Ethyl (1<i>R</i>,1'<i>S</i>,2'<i>S</i>,7a'<i>R</i>)-2-oxo-1'-[(3a<i>R</i>,5<i>R</i>,5a<i>S</i>,8a<i>S</i>,8b<i>R</i>)-2,2,7,7-tetramethyltetrahydro-3a<i>H</i>-bis[1,3]dioxolo[4,5-<i>b</i>:4',5'-<i>d</i>]pyran-5-yl]-1',2',5',6',7',7a'-hexahydro-2<i>H</i>-spiro[acenaphthylene-1,3'-pyrrolizine]-2'-carboxylate
Jagadeesan, G.; Sethusankar, K.; Prasanna, R.; Raghunathan, R.; Acta Crystallographica Section E 68 (2012) o382–o383; doi:10.1107/S1600536811055760

data_2233589
_publ_section_title
;
 Ethyl
 (1<i>R</i>,1'<i>S</i>,2'<i>S</i>,7a'<i>R</i>)-2-oxo-1'-[(3a<i>R</i>,5<i>R</i>,5a<i>S</i>,8a<i>S</i>,8b<i>R</i>)-2,2,7,7-tetramethyltetrahydro-3a<i>H</i>-bis[1,3]dioxolo[4,5-<i>b</i>:4',5'-<i>d</i>]pyran-5-yl]-1',2',5',6',7',7a'-hexahydro-2<i>H</i>-spiro[acenaphthylene-1,3'-pyrrolizine]-2'-carboxylate
;
_journal_coeditor_code           PV2491
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o382
_journal_page_last               o383
_journal_paper_doi               10.1107/S1600536811055760
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C32 H37 N O8'
_chemical_formula_moiety         'C32 H37 N O8'
_chemical_formula_sum            'C32 H37 N O8'
_chemical_formula_weight         563.63
_chemical_name_systematic
;
Ethyl (1<i>R</i>,1'<i>S</i>,2'<i>S</i>,7a'<i>R</i>)-2-oxo-
1'-[(3a<i>R</i>,5<i>R</i>,5a<i>S</i>,8a<i>S</i>,8b<i>R</i>)-2,2,7,7-
tetramethyltetrahydro-3a<i>H</i>-
bis[1,3]dioxolo[4,5-<i>b</i>:4',5'-<i>d</i>]pyran-5-yl]-1',2',5',6',7',7a'-
hexahydro-2<i>H</i>-spiro[acenaphthylene-1,3'-pyrrolizine]-2'-carboxylate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 96.990(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.4723(4)
_cell_length_b                   8.9548(2)
_cell_length_c                   15.0543(5)
_cell_measurement_reflns_used    5063
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.7
_cell_measurement_theta_min      1.4
_cell_volume                     1535.07(8)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       '\w 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  0.0256
_diffrn_reflns_av_sigmaI/netI    0.0264
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20295
_diffrn_reflns_theta_full        30.73
_diffrn_reflns_theta_max         30.73
_diffrn_reflns_theta_min         2.38
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  0.9743
_exptl_absorpt_correction_T_min  0.9659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.237
_refine_diff_density_min         -0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         5039
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0616P)^2^+0.0862P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1244
_reflns_number_gt                3469
_reflns_number_total             5063
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            pv2491.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2233589
_cod_database_fobs_code          2233589