12-Dimethylamino-2,2-difluoro-8-phenyl-1λ^5^,3-diaza-2λ^4^-boratricyclo[7.3.0.0^3,7^]dodeca-1(12),4,6,8,10-pentaen-1-ylium
Wang, Zhao-Yun; Acta Crystallographica Section E 69 (2013) o781–; doi:10.1107/S1600536813010404

data_2238001
_publ_section_title
;
 12-Dimethylamino-2,2-difluoro-8-phenyl-1\l^5^,3-diaza-2\l^4^-boratricyclo[7.3.0.0^3,7^]dodeca-1(12),4,6,8,10-pentaen-1-ylium
;
_journal_coeditor_code           RK2400
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o781
_journal_paper_doi               10.1107/S1600536813010404
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C17 H16 B F2 N3'
_chemical_formula_moiety         'C17 H16 B F2 N3'
_chemical_formula_sum            'C17 H16 B F2 N3'
_chemical_formula_weight         311.14
_chemical_name_systematic
12-Dimethylamino-2,2-difluoro-8-phenyl-1\l^5^,3-diaza-2\l^4^-boratricyclo[7.3.0.0^3,7^]dodeca-1(12),4,6,8,10-pentaen-1-ylium
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 128.671(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.8033(6)
_cell_length_b                   25.524(2)
_cell_length_c                   9.9776(5)
_cell_measurement_reflns_used    4251
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      24.34
_cell_measurement_theta_min      2.73
_cell_volume                     1551.5(2)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2002)'
_computing_data_collection       '<i>SMART</i> (Bruker, 2002)'
_computing_data_reduction        '<i>SAINT</i> (Bruker, 2002)'
_computing_molecular_graphics    '<i>SHELXTL</i> (Sheldrick, 2008)'
_computing_publication_material  '<i>SHELXTL</i> (Sheldrick, 2008)'
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0218
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11054
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  0.9810
_exptl_absorpt_correction_T_min  0.9717
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.162
_refine_diff_density_min         -0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         2736
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0582P)^2^+0.2638P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1193
_reflns_number_gt                2025
_reflns_number_total             2736
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rk2400.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2238001
_cod_database_fobs_code          2238001