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_4120496
_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            'C56 H90 B20 Ir4 N4 O11'
_chemical_formula_weight         1980.32
_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                 105.4880(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.9999(9)
_cell_length_b                   42.8479(14)
_cell_length_c                   18.1346(13)
_cell_measurement_reflns_used    4788
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      69.95
_cell_measurement_theta_min      2.86
_cell_volume                     19469.1(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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0921
_diffrn_reflns_av_sigmaI/netI    0.0966
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            44955
_diffrn_reflns_theta_full        62.50
_diffrn_reflns_theta_max         62.50
_diffrn_reflns_theta_min         2.04
_diffrn_standards_decay_%        6.60
_exptl_absorpt_coefficient_mu    10.666
_exptl_absorpt_correction_T_max  0.7403
_exptl_absorpt_correction_T_min  0.3866
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             7600
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_platon_squeeze_details          ' '
_refine_diff_density_max         1.679
_refine_diff_density_min         -3.630
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.917
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     934
_refine_ls_number_reflns         14668
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      0.917
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0610
_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^)+(0.1016P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1556
_refine_ls_wR_factor_ref         0.1699
_reflns_number_gt                9342
_reflns_number_total             14668
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4115665_si_001.cif
_cod_data_source_block           complex_3
_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_database_code               4120496