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_7712963
_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         'C24 H29 Cu N2 S'
_chemical_formula_sum            'C24 H29 Cu N2 S'
_chemical_formula_weight         441.09
_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                 109.714(3)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   8.3921(2)
_cell_length_b                   72.7477(11)
_cell_length_c                   11.9258(3)
_cell_measurement_reflns_used    25796
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      26.7090
_cell_measurement_theta_min      1.9940
_cell_volume                     6854.0(3)
_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 0.977
_diffrn_measured_fraction_theta_max 0.919
_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    -17.00 100.00   0.25   65.49    --   10.60  82.00-129.00  468
  2  \w    -46.00  78.00   0.25   65.49    --  -10.90  41.00  45.00  496
  3  \w    -79.00  31.00   0.25   65.49    --   10.60 -57.00 150.00  440
  4  \w    -13.00  94.00   0.25   65.49    --   10.60  77.00-150.00  428
  5  \w    -41.00  33.00   0.25   65.49    --  -10.90  57.00  60.00  296
;
_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  0.0523
_diffrn_reflns_av_unetI/netI     0.0580
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       59
_diffrn_reflns_limit_k_min       -93
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            63787
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.067
_diffrn_reflns_theta_min         1.680
_exptl_absorpt_coefficient_mu    1.058
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59073
_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    1.282
_exptl_crystal_description       block
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.579
_refine_diff_density_min         -0.711
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.238
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     781
_refine_ls_number_reflns         13864
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.238
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0712
_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^)+(0.0143P)^2^+22.8997P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1330
_refine_ls_wR_factor_ref         0.1388
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10714
_reflns_number_total             13864
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00474k2.cif
_cod_data_source_block           L2CuCNR
_cod_database_code               7712963
_shelx_shelxl_version_number     2018/3
_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.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C10(H10), C18(H18), C20(H20), C27(H27), C32(H32), C34(H34),
 C42(H42), C44(H44), C51(H51), C56(H56), C58(H58), C66(H66), C68(H68)
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), C22(H22a,H22b,H22c), C23(H23a,H23b,H23c), C24(H24a,H24b,
 H24c), C25(H25a,H25b,H25c), C29(H29a,H29b,H29c), C36(H36a,H36b,H36c), C37(H37a,
 H37b,H37c), C38(H38a,H38b,H38c), C46(H46a,H46b,H46c), C47(H47a,H47b,H47c),
 C48(H48a,H48b,H48c), C49(H49a,H49b,H49c), C53(H53a,H53b,H53c), C60(H60a,H60b,
 H60c), C61(H61a,H61b,H61c), C62(H62a,H62b,H62c), C70(H70a,H70b,H70c), C71(H71a,
 H71b,H71c), C72(H72a,H72b,H72c)
;
_shelx_res_checksum              45666
_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
;