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_1565156
_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         'C43 H47 Ir N2 P S'
_chemical_formula_sum            'C43 H47 Ir N2 P S'
_chemical_formula_weight         847.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 101.7624(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.41539(11)
_cell_length_b                   21.3926(2)
_cell_length_c                   18.2604(2)
_cell_measurement_reflns_used    15608
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      73.8810
_cell_measurement_theta_min      4.1260
_cell_volume                     3600.77(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_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      101(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.7110
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9845
_diffrn_measured_fraction_theta_max 0.9845
_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     -6.00  31.00   1.00    1.00    --  -40.55  38.00  30.00   37
  2  \w     19.00  45.00   1.00    1.00    --   40.55-125.00  90.00   26
  3  \w     16.00 115.00   1.00    1.00    --   40.55  38.00-120.00   99
  4  \w    -32.00  65.00   1.00    1.00    --   40.55 -77.00 -30.00   97
  5  \w     70.00 134.00   1.00    2.79    --  106.89 -61.00 -60.00   64
  6  \w     84.00 158.00   1.00    2.79    --  106.89  61.00 120.00   74
  7  \w     89.00 148.00   1.00    2.79    --  106.89  30.00-180.00   59
  8  \w     81.00 138.00   1.00    2.79    --  106.89  45.00  30.00   57
  9  \w     26.00 105.00   1.00    2.79    --  106.89 -94.00 -90.00   79
 10  \w     73.00 131.00   1.00    2.79    --  106.89 125.00  30.00   58
 11  \w     62.00  89.00   1.00    2.79    --  106.89 -45.00 -90.00   27
 12  \w      2.00  97.00   1.00    1.00    --   40.55-125.00-150.00   95
 13  \w     12.00 114.00   1.00    1.00    --   40.55  57.00  90.00  102
 14  \w     16.00 115.00   1.00    1.00    --   40.55  38.00   0.00   99
 15  \w     78.00 158.00   1.00    2.79    --  106.89  61.00-150.00   80
 16  \w     35.00 136.00   1.00    2.79    --  106.89 -61.00  60.00  101
 17  \w     78.00 158.00   1.00    2.79    --  106.89  61.00 -30.00   80
 18  \w     34.00 121.00   1.00    2.79    --  106.89-125.00 -90.00   87
 19  \w     74.00 158.00   1.00    2.79    --  106.89  77.00  60.00   84
 20  \w     78.00 158.00   1.00    2.79    --  106.89  61.00 -90.00   80
 21  \w      8.00  85.00   1.00    1.00    --   40.55  77.00-120.00   77
 22  \w      8.00 117.00   1.00    1.00    --   40.55  77.00 150.00  109
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0294642000
_diffrn_orient_matrix_UB_12      0.0610825000
_diffrn_orient_matrix_UB_13      0.0452505000
_diffrn_orient_matrix_UB_21      -0.1209400000
_diffrn_orient_matrix_UB_22      -0.0166869000
_diffrn_orient_matrix_UB_23      0.0421150000
_diffrn_orient_matrix_UB_31      0.1113628000
_diffrn_orient_matrix_UB_32      -0.0343180000
_diffrn_orient_matrix_UB_33      0.0601031000
_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  0.0487
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33630
_diffrn_reflns_theta_full        74.2072
_diffrn_reflns_theta_max         74.21
_diffrn_reflns_theta_min         4.13
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.387
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015)
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    1.5625
_exptl_crystal_description       block
_exptl_crystal_F_000             1696.4704
_exptl_crystal_size_max          0.086
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.027
_refine_diff_density_max         1.1991
_refine_diff_density_min         -0.8547
_refine_diff_density_rms         0.1278
_refine_ls_d_res_high            0.8012
_refine_ls_d_res_low             10.6963
_refine_ls_goodness_of_fit_ref   1.0222
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    77
_refine_ls_number_parameters     441
_refine_ls_number_reflns         7230
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0222
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0256
_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^)+(0.0320P)^2^+0.5740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0600
_refine_ls_wR_factor_ref         0.0640
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              26
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                6158
_reflns_number_total             7230
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            Crystal3i.cif
_cod_data_source_block           Crystal124
_cod_database_code               1565156
_reflns_odcompleteness_completeness 99.95
_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:
 C23(H23), N2(H2), C22(H22), C12(H12), C14(H14), C24(H24), C42(H42), C35(H35),
 C16(H16), C45(H45), C36(H36), C46(H46), C13(H13), C33(H33), C44(H44), C43(H43),
  C26(H26), C15(H15), C25(H25), C32(H32), C34(H34)
2.c Idealised Me refined as rotating group:
 C57(H57a,H57b,H57c), C6(H6a,H6b,H6c), C59(H59a,H59b,H59c), C5(H5a,H5b,H5c),
 C58(H58a,H58b,H58c), C8(H8a,H8b,H8c), C56(H56a,H56b,H56c), C60(H60a,H60b,H60c)
;
_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 3.107
_oxdiff_exptl_absorpt_empirical_full_min 0.617