Pyrrole thioamide complexes of the d8 metals platinum(II), palladium(II) and gold(III)
Tang, Haiming; Saunders, Graham C.; Ma, Xiaochuan; Henderson, William; Inorganica Chimica Acta 502 (2020) 119282–; doi:10.1016/j.ica.2019.119282

data_1565460
_publ_section_title
;
 Pyrrole thioamide complexes of the d8 metals platinum(II), palladium(II)
 and gold(III)
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119282
_journal_paper_doi               10.1016/j.ica.2019.119282
_journal_volume                  502
_journal_year                    2020
_chemical_formula_moiety         'C25 H22 Au N3 S, 0.75(C H2 Cl2)'
_chemical_formula_sum            'C25.75 H23.5 Au Cl1.5 N3 S'
_chemical_formula_weight         657.21
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     iterative
_cell_angle_alpha                118.107(5)
_cell_angle_beta                 98.606(4)
_cell_angle_gamma                105.272(4)
_cell_formula_units_Z            2
_cell_length_a                   10.3271(5)
_cell_length_b                   12.0211(6)
_cell_length_c                   12.2148(5)
_cell_measurement_reflns_used    7563
_cell_measurement_temperature    111(15)
_cell_measurement_theta_max      73.9180
_cell_measurement_theta_min      4.1770
_cell_volume                     1221.73(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      111(15)
_diffrn_detector_area_resol_mean 10.7110
_diffrn_measured_fraction_theta_full 0.9968
_diffrn_measured_fraction_theta_max 0.9680
_diffrn_measurement_details
;
  1 omega -112.00  -10.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.3695  -57.0000  150.0000 102

  2 omega  -51.00   39.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.3695   77.0000  -90.0000 90

  3 omega  -20.00   81.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       39.3695  -99.0000   60.0000 101

  4 omega   35.00   77.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3169  -45.0000  -90.0000 42

  5 omega   77.00  158.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3169   61.0000 -150.0000 81

  6 omega   42.00  109.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3169 -111.0000  150.0000 67

  7 omega   30.00   57.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3169  -30.0000 -120.0000 27

  8 omega   33.00   77.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3169  -45.0000   30.0000 44

  9 omega   24.00  109.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3169  -94.0000  -90.0000 85

 10 omega   34.00   69.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3169  -30.0000  -30.0000 35

 11 omega   57.00  158.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3169   15.0000 -180.0000 101

 12 omega   23.00  106.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3169  -94.0000   30.0000 83

 13 omega   23.00  103.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3169  -94.0000 -180.0000 80

 14 omega   35.00   95.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3169  178.0000    0.0000 60

 15 omega -118.00   -6.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.3695  -77.0000  -90.0000 112

 16 omega -113.00  -10.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.3695  -57.0000  -30.0000 103

 17 omega -116.00  -13.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.3695  -37.0000   30.0000 103

 18 omega  -35.00   69.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       39.3695  -57.0000  150.0000 104

 19 omega -162.00  -49.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  -77.0000  120.0000 113

 20 omega   74.00  158.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3169   77.0000   30.0000 84

 21 omega   74.00  158.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3169   77.0000  -90.0000 84

 22 omega   74.00  158.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3169   77.0000  -60.0000 84

 23 omega   80.00  158.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3169   45.0000    0.0000 78

 24 omega   74.00  158.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3169   77.0000  150.0000 84

 25 omega   33.00   77.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3169  -45.0000  150.0000 44
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0218394000
_diffrn_orient_matrix_UB_12      0.0389039000
_diffrn_orient_matrix_UB_13      0.1428871000
_diffrn_orient_matrix_UB_21      0.0516083000
_diffrn_orient_matrix_UB_22      -0.1168077000
_diffrn_orient_matrix_UB_23      -0.0272678000
_diffrn_orient_matrix_UB_31      0.1534039000
_diffrn_orient_matrix_UB_32      0.0978618000
_diffrn_orient_matrix_UB_33      0.0405492000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13537
_diffrn_reflns_theta_full        73.7219
_diffrn_reflns_theta_max         73.72
_diffrn_reflns_theta_min         4.27
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.762
_exptl_absorpt_correction_T_max  0.793
_exptl_absorpt_correction_T_min  0.622
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.7864
_exptl_crystal_description       block
_exptl_crystal_F_000             634.0710
_exptl_crystal_size_max          0.1039
_exptl_crystal_size_mid          0.0615
_exptl_crystal_size_min          0.0454
_refine_diff_density_max         4.4368
_refine_diff_density_min         -2.2165
_refine_diff_density_rms         0.2389
_refine_ls_d_res_high            0.8031
_refine_ls_d_res_low             10.3595
_refine_ls_goodness_of_fit_ref   1.0369
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    42
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4783
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0369
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0880P)^2^+3.1670P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1210
_refine_ls_wR_factor_ref         0.1240
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              12
_reflns_limit_k_min              -14
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                4433
_reflns_number_total             4783
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ICA-2020-502-119282.cif
_cod_data_source_block           crystal28
_cod_original_cell_volume        1221.73(13)
_cod_database_code               1565460
_chemical_oxdiff_formula         C25H22AuN3S
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C40(0.75) H40a(0.75) H40b(0.75) Cl2(0.75) Cl1(0.75)
3.a Secondary CH2 refined with riding coordinates:
 C26(H26a,H26b), C40(H40a,H40b)
3.b Aromatic/amide H refined with riding coordinates:
 C32(H32), C24(H24), C35(H35), C21(H21), C23(H23), C34(H34), C33(H33),
 C22(H22), C16(H16), C12(H12), C15(H15), C2(H2), C14(H14), C13(H13)
3.c Idealised Me refined as rotating group:
 C6(H6a,H6b,H6c), C5(H5a,H5b,H5c)
;