3-(2,3,5,6,7,8-Hexahydro-1<i>H</i>-cyclopenta[<i>b</i>]quinolin-9-yl)-1,5-bis(4-methoxyphenyl)biuret
Sakurai, Kaori; Noguchi, Keiichi; Nishibe, Koichiro; Acta Crystallographica Section E 66 (2010) o655–; doi:10.1107/S1600536810006057

data_2225236
_publ_section_title
3-(2,3,5,6,7,8-Hexahydro-1<i>H</i>-cyclopenta[<i>b</i>]quinolin-9-yl)-1,5-bis(4-methoxyphenyl)biuret
_journal_coeditor_code           FJ2281
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o655
_journal_paper_doi               10.1107/S1600536810006057
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C28 H30 N4 O4'
_chemical_formula_moiety         'C28 H30 N4 O4'
_chemical_formula_sum            'C28 H30 N4 O4'
_chemical_formula_weight         486.56
_chemical_name_common
;
1,5-Di-(4-methoxyphenyl)-3-hexahydrocyclopentaquinolylbiuret
;
_chemical_name_systematic
;
3-(2,3,5,6,7,8-Hexahydro-
1<i>H</i>-cyclopenta[<i>b</i>]quinolin-9-yl)-1,5-bis(4-methoxyphenyl)biuret
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 105.5260(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.4514(4)
_cell_length_b                   12.7128(2)
_cell_length_c                   8.83183(16)
_cell_measurement_reflns_used    18332
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      4.0
_cell_volume                     2428.80(7)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2004)'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla <i>et al.</i>,  2005)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0133
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            19342
_diffrn_reflns_theta_full        68.20
_diffrn_reflns_theta_max         68.20
_diffrn_reflns_theta_min         4.03
_exptl_absorpt_coefficient_mu    0.733
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.754
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(ABSCOR; Higashi, 1999)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.167
_refine_diff_density_min         -0.150
_refine_ls_extinction_coef       0.00173(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         2235
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0279
_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^)+(0.0431P)^2^+0.5591P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0710
_refine_ls_wR_factor_ref         0.0716
_reflns_number_gt                2168
_reflns_number_total             2235
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            fj2281.cif
_cod_data_source_block           I
_cod_original_cell_volume        2428.80(8)
_cod_database_code               2225236
_cod_database_fobs_code          2225236