Catalytic Activity of an Iron-Based Water Oxidation Catalyst: Substrate Effects of Graphitic Electrodes.
Kottrup, Konstantin G.; D'Agostini, Silvia; van Langevelde, Phebe H.; Siegler, Maxime A.; Hetterscheid, Dennis G. H.; ACS catalysis 8 (2018) 1052–1061; doi:10.1021/acscatal.7b03284

data_4514350
_publ_section_title
;
 Catalytic Activity of an Iron-Based Water Oxidation Catalyst: Substrate
 Effects of Graphitic Electrodes.
;
_journal_issue                   2
_journal_name_full               'ACS catalysis'
_journal_page_first              1052
_journal_page_last               1061
_journal_paper_doi               10.1021/acscatal.7b03284
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C42 H38 Fe2 N10 O3, 4(C F3 O3 S)'
_chemical_formula_sum            'C46 H38 F12 Fe2 N10 O15 S4'
_chemical_formula_weight         1438.80
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                103.183(3)
_cell_angle_beta                 102.560(3)
_cell_angle_gamma                98.477(3)
_cell_formula_units_Z            2
_cell_length_a                   11.9405(5)
_cell_length_b                   12.2853(4)
_cell_length_c                   20.3054(6)
_cell_measurement_reflns_used    11384
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      71.88
_cell_measurement_theta_min      3.75
_cell_volume                     2769.26(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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  0.0559
_diffrn_reflns_av_unetI/netI     0.0914
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            35916
_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         71.897
_diffrn_reflns_theta_min         2.315
_exptl_absorpt_coefficient_mu    6.667
_exptl_absorpt_correction_T_max  0.650
_exptl_absorpt_correction_T_min  0.400
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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            'dark red'
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_description       'small block'
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.211
_exptl_crystal_size_mid          0.171
_exptl_crystal_size_min          0.097
_refine_diff_density_max         0.894
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     878
_refine_ls_number_reflns         12230
_refine_ls_number_restraints     267
_refine_ls_restrained_S_all      0.917
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0541
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0758P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1342
_refine_ls_wR_factor_ref         0.1404
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8520
_reflns_number_total             12230
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs7b03284_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
;Adding full bibliography for 4514350.cif.

 Adding full bibliography for 4514350.cif.
;
_cod_database_code               4514350
_shelx_shelxl_version_number     2014/7
_twin_information
;

 * * * CRYSALIS TWIN DATA REDUCTION FINALIZING (38.41 (release 15-09-2015)) * * *
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 (  11.944   12.280   20.310   103.27   102.54    98.43)
Matrix 2 is taken from component 2 (  12.130   12.107   20.291   102.84   102.84    98.66)
Twin analysis: Component 1 with component 2
TL  =UB[1]-1*UB[2]:   0.0087  -0.9858  -0.0015    -1.0142  -0.0135   0.0002     0.0063   0.0006  -1.0000   det 0.999939
TL-1=UB[2]*UB[1]-1:   0.0135  -0.9858  -0.0003    -1.0143  -0.0087   0.0015    -0.0006  -0.0062  -1.0000   det 1.000061
Rot= -179.8559 deg around the following vectors: 
Reciprocal space (hkl): -0.7007 0.7134 -0.0020
Direct space (uvw)    : -0.7199 0.6941 0.0036
 
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:   1.5017   6.6697   1.9053  d=   0.0756
  2:  -1.0159   4.0942   9.9393  d=   0.0896
  3:   4.8381   2.1417   4.9819  d=   0.0930
  4:  -6.7417  -3.2147   8.0083  d=   0.0406
  5:   4.7682   5.2388  -7.0369  d=   0.0572
  6:   0.8406   8.2560  -3.0851  d=   0.0640
  7:  -2.8028  -6.2361  10.0489  d=   0.0726
  8:  -5.7974  -1.1398   9.9851  d=   0.0600
  9:  -1.0953   7.1948  -7.0731  d=   0.0740
 10:   1.8170   7.2478  -9.0638  d=   0.0708
 11:   6.3566  -4.9606   2.7028  d=   0.0697
 12:   6.2391  -1.9989  -9.0004  d=   0.0759
 13:  -3.7379   4.7647  -9.0917  d=   0.0840
 14:  -6.7386   2.7891   7.1618  d=   0.0788
 15:  -5.0111   0.5842  11.3753  d=   0.0779
 16:   5.2506   4.7717  -1.8118  d=   0.0664
 17:   6.8150   2.7291  -3.9342  d=   0.0651
 18:   3.0493  -8.1879   4.0928  d=   0.0689
 19:  -0.9617  -6.7646  -2.3592  d=   0.0342
 20:  -6.0390  -3.9318   2.7948  d=   0.0301
DC PROFFITRRPTWIN ALL INFO: Component 2
DC PROFFITRRPTWIN INFO: Face list of component 2 
  1:  -6.5555  -1.5781  -1.9475  d=   0.0756
  2:  -4.0526   1.0098  -9.9638  d=   0.0896
  3:  -2.0475  -4.9186  -4.9977  d=   0.0930
  4:   3.0762   6.8782  -7.9844  d=   0.0406
  5:  -5.0985  -4.8924   7.0015  d=   0.0572
  6:  -8.1270  -0.9288   3.0333  d=   0.0640
  7:   6.1074   2.9120 -10.0083  d=   0.0726
  8:   1.0428   5.9052  -9.9745  d=   0.0600
  9:  -7.1059   1.0381   7.0288  d=   0.0740
 10:  -7.1183  -1.9193   9.0175  d=   0.0708
 11:   4.9753  -6.4007  -2.6754  d=   0.0697
 12:   2.0571  -6.3247   9.0091  d=   0.0759
 13:  -4.7453   3.7367   9.0638  d=   0.0840
 14:  -2.8424   6.8217  -7.1752  d=   0.0788
 15:  -0.6465   5.0949 -11.3758  d=   0.0779
 16:  -4.6329  -5.3699   1.7792  d=   0.0664
 17:  -2.5976  -6.9422   3.9134  d=   0.0651
 18:   8.1121  -3.0160  -4.0435  d=   0.0689
 19:   6.6565   1.0305   2.4016  d=   0.0342
 20:   3.7940   6.1638  -2.7670  d=   0.0301
 
DC PROFFITRRPTWIN INFO: Step 4 - Analysing composite reflections of 2 components
 
Component 1: 35971 observations read
Component 2: 35735 observations read

52179 composite observations collected (32755 fully isolated, 19424 overlapped), 62 skipped due to one or more missing parts and 14 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  |       6810 |    13.1 <--- ALMOST SEPARATED
   0.20 - 0.40  |       4366 |     8.4
   0.40 - 0.60  |       3908 |     7.5
   0.60 - 0.80  |       3152 |     6.0
   0.80 - 1.00  |       1188 |     2.3 <--- FULLY OVERLAPPED
 -------------- | ---------- | ------------ 
      Total     |      19424 |    37.2

 
DC PROFFITRRPTWIN INFO: Step 5 - Scaling data & analysing twin ratios of 2 components
 
Computed twin ratios:
Twin 1: 78.18% (11799 common observations, 3624 merged)
Twin 2: 21.82% (9044 common observations, 3624 merged)

Preparing data for SCALE3 ABSPACK...

SCALING COMPONENT 1

27820 of 35916 reflections used for ABSPACK refinement
PROFFIT INFO: Inet (after scale3 abspack): min=-144655.0625 max=37698924.0000
PROFFIT INFO: sig(Inet) (after scale3 abspack): min=561.5718 max=257798.1563

SCALING COMPONENT 2

27551 of 35687 reflections used for ABSPACK refinement
PROFFIT INFO: Inet (after scale3 abspack): min=-6700436.5000 max=37698924.0000
PROFFIT INFO: sig(Inet) (after scale3 abspack): min=561.5718 max=257798.1563

Computed twin ratios:
Twin 1: 78.91% (11799 common observations, 3624 merged)
Twin 2: 21.09% (9044 common observations, 3624 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
---------------------------------------------------------------------------------------------
  37225568-   264497     2388     2388      890    2.7    669951.32    48.34    0.037    0.039
    264280-   124428     2809     2809      890    3.2    178234.04    19.93    0.050    0.055
    124296-    71759     2795     2795      890    3.1     95408.61    12.30    0.060    0.067
     71710-    45523     2970     2970      890    3.3     57302.19     8.08    0.075    0.084
     45512-    28667     2852     2852      890    3.2     36374.07     5.38    0.095    0.104
     28646-    17556     2820     2820      890    3.2     22708.32     3.54    0.134    0.145
     17542-    10374     2783     2783      890    3.1     13825.81     2.19    0.184    0.198
     10370-     5549     2774     2774      890    3.1      7735.13     1.25    0.298    0.325
      5543-     2235     2905     2905      890    3.3      3794.87     0.63    0.507    0.574
      2233-   -57927     2724     2724      894    3.0       457.29     0.09    0.882    1.593
-------------------------------------------------------------------------------------------
  37225568-   -57927    27820    27820     8904    3.1     99832.43     9.59    0.058    0.060
 

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-1.62     1992     1992      890             2.2    476338.42    33.17    0.040    0.041     0.023
1.62-1.32     1679     1679      890             1.9    196769.93    11.87    0.056    0.059     0.072
1.32-1.18     3745     3745      890             4.2    126621.59    11.91    0.066    0.079     0.083
1.18-1.08     3367     3367      890             3.8     95573.44    10.80    0.055    0.063     0.086
1.08-1.00     3253     3253      890             3.7     70482.41     8.11    0.060    0.066     0.116
1.00-0.95     3143     3143      890             3.5     53494.34     6.55    0.070    0.078     0.143
0.95-0.91     3004     3004      890             3.4     36718.99     5.15    0.082    0.092     0.186
0.91-0.87     2814     2814      890             3.2     32226.55     5.23    0.083    0.091     0.183
0.87-0.84     2620     2620      890             2.9     24064.19     4.74    0.091    0.098     0.202
0.84-0.81     2203     2203      894             2.5     18453.13     4.60    0.093    0.097     0.208
------------------------------------------------------------------------------------------------------
 inf-0.81    27820    27820     8904             3.1     99832.43     9.59    0.058    0.060     0.080
 

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-1.62     1992     1362      890   65.3      2.2    476338.42    50.43    0.040    0.014
1.62-1.32     1679     1125      890   79.1      1.9    196769.93    17.40    0.056    0.046
1.32-1.18     3745     1039      890   85.7      4.2    126621.59    22.40    0.066    0.045
1.18-1.08     3367     1100      890   80.9      3.8     95573.44    21.80    0.055    0.046
1.08-1.00     3253     1087      890   81.9      3.7     70482.41    16.18    0.060    0.062
1.00-0.95     3143     1062      890   83.8      3.5     53494.34    12.94    0.070    0.081
0.95-0.91     3004     1045      890   85.2      3.4     36718.99    10.11    0.082    0.108
0.91-0.87     2814     1031      890   86.3      3.2     32226.55     9.91    0.083    0.106
0.87-0.84     2620     1018      890   87.4      2.9     24064.19     8.64    0.091    0.121
0.84-0.81     2203     1040      894   86.0      2.5     18453.13     7.65    0.093    0.126
--------------------------------------------------------------------------------------------
 inf-0.81    27820    10910     8904   81.6      3.1     99832.43    17.18    0.058    0.044
DC PROFFITRRPTWIN INFO: Step 7 - Generating output files
 
HKLF 4
Reflections read=35916, from those 27820 with overlapping factor < 0.400 written to file C:\Users\msiegle2\Desktop\xs0888a\twin2_twin1_hklf4.hkl, 8096 skipped
Use the HKLF 4 file(s) for structure solution.

HKLF 5 merged
RINT ANALYSIS FOR ALL HKLF5 REFLECTIONS
 Components measured   unique redundancy F2/sig(F2) Rint      Rsigma
--------------------------------------------------------------------
1,2          35916     12265     2.93     11.04     0.056     0.067

RINT ANALYSIS FOR OVERLAPPED REFLECTIONS
 Components measured   unique redundancy F2/sig(F2) Rint      Rsigma
--------------------------------------------------------------------
1,2          19424      6752     2.88     14.73     0.054     0.054

RINT ANALYSIS FOR ISOLATED REFLECTIONS
 Component measured    unique redundancy F2/sig(F2) Rint      Rsigma
--------------------------------------------------------------------
     1       16492      5513     2.99      6.69     0.064     0.125
     2           0         0     0.00      0.00     0.000     0.000

12265 merged reflections saved into file: C:\Users\msiegle2\Desktop\xs0888a\twin2_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 0.21091 
;
_shelx_res_checksum              71513
_shelx_hkl_checksum              15073