(1<i>S</i>,2<i>E</i>,6<i>R</i>,7a<i>R</i>)-1,6-Dihydroxy-2-(4-nitrobenzylidene)-2,3,5,6,7,7a-hexahydro-1<i>H</i>-pyrrolizin-3-one
Oliveira, F. L.; Freire, K. R. L.; Aparicio, R.; Coelho, F.; Acta Crystallographica Section E 68 (2012) o1570–o1571; doi:10.1107/S1600536812018235

data_2234750
_publ_section_title
;
 (1<i>S</i>,2<i>E</i>,6<i>R</i>,7a<i>R</i>)-1,6-Dihydroxy-2-(4-nitrobenzylidene)-2,3,5,6,7,7a-hexahydro-1<i>H</i>-pyrrolizin-3-one
;
_journal_coeditor_code           PV2525
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1570
_journal_page_last               o1571
_journal_paper_doi               10.1107/S1600536812018235
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C14 H14 N2 O5'
_chemical_formula_moiety         'C14 H14 N2 O5'
_chemical_formula_sum            'C14 H14 N2 O5'
_chemical_formula_weight         290.27
_chemical_name_systematic
;
(1<i>S</i>,2<i>E</i>,6<i>R</i>,7a<i>R</i>)-1,6-Dihydroxy-2-
(4-nitrobenzylidene)-2,3,5,6,7,7a-hexahydro-1<i>H</i>-pyrrolizin-3-one
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_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                 92.335(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.8289(6)
_cell_length_b                   7.0433(6)
_cell_length_c                   26.618(3)
_cell_measurement_reflns_used    4038
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.75
_cell_measurement_theta_min      1.66
_cell_volume                     1279.2(2)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2010)'
_computing_data_collection       '<i>APEX2</i> (Bruker, 2010)'
_computing_data_reduction        '<i>SAINT</i> (Bruker, 2010)'
_computing_molecular_graphics    '<i>PLATON</i> (Spek, 2009)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker Kappa APEXII DUO'
_diffrn_measurement_method       'Bruker APEX CCD area-detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0215
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            41060
_diffrn_reflns_theta_full        67.75
_diffrn_reflns_theta_max         67.75
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    0.980
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8441
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(SADABS; Bruker, 2010)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.152
_refine_diff_density_min         -0.157
_refine_ls_abs_structure_details
;
Flack (1983) and Hooft <i>et al.</i> (2008);
Hooft parameter = 0.04(4), 1539 Bijvoet pairs
;
_refine_ls_abs_structure_Flack   0.03(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         4038
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0255
_refine_ls_R_factor_gt           0.0250
_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^)+(0.0419P)^2^+0.3034P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0664
_refine_ls_wR_factor_ref         0.0673
_reflns_number_gt                3986
_reflns_number_total             4038
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            pv2525.cif
_cod_data_source_block           I
_cod_database_code               2234750
_cod_database_fobs_code          2234750