Diethyl 4-methoxyoxalyl-3,5-diphenylpyrrolidine-2,2-dicarboxylate
He, Yan-Qin; Chen, Jin-Quan; Acta Crystallographica Section E 68 (2012) o1325–; doi:10.1107/S160053681201392X

data_2234563
_publ_section_title
;
 Diethyl 4-methoxyoxalyl-3,5-diphenylpyrrolidine-2,2-dicarboxylate
;
_journal_coeditor_code           CV5272
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1325
_journal_paper_doi               10.1107/S160053681201392X
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C25 H27 N O7'
_chemical_formula_moiety         'C25 H27 N O7'
_chemical_formula_sum            'C25 H27 N O7'
_chemical_formula_weight         453.48
_chemical_name_systematic
;
Diethyl 4-methoxyoxalyl-3,5-diphenylpyrrolidine-2,2-dicarboxylate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 102.213(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8779(3)
_cell_length_b                   20.3438(6)
_cell_length_c                   13.5740(5)
_cell_measurement_reflns_used    4380
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      29.0464
_cell_measurement_theta_min      3.2115
_cell_volume                     2396.12(14)
_computing_cell_refinement       'CrysAlis PRO (Oxford Diffraction, 2010)'
_computing_data_collection       'CrysAlis PRO (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis PRO (Oxford Diffraction, 2010)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      290(2)
_diffrn_detector_area_resol_mean 15.9149
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14990
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.22
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  0.9729
_exptl_absorpt_correction_T_min  0.9659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Oxford Diffraction, 2010)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.279
_refine_diff_density_min         -0.261
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         4887
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0514
_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^)+(0.0554P)^2^+0.3662P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1136
_refine_ls_wR_factor_ref         0.1334
_reflns_number_gt                3129
_reflns_number_total             4887
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cv5272.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2234563
_cod_database_fobs_code          2234563