Direct Observation of Oxygen Rebound with an Iron-Hydroxide Complex.
Zaragoza, Jan Paulo T.; Yosca, Timothy H.; Siegler, Maxime A.; Moënne-Loccoz, Pierre; Green, Michael T.; Goldberg, David P.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b07979

data_4126431
_publ_section_title
;
 Direct Observation of Oxygen Rebound with an Iron-Hydroxide Complex.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b07979
_journal_year                    2017
_chemical_formula_moiety         'C91 H60 Fe N4 O, C5 H12'
_chemical_formula_sum            'C96 H72 Fe N4 O'
_chemical_formula_weight         1353.42
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                94.8964(19)
_cell_angle_beta                 105.1209(19)
_cell_angle_gamma                109.266(2)
_cell_formula_units_Z            2
_cell_length_a                   14.1155(3)
_cell_length_b                   15.7239(4)
_cell_length_c                   21.2585(5)
_cell_measurement_reflns_used    14718
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      71.99
_cell_measurement_theta_min      3.35
_cell_volume                     4223.13(19)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL v6.10 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_av_unetI/netI     0.1051
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            51658
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.888
_diffrn_reflns_theta_min         3.031
_exptl_absorpt_coefficient_mu    1.784
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.05436
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.064
_exptl_crystal_description       'small irregular block'
_exptl_crystal_F_000             1420
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.552
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.853
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1154
_refine_ls_number_reflns         23950
_refine_ls_number_restraints     777
_refine_ls_restrained_S_all      0.859
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0568
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0655P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1341
_refine_ls_wR_factor_ref         0.1447
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13198
_reflns_number_total             23950
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b07979_si_003.cif
_cod_data_source_block           2
_cod_original_cell_volume        4223.12(18)
_cod_database_code               4126431
_shelx_shelxl_version_number     2014/7
_twin_information
;

 * * * CRYSALIS TWIN DATA REDUCTION FINALIZING (38.43 (release 21-03-2016)) * * *
Laue class: 1bar - Friedel mate is equivalent
Lattice type: P-lattice 
DC PROFFITRRPTWIN INFO: Step 1 - Loading orientation matrices (UB) of 4 components
 
DC PROFFITRRPTWIN INFO: Loading UB component 1
 
DC PROFFITRRPTWIN INFO: Loading UB component 2
 
DC PROFFITRRPTWIN INFO: Loading UB component 3
 
DC PROFFITRRPTWIN INFO: Loading UB component 4
 
DC PROFFITRRPTWIN INFO: Step 2 - Computing crossed twin laws
 
Twin law determination (relative to component 1)
Matrix 1 is taken from component 1 (  14.116   15.724   21.249    94.93   105.10   109.30)
Matrix 2 is taken from component 2 (  14.094   15.715   21.243    94.82   105.21   109.28)
Twin analysis: Component 1 with component 2
TL  =UB[1]-1*UB[2]:   0.9637   0.0020  -0.0801     0.0042   1.0054   0.0542     0.1648  -0.0484   1.0183   det 1.002491
TL-1=UB[2]*UB[1]-1:   1.0239   0.0018   0.0805     0.0047   0.9921  -0.0525    -0.1655   0.0469   0.9665   det 0.997515
Rot= 7.0880 deg around the following vectors: 
Reciprocal space (hkl): -0.2909 -0.9508 0.1063
Direct space (uvw)    : -0.5783 -0.8079 -0.1133
Matrix 2 is taken from component 3 (  14.128   15.702   21.254    94.80   105.34   109.20)
Twin analysis: Component 1 with component 3
TL  =UB[1]-1*UB[3]:   0.9989   0.0307  -0.0252    -0.0184   0.9989   0.0559     0.0326  -0.1012   0.9956   det 1.000537
TL-1=UB[3]*UB[1]-1:   0.9997  -0.0280   0.0269     0.0201   0.9949  -0.0554    -0.0307   0.1021   0.9979   det 0.999463
Rot= 4.9114 deg around the following vectors: 
Reciprocal space (hkl): -0.9112 -0.2812 -0.3012
Direct space (uvw)    : -0.8611 -0.4347 -0.2638
Matrix 2 is taken from component 4 (  14.175   15.679   21.284    94.46   105.49   109.56)
Twin analysis: Component 1 with component 4
TL  =UB[1]-1*UB[4]:   0.9875   0.0154  -0.0316    -0.0119   1.0009   0.0215     0.0740  -0.0305   1.0080   det 0.999491
TL-1=UB[4]*UB[1]-1:   1.0101  -0.0145   0.0320     0.0136   0.9982  -0.0209    -0.0737   0.0312   0.9891   det 1.000509
Rot= 3.4387 deg around the following vectors: 
Reciprocal space (hkl): -0.3549 -0.9150 -0.1918
Direct space (uvw)    : -0.6227 -0.7516 -0.2177
Twin law determination (relative to component 2)
Matrix 1 is taken from component 2 (  14.094   15.715   21.243    94.82   105.21   109.28)
Matrix 2 is taken from component 3 (  14.128   15.702   21.254    94.80   105.34   109.20)
Twin analysis: Component 2 with component 3
TL  =UB[2]-1*UB[3]:   1.0253   0.0250   0.0544    -0.0152   0.9965   0.0031    -0.1346  -0.0561   0.9691   det 0.998051
TL-1=UB[3]*UB[2]-1:   0.9678  -0.0274  -0.0542     0.0144   1.0029  -0.0041     0.1353   0.0542   1.0242   det 1.001953
Rot= 4.7674 deg around the following vectors: 
Reciprocal space (hkl): -0.3143 0.9067 -0.2812
Direct space (uvw)    : -0.1419 0.9799 -0.1400
Matrix 2 is taken from component 4 (  14.175   15.679   21.284    94.46   105.49   109.56)
Twin analysis: Component 2 with component 4
TL  =UB[2]-1*UB[4]:   1.0170   0.0151   0.0488    -0.0111   0.9947  -0.0317    -0.0925   0.0150   0.9804   det 0.997008
TL-1=UB[4]*UB[2]-1:   0.9787  -0.0141  -0.0491     0.0138   1.0046   0.0318     0.0921  -0.0167   1.0148   det 1.003001
Rot= 3.7828 deg around the following vectors: 
Reciprocal space (hkl): 0.2123 0.9221 -0.3234
Direct space (uvw)    : 0.5187 0.8549 0.0090
Twin law determination (relative to component 3)
Matrix 1 is taken from component 3 (  14.128   15.702   21.254    94.80   105.34   109.20)
Matrix 2 is taken from component 4 (  14.175   15.679   21.284    94.46   105.49   109.56)
Twin analysis: Component 3 with component 4
TL  =UB[3]-1*UB[4]:   0.9895  -0.0134  -0.0051     0.0039   0.9978  -0.0351     0.0423   0.0713   1.0090   det 0.998955
TL-1=UB[4]*UB[3]-1:   1.0103   0.0132   0.0056    -0.0054   0.9997   0.0347    -0.0420  -0.0712   0.9884   det 1.001046
Rot= 2.8477 deg around the following vectors: 
Reciprocal space (hkl): 0.8371 -0.5227 0.1615
Direct space (uvw)    : 0.9590 -0.1548 0.2375
 
DC PROFFITRRPTWIN INFO: Step 3 - Loading reflections of 4 components
 
DC PROFFITRRPTWIN ALL INFO: Component 1
DC PROFFITRRPTWIN ALL INFO: Component 2
DC PROFFITRRPTWIN ALL INFO: Component 3
DC PROFFITRRPTWIN ALL INFO: Component 4
 
DC PROFFITRRPTWIN INFO: Step 4 - Analysing composite reflections of 4 components
 
Component 1: 53559 observations read
Component 2: 53618 observations read
Component 3: 53081 observations read
Component 4: 53545 observations read

119585 composite observations collected (86124 fully isolated, 33461 overlapped), 755 skipped due to one or more missing parts and 3 skipped due to I/sig<-3.0

OVERLAP STATISTICS

2 COMPONENTS

COMPONENTS 1, 2
 Overlap factor | # in range | % of all obs 
 -------------- | ---------- | ------------ 
   0.00 - 0.20  |         99 |     0.1 <--- ALMOST SEPARATED
   0.20 - 0.40  |         49 |     0.0
   0.40 - 0.60  |         27 |     0.0
   0.60 - 0.80  |          9 |     0.0
   0.80 - 1.00  |          0 |     0.0 <--- FULLY OVERLAPPED
 -------------- | ---------- | ------------ 
      Total     |        184 |     0.2

COMPONENTS 1, 3
 Overlap factor | # in range | % of all obs 
 -------------- | ---------- | ------------ 
   0.00 - 0.20  |         56 |     0.0 <--- ALMOST SEPARATED
   0.20 - 0.40  |         16 |     0.0
   0.40 - 0.60  |          5 |     0.0
   0.60 - 0.80  |          7 |     0.0
   0.80 - 1.00  |          0 |     0.0 <--- FULLY OVERLAPPED
 -------------- | ---------- | ------------ 
      Total     |         84 |     0.1

COMPONENTS 2, 3
 Overlap factor | # in range | % of all obs 
 -------------- | ---------- | ------------ 
   0.00 - 0.20  |        189 |     0.2 <--- ALMOST SEPARATED
   0.20 - 0.40  |         93 |     0.1
   0.40 - 0.60  |         51 |     0.0
   0.60 - 0.80  |         13 |     0.0
   0.80 - 1.00  |         33 |     0.0 <--- FULLY OVERLAPPED
 -------------- | ---------- | ------------ 
      Total     |        379 |     0.3

COMPONENTS 1, 4
 Overlap factor | # in range | % of all obs 
 -------------- | ---------- | ------------ 
   0.00 - 0.20  |        185 |     0.2 <--- ALMOST SEPARATED
   0.20 - 0.40  |         37 |     0.0
   0.40 - 0.60  |         33 |     0.0
   0.60 - 0.80  |         16 |     0.0
   0.80 - 1.00  |          8 |     0.0 <--- FULLY OVERLAPPED
 -------------- | ---------- | ------------ 
      Total     |        279 |     0.2

COMPONENTS 2, 4
 Overlap factor | # in range | % of all obs 
 -------------- | ---------- | ------------ 
   0.00 - 0.20  |         73 |     0.1 <--- ALMOST SEPARATED
   0.20 - 0.40  |         52 |     0.0
   0.40 - 0.60  |         20 |     0.0
   0.60 - 0.80  |          9 |     0.0
   0.80 - 1.00  |          0 |     0.0 <--- FULLY OVERLAPPED
 -------------- | ---------- | ------------ 
      Total     |        154 |     0.1

COMPONENTS 3, 4
 Overlap factor | # in range | % of all obs 
 -------------- | ---------- | ------------ 
   0.00 - 0.20  |        133 |     0.1 <--- ALMOST SEPARATED
   0.20 - 0.40  |         55 |     0.0
   0.40 - 0.60  |         26 |     0.0
   0.60 - 0.80  |         15 |     0.0
   0.80 - 1.00  |          8 |     0.0 <--- FULLY OVERLAPPED
 -------------- | ---------- | ------------ 
      Total     |        237 |     0.2

4 COMPONENTS

COMPONENTS 1, 2, 3, 4
 Overlap factor | # in range | % of all obs 
 -------------- | ---------- | ------------ 
   0.00 - 0.20  |      10538 |     8.8 <--- ALMOST SEPARATED
   0.20 - 0.40  |       6371 |     5.3
   0.40 - 0.60  |       4779 |     4.0
   0.60 - 0.80  |       3460 |     2.9
   0.80 - 1.00  |       1350 |     1.1 <--- FULLY OVERLAPPED
 -------------- | ---------- | ------------ 
      Total     |      26498 |    22.2

 
DC PROFFITRRPTWIN INFO: Step 5 - Scaling data & analysing twin ratios of 4 components
 
Computed twin ratios:
Twin 1: 60.40% (5002 common observations, 1461 merged)
Twin 2: 17.28% (4730 common observations, 1461 merged)
Twin 3: 11.66% (3446 common observations, 1461 merged)
Twin 4: 10.66% (3119 common observations, 1461 merged)

Preparing data for SCALE3 ABSPACK...

SCALING COMPONENT 1

46804 of 52970 reflections used for ABSPACK refinement
PROFFIT INFO: Inet (after scale3 abspack): min=-35993.2305 max=7088526.0000
PROFFIT INFO: sig(Inet) (after scale3 abspack): min=281.0251 max=52419.1055

SCALING COMPONENT 2

47777 of 53101 reflections used for ABSPACK refinement
PROFFIT INFO: Inet (after scale3 abspack): min=-880108.7500 max=7088526.0000
PROFFIT INFO: sig(Inet) (after scale3 abspack): min=281.0251 max=52419.1055

SCALING COMPONENT 3

46696 of 52614 reflections used for ABSPACK refinement
PROFFIT INFO: Inet (after scale3 abspack): min=-880108.7500 max=7088526.0000
PROFFIT INFO: sig(Inet) (after scale3 abspack): min=224.0859 max=52419.1055
PROFFIT INFO: 113 observations on 'bad frames' rejected

SCALING COMPONENT 4

46438 of 53002 reflections used for ABSPACK refinement
PROFFIT INFO: Inet (after scale3 abspack): min=-880108.7500 max=7088526.0000
PROFFIT INFO: sig(Inet) (after scale3 abspack): min=176.0609 max=52419.1055
PROFFIT INFO: 47 observations on 'bad frames' rejected

Computed twin ratios:
Twin 1: 62.66% (4999 common observations, 1460 merged)
Twin 2: 18.92% (4727 common observations, 1460 merged)
Twin 3: 10.48% (3440 common observations, 1460 merged)
Twin 4: 7.94% (3113 common observations, 1460 merged)

DC PROFFITRRPTWIN INFO: Determining HKLF4 overlap threshold for completeness requirement (>=80.0%)
DC PROFFITRRPTWIN INFO: HKLF4 overlap threshold kept - 0.40

DC PROFFITRRPTWIN INFO: Step 6 - Decomposed intensities statistics (HKLF4)
 
COMPONENT 1

 
Note: The Rint, Rsigma and RsigmaB values are computed for redundant data only!
    Mean F2 and F2/sig(F2) are given for all measured values!
Note: The RsigmaA values are computed for all measured values!

Help: For more information about computations of rint and rsigma please look into Crysalis help: 
 file:__#HELP_DTheoryAlgorithm_DataReductionOutput.html
 

Statistics vs intensity - point group symmetry: P-1
                       #        #        #      average    mean      mean        
          intensity measured   kept    unique  redundancy   F2     F2/sig(F2)   Rint   Rsigma
---------------------------------------------------------------------------------------------
   6874901-    56266     4555     4555     1597    2.9    186992.97    44.98    0.050    0.053
     56233-    25110     4865     4865     1597    3.0     37745.06    14.38    0.064    0.070
     25102-    14170     5043     5043     1597    3.2     18950.94     8.09    0.078    0.085
     14164-     8497     4843     4843     1597    3.0     11002.84     5.14    0.104    0.113
      8497-     5303     4774     4774     1597    3.0      6765.13     3.34    0.139    0.149
      5301-     3285     4609     4609     1597    2.9      4218.81     2.20    0.191    0.203
      3284-     1980     4652     4652     1597    2.9      2587.81     1.36    0.284    0.300
      1978-     1056     4629     4629     1597    2.9      1488.52     0.81    0.425    0.463
      1056-      375     4582     4582     1597    2.9       709.98     0.39    0.652    0.797
       375-    -3185     4252     4252     1597    2.7       -33.44    -0.01    0.967    2.090
-------------------------------------------------------------------------------------------
   6874901-    -3185    46804    46804    15970    2.9     26878.47     8.08    0.069    0.073
 

Statistics vs resolution - point group symmetry: P-1
resolu-      #        #        #               average    mean      mean          
tion(A)   measured   kept    unique           redundancy   F2     F2/sig(F2)   Rint   Rsigma   RsigmaA
------------------------------------------------------------------------------------------------------
 inf-1.71     4388     4388     1597             2.7    143056.54    34.48    0.054    0.058     0.021
1.71-1.37     3456     3456     1597             2.2     38275.92     9.08    0.065    0.067     0.095
1.37-1.20     5827     5827     1597             3.6     26445.34     8.16    0.080    0.088     0.121
1.20-1.10     5911     5911     1597             3.7     23371.61     8.50    0.068    0.078     0.109
1.10-1.02     5313     5313     1597             3.3     13317.82     5.25    0.083    0.091     0.180
1.02-0.96     5116     5116     1597             3.2      9068.75     3.85    0.104    0.115     0.249
0.96-0.91     4803     4803     1597             3.0      7591.31     3.55    0.114    0.123     0.270
0.91-0.87     4468     4468     1597             2.8      5620.16     3.04    0.125    0.135     0.316
0.87-0.84     4086     4086     1597             2.6      3919.53     2.58    0.146    0.155     0.375
0.84-0.81     3436     3436     1597             2.2      3207.00     2.66    0.158    0.164     0.362
------------------------------------------------------------------------------------------------------
 inf-0.81    46804    46804    15970             2.9     26878.47     8.08    0.069    0.073     0.089
 

Statistics vs resolution (taking redundancy into account) - point group symmetry: P-1
resolu-      #        #        #       %       average    mean      mean          
tion(A)    kept     theory   unique complete  redundancy   F2     F2/sig(F2)   Rint  RsigmaB
--------------------------------------------------------------------------------------------
 inf-1.71     4388     1751     1597   91.2      2.7    143056.54    57.26    0.054    0.013
1.71-1.37     3456     1671     1597   95.6      2.2     38275.92    14.08    0.065    0.063
1.37-1.20     5827     1643     1597   97.2      3.6     26445.34    14.87    0.080    0.069
1.20-1.10     5911     1651     1597   96.7      3.7     23371.61    16.47    0.068    0.059
1.10-1.02     5313     1641     1597   97.3      3.3     13317.82     9.89    0.083    0.100
1.02-0.96     5116     1639     1597   97.4      3.2      9068.75     7.20    0.104    0.144
0.96-0.91     4803     1633     1597   97.8      3.0      7591.31     6.38    0.114    0.154
0.91-0.87     4468     1640     1597   97.4      2.8      5620.16     5.31    0.125    0.191
0.87-0.84     4086     1641     1597   97.3      2.6      3919.53     4.36    0.146    0.237
0.84-0.81     3436     1724     1597   92.6      2.2      3207.00     4.15    0.158    0.235
--------------------------------------------------------------------------------------------
 inf-0.81    46804    16634    15970   96.0      2.9     26878.47    14.10    0.069    0.051
DC PROFFITRRPTWIN INFO: Step 7 - Generating output files
 
HKLF 4
Reflections read=52968, from those 46803 with overlapping factor < 0.400 written to file C:\Users\Maxime Siegler\Desktop\xs0914a\twin_abs_twin1_hklf4.hkl, 6165 skipped
Use the HKLF 4 file(s) for structure solution.

HKLF 5 merged
RINT ANALYSIS FOR ALL HKLF5 REFLECTIONS
 Components measured    kept     unique redundancy F2/sig(F2) Rint      Rsigma
------------------------------------------------------------------------------
1,2,3,4      52969     51658     24000     2.15      7.69     0.062     0.113

RINT ANALYSIS FOR OVERLAPPED REFLECTIONS
 Components measured    kept     unique redundancy F2/sig(F2) Rint      Rsigma
------------------------------------------------------------------------------
1,2            186       183       129     1.42      8.28     0.053     0.073
1,3             85        85        75     1.13     14.19     0.065     0.030
1,2,3         1478      1454       771     1.89      5.37     0.081     0.153
1,4            285       283       230     1.23     16.04     0.084     0.058
1,2,4         1797      1776      1174     1.51      9.24     0.073     0.080
1,3,4         2272      2208      1256     1.76     13.11     0.066     0.065
1,2,3,4      26458     25483     10602     2.40      7.45     0.068     0.125

RINT ANALYSIS FOR ISOLATED REFLECTIONS
 Component measured     kept     unique redundancy F2/sig(F2) Rint      Rsigma
------------------------------------------------------------------------------
     1       20408     20186      9763     2.07      7.16     0.043     0.107
     2           0         0         0     0.00      0.00     0.000     0.000
     3           0         0         0     0.00      0.00     0.000     0.000
     4           0         0         0     0.00      0.00     0.000     0.000

24000 merged reflections saved into file: C:\Users\Maxime Siegler\Desktop\xs0914a\twin_abs_twin1_hklf5.hkl

Use this hkl file in SHELXL with BASF instruction, which has (components minus 1) entries, and HKLF 5 instruction.
E.g. Two component twin: 'BASF n2' in .ins file, BASF n1 can be computed as n1 = 1.0 - n2.
E.g. Three component twin: 'BASF n2 n3' in .ins file, BASF n1 can be computed as n1 = 1.0 - (n2 + n3).

BASF 0.18922 0.10482 0.07938 
;
_shelx_res_checksum              51614
_shelx_hkl_checksum              75437
_shelx_fab_checksum              75499