Ethyl 1'-methyl-2-oxo-4'-[(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]-2<i>H</i>-spiro[acenaphthylene-1,2'-pyrrolidine]-3'-carboxylate
Jagadeesan, G.; Sethusankar, K.; Prasanna, R.; Raghunathan, R.; Acta Crystallographica Section E 69 (2013) o1517–o1518; doi:10.1107/S1600536813024586

data_2238665
_publ_section_title
;
 Ethyl
 1'-methyl-2-oxo-4'-[(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]-2<i>H</i>-spiro[acenaphthylene-1,2'-pyrrolidine]-3'-carboxylate
;
_journal_coeditor_code           PV2644
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1517
_journal_page_last               o1518
_journal_paper_doi               10.1107/S1600536813024586
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C30 H35 N O8'
_chemical_formula_moiety         'C30 H35 N O8'
_chemical_formula_sum            'C30 H35 N O8'
_chemical_formula_weight         537.59
_chemical_name_systematic
;Ethyl
1'-methyl-2-oxo-4'-[(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]-2<i>H</i>-spiro[acenaphthylene-1,2'-pyrrolidine]-3'-carboxylate
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 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            4
_cell_length_a                   17.3582(15)
_cell_length_b                   18.5489(13)
_cell_length_c                   8.9213(8)
_cell_measurement_reflns_used    5184
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.24
_cell_measurement_theta_min      2.20
_cell_volume                     2872.4(4)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'ORTEP-3 for Windows (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 0.998
_diffrn_measured_fraction_theta_max 0.999
_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  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0348
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            14399
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.24
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  0.9778
_exptl_absorpt_correction_T_min  0.9735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.132
_refine_diff_density_min         -0.110
_refine_ls_extinction_coef       0.0099(8)
_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   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         5184
_refine_ls_number_restraints     332
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0476P)^2^+0.2077P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0872
_refine_ls_wR_factor_ref         0.0987
_reflns_number_gt                3771
_reflns_number_total             5184
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            pv2644.cif
_cod_data_source_block           I
_cod_database_code               2238665