Cluster Self-Assembly and Anion Binding by Metal Complexes of Non-Innocent Thiazolidinyl-Thiolate Ligands
Riffel, Madeline N.; Siegel, Lukas; Oliver, Allen Grayson; Tsui, Emily Y.; Dalton Transactions  (2022) –; doi:10.1039/D2DT01339H

data_7710455
_publ_section_title
;
 Cluster Self-Assembly and Anion Binding by Metal Complexes of
 Non-Innocent Thiazolidinyl-Thiolate Ligands
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01339H
_journal_year                    2022
_chemical_formula_moiety         'C39 H54 N9 S6 Zn3, 3(C F3 O3 S)'
_chemical_formula_sum            'C42 H54 F9 N9 O9 S9 Zn3'
_chemical_formula_weight         1484.59
_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             2022-04-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-04-20 deposited with the CCDC.	2022-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                91.153(3)
_cell_angle_beta                 104.608(3)
_cell_angle_gamma                116.404(3)
_cell_formula_units_Z            2
_cell_length_a                   12.1151(10)
_cell_length_b                   12.5801(11)
_cell_length_c                   23.7692(19)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    119.98
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.36
_cell_volume                     3103.1(5)
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      119.98
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0278
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            81797
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.270
_diffrn_reflns_theta_min         1.829
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.535
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0578 before and 0.0474 after correction.
The Ratio of minimum to maximum transmission is 0.9092.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_description       Plates
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.284
_exptl_crystal_size_mid          0.228
_exptl_crystal_size_min          0.191
_refine_diff_density_max         1.037
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     776
_refine_ls_number_reflns         15334
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0310
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0238P)^2^+4.5173P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0723
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14022
_reflns_number_total             15334
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01339h2.cif
_cod_data_source_block           mr_1_286_a
_cod_database_code               7710455
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.758
_shelx_estimated_absorpt_t_min   0.670
_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
F1 \\sim F1A \\sim F2 \\sim F2A \\sim F3 \\sim F3A \\sim C40: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
3. Others
 Sof(F1A)=Sof(F2A)=Sof(F3A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C10(H10A,H10B), C11(H11A,H11B), C14(H14A,H14B),
 C15(H15A,H15B), C23(H23A,H23B), C24(H24A,H24B), C27(H27A,H27B), C28(H28A,H28B),
  C36(H36A,H36B), C37(H37A,H37B)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7A), C18(H18), C19(H19), C20(H20), C31(H31), C32(H32),
 C33(H33)
4.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              13580
_shelx_hkl_checksum              74015
_shelx_fab_checksum              68586
_olex2_submission_special_instructions 'No special instructions were received'