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_4132140
_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 H63 Fe3 N12 O4, 3(C F3 O3 S), 0.5(C1 H2 Cl2)'
_chemical_formula_sum            'C87.5 H64 Cl F9 Fe3 N12 O13 S3'
_chemical_formula_weight         1961.68
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-06-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   23.4333(11)
_cell_length_b                   23.4333(11)
_cell_length_c                   9.7960(5)
_cell_measurement_reflns_used    9946
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.33
_cell_measurement_theta_min      2.66
_cell_volume                     4658.5(4)
_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)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.967
_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  0.0596
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            91999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.592
_diffrn_reflns_theta_min         2.309
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.640
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0945 before and 0.0573 after correction. The Ratio of minimum to maximum transmission is 0.8937. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_description       block
_exptl_crystal_F_000             2002
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.005
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         8466
_refine_ls_number_restraints     143
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0626
_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^)+(0.0930P)^2^+5.5130P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1678
_refine_ls_wR_factor_ref         0.1836
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6238
_reflns_number_total             8466
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b01825_si_001.cif
_cod_data_source_block           p17074
_cod_original_cell_volume        4658.5(5)
_cod_original_formula_sum        'C87.50 H64 Cl F9 Fe3 N12 O13 S3'
_cod_database_code               4132140
_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
 C31-Cl1 = C31-Cl2
 1.7 with sigma of 0.02
 Cl1-Cl2
 2.85 with sigma of 0.05
 S2-C30 \\sim S1-C29
 with sigma of 0.02
 S1-O3 \\sim S1-O4 \\sim S1-O5 \\sim S2-O5 \\sim S2-O4 \\sim S2-O6
 with sigma of 0.02
 F4-C30 \\sim F1-C29 \\sim F2-C30 \\sim F3-C30 \\sim F2-C29 \\sim F3-C29
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl1 \\sim C31 \\sim Cl2: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
4. Rigid body (RIGU) restrains
 S2, O4, O5, O6, F3, F4, F2, C30, S1, C29, F1, O3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(S1)=Sof(C29)=Sof(F1)=Sof(O3)=1-FVAR(1)
 Sof(S2)=Sof(O6)=Sof(F4)=Sof(C30)=FVAR(1)
 Fixed Sof: Cl1(0.16666) C31(0.16666) H31A(0.16666) H31B(0.16666) Cl2(0.16666)
6.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C11(H11), C20(H20), C14(H14), C4(H4), C12(H12), C5(H5), C22(H22),
 C13(H13), C21(H21), C7(H7), C19(H19), C6(H6), C16(H16), C28(H28), C27(H27),
 C26(H26), C25(H25), C24(H24), C18(H18), C17(H17)
6.c Fitted hexagon refined as free rotating group:
 C23(C28,C27,C26,C25,C24)
;
_olex2_submission_original_sample_id p17074
_olex2_submission_special_instructions 'No special instructions were received'