11-(2-Oxopyrrolidin-1-ylmethyl)-1,2,3,4,5,6,11,11a-octahydropyrido[2,1-<i>b</i>]quinazolin-6-one dihydrate
Samarov, Zarif U.; Okmanov, Rasul Ya.; Turgunov, Kambarali K.; Tashkhodjaev, Bakhodir; Shakhidoyatov, Khusnutdin M.; Acta Crystallographica Section E 66 (2010) o890–; doi:10.1107/S1600536810009955

data_2225441
_publ_section_title
;
 11-(2-Oxopyrrolidin-1-ylmethyl)-1,2,3,4,5,6,11,11a-octahydropyrido[2,1-<i>b</i>]quinazolin-6-one
 dihydrate
;
_journal_coeditor_code           BQ2200
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o890
_journal_paper_doi               10.1107/S1600536810009955
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C17 H21 N3 O2, 2H2 O'
_chemical_formula_moiety         'C17 H21 N3 O2, 2(H2 O)'
_chemical_formula_sum            'C17 H25 N3 O4'
_chemical_formula_weight         335.40
_chemical_melting_point          373.0(10)
_chemical_name_systematic
'11-(2-Oxopyrrolidin-1-ylmethyl)-1,2,3,4,5,6,11,11a-octahydropyrido[2,1-<i>b</i>]quinazolin-6-one dihydrate'
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.48(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.794(3)
_cell_length_b                   7.6720(15)
_cell_length_c                   15.593(3)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    300.0(10)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      10
_cell_volume                     1713.6(6)
_computing_cell_refinement       'STADI4 (Stoe & Cie, 1997)'
_computing_data_collection       'STADI4 (Stoe & Cie, 1997)'
_computing_data_reduction        'X-RED  (Stoe & Cie, 1997)'
_computing_molecular_graphics    'XP (Bruker, 1998)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      300.0(10)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Stoe Stadi-4 four-circle diffractometer D092'
_diffrn_measurement_device_type  'Stoe Stadi-4 four-circle'
_diffrn_measurement_method
;
Scan width (\w) = 1.56 - 1.68, scan ratio 2\q:\w = 1.00
I(Net) and \s(I) calculated according to Blessing (1987)
;
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0126
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3261
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.70
_diffrn_standards_decay_%        1.8
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prizm
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.179
_refine_diff_density_min         -0.144
_refine_ls_extinction_coef       0.0101(13)
_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   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         3005
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0469P)^2^+0.6922P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1074
_refine_ls_wR_factor_ref         0.1208
_reflns_number_gt                2457
_reflns_number_total             3009
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            bq2200.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2225441
_cod_database_fobs_code          2225441