Dioxygen-Derived Nonheme Mononuclear Fe<sup>III</sup>(OH) Complex and Its Reactivity with Carbon Radicals.
Yadav, Vishal; Gordon, Jesse B.; Siegler, Maxime A.; Goldberg, David P.; Journal of the American Chemical Society 141 (2019) 10148–10153; doi:10.1021/jacs.9b03329

data_4128013
_publ_section_title
;
 Dioxygen-Derived Nonheme Mononuclear Fe<sup>III</sup>(OH) Complex and Its
 Reactivity with Carbon Radicals.
;
_journal_issue                   26
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10148
_journal_page_last               10153
_journal_paper_doi               10.1021/jacs.9b03329
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C37 H46 F3 Fe N5 O4 S'
_chemical_formula_sum            'C37 H46 F3 Fe N5 O4 S'
_chemical_formula_weight         769.70
_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
_cell_angle_alpha                80.928(3)
_cell_angle_beta                 79.036(3)
_cell_angle_gamma                79.746(3)
_cell_formula_units_Z            2
_cell_length_a                   10.0166(3)
_cell_length_b                   10.6374(4)
_cell_length_c                   18.2471(6)
_cell_measurement_reflns_used    9855
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.66
_cell_measurement_theta_min      2.40
_cell_volume                     1862.77(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_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 1.000
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.1048
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28180
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.096
_exptl_absorpt_coefficient_mu    0.522
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.876
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29c (Rigaku Oxford Diffraction, 2017)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_description       block
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.587
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.812
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         9583
_refine_ls_number_restraints     268
_refine_ls_restrained_S_all      0.808
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0394
_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^)+(0.0190P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0732
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6152
_reflns_number_total             9583
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b03329_si_001.cif
_cod_data_source_block           1
_cod_database_code               4128013
_twin_information
;
 * * * CRYSALIS TWIN DATA REDUCTION FINALIZING (39.29c (release 19-06-2017)) * * *
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 (  10.017   10.638   18.246    80.93    79.03    79.76)
Matrix 2 is taken from component 2 (  10.006   10.618   18.230    80.68    79.08    79.72)
Twin analysis: Component 1 with component 2
TL  =UB[1]-1*UB[2]:  -1.0012   0.3359   0.0000    -0.0001   1.0020  -0.0003    -0.0030   0.5488  -1.0014   det 1.004320
TL-1=UB[2]*UB[1]-1:  -0.9988   0.3349  -0.0001    -0.0001   0.9983  -0.0003     0.0030   0.5460  -0.9988   det 0.995699
Rot= 179.9075 deg around the following vectors: 
Reciprocal space (hkl): 0.1596 0.9522 0.2605
Direct space (uvw)    : -0.0001 1.0000 0.0011
 
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: -11.8197   5.7021   0.2047  d=   0.0518
  2:  -1.1585   0.1734 -25.2685  d=   0.0275
  3:  11.8075  -5.6995  -0.4207  d=   0.0606
  4:   2.0734  -0.6154  25.2135  d=   0.0277
  5: -13.3556   1.3106  -8.6773  d=   0.0498
  6:  -2.7282  13.7646  -1.8886  d=   0.0579
  7:   2.2407  14.9119   1.3256  d=   0.0594
  8:  13.1857  -1.9087   8.5722  d=   0.0509
  9:  -1.7304 -14.8808  -0.9948  d=   0.0513
 10:  10.0251   6.0074 -11.7040  d=   0.0601
 11:   0.3557  10.0117 -16.5520  d=   0.0403
 12: -13.3514  -1.0019   3.4174  d=   0.0535
 13:   0.3554  10.0245  20.4994  d=   0.0534
DC PROFFITRRPTWIN ALL INFO: Component 2
DC PROFFITRRPTWIN INFO: Face list of component 2 
  1:  13.7159   5.6934   2.8742  d=   0.0518
  2:   1.2184   0.1820  25.3295  d=   0.0275
  3: -13.7028  -5.6907  -2.6571  d=   0.0606
  4:  -2.2802  -0.6233 -25.5132  d=   0.0277
  5:  13.7803   1.3127   9.3430  d=   0.0498
  6:   7.3355  13.7417   9.3943  d=   0.0579
  7:   2.7562  14.8854   6.8251  d=   0.0594
  8: -13.8108  -1.9097  -9.5651  d=   0.0509
  9:  -3.2555 -14.8545  -7.1371  d=   0.0513
 10:  -8.0000   6.0000  15.0000  d=   0.0601
 11:   3.0000  10.0000  22.0000  d=   0.0403
 12:  13.0000  -1.0000  -4.0000  d=   0.0535
 13:   3.0000  10.0000 -15.0000  d=   0.0534
 
DC PROFFITRRPTWIN INFO: Step 4 - Analysing composite reflections of 2 components
 
Component 1: 28662 observations read
Component 2: 28470 observations read

47442 composite observations collected (37946 fully isolated, 9496 overlapped), 110 skipped due to one or more missing parts

OVERLAP STATISTICS

2 COMPONENTS

COMPONENTS 1, 2
 Overlap factor | # in range | % of all obs 
 -------------- | ---------- | ------------ 
   0.00 - 0.20  |       3911 |     8.2 <--- ALMOST SEPARATED
   0.20 - 0.40  |       1567 |     3.3
   0.40 - 0.60  |       1713 |     3.6
   0.60 - 0.80  |        643 |     1.4
   0.80 - 1.00  |       1662 |     3.5 <--- FULLY OVERLAPPED
 -------------- | ---------- | ------------ 
      Total     |       9496 |    20.0

 
DC PROFFITRRPTWIN INFO: Step 5 - Scaling data & analysing twin ratios of 2 components
 
Computed twin ratios:
Twin 1: 86.46% (5695 common observations, 1380 merged)
Twin 2: 13.54% (3978 common observations, 1380 merged)

Preparing data for SCALE3 ABSPACK...

SCALING COMPONENT 1

24467 of 28554 reflections used for ABSPACK refinement
PROFFIT INFO: Inet (after scale3 abspack): min=-148226.0938 max=220110.8594
PROFFIT INFO: sig(Inet) (after scale3 abspack): min=25.7924 max=4899.2852

SCALING COMPONENT 2

24616 of 28384 reflections used for ABSPACK refinement
PROFFIT INFO: Inet (after scale3 abspack): min=-148226.0938 max=262325.8438
PROFFIT INFO: sig(Inet) (after scale3 abspack): min=24.4106 max=4899.2852

Computed twin ratios:
Twin 1: 87.21% (5695 common observations, 1380 merged)
Twin 2: 12.79% (3978 common observations, 1380 merged)

        ******************************************************************
        * GRAL PLUGIN               started at Tue Feb 13 09:42:22 2018     *
        *          version 2.4. 1                                        *
        ******************************************************************

        39.29c (release 19-06-2017),compiled Jun 19 2017,17:33:47

Original cell in Angstroms and degrees: 

  10.016601  10.637441  18.247066  80.9278  79.0363  79.7464 

   24467 Reflections read from file twin_abs_twin1_hklf4.hkl; mean (I/sigma) =   10.88

Lattice exceptions:  P      A      B      C      I      F     Obv    Rev    All
          

N (total) =           0  12228  12205  12229  12274  18331  16324  16341  24467

N (int>3sigma) =      0   7712   7512   7644   7634  11434  10223  10119  15214

Mean intensity =    0.0   39.1   39.6   39.3   39.1   39.4   40.1   40.5   39.5

Mean int/sigma =    0.0   10.8   10.7   10.9   10.9   10.8   10.9   10.9   10.9

Lattice type: P chosen          Volume:      1862.78

-------------------------------------------------------------------------------

DETERMINATION OF REDUCED (NIGGLI) CELL

Transformation from original cell (HKLF-matrix):
    1.0000  0.0000  0.0000    0.0000  1.0000  0.0000    0.0000  0.0000  1.0000

Unitcell:      10.017   10.637   18.247   80.93   79.04   79.75 

Niggli form:     a.a =   100.332      b.b =   113.155      c.c =   332.955
                 b.c =    30.606      a.c =    34.761      a.b =    18.967 

-------------------------------------------------------------------------------

SEARCH FOR HIGHER METRIC SYMMETRY

------------------------------------------------------------------------------
Option: [31]  err=   0.000     TRICLINIC P-lattice R(int) = 0.041 [ 16848] Vol =   1862.8
Cell:   10.017  10.637  18.247   80.93   79.04   79.75    Volume:      1862.78
Matrix: 1.0000  0.0000  0.0000  0.0000  1.0000  0.0000  0.0000  0.0000  1.0000

Option [31] selected

-------------------------------------------------------------------------------

SPACE GROUP DETERMINATION

Lattice exceptions:  P      A      B      C      I      F     Obv    Rev    All
          

N (total) =           0  12228  12205  12229  12274  18331  16324  16341  24467

N (int>3sigma) =      0   7712   7512   7644   7634  11434  10223  10119  15214

Mean intensity =    0.0   39.1   39.6   39.3   39.1   39.4   40.1   40.5   39.5

Mean int/sigma =    0.0   10.8   10.7   10.9   10.9   10.8   10.9   10.9   10.9

Crystal system TRICLINIC and Lattice type P selected

Mean |E*E-1| = 0.911 [expected .968 centrosym and .736 non-centrosym]

 Systematic absences not required for triclinic

  Space Group           No.   C/A   En.   O.A.  Pie.  Pyr.   CCDC    ICSD    R(int)   N(eq)

             P1 1 1     1     A     Y     Y     Y     Y     2112     239    0.035    11345
            P-1 1 1     2     C     N     N     N     N    47868    2604    0.041    16848

 P-1         -1         Triclinic

  (1)  x, y, z                            (2) -x,-y,-z 
   
Chemical formula: C37 H46 F3 Fe1 N5 O4 S1; Z=2.0 (Mo-wavelength)
   
EXPORTING .INS FILE

TITL twin_abs_twin1_hklf4 in P-1 
REM P-1 (#2 in standard setting)
CELL 0.71073  10.016601  10.637441  18.247066  80.9278  79.0363  79.7464
ZERR    2.00   0.000324   0.000403   0.000574   0.0029   0.0027   0.0029
LATT  1
SFAC C H N O F S Fe
UNIT 74.00 92.00 10.00 8.00 6.00 2.00 2.00
TREF
HKLF 4
END
 
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
---------------------------------------------------------------------------------------------
    218301-     7365     3363     3363      761    4.4     18692.00    40.40    0.026    0.031
      7360-     3876     2850     2850      761    3.7      5275.81    18.03    0.040    0.046
      3875-     2449     2430     2430      761    3.2      3106.68    11.52    0.051    0.058
      2449-     1586     2345     2345      761    3.1      1996.84     8.36    0.068    0.077
      1586-     1015     2324     2324      761    3.1      1290.79     5.87    0.090    0.101
      1015-      619     2219     2219      761    2.9       807.50     3.74    0.126    0.141
       619-      334     2246     2246      761    3.0       466.89     2.44    0.175    0.198
       334-      156     2169     2169      761    2.9       237.76     1.29    0.299    0.344
       156-       43     2273     2273      761    3.0        95.70     0.55    0.544    0.686
        43-     -515     2248     2248      770    2.9        -6.54     0.01    0.957    1.797
-------------------------------------------------------------------------------------------
    218301-     -515    24467    24467     7619    3.2      3951.77    10.88    0.042    0.053
 

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-1.65     3937     3937      761             5.2     11370.07    28.07    0.025    0.029     0.024
1.65-1.32     3638     3638      761             4.8      4957.58    15.05    0.040    0.047     0.051
1.32-1.16     2908     2908      761             3.8      3574.42    10.99    0.041    0.047     0.070
1.16-1.05     2630     2630      761             3.5      2862.48     8.84    0.049    0.056     0.090
1.05-0.97     2222     2222      761             2.9      2277.40     6.80    0.059    0.064     0.121
0.97-0.91     2080     2080      761             2.7      1632.65     4.78    0.074    0.079     0.176
0.91-0.86     1943     1943      761             2.6      1283.47     3.70    0.095    0.101     0.228
0.86-0.83     1816     1816      761             2.4      1075.73     3.02    0.117    0.121     0.284
0.83-0.79     1660     1660      761             2.2       976.39     2.63    0.127    0.130     0.325
0.79-0.77     1633     1633      770             2.1       882.51     2.27    0.141    0.144     0.378
------------------------------------------------------------------------------------------------------
 inf-0.77    24467    24467     7619             3.2      3951.77    10.88    0.042    0.053     0.071
 inf-0.80    22504    22504     6696             3.4      4218.17    11.63    0.040    0.050     0.065
 

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-1.65     3937      860      761   88.5      5.2     11370.07    62.78    0.025    0.011
1.65-1.32     3638      824      761   92.4      4.8      4957.58    32.44    0.040    0.025
1.32-1.16     2908      829      761   91.8      3.8      3574.42    21.28    0.041    0.039
1.16-1.05     2630      891      761   85.4      3.5      2862.48    16.18    0.049    0.052
1.05-0.97     2222      886      761   85.9      2.9      2277.40    11.65    0.059    0.071
0.97-0.91     2080      883      761   86.2      2.7      1632.65     8.01    0.074    0.105
0.91-0.86     1943      891      761   85.4      2.6      1283.47     6.07    0.095    0.142
0.86-0.83     1816      876      761   86.9      2.4      1075.73     4.79    0.117    0.178
0.83-0.79     1660      882      761   86.3      2.2       976.39     4.05    0.127    0.210
0.79-0.77     1633      882      770   87.3      2.1       882.51     3.46    0.141    0.251
--------------------------------------------------------------------------------------------
 inf-0.77    24467     8705     7619   87.5      3.2      3951.77    22.27    0.042    0.051
 inf-0.80    22504     7641     6696   87.6      3.4      4218.17    23.91    0.040    0.045
DC PROFFITRRPTWIN INFO: Step 7 - Generating output files
 
HKLF 4
Reflections read=28554, from those 24467 with overlapping factor < 0.400 written to file D:\Data\xs1658a\twin_abs_twin1_hklf4.hkl, 4087 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          28554     28180      9748     2.89     10.52     0.039     0.079

RINT ANALYSIS FOR OVERLAPPED REFLECTIONS
 Components measured    kept     unique redundancy F2/sig(F2) Rint      Rsigma
------------------------------------------------------------------------------
1,2           9496      9198      3522     2.61      8.76     0.054     0.112

RINT ANALYSIS FOR ISOLATED REFLECTIONS
 Component measured     kept     unique redundancy F2/sig(F2) Rint      Rsigma
------------------------------------------------------------------------------
     1       19058     18982      6226     3.05     11.48     0.033     0.066
     2           0         0         0     0.00      0.00     0.000     0.000

9748 merged reflections saved into file: D:\Data\xs1658a\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 0.12789 
;
_oxdiff_exptl_absorpt_empirical_full_min 0.619
_oxdiff_exptl_absorpt_empirical_full_max 2.029
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelxl_version_number           2014-3
_shelx_res_checksum              79738
_shelx_hkl_checksum              72982