Pyrrole thioamide complexes of organo-rhodium(III), -iridium(III) and -ruthenium(II)
Tang, Haiming; Saunders, Graham C.; Raymond, Onyekachi; Ma, Xiaochuan; Henderson, William; Inorganica Chimica Acta 506 (2020) 119545–; doi:10.1016/j.ica.2020.119545

data_1565155
_publ_section_title
;
 Pyrrole thioamide complexes of organo-rhodium(III), -iridium(III) and
 -ruthenium(II)
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119545
_journal_paper_doi               10.1016/j.ica.2020.119545
_journal_volume                  506
_journal_year                    2020
_chemical_formula_moiety         '2(C23 H27 Ir N2 S)'
_chemical_formula_sum            'C46 H54 Ir2 N4 S2'
_chemical_formula_weight         1111.533
_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                90.321(2)
_cell_angle_beta                 96.465(2)
_cell_angle_gamma                90.118(3)
_cell_formula_units_Z            2
_cell_length_a                   11.6590(4)
_cell_length_b                   12.5787(4)
_cell_length_c                   14.1070(3)
_cell_measurement_reflns_used    9717
_cell_measurement_temperature    99.97(11)
_cell_measurement_theta_max      73.9470
_cell_measurement_theta_min      3.0970
_cell_volume                     2055.67(11)
_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
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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 1.3 (Dolomanov et al., 2009)'
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_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.97(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.7110
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9697
_diffrn_measured_fraction_theta_max 0.9420
_diffrn_measurement_details
;
  1 omega  -38.00  -13.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5478  -57.0000    0.0000 25

  2 omega  -98.00  -21.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5478  -77.0000  -90.0000 77

  3 omega -107.00  -72.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5478  -57.0000    0.0000 35

  4 omega  -97.00   -8.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5478  125.0000  -30.0000 89

  5 omega   44.00   71.00   1.0000    2.4350
omega____ theta____ kappa____ phi______ frames
    -      106.8887  -45.0000  120.0000 27

  6 omega   32.00   67.00   1.0000    2.4350
omega____ theta____ kappa____ phi______ frames
    -      106.8887  -30.0000  -90.0000 35

  7 omega   32.00   69.00   1.0000    2.4350
omega____ theta____ kappa____ phi______ frames
    -      106.8887  -30.0000  -30.0000 37

  8 omega   38.00   68.00   1.0000    2.4350
omega____ theta____ kappa____ phi______ frames
    -      106.8887  -30.0000    0.0000 30

  9 omega   43.00   69.00   1.0000    2.4350
omega____ theta____ kappa____ phi______ frames
    -      106.8887  -45.0000   30.0000 26

 10 omega   36.00   66.00   1.0000    2.4350
omega____ theta____ kappa____ phi______ frames
    -      106.8887  -30.0000  -60.0000 30

 11 omega   43.00   96.00   1.0000    2.4350
omega____ theta____ kappa____ phi______ frames
    -      106.8887  -94.0000    0.0000 53

 12 omega   39.00   69.00   1.0000    2.4350
omega____ theta____ kappa____ phi______ frames
    -      106.8887  -30.0000 -150.0000 30

 13 omega   65.00  120.00   1.0000    2.4350
omega____ theta____ kappa____ phi______ frames
    -      106.8887 -125.0000   90.0000 55

 14 omega   31.00   69.00   1.0000    2.4350
omega____ theta____ kappa____ phi______ frames
    -      106.8887  -30.0000 -180.0000 38

 15 omega   51.00  113.00   1.0000    2.4350
omega____ theta____ kappa____ phi______ frames
    -      106.8887 -125.0000  -60.0000 62

 16 omega   48.00   77.00   1.0000    2.4350
omega____ theta____ kappa____ phi______ frames
    -      106.8887  -45.0000 -120.0000 29

 17 omega -117.00   -8.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5478  -77.0000  -30.0000 109

 18 omega -113.00  -12.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5478  -57.0000  120.0000 101

 19 omega   16.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5478   38.0000 -120.0000 99

 20 omega  -34.00   65.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5478  -38.0000  150.0000 99

 21 omega   81.00  158.00   1.0000    2.4350
omega____ theta____ kappa____ phi______ frames
    -      106.8887   45.0000   60.0000 77

 22 omega   79.00  158.00   1.0000    2.4350
omega____ theta____ kappa____ phi______ frames
    -      106.8887   30.0000  120.0000 79

 23 omega   79.00  158.00   1.0000    2.4350
omega____ theta____ kappa____ phi______ frames
    -      106.8887   30.0000   30.0000 79

 24 omega   24.00  109.00   1.0000    2.4350
omega____ theta____ kappa____ phi______ frames
    -      106.8887  -94.0000 -180.0000 85

 25 omega   81.00  158.00   1.0000    2.4350
omega____ theta____ kappa____ phi______ frames
    -      106.8887   45.0000  -60.0000 77

 26 omega   78.00  158.00   1.0000    2.4350
omega____ theta____ kappa____ phi______ frames
    -      106.8887   61.0000 -120.0000 80

 27 omega   79.00  158.00   1.0000    2.4350
omega____ theta____ kappa____ phi______ frames
    -      106.8887   30.0000 -150.0000 79

 28 omega   34.00   77.00   1.0000    2.4350
omega____ theta____ kappa____ phi______ frames
    -      106.8887  -45.0000   60.0000 43
;
_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      0.0595481000
_diffrn_orient_matrix_UB_12      -0.1067629000
_diffrn_orient_matrix_UB_13      -0.0161352000
_diffrn_orient_matrix_UB_21      0.1175831000
_diffrn_orient_matrix_UB_22      0.0571827000
_diffrn_orient_matrix_UB_23      0.0058589000
_diffrn_orient_matrix_UB_31      0.0176663000
_diffrn_orient_matrix_UB_32      -0.0182263000
_diffrn_orient_matrix_UB_33      0.1085578000
_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  0.0554
_diffrn_reflns_av_unetI/netI     0.0620
_diffrn_reflns_Laue_measured_fraction_full 0.9697
_diffrn_reflns_Laue_measured_fraction_max 0.9420
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19158
_diffrn_reflns_point_group_measured_fraction_full 0.9697
_diffrn_reflns_point_group_measured_fraction_max 0.9420
_diffrn_reflns_theta_full        70.0000
_diffrn_reflns_theta_max         73.99
_diffrn_reflns_theta_min         3.15
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.582
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44319
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light orange'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.796
_exptl_crystal_description       plate
_exptl_crystal_F_000             1074.783
_exptl_crystal_size_max          0.1023
_exptl_crystal_size_mid          0.0796
_exptl_crystal_size_min          0.019
_refine_diff_density_max         1.6479
_refine_diff_density_min         -2.1387
_refine_diff_density_rms         0.4028
_refine_ls_d_res_high            0.8020
_refine_ls_d_res_low             14.0170
_refine_ls_goodness_of_fit_ref   1.0383
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    80
_refine_ls_number_parameters     501
_refine_ls_number_reflns         7878
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0383
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0275P)^2^+11.7744P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0828
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                6351
_reflns_number_total             7878
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            Crystal2bnew.cif
_cod_data_source_block           Crystal111
_cod_original_cell_volume        2055.67(10)
_cod_database_code               1565155
_reflns_odcompleteness_completeness 97.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C36(H36), C35(H35), C16(H16), C12(H12), C2(H2), C32(H32), C22(H22), C15(H15),
 C33(H33), C13(H13), C34(H34), C14(H14)
2.b Idealised Me refined as rotating group:
 C59(H59a,H59b,H59c), C60(H60a,H60b,H60c), C49(H49a,H49b,H49c), C26(H26a,H26b,
 H26c), C6(H6a,H6b,H6c), C56(H56a,H56b,H56c), C48(H48a,H48b,H48c), C46(H46a,
 H46b,H46c), C50(H50a,H50b,H50c), C25(H25a,H25b,H25c), C5(H5a,H5b,H5c),
 C58(H58a,H58b,H58c), C57(H57a,H57b,H57c), C47(H47a,H47b,H47c)
;
_olex2_submission_special_instructions 'No special instructions were received'