Diverse reactions of N-heterocyclic carbenes with an alkynylborane and isolation of a reactive zwitterionic borataallene
Rudiger Bertermann; Holger Braunschweig; Christopher K. L. Brown; Alexander Damme; Rian D. Dewhurst; Christian Horl; Thomas Kramer; Ivo Krummenacher; Bernd Pfaffinger; Krzysztof Radacki; Chem.Commun. 50 (2013) 97–; doi:10.1039/c3cc46947f

data_7110158
_publ_section_title
;
 Diverse reactions of N-heterocyclic carbenes with an alkynylborane and
 isolation of a reactive zwitterionic borataallene
;
_journal_name_full               Chem.Commun.
_journal_page_first              97
_journal_paper_doi               10.1039/c3cc46947f
_journal_volume                  50
_journal_year                    2013
_chemical_formula_moiety         'C47 H59 B N2'
_chemical_formula_sum            'C47 H59 B N2'
_chemical_formula_weight         662.77
_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                 100.333(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.927(9)
_cell_length_b                   18.683(10)
_cell_length_c                   11.255(6)
_cell_measurement_temperature    100(2)
_cell_volume                     4122(4)
_computing_cell_refinement       'Saint+ ver. 7.68A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 2010.3 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. 7.68A (Bruker AXS)'
_computing_molecular_graphics    'XP ver. 5.1 (Bruker AXS, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_sigmaI/netI    0.0534
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            35318
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.78
_diffrn_reflns_theta_min         1.04
_exptl_absorpt_coefficient_mu    0.060
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6437
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'Sadabs 2008/1 (Bruker 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.068
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         8769
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1036
_refine_ls_R_factor_gt           0.0595
_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^)+(0.0833P)^2^+1.4122P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1538
_refine_ls_wR_factor_ref         0.1775
_reflns_number_gt                5573
_reflns_number_total             8769
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc46947f.txt
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7110158