4-Carboxypyridinium perchlorate 18-crown-6 dihydrate clathrate and 4-carboxypyridinium tetrafluoroborate 18-crown-6 dihydrate clathrate
Shi, Ping-ping; Zhang, Li; Ye, Qiong; Acta Crystallographica Section C 68 (2012) o266–o269; doi:10.1107/S0108270112024912

data_2018545
_publ_section_title
;
 4-Carboxypyridinium perchlorate 18-crown-6 dihydrate clathrate and
 4-carboxypyridinium tetrafluoroborate 18-crown-6 dihydrate clathrate
;
_journal_coeditor_code           KY3014
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o266
_journal_page_last               o269
_journal_paper_doi               10.1107/S0108270112024912
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C6 H6 N O2 + , Cl O4 - , C12 H24 O6 , 2H2 O'
_chemical_formula_moiety         'C6 H6 N O2 +, Cl O4 -, C12 H24 O6, 2(H2 O)'
_chemical_formula_sum            'C18 H34 Cl N O14'
_chemical_formula_weight         523.91
_chemical_name_systematic
;
4-Carboxypyridinium perchlorate 18-crown-6 dihydrate clathrate
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.668(3)
_cell_length_b                   10.242(2)
_cell_length_c                   17.191(3)
_cell_measurement_reflns_used    20523
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.02
_cell_volume                     2582.6(9)
_computing_cell_refinement       'CrystalClear (Rigaku, 2005)'
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       CCD_Profile_fitting
_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  0.0679
_diffrn_reflns_av_sigmaI/netI    0.0597
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25360
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.02
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.214
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.223
_refine_ls_abs_structure_details 'Flack (1983), with 2856 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.03(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         5913
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0645P)^2^+0.3025P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1481
_reflns_number_gt                3940
_reflns_number_total             5913
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ky3014.cif
_cod_data_source_block           I
_cod_original_cell_volume        2582.7(9)
_cod_original_sg_symbol_H-M      'P n a 21 '
_cod_database_code               2018545
_cod_database_fobs_code          2018545