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_4068225
_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 H48 B F3 N2 O3 S'
_chemical_formula_weight         620.60
_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                97.410(6)
_cell_angle_beta                 102.396(6)
_cell_angle_gamma                109.684(4)
_cell_formula_units_Z            2
_cell_length_a                   10.425(3)
_cell_length_b                   10.804(4)
_cell_length_c                   17.325(8)
_cell_measurement_reflns_used    5879
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.574
_cell_measurement_theta_min      2.170
_cell_volume                     1751.0(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0235
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18242
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.142
_exptl_absorpt_correction_T_max  0.9832
_exptl_absorpt_correction_T_min  0.9521
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.833
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6061
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1095
_refine_ls_R_factor_gt           0.0879
_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^)+(0.0907P)^2^+1.8319P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2146
_refine_ls_wR_factor_ref         0.2331
_reflns_number_gt                4506
_reflns_number_total             6061
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201259d_si_005.cif
_cod_data_source_block           j1
_cod_original_cell_volume        1751.1(11)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4068225