Hemi(4,4'-bipyridinium) hexafluoridophosphate bis(4-aminobenzoic acid) 4,4'-bipyridine monohydrate
Wu, Yi-Yi; Huang, Chun-De; Huang, Jie-Xuan; Zeng, Rong-Hua; Luo, Yi-Fan; Acta Crystallographica Section E 65 (2009) o278–; doi:10.1107/S1600536808043900

data_2220944
_publ_section_title
;
 Hemi(4,4'-bipyridinium) hexafluoridophosphate bis(4-aminobenzoic acid)
 4,4'-bipyridine monohydrate
;
_journal_coeditor_code           WN2299
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o278
_journal_paper_doi               10.1107/S1600536808043900
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac
'0.5C10 H10 N2 2+, P1 F6 -, C10 H8 N2, 2C7 H7 N O2, H2 O1'
_chemical_formula_moiety
'0.5(C10 H10 N2 2+), P1 F6 -, C10 H8 N2, 2(C7 H7 N O2), H2 O1'
_chemical_formula_sum            'C29 H29 F6 N5 O5 P'
_chemical_formula_weight         672.54
_chemical_name_systematic
;
Hemi(4,4'-bipyridinium) hexafluoridophosphate bis(4-aminobenzoic acid)
4,4'-bipyridine monohydrate
;
_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           SHELXL-97
_cell_angle_alpha                92.5570(10)
_cell_angle_beta                 98.0630(10)
_cell_angle_gamma                117.3460(10)
_cell_formula_units_Z            2
_cell_length_a                   10.1032(2)
_cell_length_b                   10.1142(2)
_cell_length_c                   16.8906(3)
_cell_measurement_reflns_used    2023
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      19.47
_cell_measurement_theta_min      2.36
_cell_volume                     1506.23(5)
_computing_cell_refinement       'APEX2 (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'APEX2 (Bruker, 2004)'
_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      296(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEXII area-detector'
_diffrn_measurement_method       '\f and \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  0.0568
_diffrn_reflns_av_sigmaI/netI    0.0678
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22618
_diffrn_reflns_theta_full        27.93
_diffrn_reflns_theta_max         27.93
_diffrn_reflns_theta_min         2.28
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.177
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             694
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.335
_refine_ls_extinction_coef       0.009(2)
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         7121
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1560
_refine_ls_R_factor_gt           0.0658
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0875P)^2^+0.1722P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1581
_refine_ls_wR_factor_ref         0.2053
_reflns_number_gt                3129
_reflns_number_total             7121
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wn2299.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C29 H29 F6 N5 O5 P1'
_cod_database_code               2220944
_cod_database_fobs_code          2220944