Trimethyl 5-(2-chloro-4-fluorophenyl)-2-phenylpyrrolidine-2,3,4-tricarboxylate
He, Long; Chen, Lian-Mei; Acta Crystallographica Section E 65 (2009) o2927–; doi:10.1107/S1600536809044274

data_2224093
_publ_section_title
;
 Trimethyl
 5-(2-chloro-4-fluorophenyl)-2-phenylpyrrolidine-2,3,4-tricarboxylate
;
_journal_coeditor_code           XU2655
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2927
_journal_paper_doi               10.1107/S1600536809044274
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C22 H21 Cl F N O6'
_chemical_formula_moiety         'C22 H21 Cl F N O6'
_chemical_formula_sum            'C22 H21 Cl F N O6'
_chemical_formula_weight         449.85
_chemical_name_systematic
;Trimethyl
 5-(2-chloro-4-fluorophenyl)-2-phenylpyrrolidine-2,3,4-tricarboxylate
;
_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                   9.474(3)
_cell_length_b                   15.057(8)
_cell_length_c                   15.182(5)
_cell_measurement_reflns_used    23516
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      62.7903
_cell_measurement_theta_min      2.9108
_cell_volume                     2165.7(15)
_computing_cell_refinement       'CrysAlis Pro (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis Pro (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis Pro (Oxford Diffraction, 2009)'
_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      298(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
_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  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0107
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            32943
_diffrn_reflns_theta_full        62.63
_diffrn_reflns_theta_max         62.63
_diffrn_reflns_theta_min         4.14
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.981
_exptl_absorpt_correction_T_max  0.9430
_exptl_absorpt_correction_T_min  0.5198
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis Pro; Oxford Diffraction, 2009)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.119
_refine_diff_density_min         -0.160
_refine_ls_abs_structure_details 'Flack (1983), 1456 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.001(11)
_refine_ls_extinction_coef       0.0055(2)
_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   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         3442
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0235
_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^)+(0.0318P)^2^+0.3155P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0603
_reflns_number_gt                3332
_reflns_number_total             3442
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            xu2655.cif
_cod_data_source_block           I
_cod_database_code               2224093
_cod_database_fobs_code          2224093