Sulfur insertion into group 12 metal dithiolate complexes: metal-dependent equilibria.
Sohail, Muhammad; Heinsen, Carsten; Oliver, Allen G.; Tsui, Emily Y.; Dalton transactions (Cambridge, England : 2003) 55 (2026) 4119–4127; doi:10.1039/d6dt00074f

data_7720033
_publ_section_title
;
 Sulfur insertion into group 12 metal dithiolate complexes:
 metal-dependent equilibria.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4119
_journal_page_last               4127
_journal_paper_doi               10.1039/d6dt00074f
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C19 H11 Cd N3 O2 S2, 2(C8 H20 N)'
_chemical_formula_sum            'C35 H51 Cd N5 O2 S2'
_chemical_formula_weight         750.32
_chemical_name_systematic
'bis(tetraethylammonium) tetrakis(4-methylbenzene-1-thiolato)-cadmium(ii)'
_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             2024-08-31
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2026-01-06 deposited with the CCDC.	2026-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.072(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5567(6)
_cell_length_b                   15.4561(11)
_cell_length_c                   24.0658(16)
_cell_measurement_reflns_used    8176
_cell_measurement_temperature    120.00
_cell_measurement_theta_max      21.271
_cell_measurement_theta_min      2.292
_cell_volume                     3554.7(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3186
_diffrn_reflns_av_unetI/netI     0.0731
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            141686
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        23.256
_diffrn_reflns_theta_max         23.256
_diffrn_reflns_theta_min         2.145
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.770
_exptl_absorpt_correction_T_max  0.8113
_exptl_absorpt_correction_T_min  0.7311
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1616 before and 0.1073 after correction.
The Ratio of minimum to maximum transmission is 0.9011.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic yellowish orange'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.174
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.697
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         5107
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0508
_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^)+(0.0302P)^2^+6.0925P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.1008
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3608
_reflns_number_total             5107
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00074f2.cif
_cod_data_source_block           ms0281_a
_cod_depositor_comments
'Adding full bibliography for 7720033--7720037.cif.'
_cod_database_code               7720033
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.878
_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
C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim
N5: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C36A \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43
\\sim N6: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C1: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
C19 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
3. Others
 Fixed Sof: C28(0.5) H28A(0.5) H28B(0.5) C29(0.5) H29A(0.5) H29B(0.5)
 H29C(0.5) C30(0.5) H30A(0.5) H30B(0.5) C31(0.5) H31A(0.5) H31B(0.5) H31C(0.5)
 C32(0.5) H32A(0.5) H32B(0.5) C33(0.5) H33A(0.5) H33B(0.5) H33C(0.5) C34(0.5)
 H34A(0.5) H34B(0.5) C35(0.5) H35A(0.5) H35B(0.5) H35C(0.5) N5(0.5) C36A(0.5)
 H36A(0.5) H36B(0.5) C37(0.5) H37A(0.5) H37B(0.5) H37C(0.5) C38(0.5) H38A(0.5)
 H38B(0.5) C39(0.5) H39A(0.5) H39B(0.5) H39C(0.5) C40(0.5) H40A(0.5) H40B(0.5)
 C41(0.5) H41A(0.5) H41B(0.5) H41C(0.5) C42(0.5) H42A(0.5) H42B(0.5) C43(0.5)
 H43A(0.5) H43B(0.5) H43C(0.5) N6(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C22(H22A,H22B), C24(H24A,H24B), C26(H26A,H26B), C28(H28A,
 H28B), C30(H30A,H30B), C32(H32A,H32B), C34(H34A,H34B), C36A(H36A,H36B),
 C38(H38A,H38B), C40(H40A,H40B), C42(H42A,H42B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C15(H15),
 C16(H16), C17(H17), C18(H18)
4.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C27(H27A,H27B,
 H27C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C35(H35A,
 H35B,H35C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C),
 C43(H43A,H43B,H43C)
;
_shelx_res_checksum              42761
_olex2_submission_special_instructions 'No special instructions were received'