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_4077986
_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         'C20 H56 B20 Cl2 P2 Pd2'
_chemical_formula_sum            'C20 H56 B20 Cl2 P2 Pd2'
_chemical_formula_weight         858.49
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.288(2)
_cell_angle_beta                 109.1240(10)
_cell_angle_gamma                107.2900(10)
_cell_formula_units_Z            2
_cell_length_a                   10.6627(8)
_cell_length_b                   14.6680(12)
_cell_length_c                   14.6944(11)
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.41
_cell_measurement_theta_min      2.40
_cell_volume                     1946.8(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT V6.02A'
_computing_molecular_graphics    'Bruker ShelXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omea 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  0.2157
_diffrn_reflns_av_sigmaI/netI    0.2068
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20304
_diffrn_reflns_theta_full        27.65
_diffrn_reflns_theta_max         27.65
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    1.160
_exptl_absorpt_correction_T_max  0.4033
_exptl_absorpt_correction_T_min  0.2168
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.792
_refine_diff_density_min         -2.077
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         8870
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.1142
_refine_ls_R_factor_gt           0.0655
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0656P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1581
_refine_ls_wR_factor_ref         0.1796
_reflns_number_gt                5194
_reflns_number_total             8870
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201198s_si_002.cif
_cod_data_source_block           1a
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4077986