Denticity Governs on the Formation of β-Thioketiminato Tri-Copper(I) and Mono-Copper(I) Complexes
Penki, Venkata Sai Sashankh; Chang, Yu-Lun; Chen, Hsing-Yin; Chu, Yu-Ting; Kuo, Yu-Ting; Dorairaj, Dorothy Priyanka Priyanka; Sudewi, Sri; Ding, Shangwu; Hsu, Sodio C. N.; Dalton Transactions  (2023) –; doi:10.1039/D3DT00474K

data_7712959
_publ_section_title
;
 Denticity Governs on the Formation of \b-Thioketiminato Tri-Copper(I) and
 Mono-Copper(I) Complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00474K
_journal_year                    2023
_chemical_formula_moiety         'C22 H26 Cu N3 S'
_chemical_formula_sum            'C22 H26 Cu N3 S'
_chemical_formula_weight         428.06
_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
_audit_creation_date             2023-03-20
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-05-02 deposited with the CCDC.	2023-05-05 downloaded from the CCDC.
;
_cell_angle_alpha                99.445(2)
_cell_angle_beta                 100.502(3)
_cell_angle_gamma                105.746(3)
_cell_formula_units_Z            4
_cell_length_a                   8.4434(3)
_cell_length_b                   13.9072(4)
_cell_length_c                   19.3518(6)
_cell_measurement_reflns_used    22426
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.0300
_cell_measurement_theta_min      1.7170
_cell_volume                     2094.98(13)
_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 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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -80.00  41.00   0.50    6.33    --    9.30 -38.00 -90.00  242
  2  \w    -18.00  99.00   0.50    6.33    --    9.30  82.00 -60.00  234
  3  \w    -20.00  99.00   0.50    6.33    --    9.30  57.00  90.00  238
  4  \w    -18.00  99.00   0.50    6.33    --    9.30  82.00 120.00  234
  5  \w    -80.00  37.00   0.50    6.33    --    9.30 -82.00-120.00  234
  6  \w    -80.00  37.00   0.50    6.33    --    9.30 -82.00-150.00  234
  7  \w    -80.00  39.00   0.50    6.33    --    9.30 -57.00 150.00  238
  8  \w    -16.00  99.00   0.50    6.33    --    9.30  77.00  30.00  230
  9  \w    -18.00  94.00   0.50    6.33    --    9.30  82.00-180.00  224
 10  \w    -11.00  14.00   0.50    6.33    --    9.30  82.00  90.00   50
 11  \w     24.00  71.00   0.50    6.33    --    9.30  82.00  90.00   94
 12  \w     -8.00  51.00   0.50    6.33    --    9.30  82.00   0.00  118
 13  \w    -19.00   8.00   0.50    6.33    --   -9.50 -82.00  90.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro II AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0598
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            43908
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.103
_exptl_absorpt_coefficient_mu    1.153
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31721
_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            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         7357
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0571P)^2^+0.4097P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1063
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6188
_reflns_number_total             7357
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00474k2.cif
_cod_data_source_block           L4CuCNR
_cod_original_cell_volume        2094.97(12)
_cod_database_code               7712959
_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.a Secondary CH2 refined with riding coordinates:
 C6(H6a,H6b), C7(H7a,H7b), C28(H28a,H28b), C29(H29a,H29b)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C9(H9), C10(H10), C11(H11), C12(H12), C16(H16), C18(H18), C25(H25),
 C31(H31), C32(H32), C33(H33), C34(H34), C38(H38), C40(H40)
2.c Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C5(H5a,H5b,H5c), C20(H20a,H20b,H20c), C21(H21a,H21b,H21c),
 C22(H22a,H22b,H22c), C23(H23a,H23b,H23c), C27(H27a,H27b,H27c), C42(H42a,H42b,
 H42c), C43(H43a,H43b,H43c), C44(H44a,H44b,H44c)
;
_shelx_res_checksum              36118
_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
;