3,4-Diaminopyridinium hydrogen squarate
Bojidarka Koleva; Tsanko Tsanev; Tsonko Kolev; Heike Mayer-Figge; William S. Sheldrick; Acta Crystallographica Section E 63 (2007) o3356–o3356; doi:10.1107/S1600536807031170

data_2214536
_publ_section_title
;
 3,4-Diaminopyridinium hydrogen squarate
;
_journal_coeditor_code           BT2412
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3356
_journal_page_last               o3356
_journal_paper_doi               10.1107/S1600536807031170
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C5 H8 N3 +, C4 H O4 -'
_chemical_formula_moiety         'C5 H8 N3 +, C4 H O4 -'
_chemical_formula_sum            'C9 H9 N3 O4'
_chemical_formula_weight         223.19
_chemical_name_systematic
;
3,4-Diaminopyridinium hydrogen squarate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 96.56(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.069(2)
_cell_length_b                   7.1925(14)
_cell_length_c                   13.480(3)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      7.5
_cell_volume                     969.8(4)
_computing_cell_refinement       R3m/V
_computing_data_collection       'R3m/V (Siemens, 1989)'
_computing_data_reduction        'XDISK (Siemens, 1989)'
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 1995)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Siemens P4 four-circle'
_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  0.0439
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            2310
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.04
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.123
_exptl_absorpt_correction_T_max  0.93837
_exptl_absorpt_correction_T_min  0.84350
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(XPREP; Sheldrick, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prsim
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.46
_refine_diff_density_max         0.243
_refine_diff_density_min         -0.375
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         1698
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0656
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0946P)^2^+0.5492P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1746
_refine_ls_wR_factor_ref         0.1890
_reflns_number_gt                1172
_reflns_number_total             1698
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt2412.cif
_cod_data_source_block           I
_cod_original_cell_volume        969.8(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2214536
_cod_database_fobs_code          2214536