Water Oxidation Catalysis by Mono- and Binuclear Iron Corroles
Sinha, Woormileela; Mahammed, Atif; Fridman, Natalia; Gross, Zeev; ACS Catalysis  (2020) 3764–; doi:10.1021/acscatal.9b05382

data_4517480
_publ_section_title
;
 Water Oxidation Catalysis by Mono- and Binuclear Iron Corroles
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              3764
_journal_paper_doi               10.1021/acscatal.9b05382
_journal_year                    2020
_chemical_formula_moiety         '2(C74 H46 Fe2 N8 O), 2(C3), C2'
_chemical_formula_sum            'C156 H92 Fe4 N16 O2'
_chemical_formula_weight         2445.86
_chemical_name_common            'Gross143 (Woormi)'
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-12-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                83.1530(10)
_cell_angle_beta                 79.3570(10)
_cell_angle_gamma                71.3010(10)
_cell_formula_units_Z            2
_cell_length_a                   15.2570(4)
_cell_length_b                   17.2020(5)
_cell_length_c                   25.3550(10)
_cell_measurement_reflns_used    21652
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.024
_cell_measurement_theta_min      0.819
_cell_volume                     6181.9(3)
_computing_cell_refinement       'DENZO HKL2000 (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius, 2006)'
_computing_data_reduction        'DENZO HKL2000 (Otwinowski & Minor 1997)'
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      200.15
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0890
_diffrn_reflns_av_unetI/netI     0.1342
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            21652
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.024
_diffrn_reflns_theta_max         25.024
_diffrn_reflns_theta_min         0.819
_exptl_absorpt_coefficient_mu    0.524
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Nonius KappaCCD'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       needle
_exptl_crystal_F_000             2520
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.747
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1520
_refine_ls_number_reflns         21652
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1915
_refine_ls_R_factor_gt           0.0913
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1375P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1951
_refine_ls_wR_factor_ref         0.2375
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18702
_reflns_number_total             21652
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs9b05382_si_003.cif
_cod_data_source_block           Gross143
_cod_database_code               4517480
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.954
_shelx_estimated_absorpt_t_min   0.872
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C84-C85
 1.5 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C26A) = Uanis(C31A)
Uanis(C64A) = Uanis(C29A)
Uanis(C66A) = Uanis(C67A)
4. Others
 Fixed Sof: C82(0.5) C83(0.5) C84(0.5) C85(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C8(H8), C9(H9), C12(H12), C13(H13), C17(H17), C18(H18),
 C25(H25), C24(H24), C23(H23), C22(H22), C21(H21), C27(H27), C28(H28), C29(H29),
  C30(H30), C31(H31), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37),
 C40(H40), C41(H41), C45(H45), C46(H46), C50(H50), C51(H51), C54(H54), C55(H55),
  C59(H59), C60(H60), C61(H61), C62(H62), C63(H63), C65(H65), C66(H66),
 C67(H67), C68(H68), C69(H69), C71(H71), C72(H72), C73(H73), C74(H74), C75(H75),
  C3A(H3A), C4A(H4A), C8A(H8A), C9A(H9A), C13A(H13A), C14A(H14A), C17A(H17A),
 C21A(H21A), C22A(H22A), C23A(H23A), C24A(H24A), C25A(H25A), C31A(H31A),
 C30A(H30A), C29A(H29A), C28A(H28A), C27A(H27A), C33A(H33A), C34A(H34A),
 C35A(H35A), C36A(H36A), C37A(H37A), C40A(H40A), C41A(H41A), C45A(H45A),
 C46A(H46A), C50A(H50A), C51A(H51A), C54A(H54A), C55A(H55A), C59A(H59A),
 C60A(H60A), C61A(H61A), C62A(H62A), C63A(H63A), C65A(H65A), C66A(H66A),
 C67A(H67A), C68A(H68A), C69A(H69A), C71A(H71A), C72A(H72A), C73A(H73A),
 C74A(H74A), C75A(H75A)
5.b Fitted hexagon refined as free rotating group:
 C20(C25,C24,C23,C22,C21), C26A(C31A,C30A,C29A,C28A,C27A), C64A(C65A,C66A,C67A,
 C68A,C69A)
;
_olex2_submission_special_instructions 'No special instructions were received'