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_7716537
_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         '2(C33 H27 Cu3 F9 N3 S3), 2(C4 H8 O)'
_chemical_formula_sum            'C74 H70 Cu6 F18 N6 O2 S6'
_chemical_formula_weight         1990.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2jmgwj
_audit_creation_date             2023-06-05
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-03-22 deposited with the CCDC.	2024-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.566(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.8952(5)
_cell_length_b                   15.8452(3)
_cell_length_c                   27.6238(8)
_cell_measurement_reflns_used    31817
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      26.4790
_cell_measurement_theta_min      1.7030
_cell_volume                     8155.5(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_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      130(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -79.00 100.00   0.50   25.30    --   10.60 -19.00 -60.00  358
  2  \w    -79.00  38.00   0.50   25.30    --   10.60 -82.00  60.00  234
  3  \w    -79.00  36.00   0.50   25.30    --   10.60 -77.00  90.00  230
  4  \w    -79.00  41.00   0.50   25.30    --   10.60 -57.00   0.00  240
  5  \w    -15.00  96.00   0.50   25.30    --   10.60  77.00 -90.00  222
  6  \w     -7.00 100.00   0.50   25.30    --   10.60  82.00   0.00  214
  7  \w     16.00  49.00   0.50   25.30    --   10.60  77.00  30.00   66
  8  \w     20.00  60.00   0.50   25.30    --   10.60  77.00-180.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro II AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0270063000
_diffrn_orient_matrix_UB_12      0.0171537000
_diffrn_orient_matrix_UB_13      0.0182546000
_diffrn_orient_matrix_UB_21      0.0205996000
_diffrn_orient_matrix_UB_22      0.0107831000
_diffrn_orient_matrix_UB_23      -0.0183563000
_diffrn_orient_matrix_UB_31      -0.0171724000
_diffrn_orient_matrix_UB_32      0.0399051000
_diffrn_orient_matrix_UB_33      -0.0029068000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0614
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            105899
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.687
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.779
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30262
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_description       block
_exptl_crystal_F_000             4016
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.589
_refine_diff_density_min         -0.892
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1021
_refine_ls_number_reflns         14310
_refine_ls_number_restraints     1861
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0622
_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^)+(0.0327P)^2^+56.1705P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1299
_refine_ls_wR_factor_ref         0.1356
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11418
_reflns_number_total             14310
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01549e2.cif
_cod_data_source_block           k11205-sodio-b_auto
_cod_depositor_comments
'Adding full bibliography for 7716532--7716537.cif.'
_cod_database_code               7716537
_shelx_shelxl_version_number     2018/3
_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
 C68-C67
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C7 \\sim C8 \\sim C1 \\sim C20 \\sim C12 \\sim C51 \\sim C9 \\sim C18 \\sim C62
\\sim C5 \\sim C56 \\sim C63 \\sim C19 \\sim C53 \\sim C61 \\sim C6 \\sim C40
\\sim C64 \\sim C34 \\sim C13 \\sim C29 \\sim C17 \\sim C21 \\sim C39 \\sim C52
\\sim C45 \\sim C37 \\sim C11 \\sim C36 \\sim C66 \\sim C65 \\sim C30 \\sim C31
\\sim C50 \\sim C23 \\sim C10 \\sim C38 \\sim C16 \\sim C32 \\sim C35 \\sim C22
\\sim C24 \\sim C60 \\sim C41 \\sim C42 \\sim C14 \\sim C74 \\sim C57 \\sim C46
\\sim C28 \\sim C44 \\sim C55 \\sim C54 \\sim C27 \\sim C73 \\sim C33 \\sim C4
\\sim C15 \\sim C49 \\sim C43 \\sim C58 \\sim C59 \\sim C26 \\sim C25 \\sim C47
\\sim C48 \\sim C2 \\sim C71 \\sim C72 \\sim C3 \\sim C68 \\sim C67 \\sim C70
\\sim C69: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 3.8A
Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C20) \\sim
Ueq, Uanis(C12) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C9) \\sim Ueq,
Uanis(C18) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C56)
\\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C53) \\sim Ueq,
Uanis(C61) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C64)
\\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C29) \\sim Ueq,
Uanis(C17) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C52)
\\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(C36) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C30)
\\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C23) \\sim Ueq,
Uanis(C10) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C32)
\\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C24) \\sim Ueq,
Uanis(C60) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C14)
\\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C46) \\sim Ueq,
Uanis(C28) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C54)
\\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C33) \\sim Ueq,
Uanis(C4) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C43)
\\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C26) \\sim Ueq,
Uanis(C25) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C2)
\\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C3) \\sim Ueq,
Uanis(C68) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C69)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
4.a Secondary CH2 refined with riding coordinates:
 C74(H74A,H74B), C73(H73A,H73B), C71(H71A,H71B), C72(H72A,H72B), C68(H68A,
 H68B), C67(H67A,H67B), C70(H70A,H70B), C69(H69A,H69B)
4.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C5(H5), C63(H63), C19(H19), C52(H52), C36(H36), C30(H30), C38(H38),
 C16(H16), C60(H60), C41(H41), C14(H14), C27(H27), C49(H49), C58(H58), C25(H25),
  C47(H47), C3(H3)
4.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C11(H11A,H11B,H11C), C66(H66A,H66B,H66C), C65(H65A,H65B,
 H65C), C10(H10A,H10B,H10C), C32(H32A,H32B,H32C), C22(H22A,H22B,H22C), C44(H44A,
 H44B,H44C), C55(H55A,H55B,H55C), C54(H54A,H54B,H54C), C33(H33A,H33B,H33C),
 C43(H43A,H43B,H43C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              87314
_shelx_fab_checksum              34631
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.744
_oxdiff_exptl_absorpt_empirical_full_min 0.450