Increased Chemical Purity Using a Hydrate
Black, Simon N.; Cuthbert, Murray W.; Roberts, Ron J.; Stensland, Birgitta; Crystal Growth & Design 4 (2004) 539–; doi:10.1021/cg034222v

data_4505330
_publ_section_title
;
 Increased Chemical Purity Using a Hydrate
;
_journal_issue                   3
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              539
_journal_paper_doi               10.1021/cg034222v
_journal_volume                  4
_journal_year                    2004
_chemical_formula_moiety         'C18 H21 Cl F2 N3 O5 '
_chemical_formula_sum            'C18 H21 Cl F2 N3 O5'
_chemical_formula_weight         432.83
_chemical_name_common            'Piperidine Hydrate'
_chemical_name_systematic
;
4-(2,6-difluoro-4-{(5R)-5-[(3-isoxazolyl]-2-oxo-1,3-
oxazolan-3-yl}phenyl)-1,2,3,6-tetrahydropyridinium 
chloride monohydrate
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'maXus & Platon'
_cell_angle_alpha                90.000(10)
_cell_angle_beta                 115.100(10)
_cell_angle_gamma                90.000(10)
_cell_formula_units_Z            4
_cell_length_a                   21.6750(10)
_cell_length_b                   5.8970(10)
_cell_length_c                   16.1290(10)
_cell_measurement_temperature    200
_cell_volume                     1866.9(4)
_computing_molecular_graphics    'Ortep (Johnson, 1976)'
_computing_publication_material  'maxus(Mackay et al., 1999)'
_computing_structure_refinement  'maxus(Mackay et al., 1999)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           ' MoK\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            3631
_diffrn_reflns_theta_max         27.49
_exptl_absorpt_coefficient_mu    0.26
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
prism: 0.14x0.17x0.29 mm 
Batch PH13177/O30, Recryst. EtOH /Birgitta Stensland
;
_exptl_crystal_F_000             900
_refine_diff_density_max         0.34
_refine_diff_density_min         -0.29
_refine_diff_density_rms         0.06
_refine_ls_abs_structure_details
;
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.714
_refine_ls_goodness_of_fit_gt    1.435
_refine_ls_goodness_of_fit_ref   1.435
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         2742
_refine_ls_R_factor_all          0.061
_refine_ls_R_factor_gt           0.041
_refine_ls_R_factor_obs          0.041
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     ' w = 1 / ( s^2^(Fo^2^) + 0.03000 * Fo^2^)'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.069
_refine_ls_wR_factor_gt          0.059
_refine_ls_wR_factor_obs         0.043
_reflns_d_resolution_high        0.62
_reflns_d_resolution_low         1.68
_reflns_limit_h_max              27
_reflns_limit_h_min              -28
_reflns_limit_k_max              7
_reflns_limit_k_min              -6
_reflns_limit_l_max              27
_reflns_limit_l_min              -28
_reflns_number_gt                2742
_reflns_number_total             3610
_reflns_threshold_expression     'I> 3.00 sigma(I)'
_cod_data_source_file            cg034222vsi20031117_065828.cif
_cod_data_source_block           "'Piperidine'HClxH2O"
_cod_original_cell_volume        1866.9(3)
_cod_original_sg_symbol_H-M      'C 2'
_cod_original_formula_sum        'C18 H21 Cl F2 N3 O5 '
_cod_database_code               4505330