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_7720034
_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
'0.667(C38 H22 Cd N6 O4 S6), 0.167(H O), 0.333(H2 O), 0.333(C6.5 H16.5 N), 0.667(C8 H20 N), 0.333(C8 H19 N), [+ solvents]'
_chemical_formula_sum            'C35.5 H40.67 Cd0.67 N5.33 O3.17 S4'
_chemical_formula_weight         795.96
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2026-01-06
_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                93.388(3)
_cell_angle_beta                 102.363(3)
_cell_angle_gamma                107.300(4)
_cell_formula_units_Z            6
_cell_length_a                   14.1642(14)
_cell_length_b                   18.917(2)
_cell_length_c                   23.983(2)
_cell_measurement_reflns_used    9534
_cell_measurement_temperature    120.00
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.20
_cell_volume                     5941.0(10)
_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 0.994
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0640
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            304390
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.358
_diffrn_reflns_theta_min         1.936
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.629
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6953
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1111 before and 0.0730 after correction.
The Ratio of minimum to maximum transmission is 0.9324.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dull yellow'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_description       block
_exptl_crystal_F_000             2474
_exptl_crystal_size_max          0.262
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.122
_refine_diff_density_max         1.418
_refine_diff_density_min         -1.277
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1441
_refine_ls_number_reflns         29528
_refine_ls_number_restraints     1033
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0421P)^2^+16.9932P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1447
_refine_ls_wR_factor_ref         0.1489
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25960
_reflns_number_total             29528
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00074f2.cif
_cod_data_source_block           ms_02_116_cdl2_heated
_cod_depositor_comments
'Adding full bibliography for 7720033--7720037.cif.'
_cod_original_cell_volume        5941.1(10)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C35.50 H40.67 Cd0.67 N5.33 O3.17 S4'
_cod_database_code               7720034
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.927
_shelx_estimated_absorpt_t_min   0.853
_diffrn_oxdiff_ac3_digest_hkl    41819cf8e6c5050afa15fb5c1d5a0a940fcb85
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 C117-C116 \\sim C119-C116
 with sigma of 0.02
 C117-C118 \\sim C119-C118
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C102 \\sim C107 \\sim C108 \\sim C114 \\sim C115 \\sim C118 \\sim C123 \\sim
C124: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
2A
C101 \\sim C105 \\sim C106 \\sim C109 \\sim C110 \\sim C116: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
N16 \\sim C123 \\sim C124 \\sim C120 \\sim C122: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
C115 \\sim N16 \\sim C107 \\sim C114 \\sim C118 \\sim C123 \\sim C105 \\sim
C109 \\sim C116 \\sim C120 \\sim H10A \\sim H10B \\sim C108 \\sim H11A \\sim
H11B \\sim H11F \\sim H11G \\sim C119 \\sim H12A \\sim H12B \\sim C124 \\sim
H10F \\sim H10G \\sim C106 \\sim H10K \\sim H10L \\sim C110 \\sim H11N \\sim
H11O \\sim C117 \\sim H12F \\sim H12G \\sim C122 \\sim H10C \\sim H10D \\sim
H10E \\sim H11C \\sim H11D \\sim H11E \\sim H11H \\sim H11I \\sim H11J \\sim
H12C \\sim H12D \\sim H12E \\sim H10H \\sim H10I \\sim H10J \\sim H11K \\sim
H11L \\sim H11M \\sim H11P \\sim H11Q \\sim H11R \\sim H12H \\sim H12I \\sim
H12J: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within
2A
4. Others
 Sof(H10M)=Sof(C101)=Sof(H10V)=Sof(H10W)=Sof(H10X)=Sof(C105)=Sof(H10F)=
 Sof(H10G)=Sof(C106)=Sof(H10H)=Sof(H10I)=Sof(H10J)=Sof(C109)=Sof(H10K)=
 Sof(H10L)=Sof(C110)=Sof(H11K)=Sof(H11L)=Sof(H11M)=Sof(C116)=Sof(H11N)=
 Sof(H11O)=1-FVAR(1)
 Sof(H100)=Sof(C102)=Sof(H10S)=Sof(H10T)=Sof(H10U)=Sof(C107)=Sof(H10A)=
 Sof(H10B)=Sof(C108)=Sof(H10C)=Sof(H10D)=Sof(H10E)=Sof(C114)=Sof(H11A)=
 Sof(H11B)=Sof(C115)=Sof(H11C)=Sof(H11D)=Sof(H11E)=Sof(C118)=Sof(H11F)=
 Sof(H11G)=Sof(C123)=Sof(H12A)=Sof(H12B)=FVAR(1)
 Fixed Sof: S8A(0.5) S8B(0.5) O5(0.5) H5A(0.5) C41(0.5) H41A(0.5) H41B(0.5)
 C42(0.5) H42A(0.5) H42B(0.5) H42C(0.5) C45(0.5) H45A(0.5) H45B(0.5) H97A(0.5)
 H97B(0.5) H97C(0.5) H97D(0.5) C99(0.5) H99A(0.5) H99B(0.5) H99C(0.5) C98(0.5)
 H98A(0.5) H98B(0.5) H98C(0.5) C119(0.5) H11H(0.5) H11I(0.5) H11J(0.5)
 C124(0.5) H12C(0.5) H12D(0.5) H12E(0.5) C117(0.5) H11P(0.5) H11Q(0.5)
 H11R(0.5) C120(0.5) H12F(0.5) H12G(0.5) C122(0.5) H12H(0.5) H12I(0.5) H12J(0.5)
5.a Free rotating group:
 O5(H5A), O10(H10Y,H)
5.b Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B), C41(H41A,H41B), C43(H43A,H43B), C45(H45A,H45B), C49(H49A,
 H49B), C51(H51A,H51B), C53(H53A,H53B), C55(H55A,H55B), C95(H95A,H95B),
 C97(H97A,H97B), C97(H97C,H97D), C103(H10N,H10O), C107(H10A,H10B), C114(H11A,
 H11B), C118(H11F,H11G), C123(H12A,H12B), C105(H10F,H10G), C109(H10K,H10L),
 C116(H11N,H11O), C120(H12F,H12G)
5.c 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), C21(H21), C22(H22), C23(H23), C24(H24), C28(H28),
  C29(H29), C30(H30), C34(H34), C35(H35), C36(H36), C37(H37), C58(H58),
 C59(H59), C60(H60), C61(H61), C65(H65), C66(H66), C67(H67), C71(H71), C72(H72),
  C73(H73), C74(H74), C77(H77), C78(H78), C79(H79), C80(H80), C84(H84),
 C85(H85), C86(H86), C90(H90), C91(H91), C92(H92), C93(H93), C100(H100),
 C100(H10M)
5.d Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C46(H46A,H46B,
 H46C), C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C56(H56A,
 H56B,H56C), C96(H96A,H96B,H96C), C104(H10P,H10Q,H10R), C99(H99A,H99B,H99C),
 C102(H10S,H10T,H10U), C98(H98A,H98B,H98C), C101(H10V,H10W,H10X), C108(H10C,
 H10D,H10E), C115(H11C,H11D,H11E), C119(H11H,H11I,H11J), C124(H12C,H12D,H12E),
 C106(H10H,H10I,H10J), C110(H11K,H11L,H11M), C117(H11P,H11Q,H11R), C122(H12H,
 H12I,H12J)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              65257
_shelx_fab_checksum              12365
_olex2_submission_original_sample_id MS-02-116
_olex2_submission_special_instructions 'No special instructions were received'