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_4129904
_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            'C24 H37 B Cl P2 Rh'
_chemical_formula_weight         536.64
_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   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 102.626(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.578(11)
_cell_length_b                   22.693(15)
_cell_length_c                   15.102(10)
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      58.309
_cell_measurement_theta_min      4.480
_cell_volume                     5210(6)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.948
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1330
_diffrn_reflns_av_unetI/netI     0.0688
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            63474
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.442
_diffrn_reflns_theta_min         1.795
_exptl_absorpt_coefficient_mu    0.890
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.5792
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       plate
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.307
_refine_diff_density_min         -1.311
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         13697
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.068
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0279P)^2^+4.1110P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0919
_refine_ls_wR_factor_ref         0.0990
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11138
_reflns_number_total             13697
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b11706_si_002.cif
_cod_data_source_block           5-Rh
_cod_depositor_comments
;

2020-05-25
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C48 H74 B2 Cl2 P4 Rh2'
_cod_original_formula_weight         1073.29
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4129904
_shelxl_version_number           2014-1
_shelx_res_checksum              78494
_shelx_hkl_checksum              43324