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_4068224
_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            'C33 H51 B N2'
_chemical_formula_weight         486.57
_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                79.110(2)
_cell_angle_beta                 81.492(2)
_cell_angle_gamma                72.090(2)
_cell_formula_units_Z            4
_cell_length_a                   11.2979(14)
_cell_length_b                   15.4458(19)
_cell_length_c                   19.384(2)
_cell_measurement_reflns_used    5353
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.812
_cell_measurement_theta_min      2.274
_cell_volume                     3146.1(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0494
_diffrn_reflns_av_sigmaI/netI    0.0565
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37009
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    0.058
_exptl_absorpt_correction_T_max  0.9942
_exptl_absorpt_correction_T_min  0.9805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.027
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.162
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.031
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         12368
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.1201
_refine_ls_R_factor_gt           0.0548
_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^)+(0.0745P)^2^+0.1182P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1592
_reflns_number_gt                6549
_reflns_number_total             12368
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201259d_si_004.cif
_cod_data_source_block           j1
_cod_original_cell_volume        3146.2(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4068224