4'-Methyl-14',19'-dioxa-4'-azaspiro[acenaphthylene-1,5'-tetracyclo[18.4.0.0^2,6^.0^8,13^]tetracosane]-1'(24'),8',10',12',20',22'-hexaene-2,7'(1<i>H</i>)-dione
Narayanan, Sibi; Srinivasan, Thothadri; Purushothaman, Santhanagopalan; Raghunathan, Raghavachary; Velmurugan, Devadasan; Acta Crystallographica Section E 68 (2012) o3345–; doi:10.1107/S1600536812046144

data_2236996
_publ_section_title
;
 4'-Methyl-14',19'-dioxa-4'-azaspiro[acenaphthylene-1,5'-tetracyclo[18.4.0.0^2,6^.0^8,13^]tetracosane]-1'(24'),8',10',12',20',22'-hexaene-2,7'(1<i>H</i>)-dione
;
_journal_coeditor_code           PV2602
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3345
_journal_paper_doi               10.1107/S1600536812046144
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C33 H29 N O4'
_chemical_formula_moiety         'C33 H29 N O4'
_chemical_formula_sum            'C33 H29 N O4'
_chemical_formula_weight         503.57
_chemical_name_systematic
;
4'-Methyl-14',19'-dioxa-4'-azaspiro[acenaphthylene-1,5'-
tetracyclo[18.4.0.0^2,6^.0^8,13^]tetracosane]-1'(24'),8',10',12',20',22'-
hexaene-2,7'(1<i>H</i>)-dione
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.965(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.248(2)
_cell_length_b                   16.609(3)
_cell_length_c                   14.037(3)
_cell_measurement_reflns_used    6363
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      1.8
_cell_volume                     2618.9(9)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2012)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\w and \f 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  0.0354
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24740
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.3
_diffrn_reflns_theta_min         1.8
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Bruker, 2008)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.222
_refine_diff_density_min         -0.210
_refine_ls_extinction_coef       0.0125(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         6363
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0523P)^2^+0.5720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1278
_reflns_number_gt                4183
_reflns_number_total             6363
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pv2602.cif
_cod_data_source_block           I
_cod_original_cell_volume        2618.8(9)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2236996
_cod_database_fobs_code          2236996