5''-(4-Chlorobenzylidene)-4'-(4-chlorophenyl)-1''-methyl-5'-phenylacenaphthene-1-spiro-2'-pyrrolidine-3'-spiro-3''-piperidine-2,4''-dione
S. Athimoolam; R. Ranjith Kumar; K. Vijaya; R. Sayee Kannan; S. Perumal; Acta Crystallographica Section E 63 (2007) o4635–o4636; doi:10.1107/S1600536807055109

data_2216775
_publ_section_title
5''-(4-Chlorobenzylidene)-4'-(4-chlorophenyl)-1''-methyl-5'-phenylacenaphthene-1-spiro-2'-pyrrolidine-3'-spiro-3''-piperidine-2,4''-dione
_journal_coeditor_code           SJ2401
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4635
_journal_page_last               o4636
_journal_paper_doi               10.1107/S1600536807055109
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C39 H30 Cl2 N2 O2'
_chemical_formula_moiety         'C39 H30 Cl2 N2 O2'
_chemical_formula_sum            'C39 H30 Cl2 N2 O2'
_chemical_formula_weight         629.55
_chemical_melting_point          190
_chemical_name_common
1-spiro-2'-pyrrolidine-3'-spiro-3''-piperidine-2,4''-dione
_chemical_name_systematic
;
4-(4-Chlorophenyl)-5-phenylpyrrolo-(spiro[2.2'']-acenaphthene-
 1''-one)-spiro[3.3']-5'-(4-chlorophenylmethylidene)-1'-
 methyltetrahydro-4'-(1H)-pyridinone
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL/PC
_cell_angle_alpha                76.025(11)
_cell_angle_beta                 75.445(9)
_cell_angle_gamma                76.220(8)
_cell_formula_units_Z            2
_cell_length_a                   9.5567(6)
_cell_length_b                   12.0442(11)
_cell_length_c                   14.8593(15)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.26
_cell_measurement_theta_min      10.27
_cell_volume                     1577.5(3)
_computing_cell_refinement       'CAD4 Express (Enraf--Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf--Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics
;
ORTEP-3  (Farrugia, 1997) and PLATON (Spek, 2003)
;
_computing_publication_material  'SHELXTL/PC (Bruker, 2000)'
_computing_structure_refinement  'SHELXTL/PC (Bruker, 2000)'
_computing_structure_solution    'SHELXTL/PC (Bruker, 2000)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius MACH3'
_diffrn_measurement_method       \w-2\q
_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  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6631
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.06
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.244
_exptl_absorpt_correction_T_max  0.9732
_exptl_absorpt_correction_T_min  0.9465
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.286
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         5538
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_gt           0.0484
_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\^)+(0.0646P)\^2\^+0.6033P] where
 P=(Fo\^2\^+2Fc\^2\^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1192
_refine_ls_wR_factor_ref         0.1424
_reflns_number_gt                3434
_reflns_number_total             5538
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj2401.cif
_cod_data_source_block           I
_cod_database_code               2216775
_cod_database_fobs_code          2216775