4,4-Difluoro-1,3,5,7-tetramethyl-4-bora-3a,4a-diaza-<i>s</i>-indacene
Xu, Hai-Jun; Acta Crystallographica Section E 64 (2008) o1672–; doi:10.1107/S1600536808024057

data_2219210
_publ_section_title
;
 4,4-Difluoro-1,3,5,7-tetramethyl-4-bora-3a,4a-diaza-<i>s</i>-indacene
;
_journal_coeditor_code           AT2574
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1672
_journal_paper_doi               10.1107/S1600536808024057
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C13 H15 B1 F2 N2'
_chemical_formula_moiety         'C13 H15 B1 F2 N2'
_chemical_formula_sum            'C13 H15 B F2 N2'
_chemical_formula_weight         248.08
_chemical_name_systematic
;
4,4-Difluoro-1,3,5,7-tetramethyl-4-bora-3a,4a-diaza-s-indacene
;
_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                 111.108(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.6909(8)
_cell_length_b                   14.3392(15)
_cell_length_c                   11.8334(10)
_cell_measurement_reflns_used    2682
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.8964
_cell_measurement_theta_min      2.8390
_cell_volume                     1217.4(2)
_computing_cell_refinement       'CrystalClear (Rigaku, 2005)'
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku Mercury2'
_diffrn_measurement_method       '\f and \w'
_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  0.0190
_diffrn_reflns_av_sigmaI/netI    0.0222
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6540
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_T_max  0.9741
_exptl_absorpt_correction_T_min  0.9614
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2005)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.236
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         2396
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0669P)^2^+0.3386P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1176
_refine_ls_wR_factor_ref         0.1259
_reflns_number_gt                1963
_reflns_number_total             2396
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            at2574.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C13 H15 B1 F2 N2'
_cod_database_code               2219210
_cod_database_fobs_code          2219210