Facile Insertion of Rh and Ir into a Boron-Phenyl Bond, Leading to Boryl/Bis(phosphine) PBP Pincer Complexes.
Shih, Wei-Chun; Gu, Weixing; MacInnis, Morgan C.; Timpa, Samuel D.; Bhuvanesh, Nattamai; Zhou, Jia; Ozerov, Oleg V.; Journal of the American Chemical Society 138 (2016) 2086–2089; doi:10.1021/jacs.5b11706

data_4129902
_publ_section_title
;
 Facile Insertion of Rh and Ir into a Boron-Phenyl Bond, Leading to
 Boryl/Bis(phosphine) PBP Pincer Complexes.
;
_journal_issue                   7
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2086
_journal_page_last               2089
_journal_paper_doi               10.1021/jacs.5b11706
_journal_volume                  138
_journal_year                    2016
_chemical_formula_sum            'C37 H48 B Cl Ir P2'
_chemical_formula_weight         793.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 99.950(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.275(5)
_cell_length_b                   10.061(4)
_cell_length_c                   31.113(13)
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      55.545
_cell_measurement_theta_min      4.844
_cell_volume                     3476(3)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            39833
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.809
_diffrn_reflns_theta_min         1.834
_exptl_absorpt_coefficient_mu    4.034
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5177
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_description       block
_exptl_crystal_F_000             1596
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.336
_refine_diff_density_min         -1.200
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         8189
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0245
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0233P)^2^+4.1465P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0548
_refine_ls_wR_factor_ref         0.0564
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7365
_reflns_number_total             8189
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b11706_si_002.cif
_cod_data_source_block           3-Ir
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4129902
_shelx_estimated_absorpt_t_min   0.471
_shelx_estimated_absorpt_t_max   0.688
_shelxl_version_number           2014-1
_shelx_res_checksum              80473
_shelx_hkl_checksum              52812