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_7029343
_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            'C28 H50 B20 Cl4 P Rh S3'
_chemical_formula_weight         974.74
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 101.332(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.916(9)
_cell_length_b                   11.926(7)
_cell_length_c                   27.143(15)
_cell_measurement_reflns_used    829
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.374
_cell_measurement_theta_min      2.241
_cell_volume                     4734(5)
_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 0.971
_diffrn_measured_fraction_theta_max 0.996
_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  0.0782
_diffrn_reflns_av_unetI/netI     0.1366
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            19120
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.008
_diffrn_reflns_theta_min         1.451
_exptl_absorpt_coefficient_mu    0.777
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       prism
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.090
_platon_squeeze_details
; 
 In asymmetric unit of 4, there were two disordered 
 dichloromethane molecules which could not be restrained 
 properly. Therefore, SQUEEZE algorithm was used to omit 
 them. 
;
_refine_diff_density_max         2.160
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.812
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         8312
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.812
_refine_ls_R_factor_all          0.1172
_refine_ls_R_factor_gt           0.0641
_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^)+(0.0782P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1411
_refine_ls_wR_factor_ref         0.1522
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3951
_reflns_number_total             8312
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt51906f.txt
_cod_data_source_block           a21114b
_cod_database_code               7029343
_shelx_estimated_absorpt_t_min   0.824
_shelx_estimated_absorpt_t_max   0.933
_shelxl_version_number           2013-2
_shelx_res_checksum              71371
_shelx_hkl_checksum              83568