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_7717393
_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 Fe2 N4 S2, 2(F6 P), C2 H3 N'
_chemical_formula_sum            'C38 H47 F12 Fe2 N5 P2 S2'
_chemical_formula_weight         1039.56
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-08-25 deposited with the CCDC.	2024-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                92.109(3)
_cell_angle_beta                 101.285(3)
_cell_angle_gamma                102.490(3)
_cell_formula_units_Z            2
_cell_length_a                   10.992(3)
_cell_length_b                   11.940(4)
_cell_length_c                   17.155(5)
_cell_measurement_reflns_used    9461
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      2.72
_cell_volume                     2148.3(11)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      200.0
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0472
_diffrn_reflns_av_unetI/netI     0.0620
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16524
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.299
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.935
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6136
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1051 before and 0.0654 after correction.
The Ratio of minimum to maximum transmission is 0.8230.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_description       block
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.671
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     616
_refine_ls_number_reflns         7423
_refine_ls_number_restraints     228
_refine_ls_restrained_S_all      1.195
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0525
_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^)+(0.0905P)^2^+0.7957P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1505
_refine_ls_wR_factor_ref         0.1610
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5925
_reflns_number_total             7423
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02484b2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7717393--7717397.cif.'
_cod_original_cell_volume        2148.2(11)
_cod_database_code               7717393
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.814
_shelx_estimated_absorpt_t_min   0.754
_olex2_refinement_description
;
1. Restrained distances
 P2-F12 \\sim P2-F11'
 with sigma of 0.02
 P2-F8 \\sim P2-F8'
 with sigma of 0.02
 P2-F7 \\sim P2-F7'
 with sigma of 0.02
 P2-F9 \\sim P2-F9'
 with sigma of 0.02
 P2-F11 \\sim P2-F12'
 with sigma of 0.02
 P2-F10 \\sim P2-F10'
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
F8 \\sim F10' \\sim F9' \\sim F12 \\sim F12' \\sim F10 \\sim F9 \\sim F11'
\\sim F11 \\sim F8' \\sim F7 \\sim F7': within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
3. Rigid body (RIGU) restrains
 F7', F12', F9', F11', F10', F8', P2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F12, F11, F9, F8, F10, F7, P2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(F7')=Sof(F11')=Sof(F8')=Sof(F9')=Sof(F12')=Sof(F10')=1-FVAR(1)
 Sof(F12)=Sof(F8)=Sof(F7)=Sof(F9)=Sof(F11)=Sof(F10)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C29(H29A,H29B)
5.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N4(H4), C28(H28), C27(H27), C25(H25), C26(H26), C36(H36), C34(H34),
 C35(H35), C33(H33)
5.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C20(H20A,H20B,H20C), C9(H9A,H9B,H9C),
 C16(H16A,H16B,H16C), C10(H10A,H10B,H10C), C19(H19A,H19B,H19C), C17(H17A,H17B,
 H17C), C8(H8A,H8B,H8C), C18(H18A,H18B,H18C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              21263
_olex2_submission_special_instructions 'No special instructions were received'