2,2-Diethyl 3,4-dimethyl 5-(4-cyanophenyl)pyrrolidine-2,2,3,4-tetracarboxylate
He, Long; Acta Crystallographica Section E 68 (2012) o2363–; doi:10.1107/S1600536812029625

data_2236019
_publ_section_title
;
 2,2-Diethyl 3,4-dimethyl
 5-(4-cyanophenyl)pyrrolidine-2,2,3,4-tetracarboxylate
;
_journal_coeditor_code           XU5557
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2363
_journal_paper_doi               10.1107/S1600536812029625
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C21 H24 N2 O8'
_chemical_formula_moiety         'C21 H24 N2 O8'
_chemical_formula_sum            'C21 H24 N2 O8'
_chemical_formula_weight         432.42
_chemical_name_systematic
;
2,2-Diethyl 3,4-dimethyl 5-(4-cyanophenyl)pyrrolidine-2,2,3,4-tetracarboxylate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   8.4720(2)
_cell_length_b                   10.3043(2)
_cell_length_c                   25.8774(5)
_cell_measurement_reflns_used    10771
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      72.2867
_cell_measurement_theta_min      1.7053
_cell_volume                     2259.05(8)
_computing_cell_refinement       'CrysAlis PRO (Oxford Diffraction, 2007)'
_computing_data_collection       'CrysAlis PRO (Oxford Diffraction, 2007)'
_computing_data_reduction        'CrysAlis PRO (Oxford Diffraction, 2007)'
_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      291(2)
_diffrn_detector_area_resol_mean 15.9149
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Oxford Diffraction Gemini S Ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0140
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            26556
_diffrn_reflns_theta_full        72.58
_diffrn_reflns_theta_max         72.58
_diffrn_reflns_theta_min         3.42
_exptl_absorpt_coefficient_mu    0.829
_exptl_absorpt_correction_T_max  0.7891
_exptl_absorpt_correction_T_min  0.7435
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Oxford Diffraction, 2007)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.220
_refine_ls_extinction_coef       0.0015(4)
_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   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         2565
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0500
_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^)+(0.0724P)^2^+0.5988P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1341
_refine_ls_wR_factor_ref         0.1413
_reflns_number_gt                2050
_reflns_number_total             2565
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            xu5557.cif
_cod_data_source_block           I
_cod_database_code               2236019
_cod_database_fobs_code          2236019