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_4089237
_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_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.332(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.246(4)
_cell_length_b                   10.695(2)
_cell_length_c                   16.624(3)
_cell_measurement_temperature    173(2)
_cell_volume                     3208.6(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0212
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34601
_diffrn_reflns_theta_full        27.68
_diffrn_reflns_theta_max         27.68
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    0.746
_exptl_absorpt_correction_T_max  0.9566
_exptl_absorpt_correction_T_min  0.5533
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         7401
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0223
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0255P)^2^+1.9775P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0545
_refine_ls_wR_factor_ref         0.0568
_reflns_number_gt                6632
_reflns_number_total             7401
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7b00070_si_002.cif
_cod_data_source_block           2-OTf
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4089237