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_7712955
_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         'C17 H25 N S'
_chemical_formula_sum            'C17 H25 N S'
_chemical_formula_weight         275.44
_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   mixed
_audit_creation_date             2023-04-09
_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                 99.025(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8498(4)
_cell_length_b                   8.9288(4)
_cell_length_c                   15.6583(6)
_cell_measurement_reflns_used    7741
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      26.9670
_cell_measurement_theta_min      1.7560
_cell_volume                     1636.21(11)
_computing_cell_refinement       'CrysAlisPro 1.171.41.36a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.41.36a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.36a (Rigaku OD, 2019)'
_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 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     -4.00  42.00   0.50    2.75    --   10.60  59.00 165.00   92
  2  \w    -26.00   0.00   0.50    2.75    --   10.60 -59.00  25.00   52
  3  \w    -42.00 -17.00   0.50    2.75    --  -10.90 -59.00  25.00   50
  4  \w    -14.00  11.00   0.50    2.75    --  -10.90  59.00 165.00   50
  5  \w    -63.00 -31.00   0.50    2.75    --   10.60 -77.00 -30.00   64
  6  \w     -6.00 100.00   0.50    2.75    --   10.60  77.00-120.00  212
  7  \w      3.00  36.00   0.50    2.75    --   10.60 -77.00 -90.00   66
  8  \w    -13.00 100.00   0.50    2.75    --   10.60  77.00-180.00  226
  9  \w     10.00  36.00   0.50    2.75    --   10.60 -77.00 -30.00   52
 10  \w     27.00  55.00   0.50    2.75    --   10.60  77.00-150.00   56
 11  \w    -20.00  16.00   0.50    2.75    --   10.60 -77.00  90.00   72
 12  \w    -78.00 -24.00   0.50    2.75    --  -10.90 -82.00  30.00  108
;
_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  0.0297
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13693
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.634
_exptl_absorpt_coefficient_mu    0.186
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.36a (Rigaku Oxford Diffraction, 2019)
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    1.118
_exptl_crystal_description       block
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.184
_refine_diff_density_min         -0.206
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2888
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0417P)^2^+0.5912P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.0952
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2467
_reflns_number_total             2888
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00474k2.cif
_cod_data_source_block           HL1
_cod_database_code               7712955
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.946
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.005
2.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              5420
_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
;