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_7716536
_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         '0.08(C33 H30 Cl6 Cu3 N3 S3), 0.08(C7 H8)'
_chemical_formula_sum            'C3.27 H3.1 Cl0.49 Cu0.24 N0.24 S0.24'
_chemical_formula_weight         86.55
_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.cc2jmgxk
_audit_creation_date             2021-12-29
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2024-03-22 deposited with the CCDC.	2024-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.1340(10)
_cell_angle_gamma                90
_cell_formula_units_Z            98
_cell_length_a                   13.1496(2)
_cell_length_b                   15.5846(2)
_cell_length_c                   43.1275(5)
_cell_measurement_reflns_used    124255
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      26.9870
_cell_measurement_theta_min      1.8020
_cell_volume                     8749.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.56a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.56a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.56a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -20.00  99.32   0.38    9.46    --   10.60  57.00 120.00  314
  2  \w    -15.00  99.00   0.38    9.46    --   10.60  77.00 120.00  300
  3  \w    -15.00  99.00   0.38    9.46    --   10.60  77.00   0.00  300
  4  \w   -100.00  19.32   0.38    9.46    --  -10.90 -57.00-180.00  314
  5  \w   -100.00  14.00   0.38    9.46    --  -10.90 -77.00-180.00  300
  6  \w   -100.00  14.00   0.38    9.46    --  -10.90 -77.00 -60.00  300
  7  \w   -100.00  16.28   0.38    9.46    --  -10.90 -82.00 120.00  306
  8  \w    -41.00  78.32   0.38    9.46    --  -10.90  57.00  30.00  314
  9  \w    -79.00  40.32   0.38    9.46    --   10.60 -57.00-180.00  314
 10  \w    -79.00  40.32   0.38    9.46    --   10.60 -57.00 -90.00  314
 11  \w    -41.00  78.32   0.38    9.46    --  -10.90  57.00 120.00  314
 12  \w    -38.00  38.00   0.38    9.46    --  -10.90  82.00 150.00  200
;
_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      -0.0319140000
_diffrn_orient_matrix_UB_12      -0.0313070000
_diffrn_orient_matrix_UB_13      0.0056746000
_diffrn_orient_matrix_UB_21      -0.0164357000
_diffrn_orient_matrix_UB_22      -0.0139154000
_diffrn_orient_matrix_UB_23      -0.0155723000
_diffrn_orient_matrix_UB_31      0.0409506000
_diffrn_orient_matrix_UB_32      -0.0299541000
_diffrn_orient_matrix_UB_33      0.0012984000
_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  0.0416
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            190634
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.564
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.988
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38510
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.56a (Rigaku Oxford Diffraction, 2020)
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    1.610
_exptl_crystal_description       block
_exptl_crystal_F_000             4288
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.936
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1135
_refine_ls_number_reflns         15434
_refine_ls_number_restraints     3942
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0291
_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^)+(0.0221P)^2^+11.3508P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0647
_refine_ls_wR_factor_ref         0.0664
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13898
_reflns_number_total             15434
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01549e2.cif
_cod_data_source_block           k11012-sodio-k(26clnscu)
_cod_depositor_comments
'Adding full bibliography for 7716532--7716537.cif.'
_cod_original_formula_sum        'C3.27 H3.10 Cl0.49 Cu0.24 N0.24 S0.24'
_cod_database_code               7716536
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C N S Cl Cu'
_diffrn_oxdiff_digest_frames
;
019f2534490375f9b81c3d383b33c853600002528c6
;
_diffrn_oxdiff_digest_hkl
;
01e6603919b53ae514a405d0793e81544c4028
;
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C80-C75 \\sim C90-C89
 with sigma of 0.02
 C80-C79 \\sim C90-C91
 with sigma of 0.02
 C77-C76 \\sim C93-C94
 with sigma of 0.02
 C77-C78 \\sim C93-C92
 with sigma of 0.02
 C76-C75 \\sim C94-C89
 with sigma of 0.02
 C75-C74 \\sim C89-C88
 with sigma of 0.02
 C78-C79 \\sim C92-C91
 with sigma of 0.02
 C80-C76 \\sim C90-C94
 with sigma of 0.04
 C80-C78 \\sim C90-C92
 with sigma of 0.04
 C80-C74 \\sim C90-C88
 with sigma of 0.04
 C77-C75 \\sim C93-C89
 with sigma of 0.04
 C77-C79 \\sim C93-C91
 with sigma of 0.04
 C76-C78 \\sim C94-C92
 with sigma of 0.04
 C76-C74 \\sim C94-C88
 with sigma of 0.04
 C75-C79 \\sim C89-C91
 with sigma of 0.04
 C83-C82 \\sim C69-C68
 with sigma of 0.02
 C83-C84 \\sim C69-C70
 with sigma of 0.02
 C82-C87 \\sim C68-C73
 with sigma of 0.02
 C82-C81 \\sim C68-C67
 with sigma of 0.02
 C87-C86 \\sim C73-C72
 with sigma of 0.02
 C86-C85 \\sim C72-C71
 with sigma of 0.02
 C84-C85 \\sim C70-C71
 with sigma of 0.02
 C83-C87 \\sim C69-C73
 with sigma of 0.04
 C83-C85 \\sim C69-C71
 with sigma of 0.04
 C83-C81 \\sim C69-C67
 with sigma of 0.04
 C82-C86 \\sim C68-C72
 with sigma of 0.04
 C82-C84 \\sim C68-C70
 with sigma of 0.04
 C87-C85 \\sim C73-C71
 with sigma of 0.04
 C87-C81 \\sim C73-C67
 with sigma of 0.04
 C86-C84 \\sim C72-C70
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49
\\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57
\\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65
\\sim C66 \\sim C81 \\sim C82 \\sim C83 \\sim C84 \\sim C85 \\sim C86 \\sim C87
\\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim C67
\\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73 \\sim C88 \\sim C89
\\sim C90 \\sim C91 \\sim C92 \\sim C93 \\sim C94 \\sim N1 \\sim N2 \\sim N3
\\sim N4 \\sim N5 \\sim N6 \\sim S1 \\sim S2 \\sim S3 \\sim S4 \\sim S5 \\sim
S6 \\sim Cl1 \\sim Cl2 \\sim Cl3 \\sim Cl4 \\sim Cl5 \\sim Cl6 \\sim Cl7 \\sim
Cl8 \\sim Cl9 \\sim Cl10 \\sim Cl11 \\sim Cl12 \\sim Cu1 \\sim Cu2 \\sim Cu3
\\sim Cu4 \\sim Cu5 \\sim Cu6: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(C88)=Sof(H88A)=Sof(H88B)=Sof(H88C)=Sof(C89)=Sof(C90)=Sof(H90)=Sof(C91)=
 Sof(H91)=Sof(C92)=Sof(H92)=Sof(C93)=Sof(H93)=Sof(C94)=Sof(H94)=1-FVAR(1)
 Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(H74C)=Sof(C75)=Sof(C76)=Sof(H76)=Sof(C77)=
 Sof(H77)=Sof(C78)=Sof(H78)=Sof(C79)=Sof(H79)=Sof(C80)=Sof(H80)=FVAR(1)
 Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(H67C)=Sof(C68)=Sof(C69)=Sof(H69)=Sof(C70)=
 Sof(H70)=Sof(C71)=Sof(H71)=Sof(C72)=Sof(H72)=Sof(C73)=Sof(H73)=1-FVAR(2)
 Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(H81C)=Sof(C82)=Sof(C83)=Sof(H83)=Sof(C84)=
 Sof(H84)=Sof(C85)=Sof(H85)=Sof(C86)=Sof(H86)=Sof(C87)=Sof(H87)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10), C14(H14), C19(H19), C20(H20), C21(H21),
 C25(H25), C30(H30), C31(H31), C32(H32), C36(H36), C41(H41), C42(H42), C43(H43),
  C47(H47), C52(H52), C53(H53), C54(H54), C58(H58), C63(H63), C64(H64),
 C65(H65), C83(H83), C84(H84), C85(H85), C86(H86), C87(H87), C76(H76), C77(H77),
  C78(H78), C79(H79), C80(H80), C69(H69), C70(H70), C71(H71), C72(H72),
 C73(H73), C90(H90), C91(H91), C92(H92), C93(H93), C94(H94)
5.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C12(H12A,H12B,H12C), C16(H16A,H16B,H16C),
 C23(H23A,H23B,H23C), C27(H27A,H27B,H27C), C34(H34A,H34B,H34C), C38(H38A,H38B,
 H38C), C45(H45A,H45B,H45C), C49(H49A,H49B,H49C), C56(H56A,H56B,H56C), C60(H60A,
 H60B,H60C), C81(H81A,H81B,H81C), C74(H74A,H74B,H74C), C67(H67A,H67B,H67C),
 C88(H88A,H88B,H88C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 2.209
_oxdiff_exptl_absorpt_empirical_full_min 0.581