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_1565461
_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         'C20 H19 Au N4 O2 S'
_chemical_formula_sum            'C20 H19 Au N4 O2 S'
_chemical_formula_weight         576.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 92.8016(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0999(2)
_cell_length_b                   8.23711(15)
_cell_length_c                   15.1811(2)
_cell_measurement_reflns_used    5110
_cell_measurement_temperature    99.95(13)
_cell_measurement_theta_max      73.9020
_cell_measurement_theta_min      4.0190
_cell_volume                     1885.96(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_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_environment      N~2~
_diffrn_ambient_temperature      99.95(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.7110
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9559
_diffrn_measured_fraction_theta_max 0.9559
_diffrn_measurement_details
;
  1 omega   16.00  115.00   1.0000    1.1100
omega____ theta____ kappa____ phi______ frames
    -       40.2978   38.0000 -150.0000 99

  2 omega   16.00  115.00   1.0000    1.1100
omega____ theta____ kappa____ phi______ frames
    -       40.2978   38.0000  -60.0000 99

  3 omega   24.00  109.00   1.0000    4.4350
omega____ theta____ kappa____ phi______ frames
    -      106.8887  -94.0000 -150.0000 85

  4 omega   31.00   69.00   1.0000    4.4350
omega____ theta____ kappa____ phi______ frames
    -      106.8887  -30.0000    0.0000 38

  5 omega   31.00   69.00   1.0000    4.4350
omega____ theta____ kappa____ phi______ frames
    -      106.8887  -30.0000  -30.0000 38

  6 omega   24.00  109.00   1.0000    4.4350
omega____ theta____ kappa____ phi______ frames
    -      106.8887  -94.0000  -90.0000 85

  7 omega   25.00  158.00   1.0000    4.4350
omega____ theta____ kappa____ phi______ frames
    -      106.8887  -15.0000   30.0000 133

  8 omega   34.00   77.00   1.0000    4.4350
omega____ theta____ kappa____ phi______ frames
    -      106.8887  -45.0000    0.0000 43

  9 omega  -96.00   -2.00   1.0000    1.1100
omega____ theta____ kappa____ phi______ frames
    -      -40.2978  125.0000  120.0000 94

 10 omega    8.00  116.00   1.0000    1.1100
omega____ theta____ kappa____ phi______ frames
    -       40.2978   77.0000   60.0000 108

 11 omega   81.00  158.00   1.0000    4.4350
omega____ theta____ kappa____ phi______ frames
    -      106.8887   45.0000  120.0000 77

 12 omega   34.00   77.00   1.0000    4.4350
omega____ theta____ kappa____ phi______ frames
    -      106.8887  -45.0000  -60.0000 43

 13 omega   79.00  104.00   1.0000    4.4350
omega____ theta____ kappa____ phi______ frames
    -      106.8887   30.0000 -150.0000 25

 14 omega   81.00  158.00   1.0000    4.4350
omega____ theta____ kappa____ phi______ frames
    -      106.8887   45.0000   60.0000 77
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0160375000
_diffrn_orient_matrix_UB_12      0.0348118000
_diffrn_orient_matrix_UB_13      -0.0991620000
_diffrn_orient_matrix_UB_21      0.1005977000
_diffrn_orient_matrix_UB_22      0.0180395000
_diffrn_orient_matrix_UB_23      -0.0094826000
_diffrn_orient_matrix_UB_31      0.0068638000
_diffrn_orient_matrix_UB_32      -0.1829686000
_diffrn_orient_matrix_UB_33      -0.0199511000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10760
_diffrn_reflns_theta_full        73.9615
_diffrn_reflns_theta_max         73.96
_diffrn_reflns_theta_min         4.03
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.900
_exptl_absorpt_correction_T_max  0.816
_exptl_absorpt_correction_T_min  0.454
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.0300
_exptl_crystal_description       plate
_exptl_crystal_F_000             1099.9832
_exptl_crystal_size_max          0.1425
_exptl_crystal_size_mid          0.0742
_exptl_crystal_size_min          0.0324
_refine_diff_density_max         1.6978
_refine_diff_density_min         -1.5974
_refine_diff_density_rms         0.2385
_refine_ls_d_res_high            0.8021
_refine_ls_d_res_low             10.9643
_refine_ls_goodness_of_fit_ref   1.0682
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    33
_refine_ls_number_parameters     255
_refine_ls_number_reflns         3659
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0682
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0263
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+4.9210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0739
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -18
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              -12
_reflns_number_gt                3233
_reflns_number_total             3659
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ICA-2020-502-119282.cif
_cod_data_source_block           Crystal95
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               1565461
_chemical_oxdiff_formula         C20H19AuN4O2S
_reflns_odcompleteness_completeness 98.92
_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.a Secondary CH2 refined with riding coordinates:
 C19(H19a,H19b)
2.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C13(H13), C1(H1), C12(H12), C15(H15), C24(H24), C26(H26), C25(H25),
 C23(H23), C2(H2), C3(H3)
2.c Idealised Me refined as rotating group:
 C18(H18a,H18b,H18c), C17(H17a,H17b,H17c)
;