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_4089238
_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_sum            'C31 H41 B F3 O3 P2 Rh S'
_chemical_formula_weight         726.36
_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
_cell_angle_alpha                90
_cell_angle_beta                 94.305(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.407(2)
_cell_length_b                   16.421(4)
_cell_length_c                   19.039(4)
_cell_measurement_reflns_used    3616
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.366
_cell_measurement_theta_min      2.309
_cell_volume                     3244.5(12)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.927
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0952
_diffrn_reflns_av_unetI/netI     0.0857
_diffrn_reflns_Laue_measured_fraction_full 0.927
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21534
_diffrn_reflns_point_group_measured_fraction_full 0.927
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.145
_exptl_absorpt_coefficient_mu    0.738
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_description       needle
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.520
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.875
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         5446
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0256P)^2^+1.9849P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.0989
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4039
_reflns_number_total             5446
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00070_si_002.cif
_cod_data_source_block           4-OTf
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4089238
_shelx_estimated_absorpt_t_min   0.700
_shelx_estimated_absorpt_t_max   0.937
_shelxl_version_number           2014-1
_shelx_res_checksum              34318
_shelx_hkl_checksum              94294