8-(4-Chlorophenyl)-11,11-dimethyl-5,9-dioxo-6,8,9,10,11,12-hexahydro-5<i>H</i>-quinolino[1,2-<i>a</i>]quinazoline-7-carbonitrile <i>N</i>,<i>N</i>-dimethylformamide solvate
Hong Jiang; Shanshan Wu; Chunmei Li; Acta Crystallographica Section E 63 (2007) o4531–o4531; doi:10.1107/S1600536807054037

data_2216357
_publ_section_title
;8-(4-Chlorophenyl)-11,11-dimethyl-5,9-dioxo-6,8,9,10,11,12-hexahydro-5<i>H</i>-quinolino[1,2-<i>a</i>]quinazoline-7-carbonitrile
 <i>N</i>,<i>N</i>-dimethylformamide solvate
;
_journal_coeditor_code           CI2492
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4531
_journal_page_last               o4531
_journal_paper_doi               10.1107/S1600536807054037
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C25 H20 Cl N3 O2, C3 H7 N O'
_chemical_formula_moiety         'C25 H20 Cl N3 O2, C3 H7 N O'
_chemical_formula_sum            'C28 H27 Cl N4 O3'
_chemical_formula_weight         502.99
_chemical_melting_point          514.0(10)
_chemical_name_systematic
;
8-(4-Chlorophenyl)-11,11-dimethyl-5,9-dioxo-6,8,9,10,11,12-hexahydro-
5<i>H</i>-quinolino[1,2-<i>a</i>]quinazoline-7-carbonitrile
<i>N</i>,<i>N</i>-dimethylformamide solvate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 102.714(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   36.340(15)
_cell_length_b                   11.780(5)
_cell_length_c                   11.870(5)
_cell_measurement_reflns_used    2136
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.315
_cell_measurement_theta_min      2.442
_cell_volume                     4957(4)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1999)'
_computing_publication_material  'SHELXTL (Bruker, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_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  0.0627
_diffrn_reflns_av_sigmaI/netI    0.0864
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12316
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.82
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.193
_exptl_absorpt_correction_T_max  0.9810
_exptl_absorpt_correction_T_min  0.9571
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.423
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         4326
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1448
_refine_ls_R_factor_gt           0.0738
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1126P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1776
_refine_ls_wR_factor_ref         0.2164
_reflns_number_gt                2288
_reflns_number_total             4326
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ci2492.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value '513-515' was changed to '514.0(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 '513-515' was changed to '514.0(10)'
- the average value was taken and precision was
estimated.

'_symmetry_cell_setting' value 'Monoclinic' changed to
'monoclinic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2216357
_cod_database_fobs_code          2216357