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_4126432
_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 H59 Cl Fe N4'
_chemical_formula_sum            'C91 H59 Cl Fe N4'
_chemical_formula_weight         1299.72
_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                95.674(3)
_cell_angle_beta                 104.611(2)
_cell_angle_gamma                109.640(2)
_cell_formula_units_Z            2
_cell_length_a                   14.2771(3)
_cell_length_b                   15.7261(5)
_cell_length_c                   21.1824(6)
_cell_measurement_reflns_used    13941
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      71.91
_cell_measurement_theta_min      4.03
_cell_volume                     4245.5(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0439
_diffrn_reflns_av_unetI/netI     0.0750
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            53816
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.895
_diffrn_reflns_theta_min         2.201
_exptl_absorpt_coefficient_mu    2.033
_exptl_absorpt_correction_T_max  0.843
_exptl_absorpt_correction_T_min  0.737
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.017
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.042
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.915
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     875
_refine_ls_number_reflns         20239
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      0.916
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0600
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0987P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1597
_refine_ls_wR_factor_ref         0.1694
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12718
_reflns_number_total             20239
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b07979_si_002.cif
_cod_data_source_block           1
_cod_database_code               4126432
_shelx_shelxl_version_number     2014/7
_twin_information
;

 * * * CRYSALIS TWIN DATA REDUCTION FINALIZING (Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)) * * *
Laue class: 1bar - Friedel mate is equivalent
Lattice type: P-lattice 
DC PROFFITRRPTWIN INFO: Step 1 - Loading orientation matrices (UB) of 2 components
 
DC PROFFITRRPTWIN INFO: Loading UB component 1
 
DC PROFFITRRPTWIN INFO: Loading UB component 2
 
DC PROFFITRRPTWIN INFO: Step 2 - Computing crossed twin laws
 
Twin law determination (relative to component 1)
Matrix 1 is taken from component 1 (  14.276   15.720   21.173    95.65   104.63   109.63)
Matrix 2 is taken from component 2 (  14.300   15.734   21.159    95.55   104.76   109.72)
Twin analysis: Component 1 with component 2
TL  =UB[1]-1*UB[2]:   0.9942  -0.0050  -0.0060    -0.0160   0.9871  -0.0429     0.0520   0.0874   1.0141   det 0.999105
TL-1=UB[2]*UB[1]-1:   1.0056   0.0045   0.0061     0.0140   1.0093   0.0427    -0.0528  -0.0872   0.9821   det 1.000895
Rot= 3.5180 deg around the following vectors: 
Reciprocal space (hkl): 0.8559 -0.4795 -0.1938
Direct space (uvw)    : 0.9845 -0.1681 0.0495
 
DC PROFFITRRPTWIN INFO: Step 3 - Loading reflections of 2 components
 
DC PROFFITRRPTWIN ALL INFO: Component 1
DC PROFFITRRPTWIN INFO: Face list of component 1 
  1:  -3.4105  -7.3316   6.9921  d=   0.0434
  2:  -1.3159   1.8855  12.8581  d=   0.0954
  3:  -8.8529   6.0594   1.7848  d=   0.0748
  4:   0.7692  -1.5169 -12.8189  d=   0.0426
  5:   8.8288  -5.9924  -1.1341  d=   0.1087
  6:   3.0123  -1.0133  10.9884  d=   0.1136
  7:   1.9986   8.9956  -2.9885  d=   0.0663
  8:   7.9985   0.9985  -6.0094  d=   0.0932
  9:   0.0100   4.9865  10.0030  d=   0.0970
 10:  -7.9945   0.9961  10.0106  d=   0.0812
 11:  -4.0007   9.9961   1.0214  d=   0.0661
 12:   3.0070 -10.0024   5.9771  d=   0.0951
 13:  -0.9881  -5.0093  12.9883  d=   0.0932
 14:   5.9976   4.9977  -6.0000  d=   0.0588
 15:  -0.9924   5.9888   8.0071  d=   0.0832
DC PROFFITRRPTWIN ALL INFO: Component 2
DC PROFFITRRPTWIN INFO: Face list of component 2 
  1:  -3.4202  -7.1492   7.6866  d=   0.0434
  2:  -1.2364   2.4342  12.5334  d=   0.0954
  3:  -8.8645   6.0681   1.6915  d=   0.0748
  4:   0.6885  -2.0681 -12.4981  d=   0.0426
  5:   8.8446  -5.9730  -1.0570  d=   0.1087
  6:   3.0917  -0.5109  10.7215  d=   0.1136
  7:   2.0323   8.9800  -3.8252  d=   0.0663
  8:   8.0115   0.8632  -6.4112  d=   0.0932
  9:   0.0936   5.4608   9.3888  d=   0.0970
 10:  -7.9740   1.3211  10.1667  d=   0.0812
 11:  -3.9718  10.0771   0.3423  d=   0.0661
 12:   3.0151  -9.7983   6.5841  d=   0.0951
 13:  -0.9371  -4.5149  13.2453  d=   0.0932
 14:   6.0175   4.8722  -6.6452  d=   0.0588
 15:  -0.9221   6.3731   7.3940  d=   0.0832
 
DC PROFFITRRPTWIN INFO: Step 4 - Analysing composite reflections of 2 components
 
Component 1: 55513 observations read
Component 2: 55442 observations read

88016 composite observations collected (65218 fully isolated, 22798 overlapped), 100 skipped due to one or more missing parts and 2 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  |      11331 |    12.9 <--- ALMOST SEPARATED
   0.20 - 0.40  |       5581 |     6.3
   0.40 - 0.60  |       3482 |     4.0
   0.60 - 0.80  |       1870 |     2.1
   0.80 - 1.00  |        534 |     0.6 <--- FULLY OVERLAPPED
 -------------- | ---------- | ------------ 
      Total     |      22798 |    25.9

 
DC PROFFITRRPTWIN INFO: Step 5 - Scaling data & analysing twin ratios of 2 components
 
Computed twin ratios:
Twin 1: 68.92% (21175 common observations, 6263 merged)
Twin 2: 31.08% (17231 common observations, 6263 merged)

Preparing data for SCALE3 ABSPACK...

SCALING COMPONENT 1

49266 of 55435 reflections used for ABSPACK refinement
PROFFIT INFO: Inet (after scale3 abspack): min=-112169.2031 max=10128993.0000
PROFFIT INFO: sig(Inet) (after scale3 abspack): min=324.2121 max=72454.9141

SCALING COMPONENT 2

50224 of 55379 reflections used for ABSPACK refinement
PROFFIT INFO: Inet (after scale3 abspack): min=-5336180.5000 max=10128993.0000
PROFFIT INFO: sig(Inet) (after scale3 abspack): min=300.9453 max=120607.6563
PROFFIT INFO: 84 observations on 'bad frames' rejected

Computed twin ratios:
Twin 1: 70.38% (21175 common observations, 6263 merged)
Twin 2: 29.62% (17228 common observations, 6263 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
--------------------------------------------------------------------------------------------
  9365628-   95892     4820     4820     1580    3.1    326628.43    60.30    0.035    0.038
    95862-   44343     5127     5127     1580    3.2     64950.13    17.14    0.048    0.052
    44314-   24780     5160     5160     1580    3.3     33109.01     9.74    0.061    0.067
    24773-   15112     5127     5127     1580    3.2     19525.52     6.23    0.080    0.087
    15108-    9390     4979     4979     1580    3.2     12068.69     4.10    0.112    0.121
     9378-    5729     5020     5020     1580    3.2      7380.08     2.59    0.156    0.167
     5728-    3409     4920     4920     1580    3.1      4531.92     1.62    0.230    0.245
     3408-    1838     4844     4844     1580    3.1      2553.46     0.94    0.357    0.383
     1836-     785     4764     4764     1580    3.0      1292.25     0.49    0.565    0.650
      785-  -10136     4505     4505     1588    2.8        97.33     0.06    0.931    1.896
------------------------------------------------------------------------------------------
  9365628-  -10136    49266    49266    15808    3.1     47024.25    10.34    0.051    0.055
 

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-1.74     4742     4742     1580             3.0    252974.68    48.65    0.035    0.038     0.016
1.74-1.38     3567     3567     1580             2.3     64907.32    11.49    0.047    0.049     0.078
1.38-1.20     6110     6110     1580             3.9     42872.05     9.00    0.069    0.076     0.109
1.20-1.09     6393     6393     1580             4.0     38508.00     9.31    0.061    0.068     0.102
1.09-1.02     5603     5603     1580             3.5     23225.12     6.13    0.069    0.076     0.156
1.02-0.96     5290     5290     1580             3.3     16503.09     4.74    0.083    0.093     0.205
0.96-0.91     5000     5000     1580             3.2     13589.29     4.42    0.090    0.098     0.223
0.91-0.87     4693     4693     1580             3.0      9549.62     3.65    0.104    0.112     0.271
0.87-0.84     4291     4291     1580             2.7      6567.89     3.07    0.125    0.132     0.322
0.84-0.81     3577     3577     1588             2.3      5328.31     3.14    0.124    0.129     0.315
------------------------------------------------------------------------------------------------------
 inf-0.81    49266    49266    15808             3.1     47024.25    10.34    0.051    0.055     0.074
 

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-1.74     4742     1676     1580   94.3      3.0    252974.68    84.45    0.035    0.010
1.74-1.38     3567     1711     1580   92.3      2.3     64907.32    17.90    0.047    0.051
1.38-1.20     6110     1701     1580   92.9      3.9     42872.05    17.41    0.069    0.060
1.20-1.09     6393     1687     1580   93.7      4.0     38508.00    18.65    0.061    0.052
1.09-1.02     5603     1689     1580   93.5      3.5     23225.12    11.83    0.069    0.083
1.02-0.96     5290     1663     1580   95.0      3.3     16503.09     8.97    0.083    0.115
0.96-0.91     5000     1654     1580   95.5      3.2     13589.29     8.16    0.090    0.128
0.91-0.87     4693     1641     1580   96.3      3.0      9549.62     6.47    0.104    0.159
0.87-0.84     4291     1632     1580   96.8      2.7      6567.89     5.25    0.125    0.198
0.84-0.81     3577     1669     1588   95.1      2.3      5328.31     4.98    0.124    0.202
--------------------------------------------------------------------------------------------
 inf-0.81    49266    16723    15808   94.5      3.1     47024.25    18.58    0.051    0.042
DC PROFFITRRPTWIN INFO: Step 7 - Generating output files
 
HKLF 4
Reflections read=55432, from those 49266 with overlapping factor < 0.400 written to file D:\Data\xs0806a\xs0806a_max_twin1_hklf4.hkl, 6166 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          55432     53816     20302     2.65     10.40     0.044     0.082

RINT ANALYSIS FOR OVERLAPPED REFLECTIONS
 Components measured    kept     unique redundancy F2/sig(F2) Rint      Rsigma
------------------------------------------------------------------------------
1,2          22714     21886      8463     2.59     11.80     0.047     0.073

RINT ANALYSIS FOR ISOLATED REFLECTIONS
 Component measured     kept     unique redundancy F2/sig(F2) Rint      Rsigma
------------------------------------------------------------------------------
     1       32718     31930     11839     2.70      9.57     0.041     0.092
     2           0         0         0     0.00      0.00     0.000     0.000

20302 merged reflections saved into file: D:\Data\xs0806a\xs0806a_max_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 0.29622 
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_shelx_res_checksum              97194
_shelx_hkl_checksum              5814
_shelx_fab_checksum              83305