A Thermodynamic Model for Redox-Dependent Binding of Carbon Monoxide at Site-Differentiated, High Spin Iron Clusters.
Arnett, Charles H.; Chalkley, Matthew J.; Agapie, Theodor; Journal of the American Chemical Society 140 (2018) 5569–5578; doi:10.1021/jacs.8b01825

data_4132144
_publ_section_title
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 A Thermodynamic Model for Redox-Dependent Binding of Carbon Monoxide at
 Site-Differentiated, High Spin Iron Clusters.
;
_journal_issue                   16
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5569
_journal_page_last               5578
_journal_paper_doi               10.1021/jacs.8b01825
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety
'C85 H59 Fe4 N12 O5, C F3 O3 S, C2 N, 2(C2 H3 N)'
_chemical_formula_sum            'C92 H65 F3 Fe4 N15 O8 S'
_chemical_formula_weight         1821.05
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-06-15
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_cell_angle_alpha                78.351(13)
_cell_angle_beta                 79.352(12)
_cell_angle_gamma                88.530(13)
_cell_formula_units_Z            2
_cell_length_a                   12.349(4)
_cell_length_b                   15.527(7)
_cell_length_c                   21.471(8)
_cell_measurement_reflns_used    9728
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.58
_cell_measurement_theta_min      2.34
_cell_volume                     3962(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker AXS D8 VENTURE KAPPA'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0856
_diffrn_reflns_av_unetI/netI     0.0597
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            145591
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.693
_diffrn_reflns_theta_min         2.134
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.823
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7412
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1248 before and 0.0812 after correction.
The Ratio of minimum to maximum transmission is 0.7412.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_description       Block
_exptl_crystal_F_000             1866
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.051
_refine_diff_density_min         -1.609
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1180
_refine_ls_number_reflns         24232
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1309
_refine_ls_R_factor_gt           0.0877
_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^)+(0.1222P)^2^+18.9589P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2192
_refine_ls_wR_factor_ref         0.2596
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16565
_reflns_number_total             24232
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b01825_si_001.cif
_cod_data_source_block           p17244
_cod_database_code               4132144
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C95-N17
 1.157 with sigma of 0.02
 C95-C96
 1.458 with sigma of 0.02
 N17-C96
 2.7 with sigma of 0.01
 C89-C88 \\sim C90-C88
 with sigma of 0.02
 N14-C90 \\sim N13-C89 \\sim N16-C94 \\sim N15-C92
 with sigma of 0.02
 N14-C88 \\sim N15-C91 \\sim N16-C93 \\sim N13-C88
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C96 \\sim C95 \\sim N17 \\sim C96 \\sim C95 \\sim N17 \\sim N16 \\sim C93 \\sim
C94 \\sim N15 \\sim C92 \\sim C91 \\sim N14 \\sim C88 \\sim C89 \\sim C90 \\sim
N13: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Others
 Sof(C87)=Sof(S2)=Sof(F4)=Sof(O6)=1-FVAR(1)
 Sof(S1)=Sof(F1)=Sof(O9)=Sof(C86)=FVAR(1)
 Sof(C92)=Sof(N15)=Sof(C91)=Sof(H91A)=Sof(H91B)=Sof(H91C)=1-FVAR(2)
 Sof(C93)=Sof(H93A)=Sof(H93B)=Sof(H93C)=Sof(N16)=Sof(C94)=FVAR(2)
 Sof(N14)=Sof(C90)=1-FVAR(3)
 Sof(C89)=Sof(N13)=FVAR(3)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C41(H41), C10(H10), C28(H28), C76(H76), C6(H6), C32(H32), C27(H27),
 C9(H9), C15(H15), C77(H77), C4(H4), C38(H38), C40(H40), C39(H39), C52(H52),
 C33(H33), C29(H29), C65(H65), C66(H66), C35(H35), C30(H30), C18(H18), C24(H24),
  C58(H58), C11(H11), C59(H59), C22(H22), C23(H23), C83(H83), C56(H56),
 C45(H45), C12(H12), C82(H82), C34(H34), C74(H74), C67(H67), C84(H84), C64(H64),
  C55(H55), C50(H50), C17(H17), C63(H63), C44(H44), C51(H51), C62(H62),
 C16(H16), C43(H43), C81(H81), C21(H21), C57(H57), C46(H46), C54(H54), C49(H49),
  C73(H73), C75(H75), C68(H68), C72(H72), C71(H71)
5.b Idealised Me refined as rotating group:
 C93(H93A,H93B,H93C), C91(H91A,H91B,H91C), C96(H96A,H96B,H96C)
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_olex2_submission_original_sample_id p17244
_olex2_submission_special_instructions 'No special instructions were received'