2-(2-Chloropyrimidin-4-yl)-3,5,6,7,8,9-hexahydro-2<i>H</i>-1,2,4-triazolo[4,3-<i>a</i>]azepin-3-one
Li, Gong-Chun; Wang, Li-Ye; Li, Zhao-Yang; Yang, Feng-Ling; Acta Crystallographica Section E 64 (2008) o1928–; doi:10.1107/S1600536808028900

data_2219484
_publ_section_title
2-(2-Chloropyrimidin-4-yl)-3,5,6,7,8,9-hexahydro-2<i>H</i>-1,2,4-triazolo[4,3-<i>a</i>]azepin-3-one
_journal_coeditor_code           AT2624
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1928
_journal_paper_doi               10.1107/S1600536808028900
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C11 H12 Cl N5 O'
_chemical_formula_moiety         'C11 H12 Cl N5 O'
_chemical_formula_sum            'C11 H12 Cl N5 O'
_chemical_formula_weight         265.71
_chemical_name_systematic
;
2-(2-Chloropyrimidin-4-yl)-3,5,6,7,8,9-hexahydro-2<i>H</i>-1,2,4-
triazolo[4,3-<i>a</i>]azepin-3-one
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 92.359(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.6810(16)
_cell_length_b                   14.718(3)
_cell_length_c                   9.4251(17)
_cell_measurement_reflns_used    1409
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      21.85
_cell_measurement_theta_min      2.57
_cell_volume                     1203.2(4)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_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      294(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and o\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  0.0473
_diffrn_reflns_av_sigmaI/netI    0.0610
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6734
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    0.313
_exptl_absorpt_correction_T_max  0.969
_exptl_absorpt_correction_T_min  0.926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.209
_refine_diff_density_min         -0.228
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2461
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1128
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0559P)^2^+0.1252P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1297
_reflns_number_gt                1291
_reflns_number_total             2461
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            at2624.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2219484
_cod_database_fobs_code          2219484