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_7712954
_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_absolute_configuration unk
_chemical_formula_moiety         'C35 H39 Cu N P S'
_chemical_formula_sum            'C35 H39 Cu N P S'
_chemical_formula_weight         600.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-01-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-06-08 deposited with the CCDC.	2023-05-05 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.780(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.7209(2)
_cell_length_b                   11.5302(2)
_cell_length_c                   15.5452(3)
_cell_measurement_reflns_used    17852
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      26.8370
_cell_measurement_theta_min      1.7660
_cell_volume                     1548.74(5)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_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    -52.00 -17.00   0.50    5.66    --   10.60 -81.00  44.00   70
  2  \w     34.00  59.00   0.50    5.66    --   10.60  81.00 166.00   50
  3  \w    -42.00 -17.00   0.50    5.66    --  -10.90 -81.00  44.00   50
  4  \w     -4.00  21.00   0.50    5.66    --  -10.90  81.00 166.00   50
  5  \w    -54.00  -8.00   0.50    5.66    --   10.60 -77.00 -30.00   92
  6  \w     -3.00  27.00   0.50    5.66    --   10.60  82.00   0.00   60
  7  \w     16.00  41.00   0.50    5.66    --   10.60  82.00 -90.00   50
  8  \w     -4.00  21.00   0.50    5.66    --   10.60  82.00 -60.00   50
  9  \w     -2.00 100.00   0.50    5.66    --   10.60  57.00  60.00  204
 10  \w    -17.00  72.00   0.50    5.66    --   10.60  82.00 150.00  178
 11  \w    -17.00 100.00   0.50    5.66    --   10.60  82.00  60.00  234
 12  \w    -12.00 100.00   0.50    5.66    --   10.60  82.00 -30.00  224
 13  \w    -17.00  13.00   0.50    5.66    --   10.60  82.00 -90.00   60
 14  \w     -7.00  18.00   0.50    5.66    --   10.60  82.00-133.92   50
 15  \w     -7.00  20.00   0.50    5.66    --   10.60  82.00-180.00   54
 16  \w     75.00 100.00   0.50    5.66    --   10.60  82.00-180.00   50
 17  \w    -50.00 -24.00   0.50    5.66    --  -10.90 -77.00-120.00   52
 18  \w    -93.00 -53.00   0.50    5.66    --  -10.90 -77.00-120.00   80
 19  \w    -28.00  69.00   0.50    5.66    --  -10.90  77.00 -90.00  194
 20  \w    -54.00  18.00   0.50    5.66    --  -10.90 -57.00 150.00  144
 21  \w     36.00  62.00   0.50    5.66    --  -10.90  77.00 120.00   52
 22  \w    -18.00  11.00   0.50    5.66    --  -10.90  77.00 120.00   58
;
_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      -0.0115849000
_diffrn_orient_matrix_UB_12      -0.0594602000
_diffrn_orient_matrix_UB_13      -0.0105592000
_diffrn_orient_matrix_UB_21      -0.0341727000
_diffrn_orient_matrix_UB_22      -0.0084086000
_diffrn_orient_matrix_UB_23      0.0384266000
_diffrn_orient_matrix_UB_31      -0.0737590000
_diffrn_orient_matrix_UB_32      0.0132343000
_diffrn_orient_matrix_UB_33      -0.0230922000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27269
_diffrn_reflns_theta_full        27.03
_diffrn_reflns_theta_max         27.03
_diffrn_reflns_theta_min         2.21
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.848
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21522
_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    1.287
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         5395
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.090
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0881P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1136
_refine_ls_wR_factor_ref         0.1147
_reflns_number_gt                5206
_reflns_number_total             5395
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d3dt00474k2.cif
_cod_data_source_block           L1CuPPh3
_cod_database_code               7712954
_chemical_oxdiff_formula         'C35 H39 N1 S1 P1 Cu1'
_diffrn_oxdiff_digest_frames
;
01db579961fd1fe35b59d37300dcd1b252000257093
;
_diffrn_oxdiff_digest_hkl
;
014b380b221c1ad04f2d7204e23a867fd66e9e
;
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.477(13)
 0.523(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10), C19(H19), C20(H20), C21(H21), C22(H22),
 C23(H23), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C31(H31), C32(H32),
  C33(H33), C34(H34), C35(H35)
3.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)
;
_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 2.133
_oxdiff_exptl_absorpt_empirical_full_min 0.445