6-Benzyl 4-ethyl 2-chloro-5,6,7,8-tetrahydropyrido[4,3-<i>d</i>]pyrimidine-4,6-dicarboxylate
Guo, Huan-Mei; Acta Crystallographica Section E 67 (2011) o2516–; doi:10.1107/S1600536811034313

data_2231499
_publ_section_title
;
 6-Benzyl 4-ethyl
 2-chloro-5,6,7,8-tetrahydropyrido[4,3-<i>d</i>]pyrimidine-4,6-dicarboxylate
;
_journal_coeditor_code           HB6350
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2516
_journal_paper_doi               10.1107/S1600536811034313
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C18 H18 Cl N3 O4'
_chemical_formula_moiety         'C18 H18 Cl N3 O4'
_chemical_formula_sum            'C18 H18 Cl N3 O4'
_chemical_formula_weight         375.80
_chemical_name_systematic
;
6-Benzyl 4-ethyl
2-chloro-5,6,7,8-tetrahydropyrido[4,3-<i>d</i>]pyrimidine-4,6-dicarboxylate
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 119.820(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.530(2)
_cell_length_b                   12.384(2)
_cell_length_c                   14.010(3)
_cell_measurement_reflns_used    6088
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.64
_cell_volume                     1735.6(6)
_computing_cell_refinement       'CrystalClear (Rigaku, 2007)'
_computing_data_collection       'CrystalClear (Rigaku, 2007)'
_computing_data_reduction        'CrystalClear (Rigaku, 2007)'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'MM007-HF CCD (Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_sigmaI/netI    0.0411
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8909
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.250
_exptl_absorpt_correction_T_max  0.9611
_exptl_absorpt_correction_T_min  0.9447
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2007)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.650
_refine_diff_density_min         -0.698
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         3925
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0580
_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^)+(0.0565P)^2^+1.1725P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1365
_refine_ls_wR_factor_ref         0.1420
_reflns_number_gt                3518
_reflns_number_total             3925
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb6350.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2231499
_cod_database_fobs_code          2231499