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_1564838
_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_moiety         'C33 H43 B N P2 Rh, C7 H8'
_chemical_formula_sum            'C40 H51 B N P2 Rh'
_chemical_formula_weight         721.47
_chemical_name_systematic        (PBP)RhQuH
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-08-07
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2020-07-06 deposited with the CCDC.	2021-10-04 downloaded from the CCDC.
;
_cell_angle_alpha                69.548(2)
_cell_angle_beta                 86.910(2)
_cell_angle_gamma                85.175(2)
_cell_formula_units_Z            2
_cell_length_a                   10.3663(14)
_cell_length_b                   11.4470(16)
_cell_length_c                   15.962(2)
_cell_measurement_reflns_used    9868
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.368
_cell_volume                     1767.8(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      110.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20337
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.521
_diffrn_reflns_theta_min         1.903
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.603
_exptl_absorpt_correction_T_max  0.4305
_exptl_absorpt_correction_T_min  0.3977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/3 (Bruker,2014/3) was used for absorption correction. wR2(int) was 0.0448 before and 0.0367 after correction. The Ratio of minimum to maximum transmission is 0.9238. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       block
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.368
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.164
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         8033
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0255
_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^)+(0.0250P)^2^+0.9574P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0583
_refine_ls_wR_factor_ref         0.0611
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7242
_reflns_number_total             8033
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc01850g3.cif
_cod_data_source_block           yhc084
_cod_original_cell_volume        1767.9(4)
_cod_database_code               1564838
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.908
_shelx_estimated_absorpt_t_min   0.809
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All Rh(H) groups
2.a Riding coordinates:
 Rh1(H)
2.b Ternary CH refined with riding coordinates:
 C16(H16), C19(H19), C28(H28), C31(H31)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13),
 C14(H14), C24(H24), C25(H25), C26(H26), C27(H27), C35(H35), C36(H36), C37(H37),
  C38(H38), C39(H39)
2.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C40(H40A,H40B,H40C)
;
_shelx_res_checksum              84679
_shelx_hkl_checksum              70438
_olex2_submission_special_instructions 'No special instructions were received'