Cooperative C-H Activation of Pyridine by PBP Complexes of Rh and Ir Can Lead to Bridging 2-Pyridyls with Different Connectivity to the B-M Unit
Cao, Yihan; Shih, Wei-Chun; Bhuvanesh, Nattamai; Zhou, Jia; Ozerov, Oleg V.; Chemical Science  (2021) –; doi:10.1039/D1SC01850G

data_1564837
_publ_section_title
;
 Cooperative C-H Activation of Pyridine by PBP Complexes of Rh and Ir Can
 Lead to Bridging 2-Pyridyls with Different Connectivity to the B-M Unit
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC01850G
_journal_year                    2021
_chemical_formula_sum            'C29 H41 B N P2 Rh'
_chemical_formula_weight         579.29
_chemical_name_systematic        (PBP)RhPyH
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2020-07-06 deposited with the CCDC.	2021-10-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.363(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.692(3)
_cell_length_b                   16.314(4)
_cell_length_c                   16.162(4)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      59.283
_cell_measurement_theta_min      4.798
_cell_volume                     2704.9(12)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33833
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.761
_diffrn_reflns_theta_min         2.049
_exptl_absorpt_coefficient_mu    0.768
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6235
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       block
_exptl_crystal_F_000             1208
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Pentane'
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         7290
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0259P)^2^+1.7670P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0580
_refine_ls_wR_factor_ref         0.0609
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6419
_reflns_number_total             7290
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc01850g3.cif
_cod_data_source_block           mo_yc052_0m
_cod_original_cell_volume        2704.9(11)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1564837
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.719
_shelx_estimated_absorpt_t_max   0.887
_shelx_res_checksum              19869
_shelx_hkl_checksum              39567