2-[3-(Trifluoromethyl)phenyl]perhydro-1,2,4-triazolo[1,2-<i>a</i>]pyridazine-1,3-dione
Zu-Guang Sun; Xiao-Qing Li; Wei Xu; Xiao-Hua Du; Acta Crystallographica Section E 63 (2007) o3840–o3840; doi:10.1107/S1600536807039748

data_2215068
_publ_section_title
2-[3-(Trifluoromethyl)phenyl]perhydro-1,2,4-triazolo[1,2-<i>a</i>]pyridazine-1,3-dione
_journal_coeditor_code           CS2041
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3840
_journal_page_last               o3840
_journal_paper_doi               10.1107/S1600536807039748
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C13 H12 F3 N3 O2'
_chemical_formula_moiety         'C13 H12 F3 N3 O2'
_chemical_formula_sum            'C13 H12 F3 N3 O2'
_chemical_formula_weight         299.26
_chemical_melting_point          417
_chemical_name_systematic
2-[3-(Trifluoromethyl)phenyl]perhydro-1,2,4-triazolo[1,2-a]pyridazine-1,3-dione
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.994(2)
_cell_angle_beta                 98.153(2)
_cell_angle_gamma                95.630(3)
_cell_formula_units_Z            2
_cell_length_a                   6.8348(9)
_cell_length_b                   8.0756(11)
_cell_length_c                   12.0770(17)
_cell_measurement_reflns_used    1670
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      52.963
_cell_measurement_theta_min      6.021
_cell_volume                     656.34(15)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker SMART APEX'
_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  0.1305
_diffrn_reflns_av_sigmaI/netI    0.0975
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3486
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.70
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 200
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.133
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             308
_exptl_crystal_size_max          0.501
_exptl_crystal_size_mid          0.373
_exptl_crystal_size_min          0.298
_refine_diff_density_max         0.278
_refine_diff_density_min         -0.271
_refine_ls_extinction_coef       0.37(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         2409
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0557
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0885P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1402
_refine_ls_wR_factor_ref         0.1476
_reflns_number_gt                1887
_reflns_number_total             2409
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cs2041.cif
_cod_data_source_block           I
_cod_database_code               2215068
_cod_database_fobs_code          2215068