Ethyl 6-(4-fluorophenyl)-4-hydroxy-2-oxo-4-trifluoromethyl-1,3-diazinane-5-carboxylate monohydrate
Li, Gong-Chun; Wu, Chang-Zeng; Guo, Li-Li; Yang, Feng-Ling; Acta Crystallographica Section E 67 (2011) o1704–o1705; doi:10.1107/S1600536811021866

data_2230752
_publ_section_title
;
 Ethyl
 6-(4-fluorophenyl)-4-hydroxy-2-oxo-4-trifluoromethyl-1,3-diazinane-5-carboxylate
 monohydrate
;
_journal_coeditor_code           JH2293
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1704
_journal_page_last               o1705
_journal_paper_doi               10.1107/S1600536811021866
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C14 H14 F4 N2 O4, H2 O1'
_chemical_formula_moiety         'C14 H14 F4 N2 O4, H2 O1'
_chemical_formula_sum            'C14 H16 F4 N2 O5'
_chemical_formula_weight         368.29
_chemical_name_systematic
;
Ethyl 6-(4-fluorophenyl)-4-hydroxy-2-oxo-4-trifluoromethyl-
1,3-diazinane-5-carboxylate monohydrate
;
_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
_cell_angle_alpha                98.463(7)
_cell_angle_beta                 103.642(8)
_cell_angle_gamma                104.400(9)
_cell_formula_units_Z            4
_cell_length_a                   10.0196(9)
_cell_length_b                   12.1718(12)
_cell_length_c                   14.3037(14)
_cell_measurement_reflns_used    5664
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      1.5
_cell_volume                     1602.2(3)
_computing_cell_refinement       'CrystalClear (Rigaku, 2009)'
_computing_data_collection       'CrystalClear (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear (Rigaku, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku Saturn CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0652
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20692
_diffrn_reflns_theta_full        27.89
_diffrn_reflns_theta_max         27.89
_diffrn_reflns_theta_min         1.50
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.144
_exptl_absorpt_correction_T_max  0.9801
_exptl_absorpt_correction_T_min  0.9717
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2009)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.870
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         7612
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.870
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0313
_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^)+(0.0267P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0692
_refine_ls_wR_factor_ref         0.0721
_reflns_number_gt                4575
_reflns_number_total             7612
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jh2293.cif
_cod_data_source_block           I
_cod_database_code               2230752
_cod_database_fobs_code          2230752