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_4132142
_publ_section_title
;
 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
'C86 H60 Fe4 N12 O6, 2(C F3 O3 S), 3.08(C H2 Cl2)'
_chemical_formula_sum            'C91.07 H66.15 Cl6.15 F6 Fe4 N12 O12 S2'
_chemical_formula_weight         2140.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                90
_cell_angle_beta                 106.580(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4988(5)
_cell_length_b                   45.032(2)
_cell_length_c                   14.6559(7)
_cell_measurement_reflns_used    9497
_cell_measurement_temperature    100
_cell_measurement_theta_max      79.43
_cell_measurement_theta_min      3.17
_cell_volume                     9171.1(7)
_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)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.97
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker AXS D8 VENTURE KAPPA'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0813
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       56
_diffrn_reflns_limit_k_min       -56
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            150997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         80.532
_diffrn_reflns_theta_min         3.180
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.732
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1327 before and 0.1024 after correction. The Ratio of minimum to maximum transmission is 0.5789. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_description       block
_exptl_crystal_F_000             4349
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.439
_refine_diff_density_min         -1.109
_refine_diff_density_rms         0.141
_refine_ls_extinction_coef       0.00105(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1230
_refine_ls_number_reflns         19794
_refine_ls_number_restraints     151
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1225
_refine_ls_R_factor_gt           0.1018
_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^)+(0.1469P)^2^+49.3094P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2745
_refine_ls_wR_factor_ref         0.2913
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15644
_reflns_number_total             19794
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b01825_si_001.cif
_cod_data_source_block           p17269
_cod_original_cell_volume        9171.2(7)
_cod_database_code               4132142
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl5-C91 \\sim Cl6-C91 \\sim Cl7_$1-C92_$1
 with sigma of 0.02
 Cl8-Cl7 \\sim Cl6_$2-Cl5_$2
 with sigma of 0.02
 Cl7-C92 \\sim Cl3_$1-C90_$1 \\sim Cl4_$1-C90_$1 \\sim Cl2_$3-C89_$3 \\sim
Cl1_$3-C89_$3
 with sigma of 0.02
 Cl8-Cl7 \\sim Cl1_$3-Cl2_$3
 with sigma of 0.02
 Cl8-Cl7 \\sim Cl4_$1-Cl3_$1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl1 \\sim C89 \\sim Cl2 \\sim Cl7 \\sim Cl8 \\sim C92 \\sim C91 \\sim Cl5 \\sim
Cl6 \\sim Cl4 \\sim Cl3 \\sim C90 \\sim C88 \\sim S2 \\sim O11 \\sim O12 \\sim
O10 \\sim F5 \\sim F4 \\sim F6 \\sim S1 \\sim O8 \\sim O7 \\sim O9 \\sim C87
\\sim F3 \\sim F1 \\sim F2: within 1.9A with sigma of 0.04 and sigma for
terminal atoms of 0.08
4. Others
 Sof(Cl3)=Sof(Cl4)=Sof(C90)=Sof(H90A)=Sof(H90B)=FVAR(1)
 Sof(Cl8)=Sof(Cl7)=Sof(C92)=Sof(H92A)=Sof(H92B)=FVAR(2)
 Sof(Cl1)=Sof(Cl2)=Sof(C89)=Sof(H89A)=Sof(H89B)=FVAR(3)
 Sof(Cl5)=Sof(Cl6)=Sof(C91)=Sof(H91A)=Sof(H91B)=FVAR(4)
5.a Secondary CH2 refined with riding coordinates:
 C92(H92A,H92B), C89(H89A,H89B), C90(H90A,H90B), C91(H91A,H91B)
5.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C52(H52), C9(H9), C12(H12), C2(H2), C38(H38), C58(H58), C23(H23),
 C18(H18), C59(H59), C22(H22), C33(H33), C76(H76), C4(H4), C67(H67), C46(H46),
 C49(H49), C11(H11), C80(H80), C35(H35), C30(H30), C17(H17), C43(H43), C54(H54),
  C45(H45), C83(H83), C51(H51), C57(H57), C32(H32), C41(H41), C15(H15),
 C77(H77), C40(H40), C10(H10), C66(H66), C24(H24), C68(H68), C27(H27), C39(H39),
  C16(H16), C21(H21), C81(H81), C56(H56), C84(H84), C29(H29), C82(H82),
 C71(H71), C50(H50), C44(H44), C28(H28), C75(H75), C34(H34), C72(H72), C73(H73),
  C62(H62), C63(H63), C65(H65), C55(H55), C64(H64), C74(H74)
;
_olex2_submission_original_sample_id p17269
_olex2_submission_special_instructions 'No special instructions were received'