6-(4-Chlorophenyl)-9,9-dimethyl-3,7-dioxo-2,3,4,6,7,8,9,10-octahydro-1<i>H</i>-pyrimido[1,2-<i>a</i>]quinoline-5-carbonitrile
Dong-Qin Chen; Chun-Mei Li; Shu-Jiang Tu; Acta Crystallographica Section E 63 (2007) o3931–o3931; doi:10.1107/S1600536807042389

data_2215419
_publ_section_title
6-(4-Chlorophenyl)-9,9-dimethyl-3,7-dioxo-2,3,4,6,7,8,9,10-octahydro-1<i>H</i>-pyrimido[1,2-<i>a</i>]quinoline-5-carbonitrile
_journal_coeditor_code           CI2454
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3931
_journal_page_last               o3931
_journal_paper_doi               10.1107/S1600536807042389
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C21 H20 Cl N3 O2'
_chemical_formula_moiety         'C21 H20 Cl N3 O2'
_chemical_formula_sum            'C21 H20 Cl N3 O2'
_chemical_formula_weight         381.85
_chemical_melting_point          540.0(10)
_chemical_name_systematic
;
6-(4-Chlorophenyl)-9,9-dimethyl-3,7-dioxo-2,3,4,6,7,8,9,10-octahydro-
1<i>H</i>-pyrimido[1,2-<i>a</i>]quinoline-5-carbonitrile
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 97.406(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.378(5)
_cell_length_b                   10.131(5)
_cell_length_c                   18.143(9)
_cell_measurement_reflns_used    981
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.139
_cell_measurement_theta_min      2.809
_cell_volume                     1891.6(16)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  'SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \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  0.0864
_diffrn_reflns_av_sigmaI/netI    0.1561
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9514
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.98
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.223
_exptl_absorpt_correction_T_max  0.9694
_exptl_absorpt_correction_T_min  0.9463
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.242
_refine_diff_density_min         -0.281
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3340
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1840
_refine_ls_R_factor_gt           0.0644
_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^)+(0.035P)^2^+2.4335P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1503
_refine_ls_wR_factor_ref         0.2226
_reflns_number_gt                1323
_reflns_number_total             3340
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ci2454.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '539-541' was changed to '540.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '539-541' was changed to '540.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1891.6(17)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2215419
_cod_database_fobs_code          2215419