Bis[2-(2-pyridylamino)pyridinium] squarate dihydrate
Ibrahim Uçar; Ahmet Bulut; Orhan Büyükgüngör; Acta Crystallographica Section E 63 (2007) o3377–o3377; doi:10.1107/S160053680703139X

data_2214675
_publ_section_title
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 Bis[2-(2-pyridylamino)pyridinium] squarate dihydrate
;
_journal_coeditor_code           HB2459
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3377
_journal_page_last               o3377
_journal_paper_doi               10.1107/S160053680703139X
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '2C10 H10 N3 + , C4 O4 2- , 2H2 O'
_chemical_formula_moiety         '2C10 H10 N3 + , C4 O4 2- , 2H2 O'
_chemical_formula_sum            'C24 H24 N6 O6'
_chemical_formula_weight         492.50
_chemical_name_systematic
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Bis[2-(2-pyridylamino)pyridinium] squarate dihydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                74.34(3)
_cell_angle_beta                 87.26(2)
_cell_angle_gamma                71.85(4)
_cell_formula_units_Z            1
_cell_length_a                   8.072(2)
_cell_length_b                   8.493(3)
_cell_length_c                   8.833(2)
_cell_measurement_reflns_used    1875
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      27.82
_cell_measurement_theta_min      2.59
_cell_volume                     553.6(3)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-RED32 (Stoe & Cie, 2002)'
_computing_molecular_graphics    'ORTEPIII (Farrugia, 1997)'
_computing_publication_material  'WinGX  (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      297(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6024
_diffrn_reflns_theta_full        28.19
_diffrn_reflns_theta_max         28.19
_diffrn_reflns_theta_min         2.62
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.109
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.947
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(X-RED32; Stoe & Cie, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             258.0
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.266
_refine_diff_density_min         -0.196
_refine_ls_extinction_coef       0.079(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         2634
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0672P)^2^+0.0549P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1159
_refine_ls_wR_factor_ref         0.1224
_reflns_number_gt                2027
_reflns_number_total             2634
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb2459.cif
_cod_data_source_block           I
_cod_database_code               2214675
_cod_database_fobs_code          2214675