Steric and electronic influence on Cu-Cu short contacts in β-thioketiminato tricopper(I) clusters.
Penki, Venkata Sai Sashankh; Chu, Yu-Ting; Chen, Hsing-Yin; Sudewi, Sri; Li, Chien-Hung; Huang, Genin Gary; Hsu, Sodio C. N.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 13160–13173; doi:10.1039/d4dt01549e

data_7716532
_publ_section_title
;
 Steric and electronic influence on Cu-Cu short contacts in
 &#x3b2;-thioketiminato tricopper(I) clusters.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13160
_journal_page_last               13173
_journal_paper_doi               10.1039/d4dt01549e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C33 H33 Cu3 N6 O6 S3, C H2 Cl2'
_chemical_formula_sum            'C34 H35 Cl2 Cu3 N6 O6 S3'
_chemical_formula_weight         981.38
_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   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2jmgvh
_audit_creation_date             2024-03-15
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-03-22 deposited with the CCDC.	2024-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                102.293(2)
_cell_angle_beta                 107.274(2)
_cell_angle_gamma                114.886(2)
_cell_formula_units_Z            2
_cell_length_a                   12.8659(8)
_cell_length_b                   14.5520(10)
_cell_length_c                   14.7553(8)
_cell_measurement_reflns_used    9332
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.31
_cell_measurement_theta_min      2.50
_cell_volume                     2203.5(2)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1002
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            64947
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.440
_diffrn_reflns_theta_min         2.503
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.744
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1136 before and 0.0801 after correction.
The Ratio of minimum to maximum transmission is 0.7711.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         8118
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0451P)^2^+2.4216P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1157
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5811
_reflns_number_total             8118
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01549e2.cif
_cod_data_source_block           d24948
_cod_depositor_comments
'Adding full bibliography for 7716532--7716537.cif.'
_cod_database_code               7716532
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.792
_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:
 C01L(H01W,H01X)
2.b Aromatic/amide H refined with riding coordinates:
 C00R(H00R), C00S(H00S), C00U(H00U), C00X(H00X), C00Y(H00Y), C00Z(H00Z),
 C013(H013), C015(H015), C016(H016), C017(H017), C019(H019), C01A(H01D),
 C01B(H01E), C01C(H01F), C01F(H01M)
2.c Idealised Me refined as rotating group:
 C018(H01A,H01B,H01C), C01D(H01G,H01H,H01I), C01E(H01J,H01K,H01L), C01G(H01N,
 H01O,H01P), C01H(H01Q,H01R,H01S), C01K(H01T,H01U,H01V)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              10012
_shelx_fab_checksum              94978
_olex2_submission_special_instructions 'No special instructions were received'