Synthesis and Structural Characterization of Carbene-Stabilized Carborane-Fused Azaborolyl Radical Cation and Dicarbollyl-Fused Azaborole
Wang, Hao; Zhang, Jiji; Lin, Zhenyang; Xie, Zuowei; Organometallics 35 (2016) 2579–; doi:10.1021/acs.organomet.6b00545

data_4088901
_publ_section_title
;
 Synthesis and Structural Characterization of Carbene-Stabilized
 Carborane-Fused Azaborolyl Radical Cation and Dicarbollyl-Fused Azaborole
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              2579
_journal_paper_doi               10.1021/acs.organomet.6b00545
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C60 H112 B22 Cu2 I4 N6'
_chemical_formula_weight         1790.05
_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   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                98.563(3)
_cell_angle_beta                 97.586(3)
_cell_angle_gamma                102.177(3)
_cell_formula_units_Z            1
_cell_length_a                   9.7240(15)
_cell_length_b                   11.0917(18)
_cell_length_c                   22.418(4)
_cell_measurement_reflns_used    101
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      15
_cell_volume                     2303.5(7)
_computing_cell_refinement       'BRUKER KAPPA APEXII DUO DIFFRACTOMETER'
_computing_data_collection       'BRUKER KAPPA APEXII DUO DIFFRACTOMETER'
_computing_data_reduction        'BRUKER KAPPA APEXII DUO DIFFRACTOMETER'
_computing_molecular_graphics    'BRUKER SHELXTL'
_computing_publication_material  'BRUKER SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'BRUKER KAPPA APEXII DUO DIFFRACTOMETER'
_diffrn_measurement_method       'Phi & Omega Scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0639
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8384
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.248
_diffrn_reflns_theta_min         0.932
_exptl_absorpt_coefficient_mu    1.836
_exptl_absorpt_correction_T_max  0.745620
_exptl_absorpt_correction_T_min  0.616516
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_description       block
_exptl_crystal_F_000             894
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_platon_squeeze_details
;
;
_refine_diff_density_max         1.375
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         8384
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.1026
_refine_ls_R_factor_gt           0.0616
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1202P)^2^+2.2522P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1870
_refine_ls_wR_factor_ref         0.2167
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5760
_reflns_number_total             8384
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00545_si_003.cif
_cod_data_source_block           '[2]2[Cu2I4]'
_cod_original_cell_volume        2303.5(6)
_cod_database_code               4088901
_shelx_estimated_absorpt_t_min   0.609
_shelx_estimated_absorpt_t_max   0.710
_shelxl_version_number           2014/6
_shelx_res_checksum              41807
_shelx_hkl_checksum              47712