Anionic N-Heterocyclic Dicarbene−Borane Binuclear Complexes
Wang, Yuzhong; Xie, Yaoming; Abraham, Mariham Y.; Wei, Pingrong; Schaefer, Henry F.; Schleyer, Paul v. R.; Robinson, Gregory H.; Organometallics 30 (2011) 1303–; doi:10.1021/om2000579

data_4064341
_publ_section_title
;
 Anionic N-Heterocyclic Dicarbene&#x2212;Borane Binuclear Complexes
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1303
_journal_paper_doi               10.1021/om2000579
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C132 H224 B8 Li4 N8 O12'
_chemical_formula_weight         2229.44
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 96.2280(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.5090(17)
_cell_length_b                   16.5228(15)
_cell_length_c                   24.285(2)
_cell_measurement_reflns_used    5683
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      18.773
_cell_measurement_theta_min      2.277
_cell_volume                     7383.0(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'BRUKER APEX II'
_diffrn_measurement_method       'OMEGA SCAN'
_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  0.2058
_diffrn_reflns_av_sigmaI/netI    0.1426
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            78082
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    0.061
_exptl_absorpt_correction_T_max  0.9975
_exptl_absorpt_correction_T_min  0.9872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.003
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2440
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       0.0018(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     899
_refine_ls_number_reflns         12985
_refine_ls_number_restraints     395
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.2631
_refine_ls_R_factor_gt           0.0828
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0840P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1766
_refine_ls_wR_factor_ref         0.2490
_reflns_number_gt                4033
_reflns_number_total             12985
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2000579_si_003.cif
_cod_data_source_block           j1
_cod_original_cell_volume        7383.0(12)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4064341