Iridium-Induced Regioselective B-H and C-H Activations at Azo-Substituted m-Carboranes: Facile Access to Polynuclear Complexes
Jin, Guo-Xin; Gao, Yang; Guo, Shu-Ting; Cui, Peng-Fei; Pemán, Francisco Aznárez; Chemical Communications  (2018) –; doi:10.1039/C8CC09084J

data_7122677
_publ_section_title
;
 Iridium-Induced Regioselective B-H and C-H Activations at Azo-Substituted
 m-Carboranes: Facile Access to Polynuclear Complexes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC09084J
_journal_year                    2018
_chemical_formula_sum            'C37 H52 B10 Cl F3 Ir2 N4 O5 S'
_chemical_formula_weight         1249.83
_space_group_crystal_system      monoclinic
_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_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-10-08 deposited with the CCDC.
2018-11-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.606(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.987(3)
_cell_length_b                   16.285(3)
_cell_length_c                   20.997(5)
_cell_measurement_reflns_used    3812
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      25.31
_cell_measurement_theta_min      2.38
_cell_volume                     4583.2(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.990
_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  0.0809
_diffrn_reflns_av_unetI/netI     0.0904
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            32345
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.169
_diffrn_reflns_theta_min         1.609
_exptl_absorpt_coefficient_mu    5.963
_exptl_absorpt_correction_T_max  0.563
_exptl_absorpt_correction_T_min  0.412
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.811
_exptl_crystal_description       block
_exptl_crystal_F_000             2424
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.130
_refine_diff_density_max         1.917
_refine_diff_density_min         -1.119
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         10072
_refine_ls_number_restraints     242
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0450P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.1045
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6743
_reflns_number_total             10072
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc09084j7.cif
_cod_data_source_block           4
_cod_original_cell_volume        4583.5(17)
_cod_database_code               7122677
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.367
_shelx_estimated_absorpt_t_max   0.511
_shelx_res_checksum              14198
_shelx_hkl_checksum              15554