Bis(4,4'-bipyridinium) dodecatungstosilicate 4,4'-bipyridine hexahydrate
Ma, Feng-Xia; Zhao, Quan; Acta Crystallographica Section E 64 (2008) m1224–; doi:10.1107/S1600536808027566

data_2219686
_publ_section_title
;
 Bis(4,4'-bipyridinium) dodecatungstosilicate 4,4'-bipyridine
 hexahydrate
;
_journal_coeditor_code           RK2097
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1224
_journal_paper_doi               10.1107/S1600536808027566
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '(C10 H10 N2)2 [Si W12 O40], C10 H8 N2, 6H2 O'
_chemical_formula_moiety
'2(C10 H10 N2 +), O40 Si W12 2-, C10 H8 N2, 6(H2 O)'
_chemical_formula_sum            'C30 H40 N6 O46 Si W12'
_chemical_formula_weight         3454.85
_chemical_name_systematic
;
Bis(4,4'-bipyridinium) dodecatungstosilicate 4,4'-bipyridine hexahydrate
;
_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           SHELXL97
_cell_angle_alpha                90.000
_cell_angle_beta                 100.834(5)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   15.491(5)
_cell_length_b                   18.096(5)
_cell_length_c                   20.921(5)
_cell_measurement_reflns_used    5214
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      1.8
_cell_volume                     5760(3)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'PROCESS-AUTO (Rigaku, 1998)'
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotor target'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0480
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15853
_diffrn_reflns_theta_full        25.98
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    23.993
_exptl_absorpt_correction_T_max  0.095
_exptl_absorpt_correction_T_min  0.041
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    3.984
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             6128
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.600
_refine_diff_density_min         -3.496
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         5652
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.049P)^2^+129.9363P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1008
_reflns_number_gt                5214
_reflns_number_total             5652
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rk2097.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2219686
_cod_database_fobs_code          2219686