Boryl/Borane Interconversion and Diversity of Binding Modes of Oxygenous Ligands in PBP Pincer Complexes of Rhodium
Shih, Wei-Chun; Gu, Weixing; MacInnis, Morgan C.; Herbert, David E.; Ozerov, Oleg V.; Organometallics 36 (2017) 1718–; doi:10.1021/acs.organomet.7b00070

data_4089235
_publ_section_title
;
 Boryl/Borane Interconversion and Diversity of Binding Modes of Oxygenous
 Ligands in PBP Pincer Complexes of Rhodium
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              1718
_journal_paper_doi               10.1021/acs.organomet.7b00070
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C35 H50 B O2 P2 Rh'
_chemical_formula_sum            'C35 H50 B O2 P2 Rh'
_chemical_formula_weight         678.41
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 96.663(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.646(3)
_cell_length_b                   16.170(4)
_cell_length_c                   19.506(5)
_cell_measurement_reflns_used    5214
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      24.01
_cell_measurement_theta_min      2.30
_cell_volume                     3335.2(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II 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  0.1145
_diffrn_reflns_av_unetI/netI     0.1031
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            36258
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.428
_diffrn_reflns_theta_min         1.640
_diffrn_source                   'normal-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.637
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.610
_refine_diff_density_min         -1.151
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.845
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         7510
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.845
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0216P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0747
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4832
_reflns_number_total             7510
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00070_si_002.cif
_cod_data_source_block           2-OPiv
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4089235
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.817
_shelx_estimated_absorpt_t_max   0.969
_shelx_res_checksum              96476
_shelx_hkl_checksum              23002