3178 
                 29 
               
               
                   
                 H(12C) 
                 24585 
                 12009 
                 4312 
                 29 
               
               
                   
                 H(12D) 
                 25726 
                 13065 
                 5083 
                 29 
               
               
                   
                 H(4BA) 
                 26714 
                 20228 
                 2451 
                 27 
               
               
                   
                 H(4BB) 
                 24412 
                 20656 
                 2462 
                 27 
               
               
                   
                 H(6BA) 
                 27544 
                 19598 
                 3608 
                 26 
               
               
                   
                 H(14B) 
                 28424 
                 17229 
                 5174 
                 25 
               
               
                   
                 H(10C) 
                 18361 
                 11726 
                 8562 
                 29 
               
               
                   
                 H(10D) 
                 19077 
                 12870 
                 8467 
                 29 
               
               
                   
                 H(11A) 
                 31562 
                 20046 
                 6148 
                 26 
               
               
                   
                 H(11B) 
                 29205 
                 20381 
                 6189 
                 26 
               
               
                   
                 H(25C) 
                 16590 
                 16751 
                 2294 
                 25 
               
               
                   
                 H(11C) 
                 26696 
                 11421 
                 5353 
                 31 
               
               
                   
                 H(11D) 
                 24327 
                 11039 
                 5303 
                 31 
               
               
                   
                 H(9AA) 
                 25631 
                 11790 
                 6817 
                 28 
               
               
                   
                 H(9AB) 
                 26460 
                 12912 
                 6716 
                 28 
               
               
                   
                 H(15A) 
                 25251 
                 16354 
                 4601 
                 35 
               
               
                   
                 H(15B) 
                 24038 
                 17434 
                 5137 
                 35 
               
               
                   
                 H(19A) 
                 21542 
                 19209 
                 194 
                 39 
               
               
                   
                 H(19B) 
                 19798 
                 18479 
                 454 
                 39 
               
               
                   
                 H(22A) 
                 25901 
                 15976 
                 7287 
                 28 
               
               
                   
                 H(22B) 
                 27952 
                 16366 
                 7953 
                 28 
               
               
                   
                 H(16A) 
                 20720 
                 15457 
                 5724 
                 29 
               
               
                   
                 H(16B) 
                 18952 
                 14489 
                 5269 
                 29 
               
               
                   
                 H(19C) 
                 19444 
                 11330 
                 11045 
                 44 
               
               
                   
                 H(19D) 
                 17576 
                 12098 
                 10868 
                 44 
               
               
                   
                 H(3AA) 
                 22660 
                 11257 
                 10408 
                 27 
               
               
                   
                 H(6AA) 
                 23960 
                 11720 
                 7861 
                 26 
               
               
                   
                 H(24A) 
                 18004 
                 16316 
                 3486 
                 29 
               
               
                   
                 H(24B) 
                 19810 
                 16327 
                 2892 
                 29 
               
               
                   
                 H(15C) 
                 20875 
                 14932 
                 6921 
                 33 
               
               
                   
                 H(15D) 
                 19488 
                 13807 
                 6380 
                 33 
               
               
                   
                 H(18D) 
                 19443 
                 12371 
                 5020 
                 41 
               
               
                   
                 H(18E) 
                 21043 
                 11501 
                 5166 
                 41 
               
               
                   
                 H(18F) 
                 20715 
                 11650 
                 4232 
                 41 
               
               
                   
                 H(20A) 
                 25243 
                 18002 
                 7690 
                 26 
               
               
                   
                 H(26A) 
                 20801 
                 15579 
                 9775 
                 41 
               
               
                   
                 H(26B) 
                 20899 
                 15098 
                 8731 
                 41 
               
               
                   
                 H(26C) 
                 21447 
                 16391 
                 9283 
                 41 
               
               
                   
                 H(25D) 
                 23893 
                 14605 
                 9451 
                 26 
               
               
                   
                 H(23A) 
                 23870 
                 16840 
                 8498 
                 32 
               
               
                   
                 H(23B) 
                 25948 
                 17163 
                 9157 
                 32 
               
               
                   
                 H(16C) 
                 25832 
                 15852 
                 5811 
                 31 
               
               
                   
                 H(16D) 
                 24128 
                 16721 
                 6241 
                 31 
               
               
                   
                 H(24B) 
                 24572 
                 14884 
                 8135 
                 28 
               
               
                   
                 H(24C) 
                 26567 
                 15235 
                 8835 
                 28 
               
               
                   
                 H(23C) 
                 17871 
                 14278 
                 2858 
                 31 
               
               
                   
                 H(23D) 
                 19853 
                 14353 
                 2365 
                 31 
               
               
                   
                 H(20B) 
                 19657 
                 13272 
                 3783 
                 29 
               
               
                   
                 H(17A) 
                 28500 
                 17005 
                 6615 
                 24 
               
               
                   
                 H(17B) 
                 23208 
                 14447 
                 4956 
                 23 
               
               
                   
                 H(22C) 
                 19938 
                 15328 
                 4253 
                 29 
               
               
                   
                 H(22D) 
                 21902 
                 15184 
                 3712 
                 29 
               
               
                   
                 H(26D) 
                 13962 
                 15360 
                 1598 
                 43 
               
               
                   
                 H(26E) 
                 14256 
                 15574 
                 2630 
                 43 
               
               
                   
                 H(26F) 
                 15183 
                 14500 
                 1945 
                 43 
               
               
                   
                 H(21A) 
                 28248 
                 19245 
                 8248 
                 49 
               
               
                   
                 H(21B) 
                 29556 
                 18246 
                 8354 
                 49 
               
               
                   
                 H(21C) 
                 27705 
                 18701 
                 8948 
                 49 
               
               
                   
                 H(21D) 
                 22673 
                 12286 
                 3278 
                 61 
               
               
                   
                 H(21E) 
                 23730 
                 13402 
                 3253 
                 61 
               
               
                   
                 H(21F) 
                 21731 
                 12827 
                 2591 
                 61 
               
               
                   
                   
               
             
          
         
       
     
     
       
         
               
             
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
             
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
               
             
           
               
                 TABLE 7 
               
             
             
               
                   
               
               
                 Observed and calculated structure factors for NEL 
               
             
          
           
               
                 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 
                 2 
                 −18 
                 48 
                 43 
                 2 
                 1 
                 0 
                 −16 
                 58 
                 59 
                 1 
                 1 
                 0 
                 −15 
                 78 
                 80 
                 1 
                 2 
                 −4 
                 −14 
                 52 
                 53 
                 1 
                 2 
                 8 
                 −14 
                 65 
                 70 
                 1 
               
               
                 1 
                 2 
                 −18 
                 75 
                 71 
                 2 
                 2 
                 0 
                 −16 
                 67 
                 68 
                 1 
                 2 
                 0 
                 −15 
                 127 
                 130 
                 2 
                 3 
                 −4 
                 −14 
                 33 
                 37 
                 2 
                 3 
                 8 
                 −14 
                 140 
                 139 
                 2 
               
               
                 0 
                 3 
                 −18 
                 30 
                 27 
                 2 
                 3 
                 0 
                 −16 
                 44 
                 45 
                 1 
                 3 
                 0 
                 −15 
                 32 
                 29 
                 1 
                 −1 
                 −3 
                 −14 
                 60 
                 62 
                 2 
                 4 
                 8 
                 −14 
                 51 
                 50 
                 2 
               
               
                 1 
                 3 
                 −18 
                 35 
                 36 
                 1 
                 −1 
                 1 
                 −16 
                 44 
                 45 
                 2 
                 4 
                 0 
                 −15 
                 9 
                 9 
                 8 
                 0 
                 −3 
                 −14 
                 21 
                 18 
                 2 
                 −3 
                 9 
                 −14 
                 28 
                 27 
                 3 
               
               
                 2 
                 3 
                 −18 
                 26 
                 28 
                 2 
                 0 
                 1 
                 −16 
                 138 
                 127 
                 3 
                 −1 
                 1 
                 −15 
                 95 
                 98 
                 2 
                 1 
                 −3 
                 −14 
                 34 
                 29 
                 1 
                 −2 
                 9 
                 −14 
                 92 
                 90 
                 2 
               
               
                 −1 
                 4 
                 −18 
                 12 
                 10 
                 6 
                 1 
                 1 
                 −16 
                 110 
                 118 
                 1 
                 0 
                 1 
                 −15 
                 39 
                 37 
                 2 
                 2 
                 −3 
                 −14 
                 37 
                 36 
                 1 
                 −1 
                 9 
                 −14 
                 53 
                 52 
                 1 
               
               
                 0 
                 4 
                 −18 
                 55 
                 56 
                 2 
                 2 
                 1 
                 −16 
                 43 
                 41 
                 1 
                 1 
                 1 
                 −15 
                 70 
                 68 
                 1 
                 3 
                 −3 
                 −14 
                 48 
                 43 
                 1 
                 0 
                 9 
                 −14 
                 116 
                 116 
                 2 
               
               
                 1 
                 4 
                 −18 
                 38 
                 40 
                 1 
                 3 
                 1 
                 −16 
                 44 
                 44 
                 1 
                 2 
                 1 
                 −15 
                 96 
                 95 
                 1 
                 −1 
                 −2 
                 −14 
                 35 
                 35 
                 2 
                 1 
                 9 
                 −14 
                 28 
                 26 
                 1 
               
               
                 2 
                 4 
                 −18 
                 36 
                 34 
                 1 
                 4 
                 1 
                 −16 
                 38 
                 41 
                 1 
                 3 
                 1 
                 −15 
                 73 
                 75 
                 1 
                 0 
                 −2 
                 −14 
                 40 
                 43 
                 1 
                 2 
                 9 
                 −14 
                 34 
                 27 
                 2 
               
               
                 −1 
                 5 
                 −18 
                 25 
                 23 
                 3 
                 −2 
                 2 
                 −16 
                 24 
                 23 
                 3 
                 4 
                 1 
                 −15 
                 31 
                 28 
                 1 
                 1 
                 −2 
                 −14 
                 44 
                 42 
                 1 
                 3 
                 9 
                 −14 
                 71 
                 66 
                 2 
               
               
                 0 
                 5 
                 −18 
                 33 
                 29 
                 2 
                 −1 
                 2 
                 −16 
                 86 
                 84 
                 2 
                 −2 
                 2 
                 −15 
                 81 
                 87 
                 2 
                 2 
                 −2 
                 −14 
                 32 
                 35 
                 1 
                 −3 
                 10 
                 −14 
                 100 
                 99 
                 2 
               
               
                 1 
                 5 
                 −18 
                 68 
                 65 
                 1 
                 0 
                 2 
                 −16 
                 106 
                 101 
                 2 
                 −1 
                 2 
                 −15 
                 79 
                 74 
                 2 
                 3 
                 −2 
                 −14 
                 43 
                 42 
                 1 
                 −2 
                 10 
                 −14 
                 70 
                 76 
                 2 
               
               
                 2 
                 5 
                 −18 
                 41 
                 37 
                 2 
                 1 
                 2 
                 −16 
                 67 
                 64 
                 1 
                 0 
                 2 
                 −15 
                 47 
                 46 
                 2 
                 4 
                 −2 
                 −14 
                 91 
                 85 
                 1 
                 −1 
                 10 
                 −14 
                 64 
                 61 
                 1 
               
               
                 −1 
                 6 
                 −18 
                 12 
                 14 
                 5 
                 2 
                 2 
                 −16 
                 63 
                 63 
                 1 
                 1 
                 2 
                 −15 
                 86 
                 83 
                 2 
                 −1 
                 −1 
                 −14 
                 68 
                 68 
                 1 
                 0 
                 10 
                 −14 
                 26 
                 25 
                 2 
               
               
                 0 
                 6 
                 −18 
                 21 
                 20 
                 3 
                 3 
                 2 
                 −16 
                 105 
                 102 
                 1 
                 2 
                 2 
                 −15 
                 72 
                 76 
                 1 
                 0 
                 −1 
                 −14 
                 59 
                 52 
                 1 
                 1 
                 10 
                 −14 
                 58 
                 51 
                 1 
               
               
                 1 
                 6 
                 −18 
                 69 
                 68 
                 1 
                 4 
                 2 
                 −16 
                 31 
                 29 
                 1 
                 3 
                 2 
                 −15 
                 35 
                 40 
                 1 
                 1 
                 −1 
                 −14 
                 72 
                 76 
                 1 
                 2 
                 10 
                 −14 
                 73 
                 74 
                 2 
               
               
                 2 
                 6 
                 −18 
                 13 
                 11 
                 5 
                 −2 
                 3 
                 −16 
                 58 
                 60 
                 2 
                 4 
                 2 
                 −15 
                 59 
                 55 
                 1 
                 2 
                 −1 
                 −14 
                 112 
                 117 
                 1 
                 3 
                 10 
                 −14 
                 12 
                 14 
                 6 
               
               
                 −1 
                 7 
                 −18 
                 22 
                 21 
                 3 
                 −1 
                 3 
                 −16 
                 72 
                 72 
                 2 
                 −2 
                 3 
                 −15 
                 79 
                 75 
                 2 
                 3 
                 −1 
                 −14 
                 46 
                 42 
                 1 
                 −2 
                 11 
                 −14 
                 47 
                 47 
                 2 
               
               
                 0 
                 7 
                 −18 
                 19 
                 22 
                 2 
                 0 
                 3 
                 −16 
                 38 
                 30 
                 2 
                 −1 
                 3 
                 −15 
                 58 
                 58 
                 2 
                 4 
                 −1 
                 −14 
                 54 
                 52 
                 1 
                 −1 
                 11 
                 −14 
                 12 
                 14 
                 4 
               
               
                 1 
                 7 
                 −18 
                 109 
                 102 
                 2 
                 1 
                 3 
                 −16 
                 52 
                 51 
                 1 
                 0 
                 3 
                 −15 
                 13 
                 10 
                 3 
                 −1 
                 0 
                 −14 
                 63 
                 63 
                 2 
                 0 
                 11 
                 −14 
                 24 
                 22 
                 1 
               
               
                 2 
                 7 
                 −18 
                 90 
                 92 
                 2 
                 2 
                 3 
                 −16 
                 35 
                 32 
                 1 
                 1 
                 3 
                 −15 
                 200 
                 198 
                 3 
                 0 
                 0 
                 −14 
                 86 
                 86 
                 1 
                 1 
                 11 
                 −14 
                 60 
                 62 
                 1 
               
               
                 1 
                 8 
                 −18 
                 58 
                 61 
                 1 
                 3 
                 3 
                 −16 
                 14 
                 15 
                 3 
                 2 
                 3 
                 −15 
                 116 
                 121 
                 1 
                 1 
                 0 
                 −14 
                 43 
                 45 
                 1 
                 2 
                 11 
                 −14 
                 66 
                 69 
                 2 
               
               
                 1 
                 −1 
                 −17 
                 77 
                 82 
                 2 
                 4 
                 3 
                 −16 
                 71 
                 71 
                 1 
                 3 
                 3 
                 −15 
                 10 
                 13 
                 4 
                 2 
                 0 
                 −14 
                 101 
                 102 
                 2 
                 −2 
                 12 
                 −14 
                 20 
                 23 
                 3 
               
               
                 0 
                 0 
                 −17 
                 39 
                 34 
                 2 
                 −2 
                 4 
                 −16 
                 31 
                 31 
                 3 
                 4 
                 3 
                 −15 
                 54 
                 53 
                 1 
                 3 
                 0 
                 −14 
                 109 
                 111 
                 1 
                 −1 
                 12 
                 −14 
                 80 
                 78 
                 2 
               
               
                 1 
                 0 
                 −17 
                 111 
                 105 
                 3 
                 −1 
                 4 
                 −16 
                 45 
                 43 
                 2 
                 5 
                 3 
                 −15 
                 105 
                 111 
                 2 
                 4 
                 0 
                 −14 
                 69 
                 66 
                 1 
                 0 
                 12 
                 −14 
                 57 
                 56 
                 1 
               
               
                 2 
                 0 
                 −17 
                 16 
                 18 
                 2 
                 0 
                 4 
                 −16 
                 90 
                 93 
                 2 
                 −2 
                 4 
                 −15 
                 39 
                 42 
                 2 
                 −2 
                 1 
                 −14 
                 57 
                 60 
                 2 
                 1 
                 12 
                 −14 
                 13 
                 19 
                 3 
               
               
                 −1 
                 1 
                 −17 
                 87 
                 83 
                 2 
                 1 
                 4 
                 −16 
                 96 
                 96 
                 2 
                 −1 
                 4 
                 −15 
                 61 
                 62 
                 2 
                 −1 
                 1 
                 −14 
                 73 
                 72 
                 2 
                 2 
                 12 
                 −14 
                 14 
                 12 
                 4 
               
               
                 0 
                 1 
                 −17 
                 211 
                 197 
                 5 
                 2 
                 4 
                 −16 
                 21 
                 22 
                 1 
                 0 
                 4 
                 −15 
                 39 
                 44 
                 1 
                 0 
                 1 
                 −14 
                 50 
                 51 
                 1 
                 0 
                 13 
                 −14 
                 66 
                 59 
                 2 
               
               
                 1 
                 1 
                 −17 
                 38 
                 33 
                 1 
                 3 
                 4 
                 −16 
                 54 
                 56 
                 1 
                 1 
                 4 
                 −15 
                 86 
                 87 
                 1 
                 1 
                 1 
                 −14 
                 9 
                 7 
                 5 
                 1 
                 13 
                 −14 
                 50 
                 53 
                 2 
               
               
                 2 
                 1 
                 −17 
                 117 
                 113 
                 1 
                 4 
                 4 
                 −16 
                 26 
                 26 
                 1 
                 2 
                 4 
                 −15 
                 109 
                 108 
                 1 
                 2 
                 1 
                 −14 
                 99 
                 102 
                 1 
                 0 
                 −6 
                 −13 
                 41 
                 37 
                 2 
               
               
                 3 
                 1 
                 −17 
                 85 
                 84 
                 2 
                 −2 
                 5 
                 −16 
                 24 
                 20 
                 3 
                 3 
                 4 
                 −15 
                 67 
                 73 
                 1 
                 3 
                 1 
                 −14 
                 115 
                 116 
                 1 
                 1 
                 −6 
                 −13 
                 41 
                 38 
                 1 
               
               
                 −1 
                 2 
                 −17 
                 53 
                 54 
                 2 
                 −1 
                 5 
                 −16 
                 97 
                 96 
                 2 
                 4 
                 4 
                 −15 
                 44 
                 43 
                 1 
                 4 
                 1 
                 −14 
                 21 
                 19 
                 2 
                 −1 
                 −5 
                 −13 
                 92 
                 84 
                 2 
               
               
                 0 
                 2 
                 −17 
                 124 
                 117 
                 3 
                 0 
                 5 
                 −16 
                 69 
                 69 
                 1 
                 5 
                 4 
                 −15 
                 31 
                 27 
                 2 
                 5 
                 1 
                 −14 
                 23 
                 23 
                 2 
                 0 
                 −5 
                 −13 
                 44 
                 43 
                 1 
               
               
                 1 
                 2 
                 −17 
                 88 
                 85 
                 1 
                 1 
                 5 
                 −16 
                 46 
                 47 
                 1 
                 −2 
                 5 
                 −15 
                 27 
                 25 
                 3 
                 −2 
                 2 
                 −14 
                 100 
                 108 
                 3 
                 1 
                 −5 
                 −13 
                 110 
                 106 
                 2 
               
               
                 2 
                 2 
                 −17 
                 49 
                 50 
                 1 
                 2 
                 5 
                 −16 
                 58 
                 56 
                 1 
                 −1 
                 5 
                 −15 
                 177 
                 181 
                 3 
                 −1 
                 2 
                 −14 
                 92 
                 92 
                 3 
                 2 
                 −5 
                 −13 
                 39 
                 41 
                 1 
               
               
                 3 
                 2 
                 −17 
                 48 
                 49 
                 1 
                 3 
                 5 
                 −16 
                 87 
                 87 
                 1 
                 0 
                 5 
                 −15 
                 162 
                 200 
                 4 
                 0 
                 2 
                 −14 
                 226 
                 229 
                 2 
                 3 
                 −5 
                 −13 
                 52 
                 55 
                 1 
               
               
                 −1 
                 3 
                 −17 
                 42 
                 35 
                 2 
                 4 
                 5 
                 −16 
                 49 
                 53 
                 1 
                 1 
                 5 
                 −15 
                 108 
                 106 
                 2 
                 1 
                 2 
                 −14 
                 91 
                 88 
                 1 
                 −2 
                 −4 
                 −13 
                 32 
                 31 
                 2 
               
               
                 0 
                 3 
                 −17 
                 100 
                 96 
                 2 
                 −2 
                 6 
                 −16 
                 89 
                 87 
                 2 
                 2 
                 5 
                 −15 
                 72 
                 72 
                 1 
                 2 
                 2 
                 −14 
                 145 
                 146 
                 2 
                 −1 
                 −4 
                 −13 
                 83 
                 86 
                 2 
               
               
                 1 
                 3 
                 −17 
                 43 
                 44 
                 1 
                 −1 
                 6 
                 −16 
                 43 
                 42 
                 2 
                 3 
                 5 
                 −15 
                 122 
                 120 
                 2 
                 3 
                 2 
                 −14 
                 73 
                 75 
                 1 
                 0 
                 −4 
                 −13 
                 44 
                 39 
                 1 
               
               
                 2 
                 3 
                 −17 
                 11 
                 7 
                 4 
                 0 
                 6 
                 −16 
                 122 
                 118 
                 2 
                 4 
                 5 
                 −15 
                 86 
                 85 
                 1 
                 4 
                 2 
                 −14 
                 21 
                 15 
                 2 
                 1 
                 −4 
                 −13 
                 85 
                 81 
                 1 
               
               
                 3 
                 3 
                 −17 
                 34 
                 34 
                 1 
                 1 
                 6 
                 −16 
                 93 
                 90 
                 2 
                 −3 
                 6 
                 −15 
                 51 
                 51 
                 2 
                 5 
                 2 
                 −14 
                 21 
                 21 
                 2 
                 2 
                 −4 
                 −13 
                 26 
                 24 
                 2 
               
               
                 −2 
                 4 
                 −17 
                 51 
                 52 
                 2 
                 2 
                 6 
                 −16 
                 18 
                 14 
                 2 
                 −2 
                 6 
                 −15 
                 48 
                 51 
                 2 
                 −2 
                 3 
                 −14 
                 145 
                 149 
                 3 
                 3 
                 −4 
                 −13 
                 81 
                 80 
                 1 
               
               
                 −1 
                 4 
                 −17 
                 46 
                 46 
                 2 
                 3 
                 6 
                 −16 
                 36 
                 34 
                 1 
                 −1 
                 6 
                 −15 
                 68 
                 68 
                 2 
                 −1 
                 3 
                 −14 
                 221 
                 227 
                 3 
                 4 
                 −4 
                 −13 
                 13 
                 14 
                 2 
               
               
                 0 
                 4 
                 −17 
                 131 
                 123 
                 3 
                 4 
                 6 
                 −16 
                 57 
                 62 
                 2 
                 0 
                 6 
                 −15 
                 154 
                 158 
                 4 
                 0 
                 3 
                 −14 
                 237 
                 243 
                 4 
                 −2 
                 −3 
                 −13 
                 80 
                 82 
                 2 
               
               
                 1 
                 4 
                 −17 
                 18 
                 16 
                 3 
                 −2 
                 7 
                 −16 
                 18 
                 25 
                 3 
                 1 
                 6 
                 −15 
                 30 
                 25 
                 2 
                 1 
                 3 
                 −14 
                 121 
                 125 
                 1 
                 −1 
                 −3 
                 −13 
                 43 
                 40 
                 2 
               
               
                 2 
                 4 
                 −17 
                 51 
                 50 
                 1 
                 −1 
                 7 
                 −16 
                 64 
                 61 
                 2 
                 2 
                 6 
                 −15 
                 42 
                 42 
                 1 
                 2 
                 3 
                 −14 
                 75 
                 80 
                 1 
                 0 
                 −3 
                 −13 
                 55 
                 53 
                 1 
               
               
                 3 
                 4 
                 −17 
                 10 
                 8 
                 7 
                 0 
                 7 
                 −16 
                 32 
                 33 
                 2 
                 3 
                 6 
                 −15 
                 84 
                 84 
                 1 
                 3 
                 3 
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                 1 
               
               
                 −4 
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                 0 
                 −8 
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                 38 
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                 1 
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                 −5 
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                 0 
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                 −3 
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                 59 
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                 −2 
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                 86 
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                 4 
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                 −3 
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                 −1 
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                 5 
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                 0 
                 8 
                 1 
                 52 
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                 6 
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                 −1 
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                 1 
                 8 
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                 1 
                 7 
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                 0 
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                 2 
                 8 
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                 25 
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                 −7 
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                 25 
                 18 
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                 1 
                 8 
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                 3 
                 8 
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                 4 
                 8 
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                 −1 
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                 −5 
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                 3 
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                 41 
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                 0 
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                 215 
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                 3 
               
               
                 5 
                 8 
                 1 
                 4 
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                 0 
                 −7 
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                 −4 
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                 4 
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                 −5 
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                 1 
                 −7 
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                 1 
                 −3 
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                 5 
                 8 
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                 81 
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                 1 
               
               
                 −4 
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                 2 
                 −7 
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                 116 
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                 −2 
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                 −5 
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                 10 
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                 −7 
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                 −3 
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                 1 
                 33 
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                 −7 
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                 82 
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                 −1 
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                 1 
               
               
                 −2 
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                 4 
                 −7 
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                 140 
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                 0 
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                 43 
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                 −1 
                 9 
                 1 
                 36 
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                 5 
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                 55 
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                 1 
                 1 
                 2 
                 2 
                 430 
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                 10 
                 11 
                 2 
               
               
                 0 
                 9 
                 1 
                 150 
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                 1 
                 6 
                 −7 
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                 11 
                 17 
                 1 
                 2 
                 2 
                 2 
                 403 
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                 −1 
                 9 
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                 175 
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                 2 
                 −1 
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                 3 
                 320 
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                 1 
                 9 
                 1 
                 80 
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                 −1 
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                 97 
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                 2 
                 3 
                 2 
                 2 
                 324 
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                 0 
                 9 
                 2 
                 65 
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                 1 
                 0 
                 −6 
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                 170 
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                 2 
               
               
                 2 
                 9 
                 1 
                 120 
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                 0 
                 −6 
                 2 
                 232 
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                 3 
                 4 
                 2 
                 2 
                 44 
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                 1 
                 1 
                 9 
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                 2 
                 1 
                 −6 
                 3 
                 383 
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                 4 
               
               
                 3 
                 9 
                 1 
                 85 
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                 2 
                 1 
                 −6 
                 2 
                 333 
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                 4 
                 5 
                 2 
                 2 
                 60 
                 57 
                 1 
                 2 
                 9 
                 2 
                 64 
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                 1 
                 2 
                 −6 
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                 47 
                 51 
                 1 
               
               
                 5 
                 9 
                 1 
                 75 
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                 −6 
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                 106 
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                 1 
                 6 
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                 119 
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                 1 
                 3 
                 9 
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                 90 
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                 1 
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                 −6 
                 3 
                 79 
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                 1 
               
               
                 −3 
                 10 
                 1 
                 26 
                 23 
                 3 
                 3 
                 −6 
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                 1 
                 7 
                 2 
                 2 
                 59 
                 55 
                 1 
                 −3 
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                 89 
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                 2 
                 4 
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                 186 
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                 2 
               
               
                 −2 
                 10 
                 1 
                 58 
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                 1 
                 4 
                 −6 
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                 150 
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                 1 
                 −7 
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                 2 
                 54 
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                 −2 
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                 35 
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                 1 
               
               
                 −1 
                 10 
                 1 
                 29 
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                 5 
                 −6 
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                 81 
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                 1 
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                 65 
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                 −1 
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                 59 
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                 1 
                 6 
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                 3 
                 43 
                 42 
                 2 
               
               
                 0 
                 10 
                 1 
                 100 
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                 2 
                 6 
                 −6 
                 2 
                 35 
                 33 
                 2 
                 −5 
                 3 
                 2 
                 47 
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                 1 
                 0 
                 10 
                 2 
                 14 
                 12 
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                 −1 
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                 381 
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                 1 
                 10 
                 1 
                 119 
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                 −1 
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                 2 
                 225 
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                 3 
                 −4 
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                 126 
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                 2 
                 1 
                 10 
                 2 
                 62 
                 63 
                 1 
                 0 
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                 3 
                 90 
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                 1 
               
               
                 2 
                 10 
                 1 
                 55 
                 53 
                 1 
                 0 
                 −5 
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                 107 
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                 1 
                 −3 
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                 2 
                 213 
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                 4 
                 2 
                 10 
                 2 
                 61 
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                 1 
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                 3 
                 202 
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                 3 
               
               
                 3 
                 10 
                 1 
                 8 
                 8 
                 7 
                 1 
                 −5 
                 2 
                 363 
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                 −2 
                 3 
                 2 
                 40 
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                 1 
                 3 
                 10 
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                 81 
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                 −5 
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                 175 
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                 2 
               
               
                 −3 
                 11 
                 1 
                 114 
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                 3 
                 2 
                 −5 
                 2 
                 68 
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                 1 
                 −1 
                 3 
                 2 
                 191 
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                 −3 
                 11 
                 2 
                 66 
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                 2 
                 3 
                 −5 
                 3 
                 43 
                 43 
                 1 
               
               
                 −2 
                 11 
                 1 
                 152 
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                 2 
                 3 
                 −5 
                 2 
                 101 
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                 1 
                 0 
                 3 
                 2 
                 115 
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                 1 
                 −2 
                 11 
                 2 
                 51 
                 48 
                 1 
                 4 
                 −5 
                 3 
                 119 
                 114 
                 1 
               
               
                 −1 
                 11 
                 1 
                 168 
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                 3 
                 4 
                 −5 
                 2 
                 51 
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                 1 
                 1 
                 3 
                 2 
                 307 
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                 −1 
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                 2 
                 56 
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                 1 
                 5 
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                 3 
                 115 
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                 2 
               
               
                 0 
                 11 
                 1 
                 72 
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                 1 
                 5 
                 −5 
                 2 
                 99 
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                 1 
                 2 
                 3 
                 2 
                 317 
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                 0 
                 11 
                 2 
                 56 
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                 1 
                 6 
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                 144 
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                 2 
               
               
                 1 
                 11 
                 1 
                 82 
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                 1 
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                 116 
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                 2 
                 3 
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                 2 
                 84 
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                 1 
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                 89 
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                 2 
                 11 
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                 −3 
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                 210 
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                 4 
                 3 
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                 11 
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                 3 
                 11 
                 1 
                 44 
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                 232 
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                 5 
                 3 
                 2 
                 57 
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                 1 
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                 25 
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                 −1 
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                 177 
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                 2 
               
               
                 −3 
                 12 
                 1 
                 47 
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                 2 
                 −1 
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                 178 
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                 2 
                 6 
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                 2 
                 68 
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                 −3 
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                 42 
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                 0 
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                 138 
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                 −2 
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                 1 
                 164 
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                 0 
                 −4 
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                 211 
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                 −7 
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                 47 
                 41 
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                 1 
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                 1 
               
               
                 −1 
                 12 
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                 1 
                 −4 
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                 53 
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                 0 
                 12 
                 1 
                 28 
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                 1 
                 2 
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                 314 
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                 −5 
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                 67 
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                 0 
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                 105 
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                 1 
                 12 
                 1 
                 47 
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                 −4 
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                 1 
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                 194 
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                 2 
                 12 
                 1 
                 90 
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                 4 
                 −4 
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                 195 
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                 −3 
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                 2 
                 145 
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                 2 
                 2 
                 12 
                 2 
                 55 
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                 5 
                 −4 
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                 28 
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                 1 
               
               
                 −2 
                 13 
                 1 
                 105 
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                 5 
                 −4 
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                 113 
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                 −2 
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                 230 
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                 −1 
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                 −4 
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                 52 
                 48 
                 1 
               
               
                 −1 
                 13 
                 1 
                 66 
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                 6 
                 −4 
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                 131 
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                 −1 
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                 102 
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                 0 
                 13 
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                 108 
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                 2 
                 7 
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                 3 
                 29 
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                 2 
               
               
                 0 
                 13 
                 1 
                 102 
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                 1 
                 7 
                 −4 
                 2 
                 28 
                 26 
                 2 
                 0 
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                 176 
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                 −1 
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                 −3 
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                 38 
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                 1 
                 13 
                 1 
                 41 
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                 2 
                 −3 
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                 197 
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                 4 
                 1 
                 4 
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                 0 
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                 34 
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                 −2 
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                 99 
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                 −1 
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                 2 
                 85 
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                 2 
                 −1 
                 −3 
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                 2 
                 4 
                 2 
                 338 
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                 3 
                 1 
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                 35 
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                 2 
                 −1 
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                 251 
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                 0 
                 −14 
                 2 
                 45 
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                 2 
                 0 
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                 69 
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                 1 
                 3 
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                 2 
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                 2 
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                 60 
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                 0 
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                 320 
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                 1 
                 −14 
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                 29 
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                 3 
                 1 
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                 73 
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                 4 
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                 2 
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                 31 
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                 2 
                 1 
                 −3 
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                 −2 
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                 −3 
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                 5 
                 4 
                 2 
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                 2 
                 2 
                 −3 
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                 88 
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                 1 
               
               
                 0 
                 −13 
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                 68 
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                 2 
                 3 
                 −3 
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                 107 
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                 1 
                 6 
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                 2 
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                 −1 
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                 20 
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                 3 
                 3 
                 −3 
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                 78 
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                 1 
               
               
                 1 
                 −13 
                 2 
                 41 
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                 3 
                 4 
                 −3 
                 2 
                 154 
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                 1 
                 −6 
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                 2 
                 29 
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                 2 
                 0 
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                 19 
                 22 
                 3 
                 4 
                 −3 
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                 124 
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                 1 
               
               
                 2 
                 −13 
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                 73 
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                 5 
                 −3 
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                 27 
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                 1 
                 −5 
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                 105 
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                 3 
                 2 
                 −13 
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                 44 
                 45 
                 3 
                 5 
                 −3 
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                 55 
                 57 
                 1 
               
               
                 3 
                 −13 
                 2 
                 54 
                 54 
                 1 
                 6 
                 −3 
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                 35 
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                 1 
                 −4 
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                 2 
                 142 
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                 2 
                 3 
                 −13 
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                 1 
                 6 
                 −3 
                 3 
                 51 
                 48 
                 1 
               
               
                 −3 
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                 2 
                 26 
                 25 
                 2 
                 7 
                 −3 
                 2 
                 58 
                 59 
                 2 
                 −3 
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                 2 
                 45 
                 47 
                 1 
                 −3 
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                 2 
                 7 
                 −3 
                 3 
                 8 
                 8 
                 6 
               
               
                 −2 
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                 97 
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                 −1 
                 −2 
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                 9 
                 −2 
                 5 
                 2 
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                 −2 
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                 3 
                 73 
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                 2 
                 −2 
                 −2 
                 3 
                 207 
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                 −1 
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                 38 
                 35 
                 2 
                 0 
                 −2 
                 2 
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                 −1 
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                 2 
                 29 
                 26 
                 1 
                 −1 
                 −12 
                 3 
                 50 
                 53 
                 2 
                 −1 
                 −2 
                 3 
                 174 
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                 2 
               
               
                 0 
                 −12 
                 2 
                 83 
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                 2 
                 1 
                 −2 
                 2 
                 430 
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                 0 
                 5 
                 2 
                 92 
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                 0 
                 −12 
                 3 
                 45 
                 47 
                 2 
                 0 
                 −2 
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                 144 
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                 2 
               
               
                 2 
                 −12 
                 2 
                 103 
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                 2 
                 2 
                 −2 
                 2 
                 224 
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                 2 
                 1 
                 5 
                 2 
                 275 
                 268 
                 2 
                 1 
                 −12 
                 3 
                 63 
                 62 
                 2 
                 1 
                 −2 
                 3 
                 446 
                 467 
                 4 
               
               
                 3 
                 −12 
                 2 
                 65 
                 64 
                 1 
                 3 
                 −2 
                 2 
                 112 
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                 1 
                 2 
                 5 
                 2 
                 100 
                 92 
                 1 
                 2 
                 −12 
                 3 
                 92 
                 93 
                 2 
                 2 
                 −2 
                 3 
                 156 
                 155 
                 1 
               
               
                 4 
                 −12 
                 2 
                 53 
                 52 
                 1 
                 4 
                 −2 
                 2 
                 53 
                 50 
                 1 
                 3 
                 5 
                 2 
                 57 
                 56 
                 1 
                 3 
                 −12 
                 3 
                 26 
                 25 
                 2 
                 3 
                 −2 
                 3 
                 6 
                 4 
                 3 
               
               
                 −4 
                 −11 
                 2 
                 53 
                 54 
                 2 
                 5 
                 −2 
                 2 
                 106 
                 99 
                 1 
                 4 
                 5 
                 2 
                 90 
                 86 
                 1 
                 4 
                 −12 
                 3 
                 56 
                 52 
                 2 
                 4 
                 −2 
                 3 
                 48 
                 52 
                 1 
               
               
                 −3 
                 −11 
                 2 
                 74 
                 75 
                 2 
                 6 
                 −2 
                 2 
                 115 
                 119 
                 2 
                 5 
                 5 
                 2 
                 78 
                 83 
                 1 
                 −3 
                 −11 
                 3 
                 172 
                 179 
                 4 
                 5 
                 −2 
                 3 
                 154 
                 154 
                 2 
               
               
                 −2 
                 −11 
                 2 
                 106 
                 104 
                 2 
                 7 
                 −2 
                 2 
                 29 
                 28 
                 2 
                 6 
                 5 
                 2 
                 30 
                 29 
                 1 
                 −2 
                 −11 
                 3 
                 116 
                 113 
                 3 
                 6 
                 −2 
                 3 
                 128 
                 129 
                 2 
               
               
                 −1 
                 −11 
                 2 
                 93 
                 109 
                 3 
                 −1 
                 −1 
                 2 
                 223 
                 236 
                 4 
                 −6 
                 6 
                 2 
                 58 
                 57 
                 2 
                 −1 
                 −11 
                 3 
                 73 
                 77 
                 2 
                 7 
                 −2 
                 3 
                 66 
                 70 
                 2 
               
               
                 0 
                 −11 
                 2 
                 95 
                 104 
                 3 
                 0 
                 −1 
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                 2 
                 −3 
                 0 
                 13 
                 60 
                 75 
                 2 
                 4 
                 −6 
                 14 
                 119 
                 115 
                 3 
               
               
                 −3 
                 −12 
                 12 
                 27 
                 24 
                 2 
                 0 
                 −2 
                 12 
                 47 
                 46 
                 1 
                 3 
                 −10 
                 13 
                 26 
                 26 
                 3 
                 −2 
                 0 
                 13 
                 14 
                 20 
                 5 
                 −4 
                 −5 
                 14 
                 63 
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                 2 
               
               
                 −2 
                 −12 
                 12 
                 67 
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                 2 
                 1 
                 −2 
                 12 
                 104 
                 105 
                 1 
                 −3 
                 −9 
                 13 
                 45 
                 43 
                 2 
                 −1 
                 0 
                 13 
                 159 
                 153 
                 4 
                 −3 
                 −5 
                 14 
                 76 
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                 2 
               
               
                 −1 
                 −12 
                 12 
                 17 
                 15 
                 4 
                 2 
                 −2 
                 12 
                 139 
                 140 
                 1 
                 −2 
                 −9 
                 13 
                 138 
                 141 
                 3 
                 0 
                 0 
                 13 
                 37 
                 39 
                 3 
                 −2 
                 −5 
                 14 
                 154 
                 173 
                 4 
               
               
                 0 
                 −12 
                 12 
                 62 
                 61 
                 2 
                 3 
                 −2 
                 12 
                 37 
                 41 
                 1 
                 −1 
                 −9 
                 13 
                 55 
                 62 
                 2 
                 1 
                 0 
                 13 
                 28 
                 30 
                 2 
                 1 
                 −5 
                 14 
                 60 
                 54 
                 3 
               
               
                 −3 
                 −11 
                 12 
                 72 
                 67 
                 2 
                 4 
                 −2 
                 12 
                 42 
                 40 
                 1 
                 0 
                 −9 
                 13 
                 98 
                 99 
                 3 
                 2 
                 0 
                 13 
                 116 
                 121 
                 1 
                 2 
                 −5 
                 14 
                 46 
                 51 
                 3 
               
               
                 −2 
                 −11 
                 12 
                 60 
                 63 
                 2 
                 5 
                 −2 
                 12 
                 95 
                 91 
                 2 
                 1 
                 −9 
                 13 
                 31 
                 26 
                 2 
                 3 
                 0 
                 13 
                 75 
                 72 
                 1 
                 3 
                 −5 
                 14 
                 98 
                 100 
                 3 
               
               
                 −1 
                 −11 
                 12 
                 40 
                 46 
                 2 
                 −5 
                 −1 
                 12 
                 88 
                 88 
                 2 
                 2 
                 −9 
                 13 
                 139 
                 144 
                 4 
                 4 
                 0 
                 13 
                 21 
                 18 
                 1 
                 4 
                 −5 
                 14 
                 25 
                 24 
                 2 
               
               
                 −5 
                 −4 
                 14 
                 49 
                 49 
                 2 
                 3 
                 1 
                 14 
                 8 
                 8 
                 8 
                 3 
                 −6 
                 15 
                 52 
                 50 
                 2 
                 0 
                 3 
                 15 
                 113 
                 106 
                 3 
                 −3 
                 −2 
                 16 
                 108 
                 102 
                 2 
               
               
                 −4 
                 −4 
                 14 
                 64 
                 65 
                 2 
                 −4 
                 2 
                 14 
                 92 
                 85 
                 2 
                 −4 
                 −5 
                 15 
                 86 
                 85 
                 2 
                 1 
                 3 
                 15 
                 65 
                 58 
                 2 
                 −2 
                 −2 
                 16 
                 66 
                 63 
                 2 
               
               
                 −2 
                 −4 
                 14 
                 110 
                 123 
                 3 
                 −3 
                 2 
                 14 
                 44 
                 41 
                 2 
                 −3 
                 −5 
                 15 
                 125 
                 120 
                 3 
                 −2 
                 −11 
                 16 
                 85 
                 85 
                 2 
                 −1 
                 −2 
                 16 
                 65 
                 64 
                 2 
               
               
                 −1 
                 −4 
                 14 
                 126 
                 138 
                 3 
                 −2 
                 2 
                 14 
                 30 
                 35 
                 2 
                 −1 
                 −5 
                 15 
                 107 
                 107 
                 3 
                 −1 
                 −11 
                 16 
                 45 
                 44 
                 2 
                 0 
                 −2 
                 16 
                 99 
                 101 
                 3 
               
               
                 0 
                 −4 
                 14 
                 331 
                 325 
                 8 
                 −1 
                 2 
                 14 
                 42 
                 41 
                 3 
                 1 
                 −5 
                 15 
                 179 
                 181 
                 4 
                 −2 
                 −10 
                 16 
                 123 
                 121 
                 3 
                 1 
                 −2 
                 16 
                 87 
                 83 
                 2 
               
               
                 1 
                 −4 
                 14 
                 186 
                 190 
                 4 
                 0 
                 2 
                 14 
                 38 
                 43 
                 3 
                 2 
                 −5 
                 15 
                 23 
                 25 
                 4 
                 −1 
                 −10 
                 16 
                 124 
                 116 
                 2 
                 2 
                 −2 
                 16 
                 26 
                 23 
                 3 
               
               
                 2 
                 −4 
                 14 
                 69 
                 63 
                 2 
                 1 
                 2 
                 14 
                 35 
                 35 
                 2 
                 3 
                 −5 
                 15 
                 39 
                 39 
                 2 
                 0 
                 −10 
                 16 
                 21 
                 17 
                 3 
                 3 
                 −2 
                 16 
                 34 
                 35 
                 2 
               
               
                 3 
                 −4 
                 14 
                 41 
                 40 
                 2 
                 2 
                 2 
                 14 
                 38 
                 37 
                 1 
                 −4 
                 −4 
                 15 
                 46 
                 43 
                 2 
                 −3 
                 −9 
                 16 
                 55 
                 58 
                 2 
                 −3 
                 −1 
                 16 
                 44 
                 44 
                 2 
               
               
                 4 
                 −4 
                 14 
                 80 
                 77 
                 1 
                 −1 
                 3 
                 14 
                 34 
                 29 
                 3 
                 −3 
                 −4 
                 15 
                 71 
                 73 
                 2 
                 −2 
                 −9 
                 16 
                 69 
                 65 
                 2 
                 −2 
                 −1 
                 16 
                 39 
                 40 
                 2 
               
               
                 −5 
                 −3 
                 14 
                 10 
                 15 
                 10 
                 0 
                 3 
                 14 
                 22 
                 18 
                 3 
                 −1 
                 −4 
                 15 
                 87 
                 87 
                 2 
                 −1 
                 −9 
                 16 
                 42 
                 37 
                 2 
                 0 
                 −1 
                 16 
                 130 
                 127 
                 3 
               
               
                 −4 
                 −3 
                 14 
                 58 
                 56 
                 2 
                 1 
                 3 
                 14 
                 64 
                 61 
                 1 
                 0 
                 −4 
                 15 
                 46 
                 44 
                 2 
                 0 
                 −9 
                 16 
                 36 
                 31 
                 2 
                 1 
                 −1 
                 16 
                 49 
                 45 
                 2 
               
               
                 −3 
                 −3 
                 14 
                 196 
                 197 
                 4 
                 2 
                 3 
                 14 
                 61 
                 54 
                 1 
                 2 
                 −4 
                 15 
                 41 
                 42 
                 2 
                 −3 
                 −8 
                 16 
                 53 
                 44 
                 2 
                 2 
                 −1 
                 16 
                 73 
                 69 
                 2 
               
               
                 −1 
                 −3 
                 14 
                 121 
                 125 
                 3 
                 −1 
                 4 
                 14 
                 80 
                 82 
                 2 
                 3 
                 −4 
                 15 
                 57 
                 54 
                 2 
                 −2 
                 −8 
                 16 
                 62 
                 61 
                 2 
                 0 
                 0 
                 16 
                 128 
                 125 
                 3 
               
               
                 0 
                 −3 
                 14 
                 238 
                 244 
                 5 
                 0 
                 4 
                 14 
                 41 
                 38 
                 1 
                 −4 
                 −3 
                 15 
                 54 
                 53 
                 2 
                 −1 
                 −8 
                 16 
                 20 
                 22 
                 3 
                 1 
                 0 
                 16 
                 94 
                 91 
                 2 
               
               
                 1 
                 −3 
                 14 
                 228 
                 227 
                 5 
                 1 
                 4 
                 14 
                 16 
                 12 
                 3 
                 −3 
                 −3 
                 15 
                 9 
                 13 
                 8 
                 0 
                 −8 
                 16 
                 61 
                 57 
                 2 
                 0 
                 1 
                 16 
                 59 
                 59 
                 2 
               
               
                 2 
                 −3 
                 14 
                 145 
                 149 
                 6 
                 0 
                 5 
                 14 
                 39 
                 49 
                 2 
                 −2 
                 −3 
                 15 
                 106 
                 121 
                 3 
                 2 
                 −8 
                 16 
                 67 
                 64 
                 2 
                 1 
                 1 
                 16 
                 17 
                 21 
                 3 
               
               
                 3 
                 −3 
                 14 
                 19 
                 18 
                 3 
                 −1 
                 −12 
                 15 
                 74 
                 67 
                 2 
                 −1 
                 −3 
                 15 
                 199 
                 198 
                 5 
                 −4 
                 −7 
                 16 
                 59 
                 59 
                 2 
                 0 
                 2 
                 16 
                 38 
                 37 
                 2 
               
               
                 4 
                 −3 
                 14 
                 69 
                 67 
                 2 
                 −2 
                 −11 
                 15 
                 30 
                 27 
                 2 
                 1 
                 −3 
                 15 
                 62 
                 58 
                 2 
                 −3 
                 −7 
                 16 
                 38 
                 35 
                 2 
                 −1 
                 −10 
                 17 
                 26 
                 20 
                 2 
               
               
                 −5 
                 −2 
                 14 
                 22 
                 21 
                 3 
                 −1 
                 −11 
                 15 
                 95 
                 87 
                 2 
                 2 
                 −3 
                 15 
                 83 
                 75 
                 2 
                 −2 
                 −7 
                 16 
                 93 
                 86 
                 2 
                 −2 
                 −9 
                 17 
                 68 
                 64 
                 2 
               
               
                 −4 
                 −2 
                 14 
                 20 
                 16 
                 3 
                 0 
                 −11 
                 15 
                 41 
                 37 
                 2 
                 3 
                 −3 
                 15 
                 84 
                 81 
                 2 
                 −1 
                 −7 
                 16 
                 107 
                 106 
                 2 
                 −1 
                 −9 
                 17 
                 49 
                 49 
                 2 
               
               
                 −3 
                 −2 
                 14 
                 69 
                 76 
                 2 
                 −3 
                 −10 
                 15 
                 105 
                 100 
                 2 
                 −4 
                 −2 
                 15 
                 59 
                 55 
                 2 
                 0 
                 −7 
                 16 
                 30 
                 33 
                 2 
                 −3 
                 −8 
                 17 
                 18 
                 18 
                 3 
               
               
                 −1 
                 −2 
                 14 
                 91 
                 88 
                 2 
                 −2 
                 −10 
                 15 
                 61 
                 62 
                 2 
                 −3 
                 −2 
                 15 
                 39 
                 39 
                 2 
                 2 
                 −7 
                 16 
                 23 
                 25 
                 3 
                 −2 
                 −8 
                 17 
                 30 
                 30 
                 2 
               
               
                 0 
                 −2 
                 14 
                 226 
                 229 
                 4 
                 −1 
                 −10 
                 15 
                 49 
                 46 
                 2 
                 −2 
                 −2 
                 15 
                 72 
                 75 
                 2 
                 3 
                 −7 
                 16 
                 74 
                 76 
                 2 
                 −1 
                 −8 
                 17 
                 76 
                 75 
                 2 
               
               
                 1 
                 −2 
                 14 
                 95 
                 93 
                 2 
                 0 
                 −10 
                 15 
                 57 
                 56 
                 2 
                 −1 
                 −2 
                 15 
                 87 
                 83 
                 2 
                 −4 
                 −6 
                 16 
                 58 
                 62 
                 2 
                 −3 
                 −7 
                 17 
                 14 
                 16 
                 4 
               
               
                 2 
                 −2 
                 14 
                 103 
                 108 
                 1 
                 2 
                 −10 
                 15 
                 60 
                 60 
                 2 
                 0 
                 −2 
                 15 
                 51 
                 47 
                 2 
                 −3 
                 −6 
                 16 
                 34 
                 34 
                 2 
                 −2 
                 −7 
                 17 
                 29 
                 30 
                 2 
               
               
                 3 
                 −2 
                 14 
                 46 
                 44 
                 1 
                 −3 
                 −9 
                 15 
                 54 
                 52 
                 2 
                 1 
                 −2 
                 15 
                 76 
                 74 
                 2 
                 −2 
                 −6 
                 16 
                 18 
                 14 
                 3 
                 −1 
                 −7 
                 17 
                 17 
                 17 
                 3 
               
               
                 4 
                 −2 
                 14 
                 43 
                 46 
                 1 
                 −2 
                 −9 
                 15 
                 112 
                 107 
                 3 
                 3 
                 −2 
                 15 
                 56 
                 54 
                 2 
                 −1 
                 −6 
                 16 
                 92 
                 90 
                 2 
                 −3 
                 −6 
                 17 
                 24 
                 19 
                 2 
               
               
                 −5 
                 −1 
                 14 
                 25 
                 24 
                 2 
                 −1 
                 −9 
                 15 
                 55 
                 56 
                 2 
                 −4 
                 −1 
                 15 
                 29 
                 28 
                 2 
                 0 
                 −6 
                 16 
                 120 
                 118 
                 3 
                 −2 
                 −6 
                 17 
                 69 
                 68 
                 2 
               
               
                 −4 
                 −1 
                 14 
                 11 
                 19 
                 10 
                 0 
                 −9 
                 15 
                 65 
                 60 
                 2 
                 −3 
                 −1 
                 15 
                 73 
                 75 
                 2 
                 1 
                 −6 
                 16 
                 42 
                 42 
                 3 
                 −1 
                 −6 
                 17 
                 104 
                 108 
                 2 
               
               
                 −3 
                 −1 
                 14 
                 109 
                 116 
                 3 
                 2 
                 −9 
                 15 
                 34 
                 37 
                 3 
                 −2 
                 −1 
                 15 
                 96 
                 96 
                 2 
                 2 
                 −6 
                 16 
                 89 
                 87 
                 2 
                 2 
                 −6 
                 17 
                 78 
                 78 
                 2 
               
               
                 −2 
                 −1 
                 14 
                 95 
                 101 
                 2 
                 3 
                 −9 
                 15 
                 43 
                 43 
                 2 
                 −1 
                 −1 
                 15 
                 71 
                 69 
                 2 
                 3 
                 −6 
                 16 
                 42 
                 41 
                 2 
                 −3 
                 −5 
                 17 
                 19 
                 17 
                 3 
               
               
                 −1 
                 −1 
                 14 
                 7 
                 7 
                 6 
                 −4 
                 −8 
                 15 
                 107 
                 102 
                 2 
                 0 
                 −1 
                 15 
                 40 
                 38 
                 3 
                 −4 
                 −5 
                 16 
                 52 
                 53 
                 2 
                 −2 
                 −5 
                 17 
                 37 
                 34 
                 2 
               
               
                 0 
                 −1 
                 14 
                 50 
                 51 
                 3 
                 −3 
                 −8 
                 15 
                 91 
                 86 
                 2 
                 1 
                 −1 
                 15 
                 92 
                 98 
                 2 
                 −3 
                 −5 
                 16 
                 87 
                 88 
                 2 
                 −1 
                 −5 
                 17 
                 59 
                 60 
                 2 
               
               
                 1 
                 −1 
                 14 
                 69 
                 72 
                 1 
                 −2 
                 −8 
                 15 
                 82 
                 78 
                 2 
                 2 
                 −1 
                 15 
                 64 
                 64 
                 1 
                 −2 
                 −5 
                 16 
                 57 
                 56 
                 2 
                 1 
                 −5 
                 17 
                 37 
                 36 
                 3 
               
               
                 2 
                 −1 
                 14 
                 57 
                 60 
                 1 
                 −1 
                 −8 
                 15 
                 33 
                 27 
                 2 
                 3 
                 −1 
                 15 
                 34 
                 33 
                 2 
                 −1 
                 −5 
                 16 
                 46 
                 46 
                 2 
                 2 
                 −5 
                 17 
                 43 
                 39 
                 2 
               
               
                 3 
                 −1 
                 14 
                 26 
                 24 
                 2 
                 0 
                 −8 
                 15 
                 122 
                 122 
                 3 
                 −4 
                 0 
                 15 
                 0 
                 9 
                 1 
                 1 
                 −5 
                 16 
                 96 
                 96 
                 3 
                 −3 
                 −4 
                 17 
                 10 
                 9 
                 9 
               
               
                 4 
                 −1 
                 14 
                 20 
                 27 
                 2 
                 2 
                 −8 
                 15 
                 42 
                 44 
                 2 
                 −3 
                 0 
                 15 
                 32 
                 28 
                 2 
                 2 
                 −5 
                 16 
                 26 
                 20 
                 3 
                 −2 
                 −4 
                 17 
                 52 
                 51 
                 2 
               
               
                 −5 
                 0 
                 14 
                 74 
                 67 
                 2 
                 3 
                 −8 
                 15 
                 89 
                 85 
                 2 
                 −2 
                 0 
                 15 
                 127 
                 131 
                 3 
                 3 
                 −5 
                 16 
                 40 
                 35 
                 2 
                 −1 
                 −4 
                 17 
                 17 
                 16 
                 4 
               
               
                 −4 
                 0 
                 14 
                 68 
                 66 
                 2 
                 −4 
                 −7 
                 15 
                 40 
                 40 
                 2 
                 0 
                 0 
                 15 
                 26 
                 26 
                 3 
                 −4 
                 −4 
                 16 
                 23 
                 26 
                 3 
                 1 
                 −4 
                 17 
                 48 
                 46 
                 2 
               
               
                 −3 
                 0 
                 14 
                 111 
                 111 
                 3 
                 −3 
                 −7 
                 15 
                 67 
                 69 
                 2 
                 1 
                 0 
                 15 
                 10 
                 7 
                 9 
                 −3 
                 −4 
                 16 
                 56 
                 56 
                 2 
                 2 
                 −4 
                 17 
                 50 
                 51 
                 2 
               
               
                 −2 
                 0 
                 14 
                 98 
                 101 
                 2 
                 −2 
                 −7 
                 15 
                 58 
                 58 
                 2 
                 2 
                 0 
                 15 
                 55 
                 56 
                 1 
                 −2 
                 −4 
                 16 
                 21 
                 22 
                 3 
                 −3 
                 −3 
                 17 
                 32 
                 34 
                 2 
               
               
                 −1 
                 0 
                 14 
                 46 
                 46 
                 2 
                 −1 
                 −7 
                 15 
                 50 
                 52 
                 2 
                 3 
                 0 
                 15 
                 34 
                 40 
                 2 
                 −1 
                 −4 
                 16 
                 98 
                 96 
                 2 
                 −2 
                 −3 
                 17 
                 13 
                 7 
                 6 
               
               
                 0 
                 0 
                 14 
                 87 
                 86 
                 2 
                 0 
                 −7 
                 15 
                 55 
                 54 
                 2 
                 −4 
                 1 
                 15 
                 23 
                 27 
                 3 
                 1 
                 −4 
                 16 
                 46 
                 43 
                 2 
                 1 
                 −3 
                 17 
                 40 
                 35 
                 2 
               
               
                 1 
                 0 
                 14 
                 64 
                 63 
                 1 
                 2 
                 −7 
                 15 
                 128 
                 127 
                 3 
                 −2 
                 1 
                 15 
                 7 
                 11 
                 6 
                 2 
                 −4 
                 16 
                 37 
                 31 
                 2 
                 2 
                 −3 
                 17 
                 49 
                 48 
                 2 
               
               
                 2 
                 0 
                 14 
                 125 
                 128 
                 2 
                 3 
                 −7 
                 15 
                 35 
                 31 
                 2 
                 0 
                 1 
                 15 
                 37 
                 36 
                 3 
                 3 
                 −4 
                 16 
                 0 
                 10 
                 1 
                 −2 
                 −2 
                 17 
                 50 
                 49 
                 2 
               
               
                 3 
                 0 
                 14 
                 11 
                 10 
                 6 
                 −4 
                 −6 
                 15 
                 110 
                 107 
                 2 
                 1 
                 1 
                 15 
                 72 
                 65 
                 1 
                 −4 
                 −3 
                 16 
                 72 
                 71 
                 2 
                 2 
                 −2 
                 17 
                 63 
                 61 
                 2 
               
               
                 −4 
                 1 
                 14 
                 57 
                 52 
                 2 
                 −3 
                 −6 
                 15 
                 86 
                 84 
                 2 
                 2 
                 1 
                 15 
                 45 
                 47 
                 1 
                 −3 
                 −3 
                 16 
                 15 
                 14 
                 5 
                 0 
                 0 
                 17 
                 30 
                 35 
                 3 
               
               
                 −3 
                 1 
                 14 
                 43 
                 42 
                 2 
                 −2 
                 −6 
                 15 
                 38 
                 42 
                 2 
                 −1 
                 2 
                 15 
                 50 
                 51 
                 2 
                 −2 
                 −3 
                 16 
                 35 
                 32 
                 2 
                 −2 
                 −6 
                 18 
                 12 
                 11 
                 6 
               
               
                 −2 
                 1 
                 14 
                 114 
                 117 
                 3 
                 −1 
                 −6 
                 15 
                 27 
                 24 
                 2 
                 0 
                 2 
                 15 
                 110 
                 103 
                 3 
                 −1 
                 −3 
                 16 
                 51 
                 51 
                 2 
               
               
                 0 
                 1 
                 14 
                 55 
                 53 
                 2 
                 0 
                 −6 
                 15 
                 158 
                 158 
                 4 
                 1 
                 2 
                 15 
                 58 
                 60 
                 1 
                 2 
                 −3 
                 16 
                 59 
                 60 
                 2 
               
               
                 1 
                 1 
                 14 
                 69 
                 69 
                 1 
                 1 
                 −6 
                 15 
                 66 
                 68 
                 2 
                 2 
                 2 
                 15 
                 21 
                 21 
                 2 
                 3 
                 −3 
                 16 
                 26 
                 29 
                 3 
               
               
                 2 
                 1 
                 14 
                 85 
                 82 
                 1 
                 2 
                 −6 
                 15 
                 46 
                 52 
                 2 
                 −1 
                 3 
                 15 
                 48 
                 48 
                 2 
                 −4 
                 −2 
                 16 
                 28 
                 28 
                 2 
               
               
                   
               
             
          
         
       
     
     EXAMPLE 3 
     Synthesis of NEL 
     The preparation of NEL having the basic structure I can be accomplished by a common general method, i.e. the condensation of a bicyclic Windaus-Grundmann type ketone II with the allylic phosphine oxide III to the corresponding 2-methylene-19-nor-vitamin D analog IV followed by deprotection at C-1, C-3 and C-25 in the latter compound IV to obtain compound I, i.e. NEL. 
     
       
                 
         
             
             
         
      
     
     In ketone II, Y 4  is preferably a hydroxy-protecting group such as a silyl protecting group. The t-butyldimethyl-silyl (TBDMS) group is an example of a particularly useful hydroxy-protecting group. In phosphine oxide III, 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. 
     Phosphine oxide III 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. 
     The overall process of the synthesis of compound I 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. Pat. No. 7,528,122 entitled “Vitamin D Analog—NEL, Methods and Uses Thereof,” the specifications of which are specifically incorporated herein by reference.