Regioselective B-Cyclometalation of a Bulkyo-Carboranyl Phosphine and the Unexpected Formation of a Dirhodium(II) Complex
Fey, Natalie; Haddow, Mairi F.; Mistry, Rakesh; Norman, Nicholas C.; Orpen, A. Guy; Reynolds, Timothy J.; Pringle, Paul G.; Organometallics 31 (2012) 2907–; doi:10.1021/om201198s

data_4077988
_publ_section_title
;
 Regioselective B-Cyclometalation of a Bulkyo-Carboranyl Phosphine and the
 Unexpected Formation of a Dirhodium(II) Complex
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              2907
_journal_paper_doi               10.1021/om201198s
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C22 H56 B20 Cl2 O2 P2 Rh2, 1.25(C7 H8)'
_chemical_formula_sum            'C30.75 H66 B20 Cl2 O2 P2 Rh2'
_chemical_formula_weight         1022.70
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.157(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3679(7)
_cell_length_b                   35.724(4)
_cell_length_c                   14.6186(13)
_cell_measurement_reflns_used    28939
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.474
_cell_measurement_theta_min      2.211
_cell_volume                     4864.0(8)
_computing_cell_refinement       'Bruker SMART V5.054 (Bruker, 1998)'
_computing_data_collection       'Bruker SMART V5.054 (Bruker, 1998)'
_computing_data_reduction        'Bruker SAINT V6.0 (Bruker, 1998)'
_computing_molecular_graphics    'Bruker SHELXTL V6.1 (Bruker AXS, 2000)'
_computing_publication_material  'Bruker SHELXTL V6.1 (Bruker AXS, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_sigmaI/netI    0.0296
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            51336
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.884
_exptl_absorpt_correction_T_max  0.920000
_exptl_absorpt_correction_T_min  0.829071
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2082
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     639
_refine_ls_number_reflns         11135
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0260
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0205P)^2^+2.6842P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0561
_refine_ls_wR_factor_ref         0.0585
_reflns_number_gt                9794
_reflns_number_total             11135
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201198s_si_002.cif
_cod_data_source_block           3_toluene
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4077988