A new family of thiolate-bridged bimetallic complexes featuring a benzimidazole moiety: synthesis, structure and redox reactivity.
Di, Kai; Yang, Dawei; Su, Linan; Du, Ronghuan; Dong, Shengbin; Wang, Baomin; Qu, Jingping; Dalton transactions (Cambridge, England : 2003) 53 (2024) 18754–18761; doi:10.1039/d4dt02484b

data_7717397
_publ_section_title
;
 A new family of thiolate-bridged bimetallic complexes featuring a
 benzimidazole moiety: synthesis, structure and redox reactivity.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18754
_journal_page_last               18761
_journal_paper_doi               10.1039/d4dt02484b
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C36 H44 Co2 N4 S2, 2(F6 P), 2(C H2 Cl2)'
_chemical_formula_sum            'C38 H48 Cl4 Co2 F12 N4 P2 S2'
_chemical_formula_weight         1174.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-04-08 deposited with the CCDC.	2024-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.113(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5804(8)
_cell_length_b                   36.884(3)
_cell_length_c                   12.2830(9)
_cell_measurement_reflns_used    4146
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      33.659
_cell_measurement_theta_min      4.527
_cell_volume                     4669.9(6)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1427
_diffrn_reflns_av_unetI/netI     0.1309
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            44435
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.943
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.180
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6329
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1177 before and 0.0970 after correction.
The Ratio of minimum to maximum transmission is 0.8493.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_description       block
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.29
_exptl_transmission_factor_max   33.659
_exptl_transmission_factor_min   4.527
_refine_diff_density_max         0.814
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.123
_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     624
_refine_ls_number_reflns         8134
_refine_ls_number_restraints     181
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1610
_refine_ls_R_factor_gt           0.0953
_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^)+(0.0479P)^2^+35.3672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1797
_refine_ls_wR_factor_ref         0.2050
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4801
_reflns_number_total             8134
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02484b2.cif
_cod_data_source_block           1_CCDC3
_cod_depositor_comments
'Adding full bibliography for 7717393--7717397.cif.'
_cod_original_cell_volume        4670.0(6)
_cod_database_code               7717397
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.726
_shelx_estimated_absorpt_t_min   0.697
_olex2_refinement_description
;
1. Restrained distances
 P2-F13 \\sim P2-F12
 with sigma of 0.02
 P2-F16 \\sim P2-F14
 with sigma of 0.02
 P2-F8 \\sim P2-F7
 with sigma of 0.02
 P2-F11 \\sim P2-F10
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
F9 \\sim F14 \\sim F13 \\sim F11 \\sim F16 \\sim F12 \\sim F7 \\sim F15 \\sim
F8 \\sim F10: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
3. Rigid body (RIGU) restrains
 F12, F7, F10, F14, F9, P2, F15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F13, F8, F11, F16, F9, P2, F15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Sof(F12)=Sof(F14)=Sof(F7)=Sof(F10)=1-FVAR(1)
 Sof(F13)=Sof(F16)=Sof(F8)=Sof(F11)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C21(H21A,H21B), C38(H38A,H38B), C37(H37A,H37B)
5.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N4(H4), C28(H28), C34(H34), C33(H33), C36(H36), C35(H35), C26(H26),
 C25(H25), C27(H27)
5.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C20(H20A,H20B,H20C), C8(H8A,H8B,H8C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C7(H7A,H7B,H7C), C17(H17A,H17B,H17C), C9(H9A,H9B,
 H9C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              19960
_olex2_submission_special_instructions 'No special instructions were received'