4,4'-Diazenediyldipyridinium 4-(4-pyridyldiazenyl)pyridinium octacyanidotungstate(V) dihydrate
Qian, Su-Yan; Liu, Wen-Yan; Yuan, Ai-Hua; Acta Crystallographica Section E 65 (2009) m1031–m1032; doi:10.1107/S1600536809030153

data_2223105
_publ_section_title
;
 4,4'-Diazenediyldipyridinium 4-(4-pyridyldiazenyl)pyridinium
 octacyanidotungstate(V) dihydrate
;
_journal_coeditor_code           HK2738
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1031
_journal_page_last               m1032
_journal_paper_doi               10.1107/S1600536809030153
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '(C10 H10 N4) (C10 H9 N4) [W (C N)8], 2H2 O'
_chemical_formula_moiety
'C10 H10 N4 2+, C10 H9 N4 +, C8 N8 W 3-, 2(H2 O)'
_chemical_formula_sum            'C28 H23 N16 O2 W'
_chemical_formula_weight         799.46
_chemical_name_systematic
;
4,4'-Diazenediyldipyridinium 4-(4-pyridyldiazenyl)pyridinium
octacyanidotungstate(V) dihydrate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.7310(16)
_cell_length_b                   16.499(2)
_cell_length_c                   30.704(4)
_cell_measurement_reflns_used    3042
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      23.31
_cell_measurement_theta_min      2.41
_cell_volume                     6449.3(14)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'SMART (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics
'SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART APEX'
_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  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0680
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            39717
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.33
_exptl_absorpt_coefficient_mu    3.636
_exptl_absorpt_correction_T_max  0.483
_exptl_absorpt_correction_T_min  0.391
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       pale
_exptl_crystal_F_000             3144
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.345
_refine_diff_density_min         -1.706
_refine_ls_abs_structure_details 'Flack (1983), 5514 Friedel pairs'
_refine_ls_abs_structure_Flack   0.045(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     847
_refine_ls_number_reflns         12501
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0468
_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^)+(0.05P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1021
_reflns_number_gt                8553
_reflns_number_total             12501
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hk2738.cif
_cod_data_source_block           I
_cod_database_code               2223105
_cod_database_fobs_code          2223105