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_4505329
_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 H18 Cl F2 N3 O4 '
_chemical_formula_sum            'C18 H18 Cl F2 N3 O4'
_chemical_formula_weight         413.808
_chemical_name_common            'Piperidine anhydrate'
_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 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'maXus & Platon'
_cell_angle_alpha                90.00(1)
_cell_angle_beta                 107.95(1)
_cell_angle_gamma                90.00(1)
_cell_formula_units_Z            4
_cell_length_a                   12.770(1)
_cell_length_b                   9.931(1)
_cell_length_c                   15.560(1)
_cell_measurement_temperature    298
_cell_volume                     1877.3(3)
_computing_data_collection       KappaCCD
_computing_data_reduction        'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_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_measurement_device       KappaCCD
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           ' MoK\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7561
_diffrn_reflns_theta_max         27.96
_exptl_absorpt_coefficient_mu    0.25
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
prism. size: 0.14x0.17x0.29 mm 
Batch PH13177/O30, Recryst. EtOH /Birgitta Stensland
;
_exptl_crystal_F_000             856
_refine_diff_density_max         0.21
_refine_diff_density_min         -0.22
_refine_diff_density_rms         0.04
_refine_ls_abs_structure_details
;
;
_refine_ls_extinction_coef       9801(1095)
_refine_ls_extinction_expression
;
 equ(22) p292 'Crystallographic Computing' (1970)
;
_refine_ls_extinction_method     Zachariasen
_refine_ls_goodness_of_fit_all   1.817
_refine_ls_goodness_of_fit_gt    1.069
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         4725
_refine_ls_R_factor_all          0.070
_refine_ls_R_factor_gt           0.036
_refine_ls_R_factor_obs          0.036
_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         0.106
_refine_ls_wR_factor_gt          0.046
_refine_ls_wR_factor_obs         0.037
_reflns_d_resolution_high        0.62
_reflns_d_resolution_low         1.93
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              13
_reflns_limit_k_min              -12
_reflns_limit_l_max              16
_reflns_limit_l_min              -16
_reflns_number_gt                4725
_reflns_number_total             7561
_reflns_threshold_expression     'I> 3.00 sigma(I)'
_cod_data_source_file            cg034222vsi20031117_065752.cif
_cod_data_source_block           "'Piperidine'HCl"
_cod_original_cell_volume        1877.2(3)
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C18 H18 Cl F2 N3 O4 '
_cod_database_code               4505329