Crystal structure of 5''-benzylidene-1'-methyl-4'-phenyltrispiro[acenaphthylene-1,2'-pyrrolidine-3',1''-cyclohexane-3'',2'''-[1,3]dioxane]-2,6''-dione
Chandralekha, Kuppan; Gavaskar, Deivasigamani; Sureshbabu, Adukamparai Rajukrishnan; Lakshmi, Srinivasakannan; Acta Crystallographica Section E 72 (2016) 387–390; doi:10.1107/S2056989016002875

data_2241575
_publ_section_title
;
 Crystal structure of
 5''-benzylidene-1'-methyl-4'-phenyltrispiro[acenaphthylene-1,2'-pyrrolidine-3',1''-cyclohexane-3'',2'''-[1,3]dioxane]-2,6''-dione
;
_journal_coeditor_code           RZ5182
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              387
_journal_page_last               390
_journal_paper_doi               10.1107/S2056989016002875
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          'C36 H31 N O4'
_chemical_formula_moiety         'C36 H31 N O4'
_chemical_formula_sum            'C36 H31 N O4'
_chemical_formula_weight         541.62
_chemical_name_systematic
5''-Benzylidene-1'-methyl-4'-phenyltrispiro[acenaphthylene-1,2'-pyrrolidine-3',1''-cyclohexane-3'',2'''-[1,3]dioxane]-2,6''-dione
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                83.830(10)
_cell_angle_beta                 65.253(8)
_cell_angle_gamma                86.397(10)
_cell_formula_units_Z            2
_cell_length_a                   10.8861(4)
_cell_length_b                   11.4899(4)
_cell_length_c                   11.9171(4)
_cell_measurement_reflns_used    43585
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.666
_cell_measurement_theta_min      4.959
_cell_volume                     1345.60(12)
_computing_cell_refinement
;
SAINT (Bruker, 2004)
;
_computing_data_collection
;
APEX2 (Bruker, 2004)
;
_computing_data_reduction
;
SAINT (Bruker, 2004)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and PLATON (Spek, 2009)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       ' bruker axs kappa axes2 CCD Diffractometer'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            33777
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.060
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.7100
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2004)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       block
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.163
_refine_diff_density_min         -0.159
_refine_ls_extinction_coef       0.0109(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         4744
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0586P)^2^+0.2573P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1217
_reflns_number_gt                3465
_reflns_number_total             4744
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            rz5182sup1.cif
_cod_data_source_block           I
_cod_database_code               2241575
_cod_database_fobs_code          2241575
_shelx_estimated_absorpt_t_min   0.974
_shelx_estimated_absorpt_t_max   0.983
_shelx_hkl_checksum              1624
_shelx_res_checksum              39538