1-Dichloroacetyl-8a-methyl-1,2,3,4,6,7,8,8a-octahydropyrrolo[1,2-<i>a</i>]pyrimidin-6-one
Gao, Shuang; Zhao, Li-xia; Ye, Fei; Fu, Ying; Xing, Zhi-yong; Acta Crystallographica Section E 68 (2012) o1982–; doi:10.1107/S1600536812024063

data_2235705
_publ_section_title
;
 1-Dichloroacetyl-8a-methyl-1,2,3,4,6,7,8,8a-octahydropyrrolo[1,2-<i>a</i>]pyrimidin-6-one
;
_journal_coeditor_code           YK2055
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1982
_journal_paper_doi               10.1107/S1600536812024063
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C10 H14 Cl2 N2 O2'
_chemical_formula_moiety         'C10 H14 Cl2 N2 O2'
_chemical_formula_sum            'C10 H14 Cl2 N2 O2'
_chemical_formula_weight         265.13
_chemical_name_systematic
;
1-Dichloroacetyl-8a-methyl-1,2,3,4,6,7,8,8a-
octahydropyrrolo[1,2-<i>a</i>]pyrimidin-6-one
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c 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            8
_cell_length_a                   10.312(2)
_cell_length_b                   14.997(3)
_cell_length_c                   15.666(3)
_cell_measurement_reflns_used    9134
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.58
_cell_measurement_theta_min      3.16
_cell_volume                     2422.7(8)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1999)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 1999)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2002)'
_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 10
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       '\w scan'
_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  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22128
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.01
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.523
_exptl_absorpt_correction_T_max  0.9224
_exptl_absorpt_correction_T_min  0.8887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.739
_refine_diff_density_min         -0.361
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         2770
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0970P)^2^+0.5072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1505
_refine_ls_wR_factor_ref         0.1558
_reflns_number_gt                2376
_reflns_number_total             2770
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            yk2055.cif
_cod_data_source_block           I
_cod_database_code               2235705
_cod_database_fobs_code          2235705