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_7717184
_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         'C23 H26 N2 S2'
_chemical_formula_sum            'C23 H26 N2 S2'
_chemical_formula_weight         394.58
_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             2022-03-02
_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                99.922(2)
_cell_angle_beta                 92.378(2)
_cell_angle_gamma                110.100(2)
_cell_formula_units_Z            2
_cell_length_a                   8.0998(3)
_cell_length_b                   10.7648(4)
_cell_length_c                   12.9362(5)
_cell_measurement_reflns_used    6799
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      66.561
_cell_measurement_theta_min      4.463
_cell_volume                     1037.20(7)
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0737
_diffrn_reflns_av_unetI/netI     0.0658
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13226
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        66.556
_diffrn_reflns_theta_max         66.556
_diffrn_reflns_theta_min         3.489
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.385
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.3754
_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 0.0869 after correction.
The Ratio of minimum to maximum transmission is 0.4987.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       block
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.206
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.109
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3616
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0548
_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^)+(0.0828P)^2^+0.5864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1441
_refine_ls_wR_factor_ref         0.1534
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2996
_reflns_number_total             3616
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02395a2.cif
_cod_data_source_block           q22038ja_0m
_cod_depositor_comments
'Adding full bibliography for 7717184--7717191.cif.'
_cod_database_code               7717184
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.781
_shelx_estimated_absorpt_t_min   0.639
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B)
2.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C3(H3), C7(H7), C8(H8), C10(H10), C11(H11), C14(H14),
 C15(H15), C17(H17), C18(H18), C21(H21)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C19(H19A,H19B,H19C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              98099
_shelx_hkl_checksum              53203
_olex2_submission_special_instructions 'No special instructions were received'