Ethyl 4-hydroxy-1-methyl-5-oxo-2-phenylpyrrolidine-3-carboxylate 1.25-hydrate
Mansor, Nurul Shulehaf; Mohammat, Mohd Fazli; Shaameri, Zurina; Khaledi, Hamid; Acta Crystallographica Section E 69 (2013) o293–o294; doi:10.1107/S1600536813001943

data_2237343
_publ_section_title
;
 Ethyl 4-hydroxy-1-methyl-5-oxo-2-phenylpyrrolidine-3-carboxylate
 1.25-hydrate
;
_journal_coeditor_code           IS5239
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o293
_journal_page_last               o294
_journal_paper_doi               10.1107/S1600536813001943
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C14 H17 N O4, 1.25H2 O'
_chemical_formula_moiety         'C14 H17 N O4, 1.25(H2 O)'
_chemical_formula_sum            'C14 H19.5 N O5.25'
_chemical_formula_weight         285.81
_chemical_name_systematic
;
Ethyl 4-hydroxy-1-methyl-5-oxo-2-phenylpyrrolidine-3-carboxylate 1.25-hydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.3730(10)
_cell_angle_beta                 80.4250(10)
_cell_angle_gamma                87.0580(10)
_cell_formula_units_Z            8
_cell_length_a                   10.3669(2)
_cell_length_b                   15.7466(3)
_cell_length_c                   18.4539(3)
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.67
_cell_measurement_theta_min      2.36
_cell_volume                     2898.31(9)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \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  0.0182
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22505
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  0.9910
_exptl_absorpt_correction_T_min  0.9792
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.752
_refine_diff_density_min         -0.283
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     780
_refine_ls_number_reflns         11260
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0387
_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^)+(0.0505P)^2^+1.2863P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1038
_reflns_number_gt                9637
_reflns_number_total             11260
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            is5239.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C14 H19.5 N1 O5.25'
_cod_database_code               2237343
_cod_database_fobs_code          2237343