Biomimics of [FeFe]-hydrogenases incorporating redox-active ligands: synthesis, redox properties and spectroelectrochemistry of diiron-dithiolate complexes with ferrocenyl-diphosphines as Fe4S4 surrogates
Orton, Georgia R. F.; Ghosh, Shishir; Alker, Lucy; Sarker, Jagodish C.; Pugh, David; Richmond, Michael G.; Hartl, František; Hogarth, Graeme; Dalton Transactions  (2022) –; doi:10.1039/D2DT00419D

data_7710491
_publ_section_title
;
 Biomimics of [FeFe]-hydrogenases incorporating redox-active ligands:
 synthesis, redox properties and spectroelectrochemistry of
 diiron-dithiolate complexes with ferrocenyl-diphosphines as Fe4S4
 surrogates
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00419D
_journal_year                    2022
_chemical_formula_moiety         'C50 H40 Fe3 N2 O4 P2 S2, 1.5[C6H12]'
_chemical_formula_sum            'C50 H40 Fe3 N2 O4 P2 S2'
_chemical_formula_weight         1026.45
_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     dual
_audit_creation_date             2022-04-17
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-05-16 deposited with the CCDC.	2022-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                79.137(4)
_cell_angle_beta                 74.698(4)
_cell_angle_gamma                83.481(4)
_cell_formula_units_Z            2
_cell_length_a                   12.2873(6)
_cell_length_b                   12.6980(6)
_cell_length_c                   18.6853(9)
_cell_measurement_reflns_used    6857
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.0150
_cell_measurement_theta_min      3.3390
_cell_volume                     2755.3(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 5.2031
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.833
_diffrn_measurement_details
;
  1 omega  -59.00   39.00   1.0000   46.0700
omega____ theta____ kappa____ phi______ frames
    -       12.2220  -57.0000  -30.0000 98

  2 omega  -20.00   54.00   1.0000   46.0700
omega____ theta____ kappa____ phi______ frames
    -       12.2220  -99.0000 -120.0000 74

  3 omega  -16.00   82.00   1.0000   46.0700
omega____ theta____ kappa____ phi______ frames
    -       12.2220   57.0000  120.0000 98
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0682
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.833
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18812
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.833
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.246
_diffrn_reflns_theta_min         3.029
_exptl_absorpt_coefficient_mu    0.953
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_correction_T_min  0.929
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_description       block
_exptl_crystal_F_000             1052
_exptl_crystal_size_max          0.2165
_exptl_crystal_size_mid          0.1939
_exptl_crystal_size_min          0.1504
_refine_diff_density_max         0.734
_refine_diff_density_min         -0.488
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         12487
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0544P)^2^+0.0048P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1228
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9542
_reflns_number_total             12487
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00419d2.cif
_cod_data_source_block           xstr0193
_cod_database_code               7710491
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2.a Rotating group:
 N2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23), C24(H24),
  C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
 C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C40(H40), C41(H41), C43(H43),
  C44(H44), C46(H46), C47(H47), C49(H49), C50(H50)
2.c X=CH2 refined with riding coordinates:
 N1(H1A,H1B)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 149 electrons were 
found in a volume of 758\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1.5[C6H12] per Asymmetric Unit 
which account for 144 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              60579
_shelx_fab_checksum              50200
_olex2_submission_special_instructions 'No special instructions were received'