##############################################################################
###                                                                        ###
###        Electronic paper (Acta Crystallographica Section E)             ###
###                                                                        ###
##############################################################################
#                                                                            #
# This CIF contains the data in a paper accepted for publication in Acta     #
# Crystallographica Section E. It conforms to the requirements of Notes      #
# for Authors for Section E, and has been peer reviewed under the auspices   #
# of the IUCr Commission on Journals.                                        #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
# ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.4.    #
#                                                                            #
# Software is freely available for graphical display of the structure(s) in  #
# this CIF.  For information consult the CIF home page http://www.iucr.org/  #
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data_global
_audit_creation_method     'SHELXL97'
_journal_date_recd_electronic     2008-06-13
_journal_date_accepted     2008-08-28
_journal_name_full     'Acta Crystallographica, Section E'
_journal_year     2008
_journal_volume     64
_journal_issue     10
_journal_page_first     m1224
_journal_page_last     m1224
_journal_paper_category     QM
_journal_coeditor_code     RK2097
_publ_contact_author_name     'Feng-Xia Ma'
_publ_contact_author_address
;
 Jilin Agricultural Science and Technology College Jilin 132101
 People's Republic of China
;
_publ_contact_author_email     'fengxia_ma@126.com'
_publ_contact_author_fax     ?
_publ_contact_author_phone     '86-432-3509527'
_publ_section_title
;
Bis(4,4'-bipyridinium) dodecatungstosilicate 4,4'-bipyridine hexahydrate
;
loop_
    _publ_author_name
    _publ_author_address
    'Feng-Xia Ma'
;
Jilin Agricultural Science and Technology College
Jilin 132101
People's Republic of China
;
    'Quan Zhao'
;
Jilin Agricultural Science and Technology College
Jilin 132101
People's Republic of China
and
Northeast Forestry University
People's Republic of China
;
data_I
_audit_creation_method     SHELXL97
_chemical_name_systematic
;
Bis(4,4'-bipyridinium) dodecatungstosilicate 4,4'-bipyridine hexahydrate
;
_chemical_name_common     ?
_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_iupac     '(C10 H10 N2)2 [Si W12 O40], C10 H8 N2, 6H2 O'
_chemical_formula_weight     3454.85
_chemical_melting_point     ?
_symmetry_cell_setting     'Monoclinic'
_symmetry_space_group_name_H-M     'C 2/c'
_symmetry_space_group_name_hall     '-C 2yc'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x, y, -z+1/2'
    'x+1/2, y+1/2, z'
    '-x+1/2, y+1/2, -z+1/2'
    '-x, -y, -z'
    'x, -y, z-1/2'
    '-x+1/2, -y+1/2, -z'
    'x+1/2, -y+1/2, z-1/2'
_cell_length_a     15.491(5)
_cell_length_b     18.096(5)
_cell_length_c     20.921(5)
_cell_angle_alpha     90.000
_cell_angle_beta     100.834(5)
_cell_angle_gamma     90.000
_cell_volume     5760(3)
_cell_formula_units_Z     4
_cell_measurement_reflns_used     5214
_cell_measurement_theta_min     1.8
_cell_measurement_theta_max     26.0
_cell_measurement_temperature     293(2)
_exptl_crystal_description     'Block'
_exptl_crystal_colour     'Black'
_exptl_crystal_size_max     0.15
_exptl_crystal_size_mid     0.12
_exptl_crystal_size_min     0.10
_exptl_crystal_density_diffrn     3.984
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'Not measured'
_exptl_crystal_F_000     6128
_exptl_absorpt_coefficient_mu     23.993
_exptl_absorpt_correction_type     'multi-scan'
_exptl_absorpt_process_details     '(ABSCOR; Higashi, 1995)'
_exptl_absorpt_correction_T_min     0.041
_exptl_absorpt_correction_T_max     0.095
_exptl_special_details
;
;
_diffrn_ambient_temperature     293(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_source     'Rotor target'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Rigaku R-AXIS RAPID'
_diffrn_measurement_method     ω
_diffrn_detector_area_resol_mean     10.0
_diffrn_reflns_number     15853
_diffrn_reflns_av_R_equivalents     0.0419
_diffrn_reflns_av_sigmaI/netI     0.0480
_diffrn_reflns_theta_min     1.75
_diffrn_reflns_theta_max     25.98
_diffrn_reflns_theta_full     25.98
_diffrn_measured_fraction_theta_max     0.999
_diffrn_measured_fraction_theta_full     0.999
_diffrn_reflns_limit_h_min     -19
_diffrn_reflns_limit_h_max     14
_diffrn_reflns_limit_k_min     -22
_diffrn_reflns_limit_k_max     22
_diffrn_reflns_limit_l_min     -23
_diffrn_reflns_limit_l_max     25
_diffrn_standards_number     ?
_diffrn_standards_interval_count     ?
_diffrn_standards_interval_time     ?
_diffrn_standards_decay_%     ?
_refine_special_details
;
 Refinement of F² against ALL reflections. The weighted
 R--factor wR and goodness of fit S are based on
 F², conventional R--factors R are based on F,
 with F set to zero for negative F². The threshold expression
 of F² > σ(F²) is used only for calculating
 R--factors(gt) etc. and is not relevant to the choice of
 reflections for refinement. R--factors based on F² are
 statistically about twice as largeas those based on F, and
 R--factors based on ALL data will be even larger.
;
_reflns_number_total     5652
_reflns_number_gt     5214
_reflns_threshold_expression     I>2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0421
_refine_ls_R_factor_gt     0.0388
_refine_ls_wR_factor_gt     0.0988
_refine_ls_wR_factor_ref     0.1008
_refine_ls_goodness_of_fit_ref     1.097
_refine_ls_restrained_S_all     0.947
_refine_ls_number_reflns     5652
_refine_ls_number_parameters     455
_refine_ls_number_restraints     8
_refine_ls_hydrogen_treatment     mixed
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
        'calc w=1/[σ²(Fo²)+(0.049P)²+129.9363P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     difmap
_refine_ls_shift/su_max     0.002
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     3.600
_refine_diff_density_min     -3.496
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     ?
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    'C' 'C' 0.0033 0.0016
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'H' 'H' 0.0000 0.0000
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'N' 'N' 0.0061 0.0033
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'O' 'O' 0.0106 0.0060
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'Si' 'Si' 0.0817 0.0704
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'W' 'W' -0.8490 6.8722
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection     'PROCESS-AUTO (Rigaku, 1998)'
_computing_cell_refinement     'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction     'PROCESS-AUTO (Rigaku, 1998)'
_computing_structure_solution     'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement     'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics     'SHELXTL-Plus (Sheldrick, 2008)'
_computing_publication_material     'SHELXL97 (Sheldrick, 2008)'
loop_
    _atom_site_type_symbol
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    Si Si1 1.0000 0.14417(15) 0.7500 0.0055(5) Uani d SU 1 . .
    W W1 0.98109(2) 0.004870(18) 0.865205(16) 0.01358(10) Uani d U 1 . .
    W W2 0.81326(2) 0.150489(19) 0.823667(17) 0.01562(10) Uani d U 1 . .
    W W3 0.83728(2) 0.008359(18) 0.701365(16) 0.01280(10) Uani d U 1 . .
    W W4 0.86857(2) 0.136541(19) 0.593364(17) 0.01711(10) Uani d U 1 . .
    W W5 0.83464(2) 0.280029(18) 0.712749(16) 0.01327(10) Uani d U 1 . .
    W W6 1.03445(2) 0.282564(18) 0.639007(16) 0.01417(10) Uani d U 1 . .
    C C1 0.7254(7) 0.6611(5) 0.4178(5) 0.0264(14) Uani d U 1 . .
    H H1 0.7714 0.6664 0.3953 0.032 Uiso calc R 1 . .
    C C2 0.6599(7) 0.7125(5) 0.4101(5) 0.0254(13) Uani d U 1 . .
    H H2 0.6598 0.7520 0.3816 0.031 Uiso calc R 1 . .
    C C3 0.5934(6) 0.7045(5) 0.4454(5) 0.0210(13) Uani d U 1 . .
    C C4 0.5952(7) 0.6445(5) 0.4877(5) 0.0223(13) Uani d U 1 . .
    H H4 0.5515 0.6386 0.5123 0.027 Uiso calc R 1 . .
    C C5 0.6624(7) 0.5948(5) 0.4922(5) 0.0266(13) Uani d U 1 . .
    H H5 0.6649 0.5544 0.5200 0.032 Uiso calc R 1 . .
    C C6 0.5183(6) 0.7587(5) 0.4376(5) 0.0210(13) Uani d U 1 . .
    C C7 0.4350(6) 0.7337(5) 0.4437(5) 0.0219(13) Uani d U 1 . .
    H H7 0.4262 0.6843 0.4530 0.026 Uiso calc R 1 . .
    C C8 0.3650(7) 0.7838(5) 0.4357(5) 0.0228(14) Uani d U 1 . .
    H H8 0.3090 0.7681 0.4396 0.027 Uiso calc R 1 . .
    C C9 0.4582(6) 0.8799(5) 0.4160(5) 0.0240(14) Uani d U 1 . .
    H H9 0.4648 0.9297 0.4069 0.029 Uiso calc R 1 . .
    C C10 0.5303(7) 0.8325(5) 0.4228(5) 0.0227(13) Uani d U 1 . .
    H H10 0.5850 0.8498 0.4175 0.027 Uiso calc R 1 . .
    C C11 0.5736(6) -0.0110(5) 0.7442(4) 0.0195(13) Uani d U 1 . .
    H H11 0.6235 -0.0379 0.7401 0.023 Uiso calc R 1 . .
    C C12 0.5755(6) 0.0660(5) 0.7443(4) 0.0174(12) Uani d U 1 . .
    H H12 0.6269 0.0908 0.7406 0.021 Uiso calc R 1 . .
    C C13 0.5000 0.1061(7) 0.7500 0.0159(14) Uani d SU 1 . .
    C C14 0.5000 0.1881(6) 0.7500 0.0146(14) Uani d SU 1 . .
    C C15 0.5682(6) 0.2278(5) 0.7320(4) 0.0174(12) Uani d U 1 . .
    H H15 0.6147 0.2029 0.7193 0.021 Uiso calc R 1 . .
    C C16 0.5676(6) 0.3045(5) 0.7328(4) 0.0206(13) Uani d U 1 . .
    H H16 0.6141 0.3307 0.7214 0.025 Uiso calc R 1 . .
    N N1 0.7246(6) 0.6045(5) 0.4565(4) 0.0265(13) Uani d DU 1 . .
    H H1N 0.770(5) 0.584(6) 0.461(6) 0.040 Uiso d D 1 . .
    N N2 0.3794(6) 0.8539(4) 0.4226(4) 0.0252(14) Uani d DU 1 . .
    H H2N 0.334(5) 0.875(6) 0.419(6) 0.038 Uiso d D 1 . .
    N N3 0.5000 -0.0457(6) 0.7500 0.0192(16) Uani d SU 1 . .
    N N4 0.5000 0.3407(6) 0.7500 0.0192(16) Uani d SU 1 . .
    O O1 0.9447(4) -0.0617(3) 0.9112(3) 0.0163(12) Uani d U 1 . .
    O O2 1.0599(4) 0.0597(3) 0.9308(3) 0.0120(10) Uani d U 1 . .
    O O3 1.0822(4) -0.0439(3) 0.8440(3) 0.0122(10) Uani d U 1 . .
    O O5 0.8959(4) 0.0815(3) 0.8665(3) 0.0116(9) Uani d U 1 . .
    O O6 0.8667(4) 0.2281(3) 0.8797(3) 0.0134(9) Uani d U 1 . .
    O O7 0.7236(4) 0.1323(3) 0.8568(3) 0.0165(11) Uani d U 1 . .
    O O8 0.7635(4) 0.2270(3) 0.7623(3) 0.0146(8) Uani d U 1 . .
    O O9 0.7957(4) 0.0824(3) 0.7520(3) 0.0141(8) Uani d U 1 . .
    O O10 0.9299(4) 0.1957(3) 0.7773(3) 0.0104(8) Uani d U 1 . .
    O O11 0.9167(4) -0.0197(3) 0.7808(3) 0.0135(9) Uani d U 1 . .
    O O12 0.7571(4) -0.0570(3) 0.6969(3) 0.0198(12) Uani d U 1 . .
    O O13 0.9484(4) 0.0926(3) 0.6913(3) 0.0096(8) Uani d U 1 . .
    O O14 0.7932(4) 0.0625(3) 0.6220(3) 0.0135(9) Uani d U 1 . .
    O O15 0.8026(4) 0.1562(3) 0.5197(3) 0.0184(12) Uani d U 1 . .
    O O16 0.9609(4) 0.2067(3) 0.5959(3) 0.0136(9) Uani d U 1 . .
    O O17 0.8220(4) 0.2048(3) 0.6488(3) 0.0146(9) Uani d U 1 . .
    O O18 0.7599(4) 0.3442(3) 0.6770(3) 0.0198(12) Uani d U 1 . .
    O O19 1.1124(4) 0.3313(3) 0.7084(3) 0.0136(10) Uani d U 1 . .
    O O20 1.0266(5) 0.3501(3) 0.5807(3) 0.0214(13) Uani d U 1 . .
    O O21 0.9400(4) 0.3087(3) 0.6807(3) 0.0159(9) Uani d U 1 . .
    O O1W 0.9247(5) 0.4797(4) 0.5870(4) 0.0332(12) Uani d DU 1 . .
    H H1A 0.890(7) 0.469(7) 0.615(4) 0.050 Uiso d D 1 . .
    H H1B 0.920(8) 0.457(6) 0.553(4) 0.050 Uiso d D 1 . .
    O O2W 0.8790(5) 0.5277(4) 0.4605(4) 0.0319(13) Uani d DU 1 . .
    H H2A 0.932(7) 0.547(6) 0.463(5) 0.048 Uiso d D 1 . .
    H H2B 0.859(7) 0.506(6) 0.427(4) 0.048 Uiso d D 1 . .
    O O3W 0.7508(5) 0.4587(4) 0.5805(4) 0.0380(13) Uani d DU 1 . .
    H H3A 0.780(8) 0.416(4) 0.594(5) 0.057 Uiso d D 1 . .
    H H3B 0.763(9) 0.487(5) 0.618(4) 0.057 Uiso d D 1 . .
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix. The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry. An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    Si1 O10 . 1.614(6) ?
    Si1 O10 2_756 1.614(6) ?
    Si1 O13 . 1.627(5) ?
    Si1 O13 2_756 1.627(5) ?
    W1 O1 . 1.703(6) ?
    W1 O11 . 1.911(5) ?
    W1 O5 . 1.918(6) ?
    W1 O3 . 1.921(6) ?
    W1 O2 . 1.931(6) ?
    W1 O13 2_756 2.366(5) ?
    W2 O7 . 1.697(6) ?
    W2 O5 . 1.889(5) ?
    W2 O6 . 1.915(6) ?
    W2 O9 . 1.921(6) ?
    W2 O8 . 1.945(6) ?
    W2 O10 . 2.353(6) ?
    W3 O12 . 1.706(6) ?
    W3 O9 . 1.894(6) ?
    W3 O14 . 1.939(6) ?
    W3 O11 . 1.940(5) ?
    W3 O3 2_756 1.948(6) ?
    W3 O13 . 2.338(5) ?
    W4 O15 . 1.719(6) ?
    W4 O2 2_756 1.904(6) ?
    W4 O16 . 1.907(6) ?
    W4 O17 . 1.924(6) ?
    W4 O14 . 1.943(6) ?
    W4 O13 . 2.325(5) ?
    W5 O18 . 1.709(6) ?
    W5 O17 . 1.894(6) ?
    W5 O8 . 1.909(6) ?
    W5 O19 2_756 1.935(6) ?
    W5 O21 . 1.948(6) ?
    W5 O10 . 2.363(5) ?
    W6 O20 . 1.715(6) ?
    W6 O21 . 1.898(6) ?
    W6 O16 . 1.900(6) ?
    W6 O19 . 1.919(6) ?
    W6 O6 2_756 1.923(6) ?
    W6 O10 2_756 2.341(5) ?
    C1 N1 . 1.306(13) ?
    C1 C2 . 1.364(14) ?
    C1 H1 . 0.9300 ?
    C2 C3 . 1.383(14) ?
    C2 H2 . 0.9300 ?
    C3 C4 . 1.397(13) ?
    C3 C6 . 1.507(13) ?
    C4 C5 . 1.366(13) ?
    C4 H4 . 0.9300 ?
    C5 N1 . 1.337(14) ?
    C5 H5 . 0.9300 ?
    C6 C10 . 1.391(13) ?
    C6 C7 . 1.395(14) ?
    C7 C8 . 1.400(13) ?
    C7 H7 . 0.9300 ?
    C8 N2 . 1.325(12) ?
    C8 H8 . 0.9300 ?
    C9 N2 . 1.340(13) ?
    C9 C10 . 1.394(14) ?
    C9 H9 . 0.9300 ?
    C10 H10 . 0.9300 ?
    C11 N3 . 1.327(11) ?
    C11 C12 . 1.395(12) ?
    C11 H11 . 0.9300 ?
    C12 C13 . 1.400(11) ?
    C12 H12 . 0.9300 ?
    C13 C12 2_656 1.400(11) ?
    C13 C14 . 1.483(17) ?
    C14 C15 2_656 1.388(11) ?
    C14 C15 . 1.388(11) ?
    C15 C16 . 1.387(12) ?
    C15 H15 . 0.9300 ?
    C16 N4 . 1.341(11) ?
    C16 H16 . 0.9300 ?
    N1 H1N . 0.79(6) ?
    N2 H2N . 0.79(6) ?
    N3 C11 2_656 1.327(11) ?
    N4 C16 2_656 1.341(11) ?
    O2 W4 2_756 1.904(6) ?
    O3 W3 2_756 1.948(6) ?
    O6 W6 2_756 1.923(6) ?
    O10 W6 2_756 2.341(5) ?
    O13 W1 2_756 2.366(5) ?
    O19 W5 2_756 1.935(6) ?
    O1W H1A . 0.89(6) ?
    O1W H1B . 0.81(6) ?
    O2W H2A . 0.88(9) ?
    O2W H2B . 0.80(6) ?
    O3W H3A . 0.92(6) ?
    O3W H3B . 0.93(6) ?
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    O10 Si1 O10 . 2_756 109.4(4) ?
    O10 Si1 O13 . . 109.3(3) ?
    O10 Si1 O13 2_756 . 109.4(3) ?
    O10 Si1 O13 . 2_756 109.4(3) ?
    O10 Si1 O13 2_756 2_756 109.3(3) ?
    O13 Si1 O13 . 2_756 110.0(4) ?
    O1 W1 O11 . . 100.7(3) ?
    O1 W1 O5 . . 101.7(3) ?
    O11 W1 O5 . . 86.6(2) ?
    O1 W1 O3 . . 100.2(3) ?
    O11 W1 O3 . . 89.2(2) ?
    O5 W1 O3 . . 158.2(2) ?
    O1 W1 O2 . . 101.2(3) ?
    O11 W1 O2 . . 158.0(2) ?
    O5 W1 O2 . . 87.9(2) ?
    O3 W1 O2 . . 88.0(2) ?
    O1 W1 O13 . 2_756 172.0(2) ?
    O11 W1 O13 . 2_756 84.5(2) ?
    O5 W1 O13 . 2_756 84.6(2) ?
    O3 W1 O13 . 2_756 73.7(2) ?
    O2 W1 O13 . 2_756 73.8(2) ?
    O7 W2 O5 . . 102.2(3) ?
    O7 W2 O6 . . 100.6(3) ?
    O5 W2 O6 . . 91.0(2) ?
    O7 W2 O9 . . 100.8(3) ?
    O5 W2 O9 . . 86.0(2) ?
    O6 W2 O9 . . 158.5(3) ?
    O7 W2 O8 . . 98.9(3) ?
    O5 W2 O8 . . 158.8(3) ?
    O6 W2 O8 . . 87.4(2) ?
    O9 W2 O8 . . 87.8(2) ?
    O7 W2 O10 . . 170.8(2) ?
    O5 W2 O10 . . 85.5(2) ?
    O6 W2 O10 . . 73.8(2) ?
    O9 W2 O10 . . 84.7(2) ?
    O8 W2 O10 . . 73.8(2) ?
    O12 W3 O9 . . 101.6(3) ?
    O12 W3 O14 . . 99.7(3) ?
    O9 W3 O14 . . 91.1(2) ?
    O12 W3 O11 . . 101.7(3) ?
    O9 W3 O11 . . 86.2(2) ?
    O14 W3 O11 . . 158.5(2) ?
    O12 W3 O3 . 2_756 99.4(3) ?
    O9 W3 O3 . 2_756 158.7(2) ?
    O14 W3 O3 . 2_756 89.0(2) ?
    O11 W3 O3 . 2_756 85.9(2) ?
    O12 W3 O13 . . 171.3(2) ?
    O9 W3 O13 . . 85.6(2) ?
    O14 W3 O13 . . 74.9(2) ?
    O11 W3 O13 . . 83.6(2) ?
    O3 W3 O13 2_756 . 73.9(2) ?
    O15 W4 O2 . 2_756 101.0(3) ?
    O15 W4 O16 . . 101.7(3) ?
    O2 W4 O16 2_756 . 91.3(2) ?
    O15 W4 O17 . . 100.4(3) ?
    O2 W4 O17 2_756 . 158.6(2) ?
    O16 W4 O17 . . 85.4(3) ?
    O15 W4 O14 . . 97.4(3) ?
    O2 W4 O14 2_756 . 89.5(2) ?
    O16 W4 O14 . . 160.3(2) ?
    O17 W4 O14 . . 86.7(2) ?
    O15 W4 O13 . . 171.5(2) ?
    O2 W4 O13 2_756 . 75.2(2) ?
    O16 W4 O13 . . 86.1(2) ?
    O17 W4 O13 . . 83.5(2) ?
    O14 W4 O13 . . 75.1(2) ?
    O18 W5 O17 . . 102.0(3) ?
    O18 W5 O8 . . 99.6(3) ?
    O17 W5 O8 . . 91.6(3) ?
    O18 W5 O19 . 2_756 101.0(3) ?
    O17 W5 O19 . 2_756 156.7(2) ?
    O8 W5 O19 . 2_756 88.5(3) ?
    O18 W5 O21 . . 102.2(3) ?
    O17 W5 O21 . . 86.0(3) ?
    O8 W5 O21 . . 158.1(2) ?
    O19 W5 O21 2_756 . 85.3(2) ?
    O18 W5 O10 . . 171.0(3) ?
    O17 W5 O10 . . 84.8(2) ?
    O8 W5 O10 . . 74.2(2) ?
    O19 W5 O10 2_756 . 72.7(2) ?
    O21 W5 O10 . . 84.0(2) ?
    O20 W6 O21 . . 101.0(3) ?
    O20 W6 O16 . . 102.7(3) ?
    O21 W6 O16 . . 87.3(3) ?
    O20 W6 O19 . . 99.3(3) ?
    O21 W6 O19 . . 88.2(3) ?
    O16 W6 O19 . . 158.0(2) ?
    O20 W6 O6 . 2_756 99.9(3) ?
    O21 W6 O6 . 2_756 159.0(2) ?
    O16 W6 O6 . 2_756 87.8(2) ?
    O19 W6 O6 . 2_756 88.7(2) ?
    O20 W6 O10 . 2_756 170.4(3) ?
    O21 W6 O10 . 2_756 85.3(2) ?
    O16 W6 O10 . 2_756 84.6(2) ?
    O19 W6 O10 . 2_756 73.5(2) ?
    O6 W6 O10 2_756 2_756 74.0(2) ?
    N1 C1 C2 . . 120.9(10) ?
    N1 C1 H1 . . 119.5 ?
    C2 C1 H1 . . 119.5 ?
    C1 C2 C3 . . 118.5(10) ?
    C1 C2 H2 . . 120.8 ?
    C3 C2 H2 . . 120.8 ?
    C2 C3 C4 . . 119.5(9) ?
    C2 C3 C6 . . 120.7(9) ?
    C4 C3 C6 . . 119.8(9) ?
    C5 C4 C3 . . 118.6(10) ?
    C5 C4 H4 . . 120.7 ?
    C3 C4 H4 . . 120.7 ?
    N1 C5 C4 . . 119.7(9) ?
    N1 C5 H5 . . 120.2 ?
    C4 C5 H5 . . 120.2 ?
    C10 C6 C7 . . 119.7(9) ?
    C10 C6 C3 . . 121.1(9) ?
    C7 C6 C3 . . 119.2(8) ?
    C6 C7 C8 . . 119.3(9) ?
    C6 C7 H7 . . 120.4 ?
    C8 C7 H7 . . 120.4 ?
    N2 C8 C7 . . 119.2(9) ?
    N2 C8 H8 . . 120.4 ?
    C7 C8 H8 . . 120.4 ?
    N2 C9 C10 . . 120.0(9) ?
    N2 C9 H9 . . 120.0 ?
    C10 C9 H9 . . 120.0 ?
    C6 C10 C9 . . 118.4(9) ?
    C6 C10 H10 . . 120.8 ?
    C9 C10 H10 . . 120.8 ?
    N3 C11 C12 . . 119.3(9) ?
    N3 C11 H11 . . 120.3 ?
    C12 C11 H11 . . 120.3 ?
    C11 C12 C13 . . 120.1(9) ?
    C11 C12 H12 . . 119.9 ?
    C13 C12 H12 . . 119.9 ?
    C12 C13 C12 2_656 . 117.5(11) ?
    C12 C13 C14 2_656 . 121.2(6) ?
    C12 C13 C14 . . 121.2(6) ?
    C15 C14 C15 2_656 . 117.5(11) ?
    C15 C14 C13 2_656 . 121.2(6) ?
    C15 C14 C13 . . 121.2(5) ?
    C16 C15 C14 . . 120.5(9) ?
    C16 C15 H15 . . 119.7 ?
    C14 C15 H15 . . 119.7 ?
    N4 C16 C15 . . 120.0(9) ?
    N4 C16 H16 . . 120.0 ?
    C15 C16 H16 . . 120.0 ?
    C1 N1 C5 . . 122.8(9) ?
    C1 N1 H1N . . 109(9) ?
    C5 N1 H1N . . 127(9) ?
    C8 N2 C9 . . 123.4(9) ?
    C8 N2 H2N . . 108(9) ?
    C9 N2 H2N . . 129(9) ?
    C11 N3 C11 2_656 . 123.6(11) ?
    C16 N4 C16 2_656 . 121.4(11) ?
    W4 O2 W1 2_756 . 120.5(3) ?
    W1 O3 W3 . 2_756 121.0(3) ?
    W2 O5 W1 . . 151.4(3) ?
    W2 O6 W6 . 2_756 121.3(3) ?
    W5 O8 W2 . . 121.2(3) ?
    W3 O9 W2 . . 151.4(3) ?
    Si1 O10 W6 . 2_756 125.0(3) ?
    Si1 O10 W2 . . 124.4(3) ?
    W6 O10 W2 2_756 . 90.93(19) ?
    Si1 O10 W5 . . 124.1(3) ?
    W6 O10 W5 2_756 . 91.59(19) ?
    W2 O10 W5 . . 90.8(2) ?
    W1 O11 W3 . . 150.2(3) ?
    Si1 O13 W4 . . 125.0(3) ?
    Si1 O13 W3 . . 124.9(3) ?
    W4 O13 W3 . . 91.37(19) ?
    Si1 O13 W1 . 2_756 123.6(3) ?
    W4 O13 W1 . 2_756 90.46(18) ?
    W3 O13 W1 . 2_756 91.39(18) ?
    W3 O14 W4 . . 118.5(3) ?
    W6 O16 W4 . . 150.9(3) ?
    W5 O17 W4 . . 152.4(3) ?
    W6 O19 W5 . 2_756 122.0(3) ?
    W6 O21 W5 . . 149.3(3) ?
    H1A O1W H1B . . 119(9) ?
    H2A O2W H2B . . 117(10) ?
    H3A O3W H3B . . 102(6) ?
loop_
    _geom_hbond_atom_site_label_D
    _geom_hbond_atom_site_label_H
    _geom_hbond_atom_site_label_A
    _geom_hbond_site_symmetry_A
    _geom_hbond_distance_DH
    _geom_hbond_distance_HA
    _geom_hbond_distance_DA
    _geom_hbond_angle_DHA
    O1W H1A O3W . 0.89(10) 2.15(11) 2.699(11) 119(7)
    O1W H1B O2W . 0.81(9) 2.31(9) 2.749(12) 115(10)
    O1W H1B O20 . 0.81(9) 2.54(11) 2.844(10) 104(8)
    N1 H1N O2W . 0.78(9) 1.97(9) 2.754(12) 172(14)
    O3W H3A O18 . 0.91(9) 2.24(10) 2.878(10) 127(9)
