Synthesis of Rhodium‒Primary Thioamide Complexes and Their Desulfurization Leading to Rhodium Sulfido Cubane-Type Clusters and Nitriles
Mutoh, Yuichiro; Sakigawara, Masahiro; Niiyama, Ippei; Saito, Shinichi; Ishii, Youichi; Organometallics 33 (2014) 5414–; doi:10.1021/om500714c

data_4084391
_publ_section_title
;
 Synthesis of Rhodium--Primary Thioamide Complexes and Their
 Desulfurization Leading to Rhodium Sulfido Cubane-Type Clusters and
 Nitriles
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5414
_journal_paper_doi               10.1021/om500714c
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C18 H21 Cl2 F3 N Rh S'
_chemical_formula_weight         514.23
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           110
_space_group_name_Hall           'I 4bw -2c'
_space_group_name_H-M_alt        'I 41 c d'
_symmetry_space_group_name_Hall  'I 4bw -2c'
_symmetry_space_group_name_H-M   'I 41 c d'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   23.591(5)
_cell_length_b                   23.591(5)
_cell_length_c                   15.839(3)
_cell_measurement_temperature    123(2)
_cell_volume                     8815(3)
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.993
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1272
_diffrn_reflns_av_unetI/netI     0.1216
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32403
_diffrn_reflns_point_group_measured_fraction_full 0.945
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.494
_diffrn_reflns_theta_min         3.098
_exptl_absorpt_coefficient_mu    1.138
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.5881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQUAB Jacobsen'
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_F_000             4128
_exptl_crystal_size_max          0.470
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.090
_refine_diff_density_max         1.741
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.167
_refine_ls_abs_structure_details
;
 Flack x determined using 1033 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.08(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         4687
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0755
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0910P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1762
_refine_ls_wR_factor_ref         0.1925
_reflns_Friedel_coverage         0.799
_reflns_Friedel_fraction_full    0.895
_reflns_Friedel_fraction_max     0.856
_reflns_number_gt                3614
_reflns_number_total             4687
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500714c_si_002.cif
_cod_data_source_block           2e
_cod_depositor_comments
'Adding full bibliography for 4084388--4084398.cif.'
_cod_original_cell_volume        8815(4)
_cod_database_code               4084391
_shelx_estimated_absorpt_t_min   0.617
_shelx_estimated_absorpt_t_max   0.904
_shelxl_version_number           2014-3
_shelx_res_checksum              79447
_shelx_hkl_checksum              98577