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_7720546
_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         'C89 H85 Co2 N11 O6, 2(B F4), C3 H7 N O'
_chemical_formula_sum            'C92 H92 B2 Co2 F8 N12 O7'
_chemical_formula_weight         1769.25
_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             2025-05-29
_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                84.734(3)
_cell_angle_beta                 71.040(3)
_cell_angle_gamma                76.279(3)
_cell_formula_units_Z            2
_cell_length_a                   14.1055(5)
_cell_length_b                   19.2368(6)
_cell_length_c                   19.9639(6)
_cell_measurement_reflns_used    15479
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.5190
_cell_measurement_theta_min      2.0820
_cell_volume                     4976.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'PHOTON II Detector'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -102.91  13.09   1.00    4.00    --  -15.95 -59.25 122.08  116
  2  \w    -59.55  22.45   1.00    4.00    --  -15.95  83.74 -83.95   82
  3  \w   -102.91  13.09   1.00    4.00    --  -15.95 -59.25  20.08  116
  4  \w    -59.55  22.45   1.00    4.00    --  -15.95  83.74 174.05   82
;
_diffrn_measurement_device       'Bruker D8VENTURE with PHOTON II Detector'
_diffrn_measurement_method       'phi, omega and kappa scan'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0204438000
_diffrn_orient_matrix_UB_12      -0.0098567000
_diffrn_orient_matrix_UB_13      -0.0361193000
_diffrn_orient_matrix_UB_21      0.0117465000
_diffrn_orient_matrix_UB_22      0.0341474000
_diffrn_orient_matrix_UB_23      -0.0094453000
_diffrn_orient_matrix_UB_31      0.0491445000
_diffrn_orient_matrix_UB_32      -0.0133325000
_diffrn_orient_matrix_UB_33      0.0042242000
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_unetI/netI     0.0698
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            47916
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         1.699
_diffrn_source_type              Micro-focus
_exptl_absorpt_coefficient_mu    0.403
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58218
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'reddish pink'
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.020
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1102
_refine_ls_number_reflns         18637
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0678
_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^)+(0.0964P)^2^+4.3709P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1823
_refine_ls_wR_factor_ref         0.1956
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14641
_reflns_number_total             18637
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02420j2.cif
_cod_data_source_block           sol2
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7720546
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O Co B F'
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.917
_reflns_odcompleteness_completeness 98.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.62
_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
 F6-B2 \\sim F8A-B2 \\sim F8B-B2 \\sim F7A-B2 \\sim F7B-B2 \\sim F5A-B2 \\sim
F5B-B2
 with sigma of 0.02
 F1-B1 \\sim F2B-B1 \\sim F2A-B1 \\sim F3A-B1 \\sim F3B-B1 \\sim F4A-B1 \\sim
F4B-B1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F6) = Uanis(F5A) = Uanis(F5B) = Uanis(F8A) = Uanis(F8B) = Uanis(F7B) =
Uanis(F7A)
Uanis(F1) = Uanis(F2A) = Uanis(F2B) = Uanis(F3A) = Uanis(F3B) = Uanis(F4A) =
Uanis(F4B)
4. Others
 Sof(F2B)=Sof(F3B)=Sof(F4B)=Sof(F5B)=Sof(F7B)=Sof(F8B)=1-FVAR(1)
 Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F7A)=Sof(F8A)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C01C(H01A,H01B), C8(H8A,H8B), C9(H9A,H9B), C26(H26A,H26B), C43(H43A,H43B),
 C60(H60A,H60B)
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), C47(H47),
 C48(H48), C49(H49), C50(H50), C51(H51), C54(H54), C55(H55), C56(H56), C57(H57),
  C58(H58), C64(H64), C65(H65), C66(H66), C67(H67), C68(H68), C71(H71),
 C72(H72), C73(H73), C74(H74), C75(H75), C80(H80), C81(H81), C82(H82), C86(H86),
  C91(H91)
5.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C25(H25A,H25B,H25C), C42(H42A,H42B,H42C), C59(H59A,H59B,
 H59C), C76(H76A,H76B,H76C), C84(H84A,H84B,H84C), C85(H85A,H85B,H85C), C87(H87A,
 H87B,H87C), C88(H88A,H88B,H88C), C89(H89A,H89B,H89C), C90(H90A,H90B,H90C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              48502
_shelx_hkl_checksum              70520
_shelx_fab_checksum              20766
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.405
_oxdiff_exptl_absorpt_empirical_full_min 0.470