4,5,8a-Triphenylperhydropyrimido[4,5-<i>d</i>]pyrimidine-2,7-dione monohydrate
Zhu, Yulin; Qiu, Wanhong; Yang, Fufen; Li, Guichan; Acta Crystallographica Section E 66 (2010) o1503–; doi:10.1107/S1600536810019525

data_2226287
_publ_section_title
;
 4,5,8a-Triphenylperhydropyrimido[4,5-<i>d</i>]pyrimidine-2,7-dione
 monohydrate
;
_journal_coeditor_code           SJ2783
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1503
_journal_paper_doi               10.1107/S1600536810019525
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C24 H22 N4 O2, H2 O'
_chemical_formula_moiety         'C24 H22 N4 O2, H2 O'
_chemical_formula_sum            'C24 H24 N4 O3'
_chemical_formula_weight         416.47
_chemical_name_systematic
;
4,5,8a-Triphenylperhydropyrimido[4,5-<i>d</i>]pyrimidine-2,7-dione monohydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.7310(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.3150(2)
_cell_length_b                   17.4935(3)
_cell_length_c                   10.5794(2)
_cell_measurement_reflns_used    5618
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      23.54
_cell_measurement_theta_min      2.26
_cell_volume                     2086.94(6)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2004)'
_computing_data_collection       '<i>APEX2</i> (Bruker, 2004)'
_computing_data_reduction        '<i>SAINT</i> (Bruker, 2004)'
_computing_molecular_graphics    '<i>SHELXTL</i> (Sheldrick, 2008)'
_computing_publication_material  '<i>SHELXTL</i> (Sheldrick, 2008)'
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII area-detector diffractometer'
_diffrn_measurement_method       '\f and \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  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            18167
_diffrn_reflns_theta_full        27.95
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         1.81
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             880.0
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.197
_refine_ls_extinction_coef       0.0066(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     '<i>SHELXL97</i> (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         3768
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_max_lt       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^)+(0.0452P)^2^+0.5316P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1099
_reflns_number_gt                2835
_reflns_number_total             3768
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj2783.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2226287
_cod_database_fobs_code          2226287