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_4132139
_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
'C60 H39 F9 Fe3 N6 O12 S3, C0.51 H1.06 Cl1.01'
_chemical_formula_sum            'C60.51 H40.06 Cl1.01 F9 Fe3 N6 O12 S3'
_chemical_formula_weight         1513.64
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2017-06-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_cell_angle_alpha                93.576(2)
_cell_angle_beta                 103.138(2)
_cell_angle_gamma                118.3998(18)
_cell_formula_units_Z            2
_cell_length_a                   12.5224(6)
_cell_length_b                   12.8854(6)
_cell_length_c                   21.9843(11)
_cell_measurement_reflns_used    9734
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      36.00
_cell_measurement_theta_min      2.30
_cell_volume                     2977.9(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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0476
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            98544
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.141
_diffrn_reflns_theta_min         2.239
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.970
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0842 before and 0.0564 after correction. The Ratio of minimum to maximum transmission is 0.8928. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_description       Block
_exptl_crystal_F_000             1531
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.440
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     941
_refine_ls_number_reflns         22669
_refine_ls_number_restraints     143
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0531P)^2^+1.9823P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1113
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17005
_reflns_number_total             22669
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b01825_si_001.cif
_cod_data_source_block           p17060
_cod_database_code               4132139
_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
 Cl2-C61 \\sim Cl1-C61
 with sigma of 0.02
 S3-O10 \\sim S3-O11 \\sim S0AA-O0AA \\sim S3-O12 \\sim S0AA-O16 \\sim S0AA-O10A
 with sigma of 0.02
 S0AA-C58A \\sim S3-C58
 with sigma of 0.02
 F18-C58A \\sim F17-C58A \\sim F19-C58A \\sim F8-C58 \\sim F7-C58 \\sim F9-C58
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 Cl2, C61, Cl1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O10, O10A, S3, O11, O16, O12, O0AA, S0AA, C58, F7, F8, C58A, F19, F17, F18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(Cl1)=Sof(Cl2)=Sof(C61)=FVAR(1)
 Sof(S0AA)=Sof(O0AA)=Sof(O16)=Sof(F17)=Sof(F18)=Sof(F19)=Sof(C58A)=Sof(O10A)=1-
 FVAR(2)
 Sof(S3)=Sof(O10)=Sof(O11)=Sof(O12)=Sof(F8)=Sof(F7)=Sof(F9)=Sof(C58)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C61(H61A,H61B)
5.b Aromatic/amide H refined with riding coordinates:
 C43(H43), C4(H4), C15(H15), C2(H2), C49(H49), C32(H32), C21(H21), C6(H6),
 C52(H52), C35(H35), C51(H51), C54(H54), C9(H9), C18(H18), C10(H10), C34(H34),
 C12(H12), C45(H45), C17(H17), C24(H24), C57(H57), C16(H16), C50(H50), C46(H46),
  C33(H33), C22(H22), C55(H55), C11(H11), C23(H23), C44(H44), C56(H56),
 C38(H38), C41(H41), C39(H39), C40(H40), C27(H27), C30(H30), C29(H29), C28(H28)
;
_olex2_submission_original_sample_id p17060
_olex2_submission_special_instructions 'No special instructions were received'