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_1565459
_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         'C15 H17 N3 O2 S'
_chemical_formula_sum            'C15 H17 N3 O2 S'
_chemical_formula_weight         303.39
_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                89.096(5)
_cell_angle_beta                 79.418(6)
_cell_angle_gamma                82.735(5)
_cell_formula_units_Z            2
_cell_length_a                   6.9323(4)
_cell_length_b                   8.5240(6)
_cell_length_c                   12.5071(8)
_cell_measurement_reflns_used    3287
_cell_measurement_temperature    100.05(16)
_cell_measurement_theta_max      73.5010
_cell_measurement_theta_min      3.5700
_cell_volume                     720.63(8)
_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      100.05(16)
_diffrn_detector_area_resol_mean 10.7110
_diffrn_measured_fraction_theta_full 0.9556
_diffrn_measured_fraction_theta_max 0.9556
_diffrn_measurement_details
;
  1 omega -109.00   -6.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.4945  -77.0000  120.0000 103

  2 omega  -34.00   63.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       39.4945  -57.0000 -150.0000 97

  3 omega  -20.00   53.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       39.4945  -37.0000  -60.0000 73

  4 omega  -84.00  -13.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000   61.0000   90.0000 71

  5 omega   29.00   69.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3169  -30.0000 -180.0000 40

  6 omega   31.00   63.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3169  -30.0000    0.0000 32

  7 omega   30.00   69.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3169  -30.0000   90.0000 39

  8 omega   23.00  109.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3169  -94.0000 -150.0000 86

  9 omega   38.00   99.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3169  -94.0000  120.0000 61

 10 omega   32.00  109.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3169  -94.0000   30.0000 77

 11 omega   30.00   61.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3169  -30.0000   30.0000 31

 12 omega   55.00  155.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3169   15.0000   30.0000 100

 13 omega   35.00  119.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3169  -61.0000 -120.0000 84

 14 omega   92.00  156.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3169   61.0000  -90.0000 64

 15 omega -113.00  -10.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.4945  -57.0000    0.0000 103

 16 omega   13.00  116.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       39.4945   37.0000 -120.0000 103

 17 omega   10.00  113.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       39.4945   57.0000  -60.0000 103

 18 omega -162.00  -49.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  -77.0000    0.0000 113

 19 omega -162.00  -49.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  -77.0000  -60.0000 113

 20 omega   77.00  158.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3169   61.0000   60.0000 81

 21 omega   77.00  158.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3169   30.0000 -120.0000 81

 22 omega   29.00   69.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3169  -30.0000 -120.0000 40

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

 24 omega   46.00  158.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.3169   15.0000 -180.0000 112
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0785243000
_diffrn_orient_matrix_UB_12      -0.1272522000
_diffrn_orient_matrix_UB_13      0.0755627000
_diffrn_orient_matrix_UB_21      0.1296086000
_diffrn_orient_matrix_UB_22      -0.0886954000
_diffrn_orient_matrix_UB_23      -0.0994484000
_diffrn_orient_matrix_UB_31      0.1701918000
_diffrn_orient_matrix_UB_32      0.0955871000
_diffrn_orient_matrix_UB_33      0.0101420000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7932
_diffrn_reflns_theta_full        73.7976
_diffrn_reflns_theta_max         73.80
_diffrn_reflns_theta_min         3.60
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.070
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67157
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.3981
_exptl_crystal_description       block
_exptl_crystal_F_000             321.5952
_exptl_crystal_size_max          0.1567
_exptl_crystal_size_mid          0.1088
_exptl_crystal_size_min          0.0666
_refine_diff_density_max         0.3603
_refine_diff_density_min         -0.4008
_refine_diff_density_rms         0.1000
_refine_ls_d_res_high            0.8028
_refine_ls_d_res_low             12.2940
_refine_ls_goodness_of_fit_ref   1.0321
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    27
_refine_ls_number_parameters     193
_refine_ls_number_reflns         2798
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0321
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0410P)^2^+0.3870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0946
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              10
_reflns_limit_k_min              -10
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                2347
_reflns_number_total             2798
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ICA-2020-502-119282.cif
_cod_data_source_block           Crystal44
_cod_original_cell_volume        720.64(8)
_cod_database_code               1565459
_chemical_oxdiff_formula         C15H17N3O2S
_reflns_odcompleteness_completeness 99.03
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7a,H7b)
2.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N1(H1), C15(H15), C12(H12), C13(H13), C16(H16)
2.c Idealised Me refined as rotating group:
 C6(H6a,H6b,H6c), C8(H8a,H8b,H8c), C5(H5a,H5b,H5c)
;