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_7712965
_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         'C12 H16 N2 S'
_chemical_formula_sum            'C12 H16 N2 S'
_chemical_formula_weight         220.33
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-30
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2022-06-08 deposited with the CCDC.	2023-05-05 downloaded from the CCDC.
;
_cell_angle_alpha                105.091(6)
_cell_angle_beta                 93.555(6)
_cell_angle_gamma                92.253(6)
_cell_formula_units_Z            2
_cell_length_a                   7.0013(5)
_cell_length_b                   7.2355(5)
_cell_length_c                   12.2312(9)
_cell_measurement_reflns_used    3797
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      26.6600
_cell_measurement_theta_min      1.7690
_cell_volume                     596.10(8)
_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 (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 0.997
_diffrn_measured_fraction_theta_max 0.940
_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     -1.00  96.00   0.50    8.83    --   10.60  57.00 120.00  194
  2  \w     57.00  89.00   0.50    8.83    --   10.60  82.00  60.00   64
  3  \w     58.00  96.00   0.50    8.83    --   10.60  82.00 -30.00   76
  4  \w    -17.00  27.00   0.50    8.83    --   10.60  82.00  60.00   88
  5  \w    -10.00  38.00   0.50    8.83    --   10.60  82.00 -30.00   96
  6  \w     37.00  95.00   0.50    8.83    --   10.60  77.00-180.00  116
  7  \w    -19.00  11.00   0.50    8.83    --   10.60  57.00 -30.00   60
  8  \w     28.00  98.00   0.50    8.83    --   10.60  57.00 -30.00  140
  9  \w    -17.00  43.00   0.50    8.83    --   10.60  82.00-120.00  120
 10  \w    -17.00  59.00   0.50    8.83    --   10.60  82.00 150.00  152
 11  \w    -35.00  71.00   0.50    8.83    --  -10.90  77.00  30.00  212
 12  \w     -6.00  22.00   0.50    8.83    --  -10.90 -38.00-180.00   56
;
_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      0.0000499000
_diffrn_orient_matrix_UB_12      -0.0141690000
_diffrn_orient_matrix_UB_13      -0.0596036000
_diffrn_orient_matrix_UB_21      -0.1016736000
_diffrn_orient_matrix_UB_22      -0.0057566000
_diffrn_orient_matrix_UB_23      -0.0045318000
_diffrn_orient_matrix_UB_31      0.0001037000
_diffrn_orient_matrix_UB_32      0.1005433000
_diffrn_orient_matrix_UB_33      0.0073944000
_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  0.0407
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6999
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.032
_diffrn_reflns_theta_min         2.920
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.241
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68633
_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    1.228
_exptl_crystal_description       block
_exptl_crystal_F_000             236
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         2447
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0698P)^2^+0.0482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1185
_refine_ls_wR_factor_ref         0.1232
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2014
_reflns_number_total             2447
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00474k2.cif
_cod_data_source_block           HL4
_cod_database_code               7712965
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C12 H16 N2 S1'
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.942
_diffrn_oxdiff_digest_frames
;
01501dafcf655fbed6ca82d2a05585482e00025d956
;
_diffrn_oxdiff_digest_hkl
;
01eb21f47998644c3f877532f5ff4c9078ec46
;
_reflns_odcompleteness_completeness 98.40
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H9,H10), C7(H11,H12)
2.b Aromatic/amide H refined with riding coordinates:
 N1(H8), C3(H4), C9(H13), C10(H14), C11(H15), C12(H16)
2.c Idealised Me refined as rotating group:
 C1(H1,H2,H3), C5(H5,H6,H7)
;
_shelx_res_checksum              27476
_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 1.438
_oxdiff_exptl_absorpt_empirical_full_min 0.666