Iridium-mediated regioselective B-h/c-h activation of carborane cage: a facile synthetic route to metallacycles with a carborane backbone.
Yao, Zi-Jian; Yu, Wei-Bin; Lin, Yue-Jian; Huang, Sheng-Li; Li, Zhen-Hua; Jin, Guo-Xin; Journal of the American Chemical Society 136 (2014) 2825–2832; doi:10.1021/ja4115665

data_4120497
_publ_section_title
;
 Iridium-mediated regioselective B-h/c-h activation of carborane cage: a
 facile synthetic route to metallacycles with a carborane backbone.
;
_journal_issue                   7
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2825
_journal_page_last               2832
_journal_paper_doi               10.1021/ja4115665
_journal_volume                  136
_journal_year                    2014
_chemical_formula_sum            'C32 H59.6 B10 Cl1.8 Ir2 N O4.8'
_chemical_formula_weight         1091.52
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 97.244(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            20
_cell_length_a                   53.686(10)
_cell_length_b                   11.179(2)
_cell_length_c                   38.356(7)
_cell_measurement_reflns_used    9784
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.18
_cell_volume                     22836(7)
_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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.1029
_diffrn_reflns_av_sigmaI/netI    0.0907
_diffrn_reflns_limit_h_max       63
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            64688
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.07
_diffrn_standards_decay_%        5.00
_exptl_absorpt_coefficient_mu    5.961
_exptl_absorpt_correction_T_max  0.6160
_exptl_absorpt_correction_T_min  0.3971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             10632
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_platon_squeeze_details          ' '
_refine_diff_density_max         2.927
_refine_diff_density_min         -4.156
_refine_diff_density_rms         0.349
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1048
_refine_ls_number_reflns         20061
_refine_ls_number_restraints     203
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.1205
_refine_ls_R_factor_gt           0.0979
_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^)+(0.0705P)^2^+2840.1123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2288
_refine_ls_wR_factor_ref         0.2404
_reflns_number_gt                15450
_reflns_number_total             20061
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4115665_si_001.cif
_cod_data_source_block           complex_4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C32 H59.60 B10 Cl1.80 Ir2 N O4.80'
_cod_database_code               4120497