(1<i>S</i>,3a<i>S</i>,4<i>S</i>,7a<i>S</i>)-Ethyl 1-benzyl-2-(4-methoxybenzyl)-6,7-dimethyl-3-oxo-2,3,3a,4,5,7a-hexahydro-1<i>H</i>-isoindole-4-carboxylate dichloromethane monosolvate
Lin, Benguo; Wu, Jin-Long; Acta Crystallographica Section E 69 (2013) o316–; doi:10.1107/S1600536813002560

data_2237294
_publ_section_title
;
 (1<i>S</i>,3a<i>S</i>,4<i>S</i>,7a<i>S</i>)-Ethyl
 1-benzyl-2-(4-methoxybenzyl)-6,7-dimethyl-3-oxo-2,3,3a,4,5,7a-hexahydro-1<i>H</i>-isoindole-4-carboxylate
 dichloromethane monosolvate
;
_journal_coeditor_code           CV5380
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o316
_journal_paper_doi               10.1107/S1600536813002560
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C28 H33 N O4, C H2 Cl2'
_chemical_formula_moiety         'C28 H33 N O4, C H2 Cl2'
_chemical_formula_sum            'C29 H35 Cl2 N O4'
_chemical_formula_weight         532.48
_chemical_name_systematic
;(1<i>S</i>,3a<i>S</i>,4<i>S</i>,7a<i>S</i>)-Ethyl 1-benzyl-2-(4-methoxybenzyl)-6,7-dimethyl-3-oxo-2,3,3a,4,5,7a-hexahydro-1<i>H</i>-isoindole-4-carboxylate
dichloromethane monosolvate
;
_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                 109.221(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.6864(5)
_cell_length_b                   15.5706(8)
_cell_length_c                   9.7460(6)
_cell_measurement_reflns_used    2239
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.0882
_cell_measurement_theta_min      2.8794
_cell_volume                     1387.98(14)
_computing_cell_refinement       'CrysAlis PRO (Oxford Diffraction, 2011)'
_computing_data_collection       'CrysAlis PRO (Oxford Diffraction, 2011)'
_computing_data_reduction        'CrysAlis PRO (Oxford Diffraction, 2011)'
_computing_molecular_graphics    'OLEX2 (Dolomanov <i>et al.</i>, 2009)'
_computing_publication_material  'OLEX2 (Dolomanov <i>et al.</i>, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Oxford Diffraction Xcalibur (Atlas, Gemini ultra)'
_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  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6260
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.89
_exptl_absorpt_coefficient_mu    0.268
_exptl_absorpt_correction_T_max  0.9409
_exptl_absorpt_correction_T_min  0.9191
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Oxford Diffraction, 2011)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.219
_refine_ls_abs_structure_details 'Flack (1983), 1789 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.05(11)
_refine_ls_extinction_coef       0.0155(19)
_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   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         3844
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0493P)^2^+0.5082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1270
_reflns_number_gt                2990
_reflns_number_total             3844
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            cv5380.cif
_cod_data_source_block           I
_cod_original_cell_volume        1387.99(14)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2237294
_cod_database_fobs_code          2237294