Electronic effects of substituents on the catalytic conversion of thiolates to alcohols by carboxylate bridged nonheme binuclear Fe(II) and Co(II) complexes.
Chakraborty, Anuj Baran; Hazra, Rajib; Mukherjee, Srimayee; Majumdar, Amit; Dalton transactions (Cambridge, England : 2003) 55 (2026) 1335–1348; doi:10.1039/d5dt02420j

data_7720547
_publ_section_title
;
 Electronic effects of substituents on the catalytic conversion of
 thiolates to alcohols by carboxylate bridged nonheme binuclear Fe(II) and
 Co(II) complexes.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1335
_journal_page_last               1348
_journal_paper_doi               10.1039/d5dt02420j
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C86 H75 F2 Fe2 N11 O3, 2(B F4), C2 H3 N'
_chemical_formula_sum            'C88 H78 B2 F10 Fe2 N12 O3'
_chemical_formula_weight         1674.94
_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
_audit_creation_date             2025-06-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2025-09-16 deposited with the CCDC.	2025-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                92.180(2)
_cell_angle_beta                 106.103(2)
_cell_angle_gamma                91.798(2)
_cell_formula_units_Z            2
_cell_length_a                   14.2379(6)
_cell_length_b                   15.3665(6)
_cell_length_c                   21.6986(9)
_cell_measurement_reflns_used    9670
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      25.61
_cell_measurement_theta_min      2.31
_cell_volume                     4553.5(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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8VENTURE with PHOTON II Detector'
_diffrn_measurement_method       'phi, omega and kappa scan'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0805
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            125731
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.690
_diffrn_reflns_theta_min         1.952
_diffrn_source_type              Micro-focus
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.391
_exptl_absorpt_correction_T_max  0.7395
_exptl_absorpt_correction_T_min  0.6902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1372 before and 0.0837 after correction.
The Ratio of minimum to maximum transmission is 0.9333.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1732
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.687
_refine_diff_density_min         -0.920
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1038
_refine_ls_number_reflns         17264
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0627
_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^)+(0.0849P)^2^+5.6185P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1624
_refine_ls_wR_factor_ref         0.1700
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13415
_reflns_number_total             17264
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02420j2.cif
_cod_data_source_block           mo_am060625a_0m
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7720547
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.926
_shelx_estimated_absorpt_t_min   0.912
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F8-B2 \\sim F7-B2 \\sim F10B-B2 \\sim F10A-B2 \\sim F9A-B2 \\sim F9B-B2
 with sigma of 0.02
 C72B-C71 \\sim C73B-C72B \\sim C74B-C73B \\sim C75B-C74B \\sim C76B-C75B \\sim
C76B-C71 \\sim C72A-
 C71 \\sim C73A-C72A \\sim C74A-C73A \\sim C75A-C74A \\sim C76A-C75A \\sim
C76A-C71
 with sigma of 0.02
 N12B-C88 \\sim N12A-C88
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C71) = Uanis(C72A) = Uanis(C73A) = Uanis(C74A) = Uanis(C75A) =
Uanis(C76A) = Uanis(C72B) = Uanis(C73B) = Uanis(C74B) = Uanis(C75B) =
Uanis(C76B)
Uanis(F7) = Uanis(F9A) = Uanis(F9B) = Uanis(F10A) = Uanis(F10B)
Uanis(N12A) = Uanis(N12B)
Uanis(C88) = Uanis(N12A) = Uanis(N12B)
4. Others
 Sof(C72B)=Sof(H72B)=Sof(C73B)=Sof(H73B)=Sof(C74B)=Sof(H74B)=Sof(C75B)=
 Sof(H75B)=Sof(C76B)=Sof(H76B)=Sof(F9B)=Sof(F10B)=Sof(N12B)=1-FVAR(1)
 Sof(C72A)=Sof(H72A)=Sof(C73A)=Sof(H73A)=Sof(C74A)=Sof(H74A)=Sof(C75A)=
 Sof(H75A)=Sof(C76A)=Sof(H76A)=Sof(F9A)=Sof(F10A)=Sof(N12A)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C26(H26A,H26B), C43(H43A,H43B), C44(H44A,H44B),
 C61(H61A,H61B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C20(H20),
 C21(H21), C22(H22), C23(H23), C24(H24), C30(H30), C31(H31), C32(H32), C33(H33),
  C34(H34), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C48(H48),
 C49(H49), C50(H50), C51(H51), C52(H52), C55(H55), C56(H56), C57(H57), C58(H58),
  C59(H59), C65(H65), C66(H66), C67(H67), C68(H68), C69(H69), C72A(H72A),
 C72B(H72B), C73A(H73A), C73B(H73B), C74A(H74A), C74B(H74B), C75A(H75A),
 C75B(H75B), C76A(H76A), C76B(H76B), C81(H81), C82(H82), C83(H83)
5.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C25(H25A,H25B,H25C), C42(H42A,H42B,H42C), C60(H60A,H60B,
 H60C), C77(H77A,H77B,H77C), C86(H86A,H86B,H86C), C87(H87A,H87B,H87C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              23461
_shelx_hkl_checksum              44339
_shelx_fab_checksum              96950
_olex2_submission_special_instructions 'No special instructions were received'