3-Ethyl 2-methyl 8-bromo-2-phenyl-1,2,3,3a,4,9b-hexahydrochromeno[4,3-<i>b</i>]pyrrole-2,3-dicarboxylate
He, Long; Acta Crystallographica Section E 66 (2010) o3075–; doi:10.1107/S1600536810044491

data_2228598
_publ_section_title
;
 3-Ethyl 2-methyl
 8-bromo-2-phenyl-1,2,3,3a,4,9b-hexahydrochromeno[4,3-<i>b</i>]pyrrole-2,3-dicarboxylate
;
_journal_coeditor_code           XU5063
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3075
_journal_paper_doi               10.1107/S1600536810044491
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C22 H22 Br N O5'
_chemical_formula_moiety         'C22 H22 Br N O5'
_chemical_formula_sum            'C22 H22 Br N O5'
_chemical_formula_weight         460.32
_chemical_name_systematic
;
3-Ethyl 2-methyl 8-bromo-2-phenyl-
1,2,3,3a,4,9b-hexahydrochromeno[4,3-<i>b</i>]pyrrole-2,3-dicarboxylate
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 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                 107.856(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1046(8)
_cell_length_b                   11.1633(6)
_cell_length_c                   17.9779(9)
_cell_measurement_reflns_used    4173
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.0808
_cell_measurement_theta_min      2.9918
_cell_volume                     2121.3(2)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2008)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2008)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2008)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 15.9149
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Oxford diffraction Gemini S Ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0564
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10601
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         3.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.970
_exptl_absorpt_correction_T_max  0.5214
_exptl_absorpt_correction_T_min  0.4391
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis Pro; Oxford Diffraction, 2009)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.358
_refine_ls_extinction_coef       0.0095(11)
_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   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         3609
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1313
_refine_ls_wR_factor_ref         0.1371
_reflns_number_gt                2015
_reflns_number_total             3609
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            xu5063.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               2228598
_cod_database_fobs_code          2228598