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Anion...π inter­actions are newly recognized weak supra­molecular forces which are relevant to many types of electron-deficient aromatic substrates. Being less competitive with respect to conventional hydrogen bonding, anion...π inter­actions are only rarely considered as a crystal-structure-defining factor. Their significance dramatically increases for polyoxometalate (POM) species, which offer extended oxide surfaces for maintaining dense aromatic/inorganic stacks. The structures of tetra­kis­(caffeinium) μ12-silicato-tetra­cosa-μ2-oxido-dodeca­oxidododeca­tungsten trihydrate, (C8H11N4O2)4[SiW12O40]·3H2O, (1), and tris­(theobrominium) μ12-phosphato-tetra­cosa-μ2-oxido-dodeca­oxidododeca­tung­sten ethanol sesquisolvate, (C7H9N4O2)3[PW12O40]·1.5C2H5OH, (2), support the utility of anion...π inter­actions as a special kind of supra­molecular synthon con­trolling the structures of ionic lattices. Both caffeinium [(HCaf)+ in (1)] and theobrominium cations [(HTbr)+ in (2)] reveal double stacking patterns at both axial sides of the aromatic frameworks, leading to the generation of anion...π...anion bridges. The latter provide the rare face-to-face linkage of the anions. In (1), every square face of the metal–oxide cubocta­hedra accepts the inter­action and the above bridges yield flat square nets, i.e. {(HCaf+)2[SiW12O40]4−}n. Two additional cations afford single stacks only and they terminate the connectivity. Salt (2) retains a two-dimensional (2D) motif of square nets, with anion...π...anion bridges involving two of the three (HTbr)+ cations. The remaining cations complete a fivefold anion...π environment of [PW12O40]3−, acting as terminal groups. This single anion...π inter­action is influenced by the specific pairing of (HTbr)+ cations by double amide-to-amide hydrogen bonding. Nevertheless, invariable 2D patterns in (1) and (2) suggest the dominant role of anion...π inter­actions as the structure-governing factor, which is applicable to the construction of noncovalent linkages involving Keggin-type oxometalates.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S205322962000950X/jx3058sup1.cif
Contains datablocks global, 1, 2

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S205322962000950X/jx30581sup2.hkl
Contains datablock 1

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S205322962000950X/jx30582sup3.hkl
Contains datablock 2

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S205322962000950X/jx3058sup4.pdf
Additional figures and characterization data

CCDC references: 2015793; 2015792

Computing details top

For both structures, data collection: IPDS Software (Stoe & Cie, 2000); cell refinement: IPDS Software (Stoe & Cie, 2000); data reduction: IPDS Software (Stoe & Cie, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2018 (Sheldrick, 2015); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: WinGX (Farrugia, 2012).

Tetrakis(1,3,7-trimethylxanthinium) µ12-silicato-tetracosa-µ2-oxido-dodecaoxidododecatungsten trihydrate (1) top
Crystal data top
(C8H11N4O2)4[SiW12O40]·3H2OF(000) = 6656
Mr = 3709.17Dx = 3.599 Mg m3
Monoclinic, CcMo Kα radiation, λ = 0.71073 Å
a = 15.8623 (4) ÅCell parameters from 34632 reflections
b = 20.7547 (6) Åθ = 1.7–26.7°
c = 21.8096 (6) ŵ = 20.21 mm1
β = 107.576 (2)°T = 173 K
V = 6844.9 (3) Å3Prism, yellow
Z = 40.22 × 0.18 × 0.16 mm
Data collection top
Stoe Image plate diffraction system
diffractometer
8741 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.026
φ oscillation scansθmax = 26.7°, θmin = 1.7°
Absorption correction: numerical
[X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)]
h = 2013
Tmin = 0.093, Tmax = 0.229k = 2620
34632 measured reflectionsl = 1827
9899 independent reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: mixed
R[F2 > 2σ(F2)] = 0.048H-atom parameters constrained
wR(F2) = 0.134 w = 1/[σ2(Fo2) + (0.082P)2 + 63.609P]
where P = (Fo2 + 2Fc2)/3
S = 1.08(Δ/σ)max = 0.002
9899 reflectionsΔρmax = 1.35 e Å3
1005 parametersΔρmin = 1.78 e Å3
58 restraintsAbsolute structure: Refined as an inversion twin.
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.40 (3)
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. Refined as a 2-component inversion twin.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Si10.7944 (5)0.3311 (2)0.3131 (4)0.0293 (8)
W10.71419 (7)0.24737 (6)0.42543 (5)0.0480 (3)
W20.71032 (8)0.41281 (6)0.42495 (6)0.0517 (3)
W30.79091 (11)0.50068 (4)0.31011 (8)0.0474 (2)
W40.86828 (9)0.42007 (6)0.20156 (6)0.0538 (3)
W50.87172 (8)0.24501 (6)0.20199 (6)0.0476 (3)
W60.79614 (10)0.16069 (4)0.31078 (8)0.0450 (2)
W70.94789 (8)0.24935 (6)0.44035 (6)0.0482 (3)
W80.94526 (7)0.41510 (6)0.44146 (6)0.0463 (3)
W91.02266 (9)0.33469 (6)0.33240 (7)0.0512 (3)
W100.56781 (9)0.32931 (6)0.30257 (7)0.0509 (3)
W110.64701 (8)0.41751 (6)0.18641 (6)0.0486 (3)
W120.64993 (7)0.24268 (6)0.18755 (5)0.0466 (3)
O90.7235 (11)0.3299 (8)0.3547 (7)0.040 (3)
O100.7786 (10)0.3938 (8)0.2713 (7)0.040 (3)
O110.7822 (11)0.2686 (7)0.2703 (8)0.039 (3)
O120.8910 (11)0.3321 (7)0.3645 (7)0.039 (3)
O130.6854 (14)0.2013 (12)0.4811 (10)0.058 (6)
O140.7031 (12)0.3294 (8)0.4673 (10)0.049 (4)
O150.8372 (13)0.2541 (10)0.4552 (9)0.050 (4)
O160.7287 (15)0.1898 (13)0.3643 (13)0.072 (7)
O170.5949 (13)0.2641 (8)0.3721 (9)0.049 (4)
O180.6842 (13)0.4609 (12)0.4800 (9)0.052 (5)
O190.7239 (11)0.4676 (8)0.3607 (8)0.044 (4)
O200.8356 (15)0.4148 (16)0.4585 (13)0.080 (9)
O210.5883 (13)0.3918 (9)0.3710 (10)0.052 (4)
O220.7942 (17)0.5818 (7)0.3209 (16)0.064 (6)
O230.8550 (13)0.4984 (9)0.2467 (9)0.051 (4)
O240.8920 (13)0.4712 (12)0.3764 (13)0.065 (6)
O250.6841 (16)0.4940 (12)0.2396 (12)0.068 (7)
O260.9131 (15)0.4560 (10)0.1503 (11)0.053 (5)
O270.8547 (13)0.3334 (8)0.1789 (10)0.054 (5)
O280.9660 (14)0.3971 (8)0.2713 (9)0.056 (5)
O290.747 (2)0.4258 (16)0.1558 (13)0.091 (11)
O300.9140 (18)0.2109 (13)0.1494 (10)0.067 (7)
O310.8621 (14)0.1696 (11)0.2513 (12)0.061 (6)
O320.9634 (12)0.2723 (9)0.2724 (9)0.046 (4)
O330.7467 (12)0.2318 (9)0.1529 (9)0.046 (4)
O340.8007 (17)0.0795 (6)0.3205 (14)0.055 (5)
O350.8980 (12)0.1931 (10)0.3742 (9)0.049 (4)
O360.6910 (14)0.1656 (10)0.2382 (10)0.056 (5)
O371.0155 (13)0.2056 (10)0.5031 (10)0.051 (5)
O380.9761 (16)0.3351 (9)0.4857 (10)0.056 (5)
O391.0362 (13)0.2720 (8)0.4019 (8)0.048 (4)
O400.9999 (13)0.4627 (12)0.5009 (11)0.061 (6)
O411.0334 (12)0.3972 (8)0.3996 (10)0.046 (4)
O421.1299 (14)0.3354 (9)0.3310 (12)0.052 (5)
O430.4572 (12)0.3260 (8)0.2842 (10)0.043 (4)
O440.5934 (12)0.3920 (10)0.2485 (12)0.056 (5)
O450.5950 (12)0.2670 (8)0.2507 (8)0.046 (4)
O460.5643 (14)0.4503 (10)0.1237 (10)0.056 (5)
O470.6498 (14)0.3308 (7)0.1666 (9)0.046 (4)
O480.5707 (15)0.2115 (10)0.1252 (9)0.051 (5)
O10.6181 (19)0.3029 (14)0.6376 (16)0.084 (9)
O20.7493 (17)0.1109 (9)0.6190 (11)0.060 (5)
N10.8868 (17)0.3083 (13)0.5979 (10)0.049 (5)
H1N0.9362810.2975020.5901090.074*
N20.773 (2)0.3639 (14)0.6095 (12)0.067 (8)
N30.6867 (18)0.2067 (12)0.6277 (12)0.049 (5)
N40.8279 (18)0.2040 (14)0.6116 (11)0.053 (6)
C10.855 (2)0.3680 (17)0.6013 (14)0.055 (6)
H10.8850730.4069210.5984260.066*
C20.755 (2)0.3033 (15)0.6174 (14)0.052 (6)
C30.680 (2)0.2716 (16)0.6302 (14)0.068 (10)
C40.748 (2)0.1702 (10)0.6220 (15)0.057 (8)
C50.8217 (19)0.2662 (13)0.6100 (13)0.048 (6)
C60.719 (3)0.4212 (12)0.6176 (17)0.080 (13)
H6A0.7476920.4606530.6086920.121*
H6B0.6595370.4180310.5875740.121*
H6C0.7164100.4225240.6617980.121*
C70.607 (2)0.1687 (15)0.639 (2)0.070 (10)
H7A0.5621550.1993150.6435260.105*
H7B0.5815830.1397580.6031770.105*
H7C0.6285300.1434810.6791540.105*
C80.898 (2)0.1647 (14)0.6010 (19)0.064 (9)
H8A0.8855120.1190470.6052630.095*
H8B0.9024570.1727830.5576890.095*
H8C0.9547610.1758750.6328970.095*
O30.5026 (19)0.1005 (13)0.1850 (11)0.071 (7)
O40.6960 (17)0.0595 (10)0.2636 (11)0.059 (6)
N50.595 (2)0.0678 (14)0.4063 (12)0.065 (8)
H5N0.6254700.0560130.4455830.097*
N60.5006 (17)0.1215 (12)0.3255 (14)0.060 (6)
N70.6024 (16)0.0216 (10)0.2275 (11)0.044 (5)
N80.6580 (16)0.0047 (11)0.3375 (12)0.045 (5)
C90.531 (2)0.1139 (17)0.387 (2)0.069 (10)
H90.5101630.1381280.4168480.083*
C100.544 (2)0.0803 (13)0.3005 (14)0.051 (6)
C110.545 (2)0.0678 (14)0.2312 (12)0.057 (7)
C120.6536 (17)0.0161 (12)0.2795 (17)0.062 (9)
C130.601 (2)0.0442 (15)0.3479 (12)0.050 (6)
C140.432 (2)0.1668 (11)0.2856 (16)0.061 (8)
H14A0.4250660.1597470.2399250.092*
H14B0.3753920.1588910.2938020.092*
H14C0.4505460.2113700.2970840.092*
C150.613 (3)0.016 (2)0.1640 (19)0.096 (16)
H15A0.6553160.0181390.1639790.144*
H15B0.5557130.0059680.1326850.144*
H15C0.6348230.0571320.1523000.144*
C160.715 (3)0.039 (2)0.3962 (14)0.080 (12)
H16A0.7051620.0201070.4347170.120*
H16B0.6996180.0846760.3935760.120*
H16C0.7773390.0339130.3985380.120*
O50.9720 (16)0.3069 (12)0.0124 (15)0.072 (7)
O60.8457 (15)0.1135 (9)0.0047 (10)0.053 (5)
N90.7074 (17)0.3086 (14)0.0243 (13)0.055 (6)
H9N0.6551630.2976730.0272510.082*
N100.8081 (17)0.3693 (10)0.0127 (12)0.048 (5)
N110.9076 (17)0.2099 (13)0.0079 (13)0.051 (6)
N120.7687 (15)0.2010 (11)0.0142 (11)0.042 (5)
C170.739 (3)0.3699 (18)0.0279 (18)0.073 (11)
H170.7118390.4068480.0399360.088*
C180.827 (2)0.3024 (13)0.0077 (14)0.055 (8)
C190.9071 (17)0.2795 (14)0.0044 (17)0.055 (7)
C200.835 (2)0.1721 (9)0.0070 (13)0.052 (7)
C210.763 (2)0.2704 (14)0.0161 (11)0.046 (6)
C220.857 (2)0.4285 (15)0.0039 (18)0.068 (9)
H22A0.9099460.4159280.0079780.102*
H22B0.8190370.4553320.0302070.102*
H22C0.8755260.4530060.0442100.102*
C230.978 (3)0.1817 (17)0.021 (2)0.068 (9)
H23A0.9703730.1347420.0224530.102*
H23B0.9803400.1966550.0634520.102*
H23C1.0325790.1932680.0117550.102*
C240.696 (3)0.165 (2)0.0255 (16)0.081 (13)
H24A0.6506370.1950410.0298260.121*
H24B0.6707180.1360120.0108750.121*
H24C0.7182700.1397230.0650270.121*
O70.5900 (16)0.6051 (11)0.4333 (12)0.067 (7)
O80.3918 (15)0.4368 (10)0.3577 (12)0.060 (5)
N130.495 (2)0.5640 (15)0.2178 (17)0.067 (8)
H13N0.4682860.5482860.1793470.100*
N140.5782 (16)0.6269 (13)0.2931 (17)0.065 (6)
N150.4899 (17)0.5258 (16)0.3919 (15)0.064 (7)
N160.4416 (19)0.4989 (12)0.2836 (12)0.051 (6)
C250.554 (3)0.615 (2)0.232 (2)0.078 (13)
H250.5733270.6383390.2011160.093*
C260.541 (2)0.5802 (17)0.325 (2)0.065 (6)
C270.5489 (17)0.5746 (12)0.3849 (12)0.048 (6)
C280.439 (2)0.4811 (13)0.3504 (15)0.055 (7)
C290.4868 (19)0.5426 (15)0.2741 (19)0.060 (8)
C300.6431 (16)0.6790 (12)0.3229 (19)0.067 (8)
H30A0.6526050.6800060.3694130.100*
H30B0.6994130.6704670.3145130.100*
H30C0.6198200.7207240.3041950.100*
C310.482 (2)0.5150 (17)0.4614 (16)0.071 (10)
H31A0.5185250.5470110.4907630.106*
H31B0.4204790.5194940.4604440.106*
H31C0.5033570.4716100.4762550.106*
C320.3735 (17)0.4645 (13)0.2345 (14)0.046 (6)
H32A0.3469770.4314770.2549740.070*
H32B0.3277200.4949940.2113440.070*
H32C0.3999690.4440850.2042400.070*
O1W0.667 (3)0.0244 (14)0.5248 (13)0.109 (13)
H1W0.6246600.0088960.5367620.163*
H2W0.6912790.0542670.5507200.163*
O2W0.416 (2)0.5248 (15)0.1006 (13)0.079 (8)
H3W0.4520670.5021830.0876240.118*
H4W0.3985460.5559750.0746450.118*
O3W0.287 (2)0.2932 (14)0.2937 (14)0.098 (9)*
H5W0.3334950.3148480.2955680.148*
H6W0.2526550.3168280.3069880.148*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Si10.031 (2)0.0279 (19)0.0261 (19)0.001 (3)0.0038 (16)0.009 (3)
W10.0532 (6)0.0481 (6)0.0402 (5)0.0043 (5)0.0106 (5)0.0062 (5)
W20.0589 (6)0.0515 (6)0.0416 (6)0.0097 (5)0.0104 (5)0.0054 (5)
W30.0580 (5)0.0361 (4)0.0476 (5)0.0029 (5)0.0152 (4)0.0005 (5)
W40.0655 (7)0.0516 (6)0.0406 (6)0.0151 (6)0.0104 (5)0.0044 (5)
W50.0553 (6)0.0452 (5)0.0400 (5)0.0015 (5)0.0109 (5)0.0066 (5)
W60.0501 (4)0.0350 (4)0.0471 (4)0.0015 (5)0.0103 (3)0.0007 (5)
W70.0528 (6)0.0497 (6)0.0398 (5)0.0079 (5)0.0107 (5)0.0037 (5)
W80.0486 (6)0.0445 (5)0.0431 (6)0.0042 (5)0.0098 (5)0.0095 (5)
W90.0447 (6)0.0434 (6)0.0625 (7)0.0027 (5)0.0116 (5)0.0028 (5)
W100.0431 (6)0.0438 (6)0.0629 (7)0.0012 (5)0.0116 (5)0.0020 (5)
W110.0522 (6)0.0469 (6)0.0434 (6)0.0026 (5)0.0096 (5)0.0077 (5)
W120.0524 (6)0.0466 (5)0.0375 (5)0.0081 (5)0.0086 (4)0.0041 (4)
O90.053 (9)0.049 (9)0.018 (6)0.007 (7)0.010 (6)0.006 (6)
O100.041 (8)0.041 (8)0.037 (7)0.014 (6)0.012 (6)0.003 (6)
O110.044 (8)0.035 (7)0.039 (7)0.008 (6)0.015 (7)0.003 (6)
O120.044 (8)0.035 (7)0.033 (7)0.003 (6)0.004 (6)0.006 (6)
O130.059 (12)0.076 (14)0.046 (11)0.038 (11)0.026 (9)0.011 (10)
O140.045 (9)0.039 (9)0.061 (11)0.003 (7)0.012 (8)0.011 (8)
O150.048 (9)0.066 (12)0.036 (9)0.019 (9)0.014 (7)0.001 (8)
O160.041 (10)0.086 (16)0.073 (15)0.021 (11)0.006 (10)0.033 (13)
O170.053 (10)0.038 (8)0.050 (10)0.001 (7)0.005 (8)0.003 (7)
O180.048 (10)0.077 (13)0.031 (8)0.009 (9)0.014 (8)0.016 (9)
O190.040 (8)0.051 (9)0.038 (8)0.018 (7)0.009 (7)0.008 (7)
O200.046 (11)0.13 (2)0.067 (14)0.040 (13)0.022 (11)0.054 (15)
O210.058 (11)0.039 (9)0.065 (12)0.002 (8)0.026 (9)0.003 (8)
O220.050 (9)0.031 (7)0.105 (18)0.002 (9)0.013 (10)0.012 (11)
O230.062 (11)0.050 (10)0.045 (9)0.012 (8)0.023 (8)0.001 (8)
O240.040 (10)0.074 (14)0.087 (16)0.015 (9)0.030 (10)0.033 (12)
O250.068 (13)0.079 (15)0.060 (12)0.025 (12)0.025 (10)0.041 (12)
O260.064 (12)0.040 (9)0.063 (13)0.010 (9)0.032 (10)0.013 (9)
O270.056 (11)0.035 (8)0.056 (11)0.004 (7)0.005 (9)0.005 (7)
O280.069 (12)0.025 (7)0.051 (10)0.009 (7)0.017 (9)0.004 (7)
O290.099 (19)0.12 (2)0.065 (15)0.064 (18)0.047 (14)0.072 (16)
O300.092 (17)0.075 (15)0.034 (10)0.027 (13)0.018 (10)0.009 (9)
O310.041 (10)0.079 (15)0.061 (12)0.002 (9)0.011 (9)0.034 (11)
O320.046 (9)0.043 (9)0.047 (9)0.005 (7)0.011 (7)0.006 (7)
O330.042 (9)0.052 (10)0.045 (10)0.004 (7)0.017 (8)0.007 (8)
O340.060 (10)0.022 (6)0.084 (14)0.003 (8)0.021 (10)0.005 (9)
O350.036 (8)0.058 (11)0.050 (10)0.006 (8)0.007 (7)0.012 (8)
O360.057 (11)0.061 (12)0.053 (11)0.011 (9)0.021 (9)0.018 (9)
O370.047 (10)0.053 (10)0.039 (10)0.019 (8)0.007 (8)0.001 (8)
O380.080 (14)0.048 (10)0.044 (10)0.003 (9)0.025 (10)0.002 (8)
O390.056 (10)0.047 (9)0.038 (9)0.014 (8)0.011 (8)0.008 (7)
O400.037 (9)0.078 (14)0.053 (11)0.022 (10)0.009 (8)0.001 (10)
O410.053 (10)0.034 (8)0.063 (11)0.002 (7)0.035 (9)0.001 (7)
O420.049 (11)0.043 (9)0.061 (12)0.001 (8)0.014 (9)0.003 (8)
O430.031 (8)0.040 (8)0.057 (11)0.000 (6)0.012 (7)0.002 (7)
O440.034 (8)0.048 (10)0.091 (16)0.000 (7)0.026 (9)0.006 (10)
O450.055 (10)0.039 (8)0.040 (9)0.004 (7)0.008 (8)0.007 (7)
O460.055 (11)0.054 (11)0.043 (10)0.012 (9)0.010 (9)0.009 (8)
O470.068 (11)0.029 (7)0.050 (10)0.011 (7)0.031 (9)0.003 (6)
O480.064 (12)0.051 (11)0.031 (9)0.003 (9)0.004 (8)0.010 (8)
O10.088 (19)0.074 (17)0.10 (2)0.044 (15)0.048 (17)0.003 (15)
O20.077 (14)0.047 (11)0.046 (11)0.002 (10)0.005 (10)0.008 (9)
N10.056 (11)0.065 (11)0.026 (8)0.012 (10)0.011 (8)0.009 (8)
N20.09 (2)0.079 (19)0.030 (11)0.010 (16)0.021 (13)0.003 (11)
N30.062 (14)0.047 (12)0.042 (11)0.004 (11)0.021 (11)0.001 (9)
N40.054 (14)0.071 (16)0.029 (10)0.013 (12)0.003 (10)0.002 (10)
C10.055 (12)0.067 (12)0.037 (10)0.016 (10)0.004 (9)0.009 (10)
C20.061 (17)0.054 (16)0.042 (14)0.005 (13)0.017 (13)0.000 (11)
C30.11 (3)0.061 (18)0.028 (12)0.000 (18)0.023 (15)0.005 (12)
C40.07 (2)0.061 (18)0.040 (14)0.017 (15)0.020 (14)0.013 (12)
C50.050 (14)0.045 (13)0.038 (13)0.019 (11)0.003 (11)0.003 (10)
C60.17 (4)0.030 (12)0.050 (17)0.011 (18)0.04 (2)0.003 (11)
C70.065 (19)0.052 (17)0.11 (3)0.009 (14)0.06 (2)0.013 (17)
C80.052 (16)0.045 (14)0.08 (2)0.001 (12)0.002 (15)0.011 (14)
O30.086 (17)0.084 (17)0.039 (11)0.001 (14)0.011 (11)0.019 (11)
O40.085 (16)0.043 (10)0.044 (11)0.005 (10)0.011 (11)0.008 (8)
N50.10 (2)0.067 (16)0.022 (10)0.004 (16)0.019 (12)0.010 (10)
N60.063 (15)0.046 (12)0.073 (18)0.002 (11)0.022 (13)0.001 (11)
N70.060 (13)0.030 (9)0.038 (10)0.013 (9)0.009 (9)0.001 (8)
N80.048 (11)0.043 (11)0.040 (11)0.003 (9)0.006 (9)0.001 (9)
C90.057 (18)0.052 (17)0.10 (3)0.007 (14)0.022 (18)0.012 (17)
C100.064 (16)0.041 (12)0.038 (13)0.003 (12)0.001 (12)0.000 (10)
C110.08 (2)0.050 (15)0.042 (14)0.008 (14)0.022 (14)0.003 (11)
C120.045 (15)0.055 (17)0.07 (2)0.033 (14)0.001 (14)0.001 (15)
C130.055 (15)0.065 (17)0.024 (11)0.001 (13)0.003 (10)0.000 (10)
C140.07 (2)0.032 (11)0.07 (2)0.008 (12)0.015 (16)0.022 (12)
C150.11 (3)0.14 (4)0.06 (2)0.07 (3)0.06 (2)0.04 (2)
C160.09 (3)0.11 (3)0.019 (11)0.02 (2)0.013 (14)0.007 (15)
O50.078 (16)0.062 (14)0.10 (2)0.007 (12)0.058 (16)0.014 (13)
O60.068 (13)0.055 (11)0.038 (10)0.004 (10)0.020 (9)0.007 (8)
N90.041 (12)0.063 (15)0.050 (13)0.003 (10)0.001 (10)0.008 (11)
N100.059 (14)0.036 (10)0.044 (12)0.002 (10)0.007 (10)0.000 (8)
N110.060 (14)0.054 (14)0.052 (13)0.008 (11)0.035 (11)0.001 (10)
N120.041 (11)0.042 (11)0.043 (11)0.000 (9)0.014 (9)0.001 (9)
C170.08 (2)0.057 (17)0.057 (18)0.012 (17)0.012 (18)0.012 (14)
C180.08 (2)0.033 (12)0.040 (13)0.016 (12)0.009 (13)0.006 (10)
C190.046 (14)0.046 (14)0.08 (2)0.010 (11)0.028 (14)0.001 (13)
C200.066 (18)0.044 (14)0.034 (12)0.020 (12)0.005 (12)0.004 (10)
C210.059 (15)0.059 (16)0.017 (9)0.002 (13)0.006 (10)0.003 (9)
C220.065 (18)0.08 (2)0.051 (18)0.008 (16)0.002 (14)0.007 (15)
C230.08 (2)0.054 (17)0.07 (2)0.011 (16)0.027 (18)0.007 (15)
C240.09 (3)0.12 (3)0.038 (15)0.04 (2)0.039 (17)0.018 (17)
O70.062 (13)0.058 (12)0.072 (15)0.015 (11)0.005 (11)0.027 (11)
O80.061 (13)0.056 (12)0.062 (13)0.002 (10)0.019 (11)0.009 (10)
N130.068 (17)0.060 (16)0.08 (2)0.026 (14)0.041 (16)0.011 (14)
N140.039 (9)0.060 (11)0.094 (17)0.010 (8)0.019 (10)0.002 (11)
N150.039 (12)0.09 (2)0.073 (18)0.006 (12)0.023 (12)0.006 (15)
N160.073 (16)0.046 (12)0.043 (12)0.001 (11)0.029 (11)0.006 (10)
C250.07 (2)0.08 (2)0.10 (3)0.022 (19)0.05 (2)0.05 (2)
C260.043 (10)0.059 (12)0.094 (18)0.015 (9)0.020 (11)0.000 (12)
C270.042 (12)0.035 (11)0.064 (17)0.006 (10)0.011 (12)0.005 (11)
C280.066 (19)0.060 (17)0.043 (14)0.001 (14)0.021 (14)0.017 (13)
C290.037 (12)0.049 (16)0.10 (3)0.022 (12)0.026 (15)0.003 (15)
C300.036 (11)0.046 (12)0.11 (2)0.021 (8)0.017 (13)0.011 (13)
C310.059 (18)0.08 (2)0.054 (17)0.052 (17)0.007 (14)0.003 (15)
C320.039 (12)0.043 (13)0.058 (16)0.003 (10)0.016 (12)0.003 (11)
O1W0.20 (4)0.071 (16)0.040 (13)0.04 (2)0.007 (18)0.007 (12)
O2W0.093 (19)0.095 (19)0.058 (14)0.017 (16)0.038 (14)0.013 (13)
Geometric parameters (Å, º) top
Si1—O101.564 (16)C6—H6A0.9800
Si1—O111.576 (16)C6—H6B0.9800
Si1—O121.602 (17)C6—H6C0.9800
Si1—O91.644 (18)C7—H7A0.9800
W1—O131.71 (2)C7—H7B0.9800
W1—O161.86 (3)C7—H7C0.9800
W1—O151.866 (19)C8—H8A0.9800
W1—O171.930 (19)C8—H8B0.9800
W1—O141.965 (17)C8—H8C0.9800
W1—O92.340 (16)O3—C111.234 (13)
W2—O181.706 (18)O4—C121.233 (13)
W2—O191.867 (17)N5—C91.37 (5)
W2—O201.90 (2)N5—C131.39 (3)
W2—O141.981 (19)N5—H5N0.8800
W2—O211.99 (2)N6—C91.30 (5)
W2—O92.355 (15)N6—C101.32 (4)
W3—O221.698 (15)N6—C141.502 (19)
W3—O191.878 (18)N7—C111.34 (4)
W3—O241.91 (2)N7—C121.42 (4)
W3—O251.92 (2)N7—C151.45 (4)
W3—O231.950 (18)N8—C121.27 (4)
W3—O102.361 (16)N8—C131.42 (4)
W4—O261.67 (2)N8—C161.50 (4)
W4—O271.861 (16)C9—H90.9500
W4—O281.876 (17)C10—C131.37 (4)
W4—O291.88 (3)C10—C111.54 (4)
W4—O231.944 (19)C14—H14A0.9800
W4—O102.438 (16)C14—H14B0.9800
W5—O301.65 (2)C14—H14C0.9800
W5—O321.855 (18)C15—H15A0.9800
W5—O271.900 (17)C15—H15B0.9800
W5—O311.93 (2)C15—H15C0.9800
W5—O331.968 (18)C16—H16A0.9800
W5—O112.399 (16)C16—H16B0.9800
W6—O341.698 (14)C16—H16C0.9800
W6—O161.90 (3)O5—C191.235 (13)
W6—O351.905 (18)O6—C201.231 (13)
W6—O311.91 (2)N9—C211.24 (4)
W6—O361.92 (2)N9—C171.36 (5)
W6—O112.393 (15)N9—H9N0.8800
W7—O371.721 (18)N10—C171.24 (5)
W7—O351.838 (18)N10—C181.43 (3)
W7—O151.882 (19)N10—C221.500 (19)
W7—O391.896 (19)N11—C231.37 (4)
W7—O382.019 (19)N11—C191.45 (4)
W7—O122.365 (14)N11—C201.50 (4)
W8—O401.65 (2)N12—C201.27 (4)
W8—O241.83 (2)N12—C211.44 (4)
W8—O201.89 (2)N12—C241.45 (4)
W8—O381.91 (2)C17—H170.9500
W8—O411.922 (17)C18—C211.27 (5)
W8—O122.378 (16)C18—C191.46 (4)
W9—O421.71 (2)C22—H22A0.9800
W9—O321.879 (18)C22—H22B0.9800
W9—O281.881 (17)C22—H22C0.9800
W9—O411.926 (18)C23—H23A0.9800
W9—O391.959 (18)C23—H23B0.9800
W9—O122.396 (17)C23—H23C0.9800
W10—O431.679 (18)C24—H24A0.9800
W10—O451.852 (19)C24—H24B0.9800
W10—O441.88 (2)C24—H24C0.9800
W10—O211.93 (2)O7—C271.235 (13)
W10—O171.980 (19)O8—C281.230 (13)
W10—O92.387 (17)N13—C291.35 (5)
W11—O461.724 (18)N13—C251.38 (5)
W11—O471.855 (15)N13—H13N0.8800
W11—O441.88 (2)N14—C251.30 (5)
W11—O291.91 (3)N14—C261.41 (5)
W11—O251.95 (2)N14—C301.500 (19)
W11—O102.387 (15)N15—C281.37 (4)
W12—O481.68 (2)N15—C271.42 (4)
W12—O471.885 (15)N15—C311.57 (4)
W12—O451.91 (2)N16—C291.21 (4)
W12—O331.917 (18)N16—C321.46 (4)
W12—O361.942 (19)N16—C281.51 (3)
W12—O112.379 (16)C25—H250.9500
O1—C31.233 (13)C26—C271.29 (5)
O2—C41.232 (13)C26—C291.41 (5)
N1—C11.35 (5)C30—H30A0.9800
N1—C51.44 (3)C30—H30B0.9800
N1—H1N0.8800C30—H30C0.9800
N2—C21.31 (4)C31—H31A0.9800
N2—C11.38 (4)C31—H31B0.9800
N2—C61.499 (19)C31—H31C0.9800
N3—C41.26 (4)C32—H32A0.9800
N3—C31.35 (4)C32—H32B0.9800
N3—C71.57 (4)C32—H32C0.9800
N4—C51.29 (4)O1W—H1W0.8500
N4—C81.46 (4)O1W—H2W0.8500
N4—C41.53 (4)O2W—H3W0.8500
C1—H10.9500O2W—H4W0.8500
C2—C51.36 (4)O3W—H5W0.8500
C2—C31.45 (5)O3W—H6W0.8500
O10—Si1—O11111.7 (10)W8—O12—W991.6 (6)
O10—Si1—O12110.4 (9)W1—O14—W2121.0 (11)
O11—Si1—O12110.2 (9)W1—O15—W7150.2 (11)
O10—Si1—O9108.5 (9)W1—O16—W6149.2 (13)
O11—Si1—O9109.4 (9)W1—O17—W10122.1 (10)
O12—Si1—O9106.4 (9)W2—O19—W3151.4 (9)
O13—W1—O16105.5 (12)W8—O20—W2147.6 (16)
O13—W1—O15105.7 (10)W10—O21—W2120.8 (10)
O16—W1—O1587.4 (9)W4—O23—W3122.6 (9)
O13—W1—O1796.0 (10)W8—O24—W3151.2 (13)
O16—W1—O1789.7 (9)W3—O25—W11124.8 (14)
O15—W1—O17158.1 (9)W4—O27—W5150.1 (11)
O13—W1—O1494.2 (10)W4—O28—W9148.3 (10)
O16—W1—O14160.0 (11)W4—O29—W11129.3 (16)
O15—W1—O1490.2 (8)W6—O31—W5127.6 (13)
O17—W1—O1485.1 (8)W5—O32—W9152.7 (10)
O13—W1—O9163.7 (10)W12—O33—W5124.4 (10)
O16—W1—O987.3 (10)W7—O35—W6149.8 (12)
O15—W1—O984.6 (8)W6—O36—W12124.7 (12)
O17—W1—O973.5 (7)W8—O38—W7122.3 (10)
O14—W1—O972.8 (7)W7—O39—W9125.8 (11)
O18—W2—O19106.2 (9)W8—O41—W9125.6 (9)
O18—W2—O2099.5 (12)W11—O44—W10151.3 (11)
O19—W2—O2086.0 (9)W10—O45—W12150.2 (10)
O18—W2—O1497.0 (10)W11—O47—W12152.0 (10)
O19—W2—O14156.7 (8)C1—N1—C5104 (3)
O20—W2—O1492.3 (10)C1—N1—H1N127.8
O18—W2—O2198.3 (9)C5—N1—H1N127.8
O19—W2—O2190.1 (8)C2—N2—C1109 (3)
O20—W2—O21162.2 (12)C2—N2—C6127 (3)
O14—W2—O2184.3 (8)C1—N2—C6124 (3)
O18—W2—O9166.8 (9)C4—N3—C3132 (3)
O19—W2—O984.5 (7)C4—N3—C7113 (2)
O20—W2—O988.8 (11)C3—N3—C7115 (3)
O14—W2—O972.2 (7)C5—N4—C8128 (3)
O21—W2—O973.5 (7)C5—N4—C4114 (3)
O22—W3—O19106.2 (12)C8—N4—C4119 (3)
O22—W3—O24103.3 (13)N1—C1—N2110 (3)
O19—W3—O2486.1 (8)N1—C1—H1125.2
O22—W3—O2599.5 (12)N2—C1—H1125.2
O19—W3—O2585.7 (9)N2—C2—C5109 (3)
O24—W3—O25157.2 (11)N2—C2—C3133 (3)
O22—W3—O2397.0 (12)C5—C2—C3118 (3)
O19—W3—O23156.6 (8)O1—C3—N3127 (3)
O24—W3—O2391.8 (9)O1—C3—C2121 (3)
O25—W3—O2387.3 (9)N3—C3—C2112 (2)
O22—W3—O10167.6 (12)O2—C4—N3129 (3)
O19—W3—O1082.4 (7)O2—C4—N4115 (3)
O24—W3—O1086.0 (9)N3—C4—N4116 (2)
O25—W3—O1071.8 (8)N4—C5—C2128 (3)
O23—W3—O1074.2 (7)N4—C5—N1124 (3)
O26—W4—O27107.0 (10)C2—C5—N1108 (3)
O26—W4—O28104.0 (11)N2—C6—H6A109.5
O27—W4—O2888.3 (7)N2—C6—H6B109.5
O26—W4—O29100.9 (13)H6A—C6—H6B109.5
O27—W4—O2984.4 (11)N2—C6—H6C109.5
O28—W4—O29155.2 (12)H6A—C6—H6C109.5
O26—W4—O2395.6 (9)H6B—C6—H6C109.5
O27—W4—O23157.1 (9)N3—C7—H7A109.5
O28—W4—O2389.5 (8)N3—C7—H7B109.5
O29—W4—O2388.1 (10)H7A—C7—H7B109.5
O26—W4—O10164.5 (8)N3—C7—H7C109.5
O27—W4—O1084.7 (8)H7A—C7—H7C109.5
O28—W4—O1086.1 (8)H7B—C7—H7C109.5
O29—W4—O1069.6 (9)N4—C8—H8A109.5
O23—W4—O1072.5 (6)N4—C8—H8B109.5
O30—W5—O32108.9 (11)H8A—C8—H8B109.5
O30—W5—O27106.5 (12)N4—C8—H8C109.5
O32—W5—O2786.5 (8)H8A—C8—H8C109.5
O30—W5—O3199.0 (13)H8B—C8—H8C109.5
O32—W5—O3187.7 (9)C9—N5—C13103 (3)
O27—W5—O31154.4 (10)C9—N5—H5N128.7
O30—W5—O3396.7 (11)C13—N5—H5N128.7
O32—W5—O33154.4 (8)C9—N6—C10106 (3)
O27—W5—O3387.2 (8)C9—N6—C14131 (3)
O31—W5—O3387.3 (8)C10—N6—C14123 (3)
O30—W5—O11163.5 (11)C11—N7—C12126 (2)
O32—W5—O1183.5 (7)C11—N7—C15113 (2)
O27—W5—O1184.5 (8)C12—N7—C15121 (3)
O31—W5—O1170.0 (8)C12—N8—C13117 (2)
O33—W5—O1171.2 (7)C12—N8—C16127 (3)
O34—W6—O16104.4 (13)C13—N8—C16117 (3)
O34—W6—O35105.4 (11)N6—C9—N5114 (4)
O16—W6—O3587.3 (8)N6—C9—H9123.0
O34—W6—O3199.7 (12)N5—C9—H9123.0
O16—W6—O31155.8 (11)N6—C10—C13110 (3)
O35—W6—O3186.6 (9)N6—C10—C11133 (3)
O34—W6—O3698.5 (11)C13—C10—C11117 (3)
O16—W6—O3688.9 (9)O3—C11—N7124 (3)
O35—W6—O36156.0 (9)O3—C11—C10123 (3)
O31—W6—O3687.3 (9)N7—C11—C10113 (2)
O34—W6—O11166.2 (11)O4—C12—N8123 (3)
O16—W6—O1185.6 (10)O4—C12—N7114 (3)
O35—W6—O1184.3 (7)N8—C12—N7123 (2)
O31—W6—O1170.5 (8)C10—C13—N5107 (3)
O36—W6—O1171.7 (7)C10—C13—N8125 (3)
O37—W7—O35107.8 (9)N5—C13—N8128 (3)
O37—W7—O15106.3 (10)N6—C14—H14A109.5
O35—W7—O1588.0 (9)N6—C14—H14B109.5
O37—W7—O3996.7 (10)H14A—C14—H14B109.5
O35—W7—O3990.7 (8)N6—C14—H14C109.5
O15—W7—O39156.2 (8)H14A—C14—H14C109.5
O37—W7—O3894.7 (9)H14B—C14—H14C109.5
O35—W7—O38157.4 (9)N7—C15—H15A109.5
O15—W7—O3887.1 (9)N7—C15—H15B109.5
O39—W7—O3885.0 (8)H15A—C15—H15B109.5
O37—W7—O12162.5 (9)N7—C15—H15C109.5
O35—W7—O1286.0 (8)H15A—C15—H15C109.5
O15—W7—O1284.4 (7)H15B—C15—H15C109.5
O39—W7—O1271.8 (7)N8—C16—H16A109.5
O38—W7—O1271.6 (7)N8—C16—H16B109.5
O40—W8—O24103.7 (12)H16A—C16—H16B109.5
O40—W8—O2098.3 (14)N8—C16—H16C109.5
O24—W8—O2085.3 (9)H16A—C16—H16C109.5
O40—W8—O3897.5 (10)H16B—C16—H16C109.5
O24—W8—O38158.8 (11)C21—N9—C17110 (3)
O20—W8—O3890.5 (11)C21—N9—H9N124.8
O40—W8—O41101.8 (10)C17—N9—H9N124.8
O24—W8—O4189.2 (9)C17—N10—C18105 (3)
O20—W8—O41160.0 (12)C17—N10—C22124 (3)
O38—W8—O4187.7 (8)C18—N10—C22131 (3)
O40—W8—O12168.4 (9)C23—N11—C19117 (3)
O24—W8—O1286.0 (10)C23—N11—C20123 (3)
O20—W8—O1288.7 (12)C19—N11—C20120 (2)
O38—W8—O1273.1 (7)C20—N12—C21123 (2)
O41—W8—O1271.7 (7)C20—N12—C24121 (3)
O42—W9—O32106.6 (9)C21—N12—C24117 (3)
O42—W9—O28104.3 (10)N10—C17—N9108 (3)
O32—W9—O2887.1 (7)N10—C17—H17125.9
O42—W9—O4198.5 (9)N9—C17—H17125.9
O32—W9—O41154.8 (8)C21—C18—N10108 (3)
O28—W9—O4189.4 (8)C21—C18—C19129 (3)
O42—W9—O3998.2 (9)N10—C18—C19123 (3)
O32—W9—O3989.8 (7)O5—C19—N11116 (3)
O28—W9—O39157.3 (10)O5—C19—C18133 (3)
O41—W9—O3984.0 (7)N11—C19—C18111 (2)
O42—W9—O12164.7 (9)O6—C20—N12127 (3)
O32—W9—O1283.7 (7)O6—C20—N11113 (3)
O28—W9—O1287.2 (8)N12—C20—N11120 (2)
O41—W9—O1271.2 (6)N9—C21—C18109 (3)
O39—W9—O1270.1 (7)N9—C21—N12134 (3)
O43—W10—O45104.2 (9)C18—C21—N12117 (3)
O43—W10—O44106.6 (9)N10—C22—H22A109.5
O45—W10—O4488.0 (8)N10—C22—H22B109.5
O43—W10—O2197.6 (9)H22A—C22—H22B109.5
O45—W10—O21157.8 (8)N10—C22—H22C109.5
O44—W10—O2190.2 (9)H22A—C22—H22C109.5
O43—W10—O1797.2 (9)H22B—C22—H22C109.5
O45—W10—O1787.4 (7)N11—C23—H23A109.5
O44—W10—O17156.1 (8)N11—C23—H23B109.5
O21—W10—O1785.4 (8)H23A—C23—H23B109.5
O43—W10—O9166.0 (8)N11—C23—H23C109.5
O45—W10—O984.0 (7)H23A—C23—H23C109.5
O44—W10—O984.6 (7)H23B—C23—H23C109.5
O21—W10—O973.7 (7)N12—C24—H24A109.5
O17—W10—O971.6 (7)N12—C24—H24B109.5
O46—W11—O47105.3 (10)H24A—C24—H24B109.5
O46—W11—O44106.4 (10)N12—C24—H24C109.5
O47—W11—O4486.7 (8)H24A—C24—H24C109.5
O46—W11—O29101.7 (14)H24B—C24—H24C109.5
O47—W11—O2985.7 (10)C29—N13—C25107 (3)
O44—W11—O29152.0 (13)C29—N13—H13N126.4
O46—W11—O2599.9 (11)C25—N13—H13N126.4
O47—W11—O25154.8 (11)C25—N14—C26110 (3)
O44—W11—O2585.5 (10)C25—N14—C30122 (3)
O29—W11—O2590.1 (10)C26—N14—C30128 (3)
O46—W11—O10167.2 (9)C28—N15—C27133 (3)
O47—W11—O1084.5 (8)C28—N15—C31110 (3)
O44—W11—O1082.1 (7)C27—N15—C31117 (3)
O29—W11—O1070.4 (11)C29—N16—C32126 (3)
O25—W11—O1070.7 (9)C29—N16—C28122 (3)
O48—W12—O47103.4 (9)C32—N16—C28111 (2)
O48—W12—O45107.1 (10)N14—C25—N13110 (3)
O47—W12—O4587.2 (7)N14—C25—H25125.0
O48—W12—O3397.4 (10)N13—C25—H25125.0
O47—W12—O3387.8 (8)C27—C26—N14129 (4)
O45—W12—O33155.6 (8)C27—C26—C29126 (4)
O48—W12—O36100.5 (10)N14—C26—C29104 (4)
O47—W12—O36156.0 (9)O7—C27—C26133 (3)
O45—W12—O3687.5 (8)O7—C27—N15118 (3)
O33—W12—O3687.5 (8)C26—C27—N15108 (3)
O48—W12—O11167.2 (9)O8—C28—N15133 (3)
O47—W12—O1184.3 (7)O8—C28—N16120 (3)
O45—W12—O1183.3 (7)N15—C28—N16107 (2)
O33—W12—O1172.4 (7)N16—C29—N13129 (4)
O36—W12—O1171.8 (8)N16—C29—C26122 (4)
Si1—O9—W1124.4 (9)N13—C29—C26109 (3)
Si1—O9—W2123.9 (8)N14—C30—H30A109.5
W1—O9—W294.0 (5)N14—C30—H30B109.5
Si1—O9—W10121.3 (8)H30A—C30—H30B109.5
W1—O9—W1092.7 (6)N14—C30—H30C109.5
W2—O9—W1091.8 (6)H30A—C30—H30C109.5
Si1—O10—W3126.2 (9)H30B—C30—H30C109.5
Si1—O10—W11124.9 (10)N15—C31—H31A109.5
W3—O10—W1192.4 (5)N15—C31—H31B109.5
Si1—O10—W4121.9 (8)H31A—C31—H31B109.5
W3—O10—W490.7 (6)N15—C31—H31C109.5
W11—O10—W490.4 (5)H31A—C31—H31C109.5
Si1—O11—W12123.9 (9)H31B—C31—H31C109.5
Si1—O11—W6124.8 (9)N16—C32—H32A109.5
W12—O11—W691.7 (6)N16—C32—H32B109.5
Si1—O11—W5123.1 (9)H32A—C32—H32B109.5
W12—O11—W592.0 (6)N16—C32—H32C109.5
W6—O11—W591.8 (5)H32A—C32—H32C109.5
Si1—O12—W7124.3 (8)H32B—C32—H32C109.5
Si1—O12—W8124.7 (8)H1W—O1W—H2W108.4
W7—O12—W893.0 (5)H3W—O2W—H4W108.4
Si1—O12—W9121.9 (9)H5W—O3W—H6W108.4
W7—O12—W992.2 (5)
O10—Si1—O9—W1179.4 (9)O45—W12—O47—W1123 (3)
O11—Si1—O9—W157.3 (12)O33—W12—O47—W11133 (3)
O12—Si1—O9—W161.7 (11)O36—W12—O47—W1154 (4)
O10—Si1—O9—W256.4 (12)O11—W12—O47—W1160 (3)
O11—Si1—O9—W2178.5 (9)C5—N1—C1—N25 (3)
O12—Si1—O9—W262.5 (11)C2—N2—C1—N16 (3)
O10—Si1—O9—W1060.5 (11)C6—N2—C1—N1178 (3)
O11—Si1—O9—W1061.6 (12)C1—N2—C2—C54 (3)
O12—Si1—O9—W10179.4 (8)C6—N2—C2—C5176 (3)
O11—Si1—O10—W3178.7 (9)C1—N2—C2—C3177 (3)
O12—Si1—O10—W355.6 (13)C6—N2—C2—C36 (6)
O9—Si1—O10—W360.6 (13)C4—N3—C3—O1178 (4)
O11—Si1—O10—W1156.1 (13)C7—N3—C3—O14 (5)
O12—Si1—O10—W11179.2 (9)C4—N3—C3—C27 (5)
O9—Si1—O10—W1164.5 (12)C7—N3—C3—C2179 (3)
O11—Si1—O10—W460.3 (13)N2—C2—C3—O12 (6)
O12—Si1—O10—W462.7 (12)C5—C2—C3—O1180 (3)
O9—Si1—O10—W4179.0 (8)N2—C2—C3—N3173 (3)
O10—Si1—O11—W1257.8 (13)C5—C2—C3—N35 (4)
O12—Si1—O11—W12179.0 (9)C3—N3—C4—O2179 (3)
O9—Si1—O11—W1262.4 (12)C7—N3—C4—O27 (5)
O10—Si1—O11—W6178.7 (9)C3—N3—C4—N45 (5)
O12—Si1—O11—W658.1 (13)C7—N3—C4—N4179 (3)
O9—Si1—O11—W658.5 (13)C5—N4—C4—O2175 (3)
O10—Si1—O11—W561.3 (13)C8—N4—C4—O21 (4)
O12—Si1—O11—W561.8 (12)C5—N4—C4—N30 (4)
O9—Si1—O11—W5178.5 (9)C8—N4—C4—N3177 (3)
O10—Si1—O12—W7179.3 (9)C8—N4—C5—C2177 (3)
O11—Si1—O12—W756.7 (13)C4—N4—C5—C21 (4)
O9—Si1—O12—W761.7 (12)C8—N4—C5—N11 (5)
O10—Si1—O12—W856.1 (13)C4—N4—C5—N1177 (2)
O11—Si1—O12—W8179.9 (9)N2—C2—C5—N4177 (3)
O9—Si1—O12—W861.5 (12)C3—C2—C5—N41 (5)
O10—Si1—O12—W962.0 (11)N2—C2—C5—N11 (3)
O11—Si1—O12—W961.9 (11)C3—C2—C5—N1180 (2)
O9—Si1—O12—W9179.6 (8)C1—N1—C5—N4179 (3)
O13—W1—O15—W7132 (2)C1—N1—C5—C22 (3)
O16—W1—O15—W727 (2)C10—N6—C9—N50 (4)
O17—W1—O15—W756 (4)C14—N6—C9—N5179 (3)
O14—W1—O15—W7133 (2)C13—N5—C9—N62 (4)
O9—W1—O15—W761 (2)C9—N6—C10—C132 (4)
O37—W7—O15—W1133 (2)C14—N6—C10—C13179 (3)
O35—W7—O15—W126 (2)C9—N6—C10—C11175 (3)
O39—W7—O15—W162 (3)C14—N6—C10—C114 (5)
O38—W7—O15—W1132 (2)C12—N7—C11—O3179 (3)
O12—W7—O15—W161 (2)C15—N7—C11—O33 (5)
O13—W1—O16—W6135 (3)C12—N7—C11—C104 (4)
O15—W1—O16—W629 (3)C15—N7—C11—C10172 (3)
O17—W1—O16—W6129 (3)N6—C10—C11—O33 (6)
O14—W1—O16—W654 (5)C13—C10—C11—O3174 (3)
O9—W1—O16—W655 (3)N6—C10—C11—N7178 (3)
O18—W2—O19—W3124 (2)C13—C10—C11—N71 (4)
O20—W2—O19—W325 (2)C13—N8—C12—O4176 (3)
O14—W2—O19—W362 (3)C16—N8—C12—O42 (5)
O21—W2—O19—W3137 (2)C13—N8—C12—N77 (4)
O9—W2—O19—W364 (2)C16—N8—C12—N7175 (3)
O22—W3—O19—W2125 (2)C11—N7—C12—O4174 (3)
O24—W3—O19—W222 (2)C15—N7—C12—O411 (4)
O25—W3—O19—W2137 (2)C11—N7—C12—N89 (4)
O23—W3—O19—W264 (3)C15—N7—C12—N8167 (3)
O10—W3—O19—W265 (2)N6—C10—C13—N54 (4)
O40—W8—O20—W2145 (3)C11—C10—C13—N5174 (3)
O24—W8—O20—W242 (3)N6—C10—C13—N8180 (3)
O38—W8—O20—W2117 (3)C11—C10—C13—N82 (5)
O41—W8—O20—W233 (5)C9—N5—C13—C103 (4)
O12—W8—O20—W244 (3)C9—N5—C13—N8179 (3)
O18—W2—O20—W8145 (3)C12—N8—C13—C102 (4)
O19—W2—O20—W839 (3)C16—N8—C13—C10180 (3)
O14—W2—O20—W8117 (3)C12—N8—C13—N5177 (3)
O21—W2—O20—W839 (6)C16—N8—C13—N55 (5)
O9—W2—O20—W845 (3)C18—N10—C17—N98 (3)
O40—W8—O24—W3133 (3)C22—N10—C17—N9173 (3)
O20—W8—O24—W335 (3)C21—N9—C17—N109 (4)
O38—W8—O24—W344 (5)C17—N10—C18—C214 (3)
O41—W8—O24—W3125 (3)C22—N10—C18—C21177 (3)
O12—W8—O24—W354 (3)C17—N10—C18—C19175 (3)
O26—W4—O27—W5129 (3)C22—N10—C18—C194 (5)
O28—W4—O27—W525 (3)C23—N11—C19—O52 (5)
O29—W4—O27—W5131 (3)C20—N11—C19—O5175 (3)
O23—W4—O27—W560 (4)C23—N11—C19—C18178 (3)
O10—W4—O27—W561 (3)C20—N11—C19—C186 (4)
O26—W4—O28—W9136 (3)C21—C18—C19—O5179 (4)
O27—W4—O28—W929 (3)N10—C18—C19—O50 (6)
O29—W4—O28—W944 (4)C21—C18—C19—N111 (5)
O23—W4—O28—W9128 (3)N10—C18—C19—N11179 (3)
O10—W4—O28—W956 (3)C21—N12—C20—O6180 (2)
O42—W9—O28—W4134 (3)C24—N12—C20—O65 (5)
O32—W9—O28—W428 (3)C21—N12—C20—N117 (4)
O41—W9—O28—W4127 (3)C24—N12—C20—N11177 (3)
O39—W9—O28—W454 (4)C23—N11—C20—O61 (4)
O12—W9—O28—W456 (3)C19—N11—C20—O6177 (3)
O26—W4—O29—W11161.8 (19)C23—N11—C20—N12174 (3)
O27—W4—O29—W1192 (2)C19—N11—C20—N129 (4)
O28—W4—O29—W1118 (4)C17—N9—C21—C186 (4)
O23—W4—O29—W1166 (2)C17—N9—C21—N12174 (3)
O10—W4—O29—W115.6 (16)N10—C18—C21—N91 (3)
O30—W5—O32—W9128 (2)C19—C18—C21—N9179 (3)
O27—W5—O32—W922 (2)N10—C18—C21—N12179 (2)
O31—W5—O32—W9133 (2)C19—C18—C21—N121 (4)
O33—W5—O32—W954 (3)C20—N12—C21—N9178 (3)
O11—W5—O32—W963 (2)C24—N12—C21—N92 (4)
O42—W9—O32—W5128 (2)C20—N12—C21—C183 (4)
O28—W9—O32—W524 (3)C24—N12—C21—C18179 (3)
O41—W9—O32—W558 (3)C26—N14—C25—N134 (4)
O39—W9—O32—W5134 (2)C30—N14—C25—N13179 (2)
O12—W9—O32—W564 (2)C29—N13—C25—N142 (4)
O37—W7—O35—W6131 (2)C25—N14—C26—C27180 (3)
O15—W7—O35—W625 (2)C30—N14—C26—C276 (5)
O39—W7—O35—W6132 (2)C25—N14—C26—C294 (3)
O38—W7—O35—W653 (4)C30—N14—C26—C29178 (2)
O12—W7—O35—W660 (2)N14—C26—C27—O72 (6)
O37—W7—O39—W9170.0 (11)C29—C26—C27—O7176 (3)
O35—W7—O39—W982.0 (11)N14—C26—C27—N15172 (3)
O15—W7—O39—W95 (3)C29—C26—C27—N153 (4)
O38—W7—O39—W975.7 (11)C28—N15—C27—O7175 (3)
O12—W7—O39—W93.5 (9)C31—N15—C27—O70 (4)
O46—W11—O44—W10125 (2)C28—N15—C27—C2610 (5)
O47—W11—O44—W1020 (3)C31—N15—C27—C26175 (2)
O29—W11—O44—W1054 (4)C27—N15—C28—O8176 (3)
O25—W11—O44—W10136 (3)C31—N15—C28—O80 (5)
O10—W11—O44—W1064 (2)C27—N15—C28—N1611 (5)
O43—W10—O44—W11124 (2)C31—N15—C28—N16174 (2)
O45—W10—O44—W1120 (3)C29—N16—C28—O8179 (3)
O21—W10—O44—W11138 (3)C32—N16—C28—O89 (4)
O17—W10—O44—W1159 (4)C29—N16—C28—N155 (4)
O9—W10—O44—W1165 (2)C32—N16—C28—N15166 (2)
O43—W10—O45—W12125 (2)C32—N16—C29—N1310 (5)
O44—W10—O45—W1218 (2)C28—N16—C29—N13180 (3)
O21—W10—O45—W1267 (3)C32—N16—C29—C26170 (3)
O17—W10—O45—W12138 (2)C28—N16—C29—C260 (4)
O9—W10—O45—W1266 (2)C25—N13—C29—N16179 (3)
O46—W11—O47—W12129 (3)C25—N13—C29—C261 (3)
O44—W11—O47—W1223 (3)C27—C26—C29—N162 (5)
O29—W11—O47—W12130 (3)N14—C26—C29—N16177 (3)
O25—W11—O47—W1249 (4)C27—C26—C29—N13178 (3)
O10—W11—O47—W1259 (3)N14—C26—C29—N133 (3)
O48—W12—O47—W11130 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1N···O48i0.882.042.82 (4)147
N1—H1N···O380.882.663.22 (3)123
N5—H5N···O1W0.881.782.65 (4)169
N9—H9N···O37ii0.882.122.95 (3)158
N13—H13N···O2W0.881.742.61 (5)174
O1W—H1W···O40iii0.852.122.84 (4)142
O1W—H2W···O20.851.902.75 (4)171
O2W—H3W···O460.852.022.73 (4)140
O2W—H4W···O6iv0.851.922.76 (3)169
O3W—H5W···O430.852.062.85 (4)153
O3W—H6W···O42v0.852.202.98 (4)153
C9—H9···O5vi0.952.153.10 (5)176
C17—H17···O290.952.452.98 (5)116
C25—H25···O1vii0.952.123.07 (4)175
C6—H6A···O29viii0.982.573.28 (5)129
C6—H6C···O25viii0.982.583.38 (4)138
C7—H7C···O4ix0.982.533.49 (5)166
C8—H8B···O370.982.533.33 (5)140
C8—H8B···O150.982.743.55 (4)141
C14—H14B···O22iii0.982.243.08 (4)143
C14—H14C···O430.982.403.33 (3)158
C14—H14C···O170.982.623.37 (3)134
C15—H15B···O26iii0.982.623.34 (5)130
C16—H16A···O1W0.982.413.39 (5)175
C16—H16B···O42iii0.982.223.08 (4)146
C16—H16C···O8x0.982.333.20 (5)147
C22—H22B···O20vii0.982.733.39 (5)125
C22—H22C···O260.982.213.10 (4)150
C23—H23B···O17xi0.982.743.57 (5)143
C23—H23C···O1xi0.982.673.53 (5)146
C24—H24A···O38ii0.982.713.33 (5)121
C24—H24A···O480.982.773.50 (4)132
C24—H24B···O41ii0.982.543.40 (4)147
C30—H30B···O220.982.353.14 (3)137
C30—H30C···O42iv0.982.443.26 (3)140
C30—H30C···O32iv0.982.603.35 (3)133
C31—H31A···O46viii0.982.773.46 (4)128
C32—H32A···O430.982.753.21 (3)109
Symmetry codes: (i) x+1/2, y+1/2, z+1/2; (ii) x1/2, y+1/2, z1/2; (iii) x1/2, y1/2, z; (iv) x1/2, y+1/2, z; (v) x1, y, z; (vi) x1/2, y+1/2, z+1/2; (vii) x, y+1, z1/2; (viii) x, y+1, z+1/2; (ix) x, y, z+1/2; (x) x+1/2, y1/2, z; (xi) x+1/2, y+1/2, z1/2.
Tris(3,7-dimethylxanthinium) µ12-phosphato-tetracosa-µ2-oxido-dodecaoxidododecatungsten ethanol sesquisolvate (2) top
Crystal data top
(C7H9N4O2)3[PW12O40]·1.5C2H6OF(000) = 6188
Mr = 3489.82Dx = 3.867 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 10.8071 (4) ÅCell parameters from 29521 reflections
b = 23.4412 (13) Åθ = 2.5–26.1°
c = 23.6644 (10) ŵ = 23.07 mm1
β = 90.720 (3)°T = 203 K
V = 5994.5 (5) Å3Prism, yellow
Z = 40.23 × 0.21 × 0.18 mm
Data collection top
Stoe Image plate diffraction system
diffractometer
7160 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.049
φ oscillation scansθmax = 26.1°, θmin = 2.5°
Absorption correction: numerical
[X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)]
h = 1113
Tmin = 0.194, Tmax = 0.231k = 2828
29521 measured reflectionsl = 2929
11783 independent reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.051Hydrogen site location: mixed
wR(F2) = 0.123H-atom parameters constrained
S = 0.93 w = 1/[σ2(Fo2) + (0.0616P)2]
where P = (Fo2 + 2Fc2)/3
11783 reflections(Δ/σ)max = 0.001
889 parametersΔρmax = 2.13 e Å3
18 restraintsΔρmin = 1.84 e Å3
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
W10.48891 (7)0.03984 (3)0.32791 (3)0.04100 (15)
W20.48800 (7)0.11740 (3)0.45730 (3)0.04284 (17)
W30.76021 (7)0.11435 (3)0.37413 (3)0.04061 (16)
W40.49793 (7)0.11484 (4)0.19726 (3)0.04805 (19)
W50.22585 (7)0.11844 (3)0.27974 (3)0.04743 (19)
W60.22332 (6)0.19564 (3)0.40993 (3)0.04050 (15)
W70.49467 (6)0.26909 (3)0.45547 (3)0.04010 (16)
W80.76745 (7)0.26620 (3)0.37255 (3)0.04415 (17)
W90.76866 (7)0.18964 (3)0.24349 (3)0.04700 (18)
W100.50376 (6)0.26703 (3)0.19552 (3)0.03815 (16)
W110.23256 (7)0.27037 (3)0.27891 (3)0.04191 (17)
W120.50288 (7)0.34422 (3)0.32475 (4)0.04439 (16)
P10.4955 (4)0.19255 (18)0.32602 (18)0.0359 (7)
O7A0.450 (2)0.1364 (8)0.2959 (8)0.032 (4)0.5
O8A0.4472 (19)0.1927 (8)0.3862 (8)0.033 (4)0.5
O9A0.641 (2)0.1887 (9)0.3286 (8)0.035 (4)0.5
O10A0.4498 (17)0.2451 (8)0.2947 (8)0.027 (4)0.5
O7B0.537 (2)0.1419 (9)0.3566 (8)0.040 (5)0.5
O8B0.351 (2)0.1963 (9)0.3269 (9)0.036 (5)0.5
O9B0.543 (2)0.1945 (9)0.2667 (9)0.039 (5)0.5
O10B0.542 (2)0.2493 (10)0.3568 (8)0.038 (5)0.5
O110.4880 (16)0.0315 (6)0.3289 (9)0.082 (5)
O120.4577 (14)0.0609 (8)0.4028 (7)0.078 (5)
O130.6575 (14)0.0554 (7)0.3432 (6)0.069 (4)
O140.5233 (15)0.0555 (10)0.2511 (7)0.099 (7)
O150.3233 (15)0.0588 (10)0.3112 (6)0.092 (6)
O160.4809 (13)0.0822 (7)0.5184 (5)0.061 (4)
O170.6580 (15)0.1128 (7)0.4379 (7)0.073 (4)
O180.5166 (13)0.1933 (6)0.4797 (9)0.086 (6)
O190.3200 (15)0.1411 (6)0.4475 (9)0.084 (6)
O200.8808 (14)0.0772 (7)0.3949 (7)0.074 (4)
O210.804 (2)0.1347 (7)0.2993 (6)0.101 (7)
O220.801 (2)0.1904 (6)0.3936 (5)0.087 (6)
O230.4978 (16)0.0792 (7)0.1362 (6)0.070 (4)
O240.3237 (15)0.1135 (10)0.2159 (8)0.098 (7)
O250.4742 (12)0.1911 (7)0.1720 (9)0.083 (5)
O260.6661 (15)0.1342 (6)0.2074 (9)0.082 (5)
O270.0982 (12)0.0837 (6)0.2573 (6)0.057 (3)
O280.197 (2)0.1948 (6)0.2586 (5)0.091 (6)
O290.187 (2)0.1412 (6)0.3550 (5)0.083 (6)
O300.0948 (12)0.1993 (5)0.4480 (6)0.054 (3)
O310.3240 (14)0.2518 (5)0.4458 (8)0.071 (5)
O320.191 (2)0.2503 (5)0.3542 (6)0.084 (6)
O330.4965 (14)0.3063 (8)0.5157 (6)0.074 (4)
O340.4707 (14)0.3288 (9)0.4019 (8)0.099 (7)
O350.6673 (16)0.2695 (9)0.4355 (8)0.106 (8)
O360.8939 (11)0.3011 (6)0.3940 (5)0.057 (3)
O370.812 (2)0.2445 (6)0.2985 (6)0.102 (8)
O380.6699 (15)0.3274 (9)0.3401 (7)0.091 (6)
O390.8957 (13)0.1885 (6)0.2053 (6)0.059 (3)
O400.6707 (15)0.2457 (6)0.2055 (8)0.079 (5)
O410.5038 (19)0.3019 (10)0.1344 (6)0.109 (8)
O420.3332 (15)0.2721 (7)0.2140 (7)0.072 (4)
O430.5356 (13)0.3261 (7)0.2480 (8)0.080 (5)
O440.1095 (12)0.3063 (7)0.2575 (5)0.061 (4)
O450.3330 (14)0.3294 (7)0.3092 (7)0.071 (5)
O460.5046 (13)0.4163 (5)0.3253 (6)0.056 (3)
O10.4129 (12)0.4920 (5)0.4361 (5)0.046 (3)
O20.3852 (14)0.3926 (5)0.5997 (5)0.053 (3)
N10.1096 (14)0.3567 (6)0.4497 (6)0.041 (3)
H1N0.0611530.3302730.4627980.062*
N20.1902 (13)0.4194 (5)0.3928 (5)0.036 (3)
N30.3954 (13)0.4403 (6)0.5160 (6)0.045 (3)
H3N0.4561890.4604240.5298940.067*
N40.2496 (13)0.3682 (6)0.5310 (5)0.038 (3)
C10.0985 (17)0.3819 (7)0.3977 (7)0.046 (4)
H10.0370750.3741490.3703170.056*
C20.2609 (16)0.4197 (7)0.4430 (6)0.038 (3)
C30.3616 (15)0.4533 (7)0.4618 (7)0.039 (4)
C40.3479 (18)0.4001 (7)0.5521 (8)0.046 (4)
C50.2079 (15)0.3794 (7)0.4772 (7)0.038 (3)
C60.2041 (19)0.4576 (8)0.3447 (7)0.049 (4)
H6A0.2773010.4809980.3503190.073*
H6B0.2125570.4353150.3104690.073*
H6C0.1317950.4819290.3414420.073*
C70.1990 (19)0.3187 (7)0.5629 (8)0.050 (4)
H7A0.2381130.3168520.5999850.074*
H7B0.1103560.3232560.5670540.074*
H7C0.2155780.2836860.5424510.074*
O30.4177 (12)0.1817 (5)0.0167 (5)0.049 (3)
O40.3727 (15)0.3733 (6)0.0310 (6)0.061 (4)
N50.1054 (14)0.2487 (6)0.1272 (6)0.044 (3)
H5N0.0554270.2711160.1453400.066*
N60.1929 (13)0.1725 (6)0.0960 (6)0.041 (3)
N70.3849 (14)0.2775 (7)0.0232 (6)0.047 (3)
H7N0.4420120.2827260.0018620.071*
N80.2367 (13)0.3194 (6)0.0818 (6)0.040 (3)
C80.1033 (16)0.1904 (7)0.1268 (7)0.040 (4)
H80.0461190.1672380.1457530.048*
C90.2561 (14)0.2178 (7)0.0736 (6)0.035 (3)
C100.3586 (15)0.2217 (9)0.0346 (6)0.042 (4)
C110.3357 (16)0.3266 (8)0.0449 (8)0.045 (4)
C120.1999 (14)0.2649 (7)0.0941 (7)0.037 (4)
C130.2136 (19)0.1107 (8)0.0830 (8)0.052 (5)
H13A0.2856840.1068240.0593390.078*
H13B0.2268310.0898690.1179590.078*
H13C0.1415420.0955470.0633220.078*
C140.1866 (18)0.3690 (8)0.1124 (9)0.055 (5)
H14A0.2234720.4036760.0979600.082*
H14B0.0975950.3704780.1069810.082*
H14C0.2059520.3653330.1523930.082*
O50.8945 (14)0.4151 (6)0.3115 (5)0.060 (3)
O60.9017 (12)0.3149 (5)0.1470 (5)0.051 (3)
N90.6153 (14)0.4618 (5)0.1714 (6)0.043 (3)
H9N0.5749330.4622420.1393630.064*
N100.6779 (16)0.4843 (7)0.2572 (7)0.055 (4)
N110.8876 (14)0.3638 (6)0.2297 (7)0.044 (3)
H11N0.9418660.3407410.2446050.067*
N120.7569 (15)0.3839 (6)0.1512 (6)0.047 (4)
C150.5972 (19)0.4964 (8)0.2152 (10)0.058 (5)
H150.5366470.5251090.2164750.069*
C160.7470 (15)0.4388 (7)0.2378 (7)0.041 (4)
C170.846 (2)0.4088 (8)0.2654 (8)0.054 (5)
C180.8528 (16)0.3523 (6)0.1742 (8)0.042 (4)
C190.7075 (15)0.4260 (7)0.1860 (7)0.040 (4)
C200.684 (2)0.5135 (9)0.3110 (9)0.062 (5)
H20A0.7497160.4971020.3340870.093*
H20B0.7007550.5536850.3048390.093*
H20C0.6057250.5093590.3301660.093*
C210.722 (2)0.3781 (8)0.0913 (8)0.055 (5)
H21A0.6527990.4034430.0827440.082*
H21B0.7913510.3880670.0678730.082*
H21C0.6970270.3390220.0836110.082*
O470.4514 (16)0.4661 (7)0.0892 (7)0.082 (5)*
H1O0.4267580.4369710.0708900.124*
C220.364 (3)0.5112 (11)0.0809 (11)0.100 (9)*
H22A0.4044960.5476920.0895020.120*
H22B0.2957670.5062790.1072050.120*
C230.314 (4)0.5126 (19)0.0220 (14)0.171 (19)*
H23A0.2557670.5437160.0181690.256*
H23B0.3817980.5181810.0040950.256*
H23C0.2731110.4767830.0136010.256*
O480.891 (5)0.501 (2)0.458 (3)0.166 (19)*0.5
H2O0.9197110.5192620.4299340.249*0.5
C240.862 (5)0.442 (2)0.439 (4)0.159 (19)*0.5
H24A0.8941940.4366190.4012300.191*0.5
H24B0.9046890.4152440.4646090.191*0.5
C250.733 (6)0.430 (3)0.439 (3)0.120 (19)*0.5
H25A0.7188920.3915400.4267320.180*0.5
H25B0.7011390.4351880.4770820.180*0.5
H25C0.6906430.4565630.4137040.180*0.5
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
W10.0420 (4)0.0382 (3)0.0428 (3)0.0024 (3)0.0017 (3)0.0015 (3)
W20.0446 (4)0.0497 (4)0.0341 (4)0.0023 (3)0.0023 (3)0.0092 (3)
W30.0408 (4)0.0455 (4)0.0354 (3)0.0084 (3)0.0026 (3)0.0004 (3)
W40.0383 (4)0.0700 (5)0.0358 (4)0.0016 (3)0.0033 (3)0.0178 (3)
W50.0417 (4)0.0616 (4)0.0389 (4)0.0165 (3)0.0045 (3)0.0001 (3)
W60.0385 (3)0.0452 (3)0.0380 (3)0.0000 (3)0.0072 (3)0.0015 (3)
W70.0377 (4)0.0526 (4)0.0300 (3)0.0058 (3)0.0039 (3)0.0078 (3)
W80.0387 (4)0.0586 (4)0.0349 (4)0.0120 (3)0.0076 (3)0.0000 (3)
W90.0408 (4)0.0576 (4)0.0428 (4)0.0094 (3)0.0112 (3)0.0135 (3)
W100.0401 (4)0.0453 (3)0.0289 (3)0.0024 (3)0.0038 (3)0.0038 (3)
W110.0434 (4)0.0417 (3)0.0403 (4)0.0036 (3)0.0131 (3)0.0010 (3)
W120.0404 (4)0.0391 (3)0.0537 (4)0.0006 (3)0.0014 (3)0.0061 (3)
P10.0372 (19)0.0366 (17)0.0340 (18)0.0035 (19)0.0018 (15)0.0029 (19)
O7A0.048 (11)0.034 (7)0.015 (8)0.014 (8)0.003 (8)0.009 (7)
O8A0.035 (10)0.033 (9)0.029 (7)0.017 (9)0.005 (7)0.004 (7)
O9A0.040 (7)0.038 (10)0.027 (9)0.014 (8)0.005 (7)0.001 (9)
O10A0.018 (8)0.042 (7)0.021 (8)0.006 (7)0.004 (7)0.000 (7)
O7B0.053 (14)0.046 (12)0.022 (10)0.032 (10)0.009 (10)0.006 (9)
O8B0.035 (11)0.042 (11)0.031 (10)0.008 (9)0.005 (9)0.010 (9)
O9B0.055 (14)0.029 (9)0.033 (10)0.002 (10)0.014 (10)0.006 (9)
O10B0.032 (11)0.064 (14)0.017 (9)0.003 (10)0.002 (8)0.017 (9)
O110.072 (10)0.055 (8)0.119 (14)0.016 (8)0.036 (10)0.030 (9)
O120.044 (8)0.122 (13)0.067 (10)0.008 (9)0.011 (7)0.021 (10)
O130.063 (9)0.100 (11)0.044 (8)0.010 (8)0.006 (7)0.014 (7)
O140.050 (9)0.19 (2)0.052 (9)0.035 (11)0.007 (7)0.026 (11)
O150.054 (9)0.183 (19)0.041 (8)0.035 (11)0.015 (7)0.038 (10)
O160.058 (8)0.087 (9)0.037 (7)0.009 (7)0.002 (6)0.012 (7)
O170.068 (10)0.087 (10)0.063 (9)0.019 (8)0.012 (8)0.032 (8)
O180.039 (8)0.054 (7)0.163 (17)0.001 (6)0.029 (9)0.006 (10)
O190.061 (10)0.048 (8)0.141 (17)0.013 (7)0.040 (10)0.010 (9)
O200.064 (10)0.081 (10)0.075 (10)0.032 (8)0.026 (8)0.017 (9)
O210.20 (2)0.066 (9)0.037 (8)0.045 (12)0.024 (11)0.016 (7)
O220.19 (2)0.048 (7)0.025 (6)0.031 (10)0.021 (8)0.001 (6)
O230.087 (12)0.076 (9)0.048 (8)0.000 (9)0.003 (7)0.023 (8)
O240.043 (9)0.170 (18)0.081 (12)0.026 (10)0.013 (8)0.043 (12)
O250.035 (8)0.066 (8)0.147 (16)0.009 (7)0.022 (9)0.036 (10)
O260.063 (10)0.038 (7)0.144 (16)0.003 (6)0.040 (10)0.010 (9)
O270.034 (6)0.065 (8)0.073 (9)0.017 (6)0.006 (6)0.008 (7)
O280.20 (2)0.045 (7)0.025 (6)0.032 (10)0.006 (9)0.003 (6)
O290.177 (19)0.046 (7)0.025 (6)0.007 (9)0.002 (9)0.013 (5)
O300.049 (7)0.044 (6)0.070 (9)0.011 (5)0.010 (6)0.011 (6)
O310.054 (9)0.045 (7)0.114 (13)0.006 (6)0.035 (8)0.003 (8)
O320.176 (19)0.037 (7)0.037 (7)0.022 (9)0.025 (9)0.010 (6)
O330.059 (9)0.108 (11)0.053 (8)0.031 (9)0.022 (7)0.020 (9)
O340.047 (9)0.154 (16)0.099 (13)0.046 (10)0.014 (9)0.081 (12)
O350.062 (10)0.159 (18)0.098 (14)0.032 (11)0.021 (10)0.093 (13)
O360.036 (6)0.083 (9)0.052 (7)0.022 (7)0.005 (6)0.011 (7)
O370.22 (2)0.050 (8)0.037 (8)0.034 (11)0.006 (11)0.006 (6)
O380.056 (10)0.152 (17)0.064 (10)0.025 (10)0.014 (8)0.052 (11)
O390.048 (7)0.072 (8)0.056 (8)0.009 (7)0.006 (6)0.004 (7)
O400.064 (10)0.052 (8)0.122 (15)0.003 (7)0.025 (9)0.035 (9)
O410.117 (15)0.164 (18)0.046 (8)0.079 (14)0.036 (9)0.054 (11)
O420.063 (9)0.078 (10)0.077 (10)0.013 (7)0.015 (8)0.041 (8)
O430.035 (7)0.106 (12)0.101 (12)0.022 (7)0.023 (8)0.059 (10)
O440.043 (7)0.089 (10)0.049 (7)0.023 (7)0.007 (6)0.004 (8)
O450.056 (9)0.090 (10)0.067 (9)0.027 (8)0.019 (7)0.046 (8)
O460.050 (7)0.047 (6)0.070 (8)0.019 (6)0.005 (6)0.013 (7)
O10.060 (8)0.038 (6)0.039 (6)0.008 (5)0.011 (6)0.004 (5)
O20.075 (9)0.046 (6)0.036 (6)0.001 (6)0.017 (6)0.002 (5)
N10.044 (8)0.047 (7)0.033 (7)0.009 (6)0.002 (6)0.002 (6)
N20.044 (8)0.030 (6)0.034 (6)0.004 (5)0.016 (6)0.001 (5)
N30.038 (8)0.040 (7)0.056 (9)0.007 (6)0.004 (7)0.008 (6)
N40.043 (8)0.052 (7)0.019 (6)0.005 (6)0.001 (5)0.008 (6)
C10.044 (10)0.058 (10)0.036 (9)0.003 (8)0.013 (8)0.008 (8)
C20.048 (9)0.041 (8)0.025 (7)0.011 (7)0.002 (7)0.005 (6)
C30.033 (8)0.046 (9)0.037 (8)0.005 (7)0.007 (7)0.002 (7)
C40.052 (11)0.036 (8)0.051 (11)0.007 (7)0.004 (8)0.004 (7)
C50.036 (9)0.043 (8)0.034 (8)0.003 (6)0.009 (7)0.004 (6)
C60.058 (12)0.048 (9)0.039 (9)0.005 (8)0.005 (8)0.004 (8)
C70.062 (12)0.044 (9)0.044 (9)0.009 (8)0.016 (9)0.009 (7)
O30.045 (7)0.061 (7)0.042 (6)0.016 (6)0.011 (5)0.009 (6)
O40.078 (10)0.050 (7)0.055 (8)0.013 (7)0.006 (7)0.002 (6)
N50.041 (8)0.060 (8)0.030 (7)0.003 (7)0.008 (6)0.011 (6)
N60.028 (7)0.045 (7)0.049 (8)0.006 (6)0.002 (6)0.001 (6)
N70.037 (8)0.062 (9)0.043 (8)0.010 (7)0.002 (6)0.007 (7)
N80.041 (8)0.046 (8)0.034 (7)0.005 (6)0.008 (6)0.003 (6)
C80.046 (9)0.037 (8)0.038 (8)0.011 (7)0.006 (7)0.016 (7)
C90.030 (8)0.045 (8)0.031 (8)0.004 (6)0.010 (6)0.010 (6)
C100.028 (8)0.090 (13)0.010 (6)0.001 (8)0.004 (6)0.002 (7)
C110.034 (9)0.064 (11)0.038 (9)0.000 (8)0.005 (7)0.006 (8)
C120.023 (7)0.046 (8)0.041 (9)0.003 (6)0.013 (7)0.017 (7)
C130.051 (11)0.063 (11)0.042 (10)0.015 (9)0.007 (8)0.011 (8)
C140.043 (10)0.058 (10)0.062 (12)0.006 (8)0.002 (9)0.028 (9)
O50.066 (9)0.070 (8)0.044 (7)0.006 (7)0.012 (6)0.000 (6)
O60.046 (7)0.057 (7)0.051 (7)0.007 (6)0.006 (6)0.004 (6)
N90.052 (9)0.035 (7)0.040 (8)0.003 (6)0.004 (6)0.002 (6)
N100.051 (9)0.053 (9)0.061 (10)0.004 (7)0.008 (8)0.005 (8)
N110.043 (8)0.033 (7)0.056 (9)0.007 (6)0.019 (7)0.013 (6)
N120.049 (9)0.046 (8)0.045 (8)0.006 (6)0.009 (7)0.008 (6)
C150.042 (11)0.050 (10)0.081 (15)0.005 (8)0.001 (10)0.002 (10)
C160.028 (8)0.055 (9)0.039 (9)0.006 (7)0.002 (7)0.016 (8)
C170.069 (13)0.045 (10)0.048 (11)0.014 (9)0.004 (10)0.018 (8)
C180.043 (9)0.031 (7)0.052 (10)0.006 (7)0.008 (8)0.003 (7)
C190.036 (8)0.034 (8)0.050 (9)0.004 (6)0.002 (7)0.015 (7)
C200.071 (14)0.056 (11)0.059 (12)0.014 (10)0.008 (11)0.017 (10)
C210.064 (13)0.055 (10)0.046 (10)0.007 (9)0.016 (9)0.016 (8)
Geometric parameters (Å, º) top
W1—O111.673 (14)P1—O9A1.58 (2)
W1—O121.875 (15)P1—O10B1.59 (2)
W1—O151.881 (15)O1—C31.23 (2)
W1—O131.888 (15)O2—C41.21 (2)
W1—O141.896 (16)N1—C51.35 (2)
W1—O7A2.424 (19)N1—C11.37 (2)
W2—O161.668 (13)N1—H1N0.8700
W2—O121.875 (16)N2—C11.33 (2)
W2—O181.881 (15)N2—C21.403 (19)
W2—O171.903 (16)N2—C61.46 (2)
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O32—W11—O8B60.9 (8)C22—C23—H23A109.5
O44—W11—O10A160.0 (7)C22—C23—H23B109.5
O28—W11—O10A90.2 (8)H23A—C23—H23B109.5
O45—W11—O10A64.8 (7)C22—C23—H23C109.5
O42—W11—O10A64.5 (7)H23A—C23—H23C109.5
O32—W11—O10A92.0 (8)H23B—C23—H23C109.5
O46—W12—O38101.4 (8)C24—O48—H2O107.5
O46—W12—O34100.7 (8)C25—C24—O48112.5 (11)
O38—W12—O3487.8 (7)C25—C24—H24A109.1
O46—W12—O45101.3 (7)O48—C24—H24A109.1
O38—W12—O45157.3 (8)C25—C24—H24B109.1
O34—W12—O4587.9 (7)O48—C24—H24B108.0
O46—W12—O43103.2 (7)H24A—C24—H24B107.8
O38—W12—O4387.0 (7)C24—C25—H25A109.5
O34—W12—O43156.1 (8)C24—C25—H25B109.5
O45—W12—O4388.0 (6)H25A—C25—H25B109.5
O46—W12—O10B158.1 (7)C24—C25—H25C109.5
O38—W12—O10B64.9 (8)H25A—C25—H25C109.5
O34—W12—O10B63.3 (7)H25B—C25—H25C109.5
O10A—P1—O7A—W1178.3 (12)O29—W5—O28—W1147 (2)
O8A—P1—O7A—W157.4 (16)O7A—W5—O28—W1145 (2)
O9A—P1—O7A—W159.1 (15)O8B—W5—O28—W1110.9 (17)
O10A—P1—O7A—W458.1 (14)O30—W6—O29—W5152.2 (16)
O8A—P1—O7A—W4179.0 (11)O19—W6—O29—W5103.7 (18)
O9A—P1—O7A—W464.5 (13)O32—W6—O29—W551.3 (17)
O10A—P1—O7A—W557.4 (14)O31—W6—O29—W524 (3)
O8A—P1—O7A—W563.5 (13)O8B—W6—O29—W58.5 (15)
O9A—P1—O7A—W5180.0 (11)O8A—W6—O29—W540.5 (17)
O10A—P1—O8A—W2179.0 (11)O33—W7—O31—W6154.3 (14)
O7A—P1—O8A—W257.6 (15)O18—W7—O31—W651.1 (15)
O9A—P1—O8A—W257.4 (16)O34—W7—O31—W6105.4 (15)
O10A—P1—O8A—W760.4 (13)O35—W7—O31—W628 (2)
O7A—P1—O8A—W7178.1 (11)O10B—W7—O31—W643.6 (15)
O9A—P1—O8A—W763.2 (13)O8A—W7—O31—W69.9 (12)
O10A—P1—O8A—W658.0 (15)O30—W6—O32—W11154.5 (15)
O7A—P1—O8A—W663.5 (14)O29—W6—O32—W1150.9 (16)
O9A—P1—O8A—W6178.4 (11)O19—W6—O32—W1129 (2)
O10A—P1—O9A—W3179.4 (11)O31—W6—O32—W11104.4 (16)
O8A—P1—O9A—W357.4 (15)O8B—W6—O32—W1110.7 (14)
O7A—P1—O9A—W359.0 (14)O8A—W6—O32—W1140.2 (15)
O10A—P1—O9A—W956.3 (15)O46—W12—O34—W7156.1 (16)
O8A—P1—O9A—W9178.3 (11)O38—W12—O34—W754.9 (17)
O7A—P1—O9A—W965.3 (14)O45—W12—O34—W7102.9 (17)
O10A—P1—O9A—W858.6 (14)O43—W12—O34—W723 (3)
O8A—P1—O9A—W863.4 (14)O10B—W12—O34—W78.1 (14)
O7A—P1—O9A—W8179.8 (11)O10A—W12—O34—W739.4 (17)
O8A—P1—O10A—W1159.0 (15)O36—W8—O35—W7152.6 (18)
O7A—P1—O10A—W1161.0 (14)O22—W8—O35—W7104.6 (19)
O9A—P1—O10A—W11179.8 (11)O37—W8—O35—W731 (3)
O8A—P1—O10A—W10179.0 (11)O38—W8—O35—W751.3 (19)
O7A—P1—O10A—W1061.1 (13)O9A—W8—O35—W743.3 (19)
O9A—P1—O10A—W1057.8 (14)O10B—W8—O35—W78.1 (16)
O8A—P1—O10A—W1261.6 (14)O39—W9—O37—W8157.3 (19)
O7A—P1—O10A—W12178.4 (11)O21—W9—O37—W855.8 (19)
O9A—P1—O10A—W1259.6 (14)O26—W9—O37—W820 (3)
O9B—P1—O7B—W2179.0 (14)O40—W9—O37—W8100 (2)
O8A—P1—O7B—W20.1 (14)O9A—W9—O37—W84.9 (17)
O8B—P1—O7B—W256.2 (18)O9B—W9—O37—W838 (2)
O10B—P1—O7B—W259.3 (19)O36—W8—O37—W9157.9 (18)
O9B—P1—O7B—W358.3 (16)O35—W8—O37—W919 (3)
O8A—P1—O7B—W3120.7 (16)O22—W8—O37—W955 (2)
O8B—P1—O7B—W3177.0 (11)O38—W8—O37—W9101 (2)
O10B—P1—O7B—W361.4 (15)O9A—W8—O37—W94.8 (16)
O7B—P1—O8B—W655.1 (16)O10B—W8—O37—W939 (2)
O9B—P1—O8B—W6179.7 (12)O46—W12—O38—W8154.4 (16)
O10B—P1—O8B—W664.4 (16)O34—W12—O38—W853.9 (17)
O7B—P1—O8B—W11177.4 (11)O45—W12—O38—W825 (3)
O9B—P1—O8B—W1152.1 (15)O43—W12—O38—W8102.7 (17)
O10B—P1—O8B—W1163.2 (14)O10B—W12—O38—W87.5 (14)
O7B—P1—O8B—W563.0 (14)O10A—W12—O38—W838.9 (17)
O9B—P1—O8B—W562.2 (15)O41—W10—O40—W9155.5 (15)
O10B—P1—O8B—W5177.6 (11)O43—W10—O40—W9102.8 (15)
O7B—P1—O9B—W10179.1 (14)O25—W10—O40—W953.9 (14)
O8B—P1—O9B—W1055.2 (17)O42—W10—O40—W924 (2)
O10B—P1—O9B—W1058.9 (17)O9B—W10—O40—W99.5 (12)
O7B—P1—O9B—W956.0 (17)O10A—W10—O40—W938.4 (14)
O10A—P1—O9B—W9124.8 (15)O44—W11—O42—W10155.1 (12)
O8B—P1—O9B—W9179.9 (11)O28—W11—O42—W10101.4 (14)
O10B—P1—O9B—W966.0 (15)O45—W11—O42—W1053.8 (13)
O7B—P1—O10B—W12179.4 (14)O32—W11—O42—W1026 (2)
O9B—P1—O10B—W1256.5 (16)O8B—W11—O42—W1038.8 (13)
O8B—P1—O10B—W1262.0 (15)O10A—W11—O42—W109.3 (11)
O7B—P1—O10B—W756.2 (16)O41—W10—O43—W12152.1 (16)
O9B—P1—O10B—W7179.1 (12)O40—W10—O43—W12105.1 (16)
O8B—P1—O10B—W762.4 (15)O25—W10—O43—W1230 (2)
O7B—P1—O10B—W858.6 (16)O42—W10—O43—W1251.8 (15)
O9B—P1—O10B—W864.3 (15)O9B—W10—O43—W1240.9 (15)
O8B—P1—O10B—W8177.2 (12)O10A—W10—O43—W129.6 (13)
O16—W2—O12—W1152.1 (16)O44—W11—O45—W12156.5 (14)
O18—W2—O12—W132 (3)O28—W11—O45—W1221 (3)
O17—W2—O12—W148.6 (16)O42—W11—O45—W1254.7 (15)
O19—W2—O12—W1106.8 (17)O32—W11—O45—W12101.2 (15)
O8A—W2—O12—W143.7 (16)O8B—W11—O45—W1240.4 (15)
O7B—W2—O12—W113.9 (14)O10A—W11—O45—W128.1 (12)
O11—W1—O12—W2150.0 (16)O46—W12—O45—W11157.1 (14)
O15—W1—O12—W2106.8 (17)O38—W12—O45—W1123 (3)
O13—W1—O12—W248.9 (16)O34—W12—O45—W11102.5 (15)
O14—W1—O12—W228 (3)O43—W12—O45—W1154.0 (15)
O7A—W1—O12—W243.5 (17)O10B—W12—O45—W1139.3 (15)
O11—W1—O13—W3154.9 (14)O10A—W12—O45—W118.0 (12)
O12—W1—O13—W350.7 (14)C2—N2—C1—N11 (2)
O15—W1—O13—W327 (2)C6—N2—C1—N1175.5 (15)
O14—W1—O13—W3103.5 (15)C5—N1—C1—N21 (2)
O7A—W1—O13—W340.2 (13)C1—N2—C2—C51.5 (19)
O11—W1—O14—W4155.1 (17)C6—N2—C2—C5175.3 (16)
O12—W1—O14—W426 (3)C1—N2—C2—C3175.1 (19)
O15—W1—O14—W451.9 (17)C6—N2—C2—C31 (3)
O13—W1—O14—W4104.0 (17)C4—N3—C3—O1178.1 (16)
O7A—W1—O14—W49.6 (15)C4—N3—C3—C21 (3)
O11—W1—O15—W5155.9 (16)C5—C2—C3—O1176.7 (17)
O12—W1—O15—W599.9 (16)N2—C2—C3—O11 (3)
O13—W1—O15—W522 (3)C5—C2—C3—N30 (2)
O14—W1—O15—W554.2 (17)N2—C2—C3—N3175.9 (17)
O7A—W1—O15—W57.5 (13)C3—N3—C4—O2179.5 (18)
O27—W5—O15—W1155.5 (15)C3—N3—C4—N41 (3)
O24—W5—O15—W155.1 (17)C5—N4—C4—O2178.0 (16)
O28—W5—O15—W122 (3)C7—N4—C4—O29 (3)
O29—W5—O15—W1100.7 (16)C5—N4—C4—N31 (2)
O7A—W5—O15—W17.4 (13)C7—N4—C4—N3172.7 (15)
O8B—W5—O15—W140.4 (16)C1—N1—C5—N4177.3 (17)
O20—W3—O17—W2153.1 (14)C1—N1—C5—C20 (2)
O22—W3—O17—W2102.8 (15)C4—N4—C5—N1175.2 (16)
O21—W3—O17—W228 (2)C7—N4—C5—N111 (3)
O13—W3—O17—W252.6 (14)C4—N4—C5—C22 (2)
O9A—W3—O17—W239.9 (14)C7—N4—C5—C2171.8 (16)
O7B—W3—O17—W210.6 (12)N2—C2—C5—N10.9 (19)
O16—W2—O18—W7154.7 (15)C3—C2—C5—N1176.1 (15)
O12—W2—O18—W721 (3)N2—C2—C5—N4178.3 (15)
O17—W2—O18—W7101.7 (16)C3—C2—C5—N41 (3)
O19—W2—O18—W754.3 (16)C9—N6—C8—N51.6 (19)
O8A—W2—O18—W78.1 (14)C13—N6—C8—N5175.8 (15)
O7B—W2—O18—W737.4 (16)C12—N5—C8—N61.1 (19)
O33—W7—O18—W2156.9 (15)C8—N6—C9—C121.3 (18)
O31—W7—O18—W254.8 (16)C13—N6—C9—C12175.4 (15)
O34—W7—O18—W223 (3)C8—N6—C9—C10176.4 (16)
O35—W7—O18—W2101.5 (17)C13—N6—C9—C102 (3)
O10B—W7—O18—W238.5 (16)C11—N7—C10—O3172.1 (17)
O8A—W7—O18—W28.1 (14)C11—N7—C10—C94 (2)
O30—W6—O19—W2157.0 (15)C12—C9—C10—O3176.0 (15)
O29—W6—O19—W298.9 (16)N6—C9—C10—O37 (3)
O32—W6—O19—W220 (3)C12—C9—C10—N70 (2)
O31—W6—O19—W255.9 (16)N6—C9—C10—N7177.2 (16)
O8B—W6—O19—W235.6 (16)C10—N7—C11—O4177.9 (17)
O8A—W6—O19—W26.8 (14)C10—N7—C11—N85 (3)
O39—W9—O21—W3155.7 (17)C12—N8—C11—O4178.6 (16)
O37—W9—O21—W355.4 (18)C14—N8—C11—O410 (3)
O26—W9—O21—W3101.4 (18)C12—N8—C11—N72 (2)
O40—W9—O21—W325 (3)C14—N8—C11—N7173.1 (15)
O9A—W9—O21—W38.1 (15)C8—N5—C12—C90.3 (18)
O9B—W9—O21—W337.3 (18)C8—N5—C12—N8179.7 (15)
O36—W8—O22—W3154.0 (15)N6—C9—C12—N50.6 (17)
O35—W8—O22—W3103.7 (17)C10—C9—C12—N5177.5 (13)
O37—W8—O22—W353.2 (17)N6—C9—C12—N8179.4 (14)
O38—W8—O22—W326 (3)C10—C9—C12—N83 (2)
O9A—W8—O22—W38.9 (14)C11—N8—C12—N5178.2 (15)
O10B—W8—O22—W341.1 (16)C14—N8—C12—N510 (2)
O20—W3—O22—W8153.4 (16)C11—N8—C12—C92 (2)
O17—W3—O22—W8104.0 (17)C14—N8—C12—C9169.6 (15)
O21—W3—O22—W852.2 (17)C19—N9—C15—N101 (2)
O13—W3—O22—W826 (3)C16—N10—C15—N91 (2)
O9A—W3—O22—W89.1 (14)C20—N10—C15—N9179.8 (17)
O7B—W3—O22—W839.7 (16)C15—N10—C16—C191 (2)
O27—W5—O24—W4155.0 (17)C20—N10—C16—C19179.2 (18)
O28—W5—O24—W4101.3 (19)C15—N10—C16—C17180.0 (18)
O15—W5—O24—W452.8 (19)C20—N10—C16—C172 (3)
O29—W5—O24—W427 (3)C18—N11—C17—O5173.9 (17)
O7A—W5—O24—W47.2 (15)C18—N11—C17—C167 (2)
O8B—W5—O24—W440.9 (19)C19—C16—C17—O5179 (2)
O41—W10—O25—W4157.1 (15)N10—C16—C17—O50 (3)
O40—W10—O25—W454.2 (15)C19—C16—C17—N112 (2)
O43—W10—O25—W421 (2)N10—C16—C17—N11178.7 (16)
O42—W10—O25—W4102.7 (15)C19—N12—C18—O6179.6 (15)
O9B—W10—O25—W48.8 (13)C21—N12—C18—O67 (3)
O10A—W10—O25—W439.2 (14)C19—N12—C18—N112 (2)
O23—W4—O26—W9154.1 (16)C21—N12—C18—N11174.4 (16)
O25—W4—O26—W953.0 (17)C17—N11—C18—O6174.7 (16)
O14—W4—O26—W9103.9 (18)C17—N11—C18—N127 (3)
O24—W4—O26—W923 (3)N10—C16—C19—N90.1 (19)
O7A—W4—O26—W941.2 (17)C17—C16—C19—N9179.3 (16)
O44—W11—O28—W5149.6 (19)N10—C16—C19—N12177.5 (15)
O45—W11—O28—W533 (3)C17—C16—C19—N122 (3)
O42—W11—O28—W5109 (2)C15—N9—C19—C161 (2)
O32—W11—O28—W547 (2)C15—N9—C19—N12178.3 (16)
O8B—W11—O28—W511.1 (17)C18—N12—C19—C162 (3)
O10A—W11—O28—W544.6 (19)C21—N12—C19—C16170.1 (18)
O27—W5—O28—W11150.5 (19)C18—N12—C19—N9179.0 (16)
O24—W5—O28—W11109 (2)C21—N12—C19—N97 (3)
O15—W5—O28—W1132 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1N···O3i0.872.042.776 (18)142
N1—H1N···O36ii0.872.512.965 (18)113
N3—H3N···O1iii0.871.972.835 (18)177
N5—H5N···O6ii0.871.952.738 (19)149
N7—H7N···O30iv0.872.092.95 (2)171
N9—H9N···O470.871.782.62 (2)161
N11—H11N···O44v0.872.002.822 (19)156
O47—H1O···O40.851.862.71 (2)180
O48—H2O···O23vi0.852.293.13 (7)171
C1—H1···O5ii0.942.283.08 (2)144
C1—H1···O36ii0.942.382.91 (2)116
C8—H8···O39ii0.942.222.93 (2)132
C8—H8···O2vii0.942.483.12 (2)125
C15—H15···O27viii0.942.103.02 (2)165
C7—H7B···O3i0.972.393.22 (2)143
C7—H7C···O310.972.693.47 (2)138
C13—H13B···O240.972.593.35 (3)135
C13—H13C···O1ix0.972.503.13 (2)123
C14—H14B···O6ii0.972.673.44 (2)136
C14—H14B···O16vii0.972.673.33 (2)125
C20—H20B···O26vi0.972.393.29 (2)154
C20—H20C···O460.972.443.01 (2)117
C21—H21A···O470.972.633.57 (3)164
C21—H21B···O16iv0.972.473.44 (3)173
C21—H21C···O410.972.573.14 (3)117
C22—H22A···O20vi0.982.443.20 (3)134
C22—H22B···O15viii0.982.643.46 (3)142
C23—H23A···O19viii0.972.563.43 (4)148
C23—H23C···O40.972.683.33 (4)125
C24—H24A···O50.982.183.12 (9)159
C24—H24B···O3x0.982.593.48 (8)152
C25—H25A···O380.972.593.43 (6)145
Symmetry codes: (i) x1/2, y+1/2, z+1/2; (ii) x1, y, z; (iii) x+1, y+1, z+1; (iv) x+1/2, y+1/2, z1/2; (v) x+1, y, z; (vi) x+3/2, y+1/2, z+1/2; (vii) x1/2, y+1/2, z1/2; (viii) x+1/2, y+1/2, z+1/2; (ix) x+1/2, y1/2, z+1/2; (x) x+1/2, y+1/2, z+1/2.
Geometry of anion···π interactions (Å, °) for (1) and (2) top
CationFaceaShortest contactsO···plane distancesφ
C···ON···OCH3···ORangeMean
(HCaf)4(SiW12O40).3H2O, (1)
AO13/O34/O43/O482.99 (3)2.97 (3)3.33 (3)2.45 (5)–3.45 (3)2.94 (5)3.4 (8)
(O22/O26/O40/O42)iii3.26 (4)3.26 (3)3.08 (4)2.56 (4)–3.57 (3)3.05 (4)3.4 (8)
BO18/O22/O43/O462.93 (4)3.23 (4)3.14 (3)2.45 (4)–3.64 (2)3.02 (4)5.7 (9)
(O30/O34/O37/O42)iv2.93 (4)3.09 (4)3.26 (3)2.23 (5)–3.32 (3)2.84 (5)5.6 (9)
CO13/O14/O15/O18/O20b3.00 (4)3.05 (3)3.00 (4)2.71 (4)–3.01 (2)2.87 (4)2.3 (8)
DO26/O27/O29/O30/O32b2.98 (4)3.12 (3)2.99 (4)2.53 (4)–3.34 (2)2.87 (4)9.5 (8)
(HTbr)3(PW12O40).1.5H2O, (2)
AO30/O33/O44/O462.86 (2)3.06 (2)3.42 (2)2.45 (2)–3.29 (2)2.91 (2)3.5 (6)
BO23/O27/O41/O442.83 (2)2.97 (2)3.35 (3)2.36 (2)–3.304 (18)2.86 (2)4.9 (4)
(O16/O20/O33/O36)vii2.86 (2)2.856 (19)3.33 (2)2.32 (2)–3.331 (19)2.88 (2)5.0 (4)
CO36/O39/O41/O463.24 (2)2.95 (2)3.01 (2)2.41 (3)–3.322 (17)2.91 (2)5.2 (6)
(O11/O20/O23/O39)vi3.20 (2)3.13 (2)3.29 (2)2.24 (3)–3.33 (2)2.87 (2)6.8 (5)
Notes: (a) the face of the anion if defined by four terminal O atoms; O···plane is the distance between the anion O atoms and the mean plane of the cations; φ is an angle subtended by the mean planes of the cation and the square face of the stacked anion. (b) Only two of the four WO6 octahedra are considered as components of the stack. For details, see Fig. 6.

Symmetry codes for (1): (iii) x-1/2, y-1/2, z; (iv) x-1/2, y+1/2, z; for (2): (vi) -x+3/2, y+1/2, -z+1/2; (vii) x-1/2, -y+1/2, z-1/2.
 

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