Bis(4-aminopyridinium) bis(hydrogen oxalate) monohydrate
Fun, Hoong-Kun; John, Jain; Jebas, Samuel Robinson; Balasubramanian, T; Acta Crystallographica Section E 65 (2009) o748–o749; doi:10.1107/S1600536809007247

data_2221241
_publ_section_title
;
 Bis(4-aminopyridinium) bis(hydrogen oxalate) monohydrate
;
_journal_coeditor_code           AT2732
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o748
_journal_page_last               o749
_journal_paper_doi               10.1107/S1600536809007247
_journal_volume                  65
_journal_year                    2009
_chemical_formula_moiety         'C5 H7 N2 + , C2 H O4 - , 0.5(H2 O)'
_chemical_formula_sum            'C7 H9 N2 O4.5'
_chemical_formula_weight         193.16
_chemical_name_common            '4-aminopyridinium oxalate'
_chemical_name_systematic
;
Bis(4-aminopyridinium) bis(hydrogen oxalate) monohydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.617(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.6429(6)
_cell_length_b                   5.6929(2)
_cell_length_c                   19.9091(7)
_cell_measurement_reflns_used    7009
_cell_measurement_temperature    100
_cell_measurement_theta_max      38.77
_cell_measurement_theta_min      2.70
_cell_volume                     1707.52(11)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            12438
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.12
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.127
_exptl_absorpt_correction_T_max  0.9859
_exptl_absorpt_correction_T_min  0.9061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.243
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         2467
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max_lt       0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+0.8323P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0958
_reflns_number_gt                2159
_reflns_number_total             2467
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            at2732.cif
_cod_data_source_block           I
_cod_depositor_comments
;

2017-04-07
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_moiety     '2C5 H7 N2 + , 2C2 H O4 - , H2 O'
_cod_original_formula_sum        'C14 H18 N4 O9'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     386.32
_cod_database_code               2221241
_cod_database_fobs_code          2221241