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_7122673
_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            'C32 H53 B10 Cl2 Ir2 N2 O'
_chemical_formula_weight         1045.16
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_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                75.448(2)
_cell_angle_beta                 79.942(2)
_cell_angle_gamma                85.845(2)
_cell_formula_units_Z            2
_cell_length_a                   8.3378(11)
_cell_length_b                   12.0979(16)
_cell_length_c                   20.336(3)
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.24
_cell_volume                     1954.1(5)
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0325
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            13592
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_min         1.740
_exptl_absorpt_coefficient_mu    6.969
_exptl_absorpt_correction_T_max  0.563
_exptl_absorpt_correction_T_min  0.274
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.776
_exptl_crystal_description       sheet
_exptl_crystal_F_000             1010
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.080
_refine_diff_density_max         2.463
_refine_diff_density_min         -1.869
_refine_diff_density_rms         0.218
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         8432
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+5.4744P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1034
_refine_ls_wR_factor_ref         0.1099
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7217
_reflns_number_total             8432
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc09084j4.cif
_cod_data_source_block           2b
_cod_original_cell_volume        1954.1(4)
_cod_database_code               7122673
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.194
_shelx_estimated_absorpt_t_max   0.606
_shelx_res_checksum              28410
_shelx_hkl_checksum              74505