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_7712957
_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         'C32 H33 Cu N P S'
_chemical_formula_sum            'C32 H33 Cu N P S'
_chemical_formula_weight         558.16
_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
_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                90
_cell_angle_beta                 102.842(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.0853(6)
_cell_length_b                   10.8570(2)
_cell_length_c                   15.8802(4)
_cell_measurement_reflns_used    17974
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      26.5930
_cell_measurement_theta_min      2.2810
_cell_volume                     5729.7(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 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      113(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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     14.00  46.30   0.38   96.06    --   10.60  82.00  60.00   85
  2  \w    -20.00  44.22   0.38   96.06    --   10.60  57.00 -90.00  169
  3  \w    -34.00   9.32   0.38   96.06    --   10.60 -82.00-180.00  114
  4  \w    -15.00  77.72   0.38   96.06    --   10.60  82.00  90.00  244
  5  \w    -74.00  40.00   0.38   96.06    --   10.60 -57.00-120.00  300
  6  \w     71.00  98.36   0.38   96.06    --   10.60  57.00 -90.00   72
  7  \w    -14.00  26.28   0.38   96.06    --   10.60  82.00  30.00  106
  8  \w     66.00  91.08   0.38   96.06    --   10.60  82.00  30.00   66
  9  \w    -29.00  15.08   0.38   96.06    --  -10.90 -82.00-120.00  116
 10  \w    -81.00 -37.68   0.38   96.06    --  -10.90 -82.00-120.00  114
 11  \w    -38.00  13.30   0.38   96.06    --  -10.90 -57.00 -60.00  135
;
_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      0.0002138000
_diffrn_orient_matrix_UB_12      0.0648209000
_diffrn_orient_matrix_UB_13      -0.0055170000
_diffrn_orient_matrix_UB_21      0.0212822000
_diffrn_orient_matrix_UB_22      -0.0000586000
_diffrn_orient_matrix_UB_23      0.0130715000
_diffrn_orient_matrix_UB_31      0.0013917000
_diffrn_orient_matrix_UB_32      -0.0082243000
_diffrn_orient_matrix_UB_33      -0.0435761000
_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  0.0828
_diffrn_reflns_av_unetI/netI     0.0680
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            48453
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.570
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.912
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62181
_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            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_description       block
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.182
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     660
_refine_ls_number_reflns         10040
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.1121
_refine_ls_R_factor_gt           0.0873
_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^)+(0.0270P)^2^+43.1914P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1782
_refine_ls_wR_factor_ref         0.1873
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7735
_reflns_number_total             10040
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00474k2.cif
_cod_data_source_block           L2CuPPh3
_cod_database_code               7712957
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C32 H33 N2 P Cu'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.96245
 0.03755
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C10(H10), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20),
 C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30),
  C31(H31), C32(H32), C35(H35), C40(H40), C42(H42), C48(H48), C49(H49),
 C50(H50), C51(H51), C52(H52), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58),
  C60(H60), C61(H61), C62(H62), C63(H63), C64(H64)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C), C33(H33A,H33B,H33C), C37(H37A,H37B,H37C), C44(H44A,H44B,
 H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C)
;
_shelx_res_checksum              12537
_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 1.495
_oxdiff_exptl_absorpt_empirical_full_min 0.715