From Anionic N-Heterocyclic Dicarbenes to Abnormal Carbene–Borane Complexes: A Logical Synthetic Route
Wang, Yuzhong; Abraham, Mariham Y.; Gilliard, Robert J.; Wei, Pingrong; Smith, Jared C.; Robinson, Gregory H.; Organometallics 31 (2012) 791–; doi:10.1021/om201259d

data_4068222
_publ_section_title
;
 From Anionic N-Heterocyclic Dicarbenes to Abnormal Carbene--Borane
 Complexes: A Logical Synthetic Route
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              791
_journal_paper_doi               10.1021/om201259d
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C43 H67 B N2 Si'
_chemical_formula_weight         650.89
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.1050(10)
_cell_angle_beta                 95.3380(10)
_cell_angle_gamma                95.7620(10)
_cell_formula_units_Z            2
_cell_length_a                   11.6738(10)
_cell_length_b                   12.7915(11)
_cell_length_c                   14.4424(12)
_cell_measurement_reflns_used    4446
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.617
_cell_measurement_theta_min      2.257
_cell_volume                     2136.3(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'BRUKER SMART 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  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22968
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  0.9917
_exptl_absorpt_correction_T_min  0.9794
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.012
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.035
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     519
_refine_ls_number_reflns         7494
_refine_ls_number_restraints     363
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.1052
_refine_ls_R_factor_gt           0.0655
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0926P)^2^+0.6545P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1786
_refine_ls_wR_factor_ref         0.2061
_reflns_number_gt                4584
_reflns_number_total             7494
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201259d_si_002.cif
_cod_data_source_block           y1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4068222