Reversible phase transition of 2-carboxypyridinium perchlorate‒pyridinium-2-carboxylate (1/1)
Wang, Bi-Qin; Yan, Hai-Biao; Huang, Zheng-Qing; Zhang, Yun-Hua; Sun, Jing; Acta Crystallographica Section C 71 (2015) –; doi:10.1107/S2053229615003691

data_2019886
_publ_section_title
;
 Reversible phase transition of 2-carboxypyridinium
 perchlorate--pyridinium-2-carboxylate (1/1)
;
_journal_coeditor_code           KU3149
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229615003691
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C6 H6 N O2 + , Cl O4 - , C6 H5 N O2'
_chemical_formula_moiety         'C6 H6 N O2 +, Cl O4 -, C6 H5 N O2'
_chemical_formula_sum            'C12 H11 Cl N2 O8'
_chemical_formula_weight         346.68
_chemical_name_systematic
;
2-Carboxypyridinium perchlorate--pyridinium-2-carboxylate (1/1)
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_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                 106.29(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.252(2)
_cell_length_b                   5.8362(12)
_cell_length_c                   12.656(3)
_cell_measurement_reflns_used    5941
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      3.01
_cell_volume                     726.8(3)
_computing_cell_refinement
;
RAPID-AUTO (Rigaku, 2000)
;
_computing_data_collection
;
RAPID-AUTO (Rigaku, 2000)
;
_computing_data_reduction
;
RAPID-AUTO (Rigaku, 2000)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008), DIAMOND (Brandenburg & Putz, 2005),
<i>Marvinsketch</i> (ChemAxon, 2010)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXTL (Sheldrick, 2008)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku RAPID'
_diffrn_measurement_method       \w
_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  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0246
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6708
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         3.35
_exptl_absorpt_coefficient_mu    0.309
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.854
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(RAPID-AUTO; Rigaku, 2000)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.857
_refine_diff_density_min         -0.505
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         1653
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.232
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0785
_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^)+(0.1651P)^2^+0.3529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2523
_refine_ls_wR_factor_ref         0.2578
_reflns_number_gt                1460
_reflns_number_total             1653
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ku3149sup1.cif
_cod_data_source_block           296K
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               2019886
_cod_database_fobs_code          2019886