(3a<i>S</i>,5a<i>R</i>,10a<i>S</i>,11a<i>R</i>)-2,2-Dimethyl-3a,9,10,10a,11,11a-hexahydro-5a<i>H</i>-1,3-dioxolo[4,5:3',4']furo[2',3'-<i>f</i>]indolizin-8(4<i>H</i>)-one
Vrábel, Viktor; Kožíšek, Jozef; Langer, Vratislav; Marchalín, Štefan; Bobošíková, Maria; Acta Crystallographica Section E 60 (2004) o1069–o1071; doi:10.1107/S1600536804012139

data_2203721
_publ_section_title
(3a<i>S</i>,5a<i>R</i>,10a<i>S</i>,11a<i>R</i>)-2,2-Dimethyl-3a,9,10,10a,11,11a-hexahydro-5a<i>H</i>-1,3-dioxolo[4,5:3',4']furo[2',3'-<i>f</i>]indolizin-8(4<i>H</i>)-one
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1069
_journal_page_last               o1071
_journal_paper_doi               10.1107/S1600536804012139
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C13 H19 N O4'
_chemical_formula_moiety         'C13 H19 N O4'
_chemical_formula_sum            'C13 H19 N O4'
_chemical_formula_weight         253.29
_chemical_name_systematic
;
(3aS,5aR,10aS,11aR)-2,2-Dimethyl-3a,9,10,10a,11,11a-hexahydro-
5aH-1,3-dioxolo[4,5:3',4']furo[2',3'-f]indolizin-8(4H)-one
;
_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                 90.0370(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.94650(10)
_cell_length_b                   17.7167(3)
_cell_length_c                   11.8918(2)
_cell_measurement_reflns_used    6898
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      30.94
_cell_measurement_theta_min      3.15
_cell_volume                     1252.83(4)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL (Bruker, 2001)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       \w
_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  0.0427
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22580
_diffrn_reflns_theta_full        32.94
_diffrn_reflns_theta_max         32.94
_diffrn_reflns_theta_min         1.15
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_T_max  0.9921
_exptl_absorpt_correction_T_min  0.9204
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2002)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.85
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         4637
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0447P)^2^+0.0464P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0822
_reflns_number_gt                4190
_reflns_number_total             4637
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cf6347.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2203721
_cod_database_fobs_code          2203721