Helical dinuclear 3d metal complexes with bis(bidentate) [S,N] ligands: synthesis, structural and computational studies.
Allen, Jamie; Saßmannshausen, Jörg; Singh, Kuldip; Kilpatrick, Alexander F. R.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 17608–17619; doi:10.1039/d4dt02395a

data_7717189
_publ_section_title
;
 Helical dinuclear 3d metal complexes with bis(bidentate) [S,N] ligands:
 synthesis, structural and computational studies.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17608
_journal_page_last               17619
_journal_paper_doi               10.1039/d4dt02395a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C46 H48 Co2 N4 S4, 3[C7H8]'
_chemical_formula_sum            'C67 H72 Co2 N4 S4'
_chemical_formula_weight         1179.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6403)
;
_audit_update_record
;
2024-02-01 deposited with the CCDC.	2024-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.482(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9936(6)
_cell_length_b                   21.8180(12)
_cell_length_c                   28.6124(15)
_cell_measurement_reflns_used    9822
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      70.287
_cell_measurement_theta_min      4.053
_cell_volume                     6236.6(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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Quest Photon III'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0783
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            42785
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.318
_diffrn_reflns_theta_min         4.052
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.737
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.4414
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1416 before and 0.0893 after correction.
The Ratio of minimum to maximum transmission is 0.5860.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_description       plate
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.267
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.065
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.069
_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     257
_refine_ls_number_reflns         5935
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0643
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0619P)^2^+27.2534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1556
_refine_ls_wR_factor_ref         0.1630
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5058
_reflns_number_total             5935
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02395a2.cif
_cod_data_source_block           q22063ja_0m
_cod_depositor_comments
'Adding full bibliography for 7717184--7717191.cif.'
_cod_database_code               7717189
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.707
_shelx_estimated_absorpt_t_min   0.310
_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. Uiso/Uaniso restraints and constraints
C12 \\sim C13 \\sim C12 \\sim C9: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01 within 2A
3.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C8(H8), C10(H10), C11(H11), C14(H14), C15(H15), C17(H17),
 C18(H18), C20(H20)
3.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 620 electrons were 
found in a volume of 2600\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
3[C7H8] per Formula Unit 
which account for 600 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              25533
_shelx_hkl_checksum              39725
_shelx_fab_checksum              36670
_olex2_submission_special_instructions 'No special instructions were received'