5-Benzyl-2-phenyl-6,8-dihydro-5<i>H</i>-1,2,4-triazolo[3,4-<i>c</i>][1,4]oxazin-2-ium hexafluoridophosphate
Huang, Yumin; Wei, Siping; Wang, Zhen; Mao, Zhihua; Su, Xiaoyu; Acta Crystallographica Section E 65 (2009) o1328–; doi:10.1107/S1600536809018005

data_2221905
_publ_section_title
;5-Benzyl-2-phenyl-6,8-dihydro-5<i>H</i>-1,2,4-triazolo[3,4-<i>c</i>][1,4]oxazin-2-ium
 hexafluoridophosphate
;
_journal_coeditor_code           BG2257
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1328
_journal_paper_doi               10.1107/S1600536809018005
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C18 H18 N3 O +, F6 P -'
_chemical_formula_moiety         'C18 H18 N3 O +, F6 P -'
_chemical_formula_sum            'C18 H18 F6 N3 O P'
_chemical_formula_weight         437.32
_chemical_name_common            triazolium
_chemical_name_systematic
;
5-Benzyl-2-phenyl-6,8-dihydro-5<i>H</i>-1,2,4-
triazolo[3,4-<i>c</i>][1,4]oxazin-2-ium hexafluoridophosphate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 118.678(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.4054(13)
_cell_length_b                   8.1243(9)
_cell_length_c                   11.8593(14)
_cell_measurement_reflns_used    3172
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      26.013
_cell_measurement_theta_min      3.078
_cell_volume                     964.09(19)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5505
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.213
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.200
_refine_diff_density_min         -0.204
_refine_ls_abs_structure_details 'Flack (1983), 1368 Friedel pairs'
_refine_ls_abs_structure_Flack   0.01(10)
_refine_ls_extinction_coef       0.019(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         3406
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.075P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1059
_refine_ls_wR_factor_ref         0.1142
_reflns_number_gt                2984
_reflns_number_total             3406
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bg2257.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2221905
_cod_database_fobs_code          2221905