(1<i>S</i>,1'<i>S</i>,2'<i>R</i>,4a'<i>S</i>,9a'<i>S</i>,9b'<i>R</i>)-1'-Acetyloxy-2,4'-dioxo-2',4',4a',7',8',9',9a',9b'-octahydro-1'<i>H</i>,2<i>H</i>-spiro[acenaphthylene-1,5'-pyrano[4,3-<i>a</i>]pyrrolizin]-2'-ylmethyl acetate
Santhiya, S.; Naga Siva Rao, J.; Raghunathan, R.; Latha, N.; Lakshmi, S.; Acta Crystallographica Section E 69 (2013) o1601–; doi:10.1107/S1600536813026111

data_2238769
_publ_section_title
;
 (1<i>S</i>,1'<i>S</i>,2'<i>R</i>,4a'<i>S</i>,9a'<i>S</i>,9b'<i>R</i>)-1'-Acetyloxy-2,4'-dioxo-2',4',4a',7',8',9',9a',9b'-octahydro-1'<i>H</i>,2<i>H</i>-spiro[acenaphthylene-1,5'-pyrano[4,3-<i>a</i>]pyrrolizin]-2'-ylmethyl
 acetate
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1601
_journal_paper_doi               10.1107/S1600536813026111
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C26 H25 N O7'
_chemical_formula_moiety         'C26 H25 N O7'
_chemical_formula_sum            'C26 H25 N O7'
_chemical_formula_weight         463.47
_chemical_melting_point          481.15
_chemical_name_systematic
'(1<i>S</i>,1'<i>S</i>,2'<i>R</i>,4a'<i>S</i>,9a'<i>S</i>,9b'<i>R</i>)-1'-Acetyloxy-2,4'-dioxo-2',4',4a',7',8',9',9a',9b'-octahydro-1'<i>H</i>,2<i>H</i>-spiro[acenaphthylene-1,5'-pyrano[4,3-<i>a</i>]pyrrolizin]-2'-ylmethyl acetate'
_space_group_IT_number           96
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.6792(3)
_cell_length_b                   13.6792(3)
_cell_length_c                   24.9625(13)
_cell_measurement_reflns_used    5405
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      22.16
_cell_measurement_theta_min      2.20
_cell_volume                     4671.0(3)
_computing_cell_refinement       'APEX2 and SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT and XPREP (Bruker, 2004)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       '\w and \f scan'
_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  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            21173
_diffrn_reflns_theta_full        25.09
_diffrn_reflns_theta_max         25.09
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  0.9763
_exptl_absorpt_correction_T_min  0.9017
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.120
_refine_ls_extinction_coef       0.0038(5)
_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   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         4010
_refine_ls_number_restraints     138
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0494P)^2^+0.4380P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.1041
_reflns_number_gt                2923
_reflns_number_total             4010
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            nc2316.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     P4nw2abw
_cod_database_code               2238769