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_4132143
_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         'C84 H60 Fe4 N12 O4, C F3 O3 S, 2.67(C2 N)'
_chemical_formula_sum            'C90.34 H60 F3 Fe4 N14.67 O7 S'
_chemical_formula_weight         1775.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-06-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_cell_angle_alpha                90
_cell_angle_beta                 115.389(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   40.403(4)
_cell_length_b                   17.5931(17)
_cell_length_c                   25.468(3)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    100
_cell_measurement_theta_max      78.659
_cell_measurement_theta_min      2.794
_cell_volume                     16355(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      100.03
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.1060
_diffrn_reflns_av_unetI/netI     0.0565
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            115838
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        66.547
_diffrn_reflns_theta_max         66.547
_diffrn_reflns_theta_min         2.788
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.422
_exptl_absorpt_correction_T_max  0.9682
_exptl_absorpt_correction_T_min  0.5266
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1414 before and 0.0887 after correction. The Ratio of minimum to maximum transmission is 0.5439. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_description       needle
_exptl_crystal_F_000             7262
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.253
_refine_diff_density_min         -1.691
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1071
_refine_ls_number_reflns         14365
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1124
_refine_ls_R_factor_gt           0.0847
_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^)+(0.1437P)^2^+150.0401P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2283
_refine_ls_wR_factor_ref         0.2541
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10798
_reflns_number_total             14365
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b01825_si_001.cif
_cod_data_source_block           p17223
_cod_database_code               4132143
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 N14-C89 = N13_$1-C87_$1 = C93_$2-N16_$2 = N15_$3-C91_$3
 2.71 with sigma of 0.01
 C89-C88 = C86_$1-C87_$1 = C93_$2-C92_$2 = C90_$3-C91_$3 = C94-C95
 1.458 with sigma of 0.01
 N14-C88 = N13_$1-C86_$1 = N16_$2-C92_$2 = N15_$3-C90_$3 = C94-N17
 1.157 with sigma of 0.01
 N17-C95
 2.71 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
N14 \\sim C89 \\sim C88: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
N14 \\sim C89 \\sim C88 \\sim C87 \\sim C86 \\sim N13: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C93 \\sim C92 \\sim N16: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C91 \\sim C94 \\sim N17 \\sim C95 \\sim N16 \\sim C92 \\sim C93 \\sim C90 \\sim
N15 \\sim C89 \\sim N14 \\sim C88 \\sim N13 \\sim C87 \\sim C86: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Others
 Sof(C87)=Sof(C86)=Sof(N13)=1-FVAR(1)
 Sof(N14)=Sof(C89)=Sof(C88)=FVAR(1)
 Sof(C94)=Sof(N17)=Sof(C90)=Sof(N15)=Sof(C91)=Sof(C95)=1-FVAR(2)
 Sof(N16)=Sof(C92)=Sof(C93)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C72(H72), C12(H12), C2(H2), C24(H24), C63(H63), C39(H39), C59(H59),
 C16(H16), C28(H28), C67(H67), C75(H75), C50(H50), C10(H10), C18(H18), C49(H49),
  C6(H6), C46(H46), C53(H53), C76(H76), C43(H43), C17(H17), C34(H34), C38(H38),
 C30(H30), C11(H11), C21(H21), C73(H73), C32(H32), C15(H15), C48(H48), C74(H74),
  C44(H44), C54(H54), C62(H62), C64(H64), C35(H35), C83(H83), C71(H71),
 C41(H41), C56(H56), C66(H66), C9(H9), C58(H58), C81(H81), C82(H82), C68(H68),
 C29(H29), C23(H23), C65(H65), C77(H77), C27(H27), C80(H80), C51(H51), C45(H45),
  C33(H33), C84(H84), C22(H22), C55(H55), C40(H40)
;
_olex2_submission_original_sample_id p17223
_olex2_submission_special_instructions 'No special instructions were received'