Crystal structure of 9-(dibromomethyl)-1,1-difluoro-3,7-dimethyl-1<i>H</i>-[1,3,5,2]oxadiazaborinino[3,4-<i>a</i>][1,8]naphthyridin-11-ium-1-uide
Wang, Bang Zhong; Zhou, Jun Ping; Zhou, Yong; Luo, Jian Song; Chi, Shao Ming; Acta Crystallographica Section E 72 (2016) 1642–1644; doi:10.1107/S2056989016016704

data_2241899
_publ_section_title
;
 Crystal structure of
 9-(dibromomethyl)-1,1-difluoro-3,7-dimethyl-1<i>H</i>-[1,3,5,2]oxadiazaborinino[3,4-<i>a</i>][1,8]naphthyridin-11-ium-1-uide
;
_journal_coeditor_code           WM5325
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1642
_journal_page_last               1644
_journal_paper_doi               10.1107/S2056989016016704
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          'C12 H10 B Br2 F2 N3 O'
_chemical_formula_moiety         'C12 H10 B Br2 F2 N3 O'
_chemical_formula_sum            'C12 H10 B Br2 F2 N3 O'
_chemical_formula_weight         420.86
_chemical_name_systematic
9-(Dibromomethyl)-1,1-difluoro-3,7-dimethyl-1<i>H</i>-[1,3,5,2]oxadiazaborinino[3,4-<i>a</i>][1,8]naphthyridin-11-ium-1-uide
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.161(3)
_cell_length_b                   7.2169(14)
_cell_length_c                   11.678(2)
_cell_measurement_reflns_used    1765
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      3.09
_cell_volume                     1446.3(5)
_computing_cell_refinement
;
PROCESS-AUTO (Rigaku, 1998)
;
_computing_data_collection
;
PROCESS-AUTO (Rigaku, 1998)
;
_computing_data_reduction
;
CrystalStructure (Rigaku/MSC, 2006)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXL-97 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL-97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS-97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       '\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  0.1392
_diffrn_reflns_av_sigmaI/netI    0.0748
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13517
_diffrn_reflns_theta_full        27.39
_diffrn_reflns_theta_max         27.39
_diffrn_reflns_theta_min         3.32
_exptl_absorpt_coefficient_mu    5.627
_exptl_absorpt_correction_T_max  0.3018
_exptl_absorpt_correction_T_min  0.2661
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>ABSCOR</i>; Higashi, 1995)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.933
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.503
_refine_diff_density_min         -0.366
_refine_ls_extinction_coef       0.0042(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         1765
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.1220
_refine_ls_R_factor_gt           0.0535
_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^)+(0.0519P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1196
_reflns_number_gt                937
_reflns_number_total             1765
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            wm5325sup1.cif
_cod_data_source_block           I
_cod_database_code               2241899
_cod_database_fobs_code          2241899