1-Ethoxymethyl-5-methyl-9-phenyl-6,7,8,9-tetrahydro-1<i>H</i>-pyrimido[4,5-<i>b</i>][1,4]diazepine-2,4(3<i>H</i>,5<i>H</i>)-dione
Li, Gong; Wang, Xiaowei; Zhang, Zhili; Liu, Junyi; Acta Crystallographica Section E 68 (2012) o1396–; doi:10.1107/S1600536812014985

data_2234705
_publ_section_title
;
 1-Ethoxymethyl-5-methyl-9-phenyl-6,7,8,9-tetrahydro-1<i>H</i>-pyrimido[4,5-<i>b</i>][1,4]diazepine-2,4(3<i>H</i>,5<i>H</i>)-dione
;
_journal_coeditor_code           KP2397
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1396
_journal_paper_doi               10.1107/S1600536812014985
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C17 H22 N4 O3'
_chemical_formula_moiety         'C17 H22 N4 O3'
_chemical_formula_sum            'C17 H22 N4 O3'
_chemical_formula_weight         330.39
_chemical_name_systematic
;
1-Ethoxymethyl-5-methyl-9-phenyl-6,7,8,9-tetrahydro-1<i>H</i>-
pyrimido[4,5-<i>b</i>][1,4]diazepine-2,4(3<i>H</i>,5<i>H</i>)-dione
;
_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                 112.79(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.831(3)
_cell_length_b                   8.9904(18)
_cell_length_c                   14.978(3)
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.56
_cell_volume                     1717.1(7)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 2000)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 2000)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2000)'
_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      298(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       \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  0.0407
_diffrn_reflns_av_sigmaI/netI    0.0987
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7151
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.56
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  0.9736
_exptl_absorpt_correction_T_min  0.9650
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(ABSCOR; Higashi, 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.585
_refine_ls_extinction_coef       0.062(7)
_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   0.863
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3921
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.863
_refine_ls_R_factor_all          0.1481
_refine_ls_R_factor_gt           0.0791
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1510P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2249
_refine_ls_wR_factor_ref         0.2504
_reflns_number_gt                1601
_reflns_number_total             3921
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            kp2397.cif
_cod_data_source_block           I
_cod_original_cell_volume        1717.1(6)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2234705
_cod_database_fobs_code          2234705