Nucleophilic addition of carborane anion to Ir, Rh-coordinated Cp* ring: C-C bond formation accompanied by reduction of metal center.
Yao, Zi-Jian; Lin, Yue-Jian; Xu, Bin; Jin, Guo-Xin; Dalton transactions (Cambridge, England : 2003) 43 (2014) 4938–4940; doi:10.1039/c3dt51906f

data_7029342
_publ_section_title
;
 Nucleophilic addition of carborane anion to Ir, Rh-coordinated Cp* ring:
 C-C bond formation accompanied by reduction of metal center.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4938
_journal_page_last               4940
_journal_paper_doi               10.1039/c3dt51906f
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C27 H48 B20 Cl2 P Rh S2'
_chemical_formula_weight         857.75
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 96.824(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.013(4)
_cell_length_b                   29.317(9)
_cell_length_c                   12.157(4)
_cell_measurement_reflns_used    977
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.894
_cell_measurement_theta_min      2.254
_cell_volume                     4251(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0730
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19307
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.010
_diffrn_reflns_theta_min         1.389
_exptl_absorpt_coefficient_mu    0.686
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_description       sheet
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_platon_squeeze_details
; 
 In asymmetric unit of 3, there was one disordered 
 dichloromethane molecule which could not be restrained 
 properly. Therefore, SQUEEZE algorithm was used to omit it. 
;
_refine_diff_density_max         0.673
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.26(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     920
_refine_ls_number_reflns         12762
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0470P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.0968
_reflns_Friedel_coverage         0.962
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                9503
_reflns_number_total             12762
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt51906f.txt
_cod_data_source_block           a10120a
_cod_database_code               7029342
_shelx_estimated_absorpt_t_min   0.904
_shelx_estimated_absorpt_t_max   0.947
_shelxl_version_number           2013-2
_shelx_res_checksum              34117
_shelx_hkl_checksum              39488