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_7717185
_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 N4 S4 Zn2, 1[C4H8O], 1[C6H14]'
_chemical_formula_sum            'C56 H70 N4 O S4 Zn2'
_chemical_formula_weight         1074.14
_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             2022-07-11
_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                 100.9930(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9162(5)
_cell_length_b                   19.8942(7)
_cell_length_c                   22.5497(10)
_cell_measurement_reflns_used    9932
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      72.145
_cell_measurement_theta_min      3.994
_cell_volume                     6128.4(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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 0.995
_diffrn_measured_fraction_theta_max 0.994
_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  0.0363
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            34406
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.206
_diffrn_reflns_theta_min         3.925
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.515
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.6197
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1283 before and 0.0536 after correction.
The Ratio of minimum to maximum transmission is 0.8223.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_description       plate
_exptl_crystal_F_000             2264
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF / hexane'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.188
_exptl_crystal_size_min          0.081
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         5994
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0789P)^2^+5.6082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1179
_refine_ls_wR_factor_ref         0.1222
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5484
_reflns_number_total             5994
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02395a2.cif
_cod_data_source_block           q22067ja_0ma
_cod_depositor_comments
'Adding full bibliography for 7717184--7717191.cif.'
_cod_database_code               7717185
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.822
_shelx_estimated_absorpt_t_min   0.500
_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.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B)
2.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)
2.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 396 electrons were 
found in a volume of 2532\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[C4H8O], 1[C6H14] per Formula Unit 
which account for 360 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              93047
_shelx_hkl_checksum              23979
_shelx_fab_checksum              20655
_olex2_submission_special_instructions 'No special instructions were received'