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_7720036
_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
'C27 H21 Cd N3 O2 S3, 2(C8 H20 N), 0.5(C2 H3 N)'
_chemical_formula_sum            'C44 H62.5 Cd N5.5 O2 S3'
_chemical_formula_weight         909.07
_chemical_name_systematic        '[Et4N]2[3Me-Cd(Stol)]'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-10-28
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_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
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.8332(15)
_cell_length_b                   18.2888(17)
_cell_length_c                   30.014(3)
_cell_measurement_reflns_used    9170
_cell_measurement_temperature    120.00
_cell_measurement_theta_max      26.32
_cell_measurement_theta_min      2.61
_cell_volume                     9240.1(15)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0539
_diffrn_reflns_av_unetI/netI     0.0122
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            401389
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.384
_diffrn_reflns_theta_min         2.132
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.649
_exptl_absorpt_correction_T_max  0.7985
_exptl_absorpt_correction_T_min  0.7257
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0854 before and 0.0564 after correction.
The Ratio of minimum to maximum transmission is 0.9088.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_description       block
_exptl_crystal_F_000             3816
_exptl_crystal_size_max          0.322
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.327
_refine_diff_density_min         -1.248
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         9445
_refine_ls_number_restraints     147
_refine_ls_restrained_S_all      1.168
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0748
_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^)+(0.0670P)^2^+42.8994P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1872
_refine_ls_wR_factor_ref         0.1904
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8776
_reflns_number_total             9445
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00074f2.cif
_cod_data_source_block           ms03151
_cod_depositor_comments
'Adding full bibliography for 7720033--7720037.cif.'
_cod_original_cell_volume        9240.2(15)
_cod_original_sg_symbol_H-M      Pbca
_cod_original_formula_sum        'C44 H62.50 Cd N5.50 O2 S3'
_cod_database_code               7720036
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.926
_shelx_estimated_absorpt_t_min   0.818
_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. Restrained distances
 C36-C37 \\sim C42-C43 \\sim C42A-C43A \\sim C40A-C41A \\sim C40-C41 \\sim
C38-C39
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N6 \\sim C44 \\sim C45: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
N5 \\sim C36 \\sim C38 \\sim C40 \\sim C42 \\sim C40A \\sim C42A \\sim C37
\\sim C39 \\sim C41 \\sim C43 \\sim C41A \\sim C43A: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
4. Others
 Fixed Sof: 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)
 C40A(0.5) H40C(0.5) H40D(0.5) C41A(0.5) H41D(0.5) H41E(0.5) H41F(0.5)
 C42A(0.5) H42C(0.5) H42D(0.5) C43A(0.5) H43D(0.5) H43E(0.5) H43F(0.5) N6(0.5)
 C44(0.5) C45(0.5) H45A(0.5) H45B(0.5) H45C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C30(H30A,H30B), C32(H32A,H32B), C34(H34A,H34B), C36(H36A,
 H36B), C38(H38A,H38B), C40(H40A,H40B), C42(H42A,H42B), C40A(H40C,H40D),
 C42A(H42C,H42D)
5.b Me refined with riding coordinates:
 C43A(H43D,H43E,H43F)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C16(H16),
 C17(H17), C18(H18), C19(H19), C22(H22), C23(H23), C25(H25), C26(H26)
5.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), 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), C41A(H41D,H41E,H41F),
 C45(H45A,H45B,H45C)
;
_shelx_res_checksum              13751
_olex2_submission_original_sample_id 'MS-03-151 [Et4N]2[3Me-Cd(Stol)]'
_olex2_submission_special_instructions 'No special instructions were received'