Supra­molecular networks supported by the anion...π linkage of Keggin-type heteropolyoxotungstates

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.

Computing details

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)

Crystal data

(C8H11N4O2)4[SiW12O40]·3H2O	F(000) = 6656
Mr = 3709.17	Dx = 3.599 Mg m^−3
Monoclinic, Cc	Mo Kα radiation, λ = 0.71073 Å
a = 15.8623 (4) Å	Cell parameters from 34632 reflections
b = 20.7547 (6) Å	θ = 1.7–26.7°
c = 21.8096 (6) Å	µ = 20.21 mm^−1
β = 107.576 (2)°	T = 173 K
V = 6844.9 (3) Å^3	Prism, yellow
Z = 4	0.22 × 0.18 × 0.16 mm

Data collection

Stoe Image plate diffraction system diffractometer	8741 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.026
φ oscillation scans	θmax = 26.7°, θmin = 1.7°
Absorption correction: numerical [X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)]	h = −20→13
Tmin = 0.093, Tmax = 0.229	k = −26→20
34632 measured reflections	l = −18→27
9899 independent reflections

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.048	H-atom parameters constrained
wR(F^2) = 0.134	w = 1/[σ^2(Fo^2) + (0.082P)^2 + 63.609P] where P = (Fo^2 + 2Fc^2)/3
S = 1.08	(Δ/σ)max = 0.002
9899 reflections	Δρmax = 1.35 e Å^−3
1005 parameters	Δρmin = −1.78 e Å^−3
58 restraints	Absolute structure: Refined as an inversion twin.
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.40 (3)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Si1	0.7944 (5)	0.3311 (2)	0.3131 (4)	0.0293 (8)
W1	0.71419 (7)	0.24737 (6)	0.42543 (5)	0.0480 (3)
W2	0.71032 (8)	0.41281 (6)	0.42495 (6)	0.0517 (3)
W3	0.79091 (11)	0.50068 (4)	0.31011 (8)	0.0474 (2)
W4	0.86828 (9)	0.42007 (6)	0.20156 (6)	0.0538 (3)
W5	0.87172 (8)	0.24501 (6)	0.20199 (6)	0.0476 (3)
W6	0.79614 (10)	0.16069 (4)	0.31078 (8)	0.0450 (2)
W7	0.94789 (8)	0.24935 (6)	0.44035 (6)	0.0482 (3)
W8	0.94526 (7)	0.41510 (6)	0.44146 (6)	0.0463 (3)
W9	1.02266 (9)	0.33469 (6)	0.33240 (7)	0.0512 (3)
W10	0.56781 (9)	0.32931 (6)	0.30257 (7)	0.0509 (3)
W11	0.64701 (8)	0.41751 (6)	0.18641 (6)	0.0486 (3)
W12	0.64993 (7)	0.24268 (6)	0.18755 (5)	0.0466 (3)
O9	0.7235 (11)	0.3299 (8)	0.3547 (7)	0.040 (3)
O10	0.7786 (10)	0.3938 (8)	0.2713 (7)	0.040 (3)
O11	0.7822 (11)	0.2686 (7)	0.2703 (8)	0.039 (3)
O12	0.8910 (11)	0.3321 (7)	0.3645 (7)	0.039 (3)
O13	0.6854 (14)	0.2013 (12)	0.4811 (10)	0.058 (6)
O14	0.7031 (12)	0.3294 (8)	0.4673 (10)	0.049 (4)
O15	0.8372 (13)	0.2541 (10)	0.4552 (9)	0.050 (4)
O16	0.7287 (15)	0.1898 (13)	0.3643 (13)	0.072 (7)
O17	0.5949 (13)	0.2641 (8)	0.3721 (9)	0.049 (4)
O18	0.6842 (13)	0.4609 (12)	0.4800 (9)	0.052 (5)
O19	0.7239 (11)	0.4676 (8)	0.3607 (8)	0.044 (4)
O20	0.8356 (15)	0.4148 (16)	0.4585 (13)	0.080 (9)
O21	0.5883 (13)	0.3918 (9)	0.3710 (10)	0.052 (4)
O22	0.7942 (17)	0.5818 (7)	0.3209 (16)	0.064 (6)
O23	0.8550 (13)	0.4984 (9)	0.2467 (9)	0.051 (4)
O24	0.8920 (13)	0.4712 (12)	0.3764 (13)	0.065 (6)
O25	0.6841 (16)	0.4940 (12)	0.2396 (12)	0.068 (7)
O26	0.9131 (15)	0.4560 (10)	0.1503 (11)	0.053 (5)
O27	0.8547 (13)	0.3334 (8)	0.1789 (10)	0.054 (5)
O28	0.9660 (14)	0.3971 (8)	0.2713 (9)	0.056 (5)
O29	0.747 (2)	0.4258 (16)	0.1558 (13)	0.091 (11)
O30	0.9140 (18)	0.2109 (13)	0.1494 (10)	0.067 (7)
O31	0.8621 (14)	0.1696 (11)	0.2513 (12)	0.061 (6)
O32	0.9634 (12)	0.2723 (9)	0.2724 (9)	0.046 (4)
O33	0.7467 (12)	0.2318 (9)	0.1529 (9)	0.046 (4)
O34	0.8007 (17)	0.0795 (6)	0.3205 (14)	0.055 (5)
O35	0.8980 (12)	0.1931 (10)	0.3742 (9)	0.049 (4)
O36	0.6910 (14)	0.1656 (10)	0.2382 (10)	0.056 (5)
O37	1.0155 (13)	0.2056 (10)	0.5031 (10)	0.051 (5)
O38	0.9761 (16)	0.3351 (9)	0.4857 (10)	0.056 (5)
O39	1.0362 (13)	0.2720 (8)	0.4019 (8)	0.048 (4)
O40	0.9999 (13)	0.4627 (12)	0.5009 (11)	0.061 (6)
O41	1.0334 (12)	0.3972 (8)	0.3996 (10)	0.046 (4)
O42	1.1299 (14)	0.3354 (9)	0.3310 (12)	0.052 (5)
O43	0.4572 (12)	0.3260 (8)	0.2842 (10)	0.043 (4)
O44	0.5934 (12)	0.3920 (10)	0.2485 (12)	0.056 (5)
O45	0.5950 (12)	0.2670 (8)	0.2507 (8)	0.046 (4)
O46	0.5643 (14)	0.4503 (10)	0.1237 (10)	0.056 (5)
O47	0.6498 (14)	0.3308 (7)	0.1666 (9)	0.046 (4)
O48	0.5707 (15)	0.2115 (10)	0.1252 (9)	0.051 (5)
O1	0.6181 (19)	0.3029 (14)	0.6376 (16)	0.084 (9)
O2	0.7493 (17)	0.1109 (9)	0.6190 (11)	0.060 (5)
N1	0.8868 (17)	0.3083 (13)	0.5979 (10)	0.049 (5)
H1N	0.936281	0.297502	0.590109	0.074*
N2	0.773 (2)	0.3639 (14)	0.6095 (12)	0.067 (8)
N3	0.6867 (18)	0.2067 (12)	0.6277 (12)	0.049 (5)
N4	0.8279 (18)	0.2040 (14)	0.6116 (11)	0.053 (6)
C1	0.855 (2)	0.3680 (17)	0.6013 (14)	0.055 (6)
H1	0.885073	0.406921	0.598426	0.066*
C2	0.755 (2)	0.3033 (15)	0.6174 (14)	0.052 (6)
C3	0.680 (2)	0.2716 (16)	0.6302 (14)	0.068 (10)
C4	0.748 (2)	0.1702 (10)	0.6220 (15)	0.057 (8)
C5	0.8217 (19)	0.2662 (13)	0.6100 (13)	0.048 (6)
C6	0.719 (3)	0.4212 (12)	0.6176 (17)	0.080 (13)
H6A	0.747692	0.460653	0.608692	0.121*
H6B	0.659537	0.418031	0.587574	0.121*
H6C	0.716410	0.422524	0.661798	0.121*
C7	0.607 (2)	0.1687 (15)	0.639 (2)	0.070 (10)
H7A	0.562155	0.199315	0.643526	0.105*
H7B	0.581583	0.139758	0.603177	0.105*
H7C	0.628530	0.143481	0.679154	0.105*
C8	0.898 (2)	0.1647 (14)	0.6010 (19)	0.064 (9)
H8A	0.885512	0.119047	0.605263	0.095*
H8B	0.902457	0.172783	0.557689	0.095*
H8C	0.954761	0.175875	0.632897	0.095*
O3	0.5026 (19)	0.1005 (13)	0.1850 (11)	0.071 (7)
O4	0.6960 (17)	−0.0595 (10)	0.2636 (11)	0.059 (6)
N5	0.595 (2)	0.0678 (14)	0.4063 (12)	0.065 (8)
H5N	0.625470	0.056013	0.445583	0.097*
N6	0.5006 (17)	0.1215 (12)	0.3255 (14)	0.060 (6)
N7	0.6024 (16)	0.0216 (10)	0.2275 (11)	0.044 (5)
N8	0.6580 (16)	−0.0047 (11)	0.3375 (12)	0.045 (5)
C9	0.531 (2)	0.1139 (17)	0.387 (2)	0.069 (10)
H9	0.510163	0.138128	0.416848	0.083*
C10	0.544 (2)	0.0803 (13)	0.3005 (14)	0.051 (6)
C11	0.545 (2)	0.0678 (14)	0.2312 (12)	0.057 (7)
C12	0.6536 (17)	−0.0161 (12)	0.2795 (17)	0.062 (9)
C13	0.601 (2)	0.0442 (15)	0.3479 (12)	0.050 (6)
C14	0.432 (2)	0.1668 (11)	0.2856 (16)	0.061 (8)
H14A	0.425066	0.159747	0.239925	0.092*
H14B	0.375392	0.158891	0.293802	0.092*
H14C	0.450546	0.211370	0.297084	0.092*
C15	0.613 (3)	0.016 (2)	0.1640 (19)	0.096 (16)
H15A	0.655316	−0.018139	0.163979	0.144*
H15B	0.555713	0.005968	0.132685	0.144*
H15C	0.634823	0.057132	0.152300	0.144*
C16	0.715 (3)	−0.039 (2)	0.3962 (14)	0.080 (12)
H16A	0.705162	−0.020107	0.434717	0.120*
H16B	0.699618	−0.084676	0.393576	0.120*
H16C	0.777339	−0.033913	0.398538	0.120*
O5	0.9720 (16)	0.3069 (12)	−0.0124 (15)	0.072 (7)
O6	0.8457 (15)	0.1135 (9)	0.0047 (10)	0.053 (5)
N9	0.7074 (17)	0.3086 (14)	0.0243 (13)	0.055 (6)
H9N	0.655163	0.297673	0.027251	0.082*
N10	0.8081 (17)	0.3693 (10)	0.0127 (12)	0.048 (5)
N11	0.9076 (17)	0.2099 (13)	−0.0079 (13)	0.051 (6)
N12	0.7687 (15)	0.2010 (11)	0.0142 (11)	0.042 (5)
C17	0.739 (3)	0.3699 (18)	0.0279 (18)	0.073 (11)
H17	0.711839	0.406848	0.039936	0.088*
C18	0.827 (2)	0.3024 (13)	0.0077 (14)	0.055 (8)
C19	0.9071 (17)	0.2795 (14)	−0.0044 (17)	0.055 (7)
C20	0.835 (2)	0.1721 (9)	0.0070 (13)	0.052 (7)
C21	0.763 (2)	0.2704 (14)	0.0161 (11)	0.046 (6)
C22	0.857 (2)	0.4285 (15)	0.0039 (18)	0.068 (9)
H22A	0.909946	0.415928	−0.007978	0.102*
H22B	0.819037	0.455332	−0.030207	0.102*
H22C	0.875526	0.453006	0.044210	0.102*
C23	0.978 (3)	0.1817 (17)	−0.021 (2)	0.068 (9)
H23A	0.970373	0.134742	−0.022453	0.102*
H23B	0.980340	0.196655	−0.063452	0.102*
H23C	1.032579	0.193268	0.011755	0.102*
C24	0.696 (3)	0.165 (2)	0.0255 (16)	0.081 (13)
H24A	0.650637	0.195041	0.029826	0.121*
H24B	0.670718	0.136012	−0.010875	0.121*
H24C	0.718270	0.139723	0.065027	0.121*
O7	0.5900 (16)	0.6051 (11)	0.4333 (12)	0.067 (7)
O8	0.3918 (15)	0.4368 (10)	0.3577 (12)	0.060 (5)
N13	0.495 (2)	0.5640 (15)	0.2178 (17)	0.067 (8)
H13N	0.468286	0.548286	0.179347	0.100*
N14	0.5782 (16)	0.6269 (13)	0.2931 (17)	0.065 (6)
N15	0.4899 (17)	0.5258 (16)	0.3919 (15)	0.064 (7)
N16	0.4416 (19)	0.4989 (12)	0.2836 (12)	0.051 (6)
C25	0.554 (3)	0.615 (2)	0.232 (2)	0.078 (13)
H25	0.573327	0.638339	0.201116	0.093*
C26	0.541 (2)	0.5802 (17)	0.325 (2)	0.065 (6)
C27	0.5489 (17)	0.5746 (12)	0.3849 (12)	0.048 (6)
C28	0.439 (2)	0.4811 (13)	0.3504 (15)	0.055 (7)
C29	0.4868 (19)	0.5426 (15)	0.2741 (19)	0.060 (8)
C30	0.6431 (16)	0.6790 (12)	0.3229 (19)	0.067 (8)
H30A	0.652605	0.680006	0.369413	0.100*
H30B	0.699413	0.670467	0.314513	0.100*
H30C	0.619820	0.720724	0.304195	0.100*
C31	0.482 (2)	0.5150 (17)	0.4614 (16)	0.071 (10)
H31A	0.518525	0.547011	0.490763	0.106*
H31B	0.420479	0.519494	0.460444	0.106*
H31C	0.503357	0.471610	0.476255	0.106*
C32	0.3735 (17)	0.4645 (13)	0.2345 (14)	0.046 (6)
H32A	0.346977	0.431477	0.254974	0.070*
H32B	0.327720	0.494994	0.211344	0.070*
H32C	0.399969	0.444085	0.204240	0.070*
O1W	0.667 (3)	0.0244 (14)	0.5248 (13)	0.109 (13)
H1W	0.624660	0.008896	0.536762	0.163*
H2W	0.691279	0.054267	0.550720	0.163*
O2W	0.416 (2)	0.5248 (15)	0.1006 (13)	0.079 (8)
H3W	0.452067	0.502183	0.087624	0.118*
H4W	0.398546	0.555975	0.074645	0.118*
O3W	0.287 (2)	0.2932 (14)	0.2937 (14)	0.098 (9)*
H5W	0.333495	0.314848	0.295568	0.148*
H6W	0.252655	0.316828	0.306988	0.148*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Si1	0.031 (2)	0.0279 (19)	0.0261 (19)	−0.001 (3)	0.0038 (16)	0.009 (3)
W1	0.0532 (6)	0.0481 (6)	0.0402 (5)	−0.0043 (5)	0.0106 (5)	0.0062 (5)
W2	0.0589 (6)	0.0515 (6)	0.0416 (6)	0.0097 (5)	0.0104 (5)	−0.0054 (5)
W3	0.0580 (5)	0.0361 (4)	0.0476 (5)	−0.0029 (5)	0.0152 (4)	0.0005 (5)
W4	0.0655 (7)	0.0516 (6)	0.0406 (6)	−0.0151 (6)	0.0104 (5)	0.0044 (5)
W5	0.0553 (6)	0.0452 (5)	0.0400 (5)	0.0015 (5)	0.0109 (5)	−0.0066 (5)
W6	0.0501 (4)	0.0350 (4)	0.0471 (4)	−0.0015 (5)	0.0103 (3)	0.0007 (5)
W7	0.0528 (6)	0.0497 (6)	0.0398 (5)	0.0079 (5)	0.0107 (5)	0.0037 (5)
W8	0.0486 (6)	0.0445 (5)	0.0431 (6)	−0.0042 (5)	0.0098 (5)	−0.0095 (5)
W9	0.0447 (6)	0.0434 (6)	0.0625 (7)	−0.0027 (5)	0.0116 (5)	0.0028 (5)
W10	0.0431 (6)	0.0438 (6)	0.0629 (7)	−0.0012 (5)	0.0116 (5)	−0.0020 (5)
W11	0.0522 (6)	0.0469 (6)	0.0434 (6)	0.0026 (5)	0.0096 (5)	0.0077 (5)
W12	0.0524 (6)	0.0466 (5)	0.0375 (5)	−0.0081 (5)	0.0086 (4)	−0.0041 (4)
O9	0.053 (9)	0.049 (9)	0.018 (6)	−0.007 (7)	0.010 (6)	−0.006 (6)
O10	0.041 (8)	0.041 (8)	0.037 (7)	0.014 (6)	0.012 (6)	0.003 (6)
O11	0.044 (8)	0.035 (7)	0.039 (7)	0.008 (6)	0.015 (7)	0.003 (6)
O12	0.044 (8)	0.035 (7)	0.033 (7)	0.003 (6)	0.004 (6)	0.006 (6)
O13	0.059 (12)	0.076 (14)	0.046 (11)	−0.038 (11)	0.026 (9)	−0.011 (10)
O14	0.045 (9)	0.039 (9)	0.061 (11)	−0.003 (7)	0.012 (8)	−0.011 (8)
O15	0.048 (9)	0.066 (12)	0.036 (9)	0.019 (9)	0.014 (7)	−0.001 (8)
O16	0.041 (10)	0.086 (16)	0.073 (15)	−0.021 (11)	−0.006 (10)	−0.033 (13)
O17	0.053 (10)	0.038 (8)	0.050 (10)	−0.001 (7)	0.005 (8)	−0.003 (7)
O18	0.048 (10)	0.077 (13)	0.031 (8)	0.009 (9)	0.014 (8)	−0.016 (9)
O19	0.040 (8)	0.051 (9)	0.038 (8)	0.018 (7)	0.009 (7)	0.008 (7)
O20	0.046 (11)	0.13 (2)	0.067 (14)	0.040 (13)	0.022 (11)	0.054 (15)
O21	0.058 (11)	0.039 (9)	0.065 (12)	0.002 (8)	0.026 (9)	0.003 (8)
O22	0.050 (9)	0.031 (7)	0.105 (18)	−0.002 (9)	0.013 (10)	−0.012 (11)
O23	0.062 (11)	0.050 (10)	0.045 (9)	−0.012 (8)	0.023 (8)	−0.001 (8)
O24	0.040 (10)	0.074 (14)	0.087 (16)	0.015 (9)	0.030 (10)	0.033 (12)
O25	0.068 (13)	0.079 (15)	0.060 (12)	−0.025 (12)	0.025 (10)	−0.041 (12)
O26	0.064 (12)	0.040 (9)	0.063 (13)	−0.010 (9)	0.032 (10)	−0.013 (9)
O27	0.056 (11)	0.035 (8)	0.056 (11)	−0.004 (7)	−0.005 (9)	−0.005 (7)
O28	0.069 (12)	0.025 (7)	0.051 (10)	−0.009 (7)	−0.017 (9)	−0.004 (7)
O29	0.099 (19)	0.12 (2)	0.065 (15)	−0.064 (18)	0.047 (14)	−0.072 (16)
O30	0.092 (17)	0.075 (15)	0.034 (10)	0.027 (13)	0.018 (10)	−0.009 (9)
O31	0.041 (10)	0.079 (15)	0.061 (12)	−0.002 (9)	0.011 (9)	0.034 (11)
O32	0.046 (9)	0.043 (9)	0.047 (9)	0.005 (7)	0.011 (7)	0.006 (7)
O33	0.042 (9)	0.052 (10)	0.045 (10)	−0.004 (7)	0.017 (8)	0.007 (8)
O34	0.060 (10)	0.022 (6)	0.084 (14)	−0.003 (8)	0.021 (10)	0.005 (9)
O35	0.036 (8)	0.058 (11)	0.050 (10)	−0.006 (8)	0.007 (7)	−0.012 (8)
O36	0.057 (11)	0.061 (12)	0.053 (11)	0.011 (9)	0.021 (9)	0.018 (9)
O37	0.047 (10)	0.053 (10)	0.039 (10)	0.019 (8)	−0.007 (8)	0.001 (8)
O38	0.080 (14)	0.048 (10)	0.044 (10)	0.003 (9)	0.025 (10)	−0.002 (8)
O39	0.056 (10)	0.047 (9)	0.038 (9)	−0.014 (8)	0.011 (8)	−0.008 (7)
O40	0.037 (9)	0.078 (14)	0.053 (11)	−0.022 (10)	−0.009 (8)	0.001 (10)
O41	0.053 (10)	0.034 (8)	0.063 (11)	−0.002 (7)	0.035 (9)	0.001 (7)
O42	0.049 (11)	0.043 (9)	0.061 (12)	−0.001 (8)	0.014 (9)	−0.003 (8)
O43	0.031 (8)	0.040 (8)	0.057 (11)	0.000 (6)	0.012 (7)	0.002 (7)
O44	0.034 (8)	0.048 (10)	0.091 (16)	0.000 (7)	0.026 (9)	−0.006 (10)
O45	0.055 (10)	0.039 (8)	0.040 (9)	−0.004 (7)	0.008 (8)	0.007 (7)
O46	0.055 (11)	0.054 (11)	0.043 (10)	0.012 (9)	−0.010 (9)	0.009 (8)
O47	0.068 (11)	0.029 (7)	0.050 (10)	−0.011 (7)	0.031 (9)	−0.003 (6)
O48	0.064 (12)	0.051 (11)	0.031 (9)	−0.003 (9)	0.004 (8)	0.010 (8)
O1	0.088 (19)	0.074 (17)	0.10 (2)	0.044 (15)	0.048 (17)	0.003 (15)
O2	0.077 (14)	0.047 (11)	0.046 (11)	−0.002 (10)	0.005 (10)	0.008 (9)
N1	0.056 (11)	0.065 (11)	0.026 (8)	−0.012 (10)	0.011 (8)	0.009 (8)
N2	0.09 (2)	0.079 (19)	0.030 (11)	−0.010 (16)	0.021 (13)	−0.003 (11)
N3	0.062 (14)	0.047 (12)	0.042 (11)	−0.004 (11)	0.021 (11)	0.001 (9)
N4	0.054 (14)	0.071 (16)	0.029 (10)	−0.013 (12)	0.003 (10)	−0.002 (10)
C1	0.055 (12)	0.067 (12)	0.037 (10)	−0.016 (10)	0.004 (9)	0.009 (10)
C2	0.061 (17)	0.054 (16)	0.042 (14)	0.005 (13)	0.017 (13)	0.000 (11)
C3	0.11 (3)	0.061 (18)	0.028 (12)	0.000 (18)	0.023 (15)	0.005 (12)
C4	0.07 (2)	0.061 (18)	0.040 (14)	−0.017 (15)	0.020 (14)	−0.013 (12)
C5	0.050 (14)	0.045 (13)	0.038 (13)	−0.019 (11)	−0.003 (11)	0.003 (10)
C6	0.17 (4)	0.030 (12)	0.050 (17)	0.011 (18)	0.04 (2)	0.003 (11)
C7	0.065 (19)	0.052 (17)	0.11 (3)	−0.009 (14)	0.06 (2)	0.013 (17)
C8	0.052 (16)	0.045 (14)	0.08 (2)	−0.001 (12)	0.002 (15)	−0.011 (14)
O3	0.086 (17)	0.084 (17)	0.039 (11)	−0.001 (14)	0.011 (11)	0.019 (11)
O4	0.085 (16)	0.043 (10)	0.044 (11)	0.005 (10)	0.011 (11)	−0.008 (8)
N5	0.10 (2)	0.067 (16)	0.022 (10)	−0.004 (16)	0.019 (12)	−0.010 (10)
N6	0.063 (15)	0.046 (12)	0.073 (18)	−0.002 (11)	0.022 (13)	−0.001 (11)
N7	0.060 (13)	0.030 (9)	0.038 (10)	−0.013 (9)	0.009 (9)	−0.001 (8)
N8	0.048 (11)	0.043 (11)	0.040 (11)	−0.003 (9)	0.006 (9)	−0.001 (9)
C9	0.057 (18)	0.052 (17)	0.10 (3)	−0.007 (14)	0.022 (18)	0.012 (17)
C10	0.064 (16)	0.041 (12)	0.038 (13)	0.003 (12)	0.001 (12)	0.000 (10)
C11	0.08 (2)	0.050 (15)	0.042 (14)	−0.008 (14)	0.022 (14)	−0.003 (11)
C12	0.045 (15)	0.055 (17)	0.07 (2)	−0.033 (14)	0.001 (14)	0.001 (15)
C13	0.055 (15)	0.065 (17)	0.024 (11)	−0.001 (13)	0.003 (10)	0.000 (10)
C14	0.07 (2)	0.032 (11)	0.07 (2)	−0.008 (12)	0.015 (16)	−0.022 (12)
C15	0.11 (3)	0.14 (4)	0.06 (2)	0.07 (3)	0.06 (2)	0.04 (2)
C16	0.09 (3)	0.11 (3)	0.019 (11)	−0.02 (2)	−0.013 (14)	−0.007 (15)
O5	0.078 (16)	0.062 (14)	0.10 (2)	0.007 (12)	0.058 (16)	−0.014 (13)
O6	0.068 (13)	0.055 (11)	0.038 (10)	0.004 (10)	0.020 (9)	0.007 (8)
N9	0.041 (12)	0.063 (15)	0.050 (13)	−0.003 (10)	−0.001 (10)	−0.008 (11)
N10	0.059 (14)	0.036 (10)	0.044 (12)	−0.002 (10)	0.007 (10)	0.000 (8)
N11	0.060 (14)	0.054 (14)	0.052 (13)	0.008 (11)	0.035 (11)	0.001 (10)
N12	0.041 (11)	0.042 (11)	0.043 (11)	0.000 (9)	0.014 (9)	−0.001 (9)
C17	0.08 (2)	0.057 (17)	0.057 (18)	0.012 (17)	−0.012 (18)	−0.012 (14)
C18	0.08 (2)	0.033 (12)	0.040 (13)	0.016 (12)	−0.009 (13)	−0.006 (10)
C19	0.046 (14)	0.046 (14)	0.08 (2)	−0.010 (11)	0.028 (14)	0.001 (13)
C20	0.066 (18)	0.044 (14)	0.034 (12)	−0.020 (12)	−0.005 (12)	−0.004 (10)
C21	0.059 (15)	0.059 (16)	0.017 (9)	−0.002 (13)	0.006 (10)	−0.003 (9)
C22	0.065 (18)	0.08 (2)	0.051 (18)	−0.008 (16)	0.002 (14)	0.007 (15)
C23	0.08 (2)	0.054 (17)	0.07 (2)	0.011 (16)	0.027 (18)	0.007 (15)
C24	0.09 (3)	0.12 (3)	0.038 (15)	−0.04 (2)	0.039 (17)	−0.018 (17)
O7	0.062 (13)	0.058 (12)	0.072 (15)	0.015 (11)	0.005 (11)	−0.027 (11)
O8	0.061 (13)	0.056 (12)	0.062 (13)	0.002 (10)	0.019 (11)	0.009 (10)
N13	0.068 (17)	0.060 (16)	0.08 (2)	0.026 (14)	0.041 (16)	0.011 (14)
N14	0.039 (9)	0.060 (11)	0.094 (17)	0.010 (8)	0.019 (10)	0.002 (11)
N15	0.039 (12)	0.09 (2)	0.073 (18)	−0.006 (12)	0.023 (12)	−0.006 (15)
N16	0.073 (16)	0.046 (12)	0.043 (12)	0.001 (11)	0.029 (11)	−0.006 (10)
C25	0.07 (2)	0.08 (2)	0.10 (3)	0.022 (19)	0.05 (2)	0.05 (2)
C26	0.043 (10)	0.059 (12)	0.094 (18)	0.015 (9)	0.020 (11)	0.000 (12)
C27	0.042 (12)	0.035 (11)	0.064 (17)	0.006 (10)	0.011 (12)	−0.005 (11)
C28	0.066 (19)	0.060 (17)	0.043 (14)	−0.001 (14)	0.021 (14)	0.017 (13)
C29	0.037 (12)	0.049 (16)	0.10 (3)	0.022 (12)	0.026 (15)	−0.003 (15)
C30	0.036 (11)	0.046 (12)	0.11 (2)	0.021 (8)	0.017 (13)	−0.011 (13)
C31	0.059 (18)	0.08 (2)	0.054 (17)	0.052 (17)	−0.007 (14)	0.003 (15)
C32	0.039 (12)	0.043 (13)	0.058 (16)	0.003 (10)	0.016 (12)	−0.003 (11)
O1W	0.20 (4)	0.071 (16)	0.040 (13)	−0.04 (2)	0.007 (18)	0.007 (12)
O2W	0.093 (19)	0.095 (19)	0.058 (14)	0.017 (16)	0.038 (14)	0.013 (13)

Geometric parameters (Å, º)

Si1—O10	1.564 (16)	C6—H6A	0.9800
Si1—O11	1.576 (16)	C6—H6B	0.9800
Si1—O12	1.602 (17)	C6—H6C	0.9800
Si1—O9	1.644 (18)	C7—H7A	0.9800
W1—O13	1.71 (2)	C7—H7B	0.9800
W1—O16	1.86 (3)	C7—H7C	0.9800
W1—O15	1.866 (19)	C8—H8A	0.9800
W1—O17	1.930 (19)	C8—H8B	0.9800
W1—O14	1.965 (17)	C8—H8C	0.9800
W1—O9	2.340 (16)	O3—C11	1.234 (13)
W2—O18	1.706 (18)	O4—C12	1.233 (13)
W2—O19	1.867 (17)	N5—C9	1.37 (5)
W2—O20	1.90 (2)	N5—C13	1.39 (3)
W2—O14	1.981 (19)	N5—H5N	0.8800
W2—O21	1.99 (2)	N6—C9	1.30 (5)
W2—O9	2.355 (15)	N6—C10	1.32 (4)
W3—O22	1.698 (15)	N6—C14	1.502 (19)
W3—O19	1.878 (18)	N7—C11	1.34 (4)
W3—O24	1.91 (2)	N7—C12	1.42 (4)
W3—O25	1.92 (2)	N7—C15	1.45 (4)
W3—O23	1.950 (18)	N8—C12	1.27 (4)
W3—O10	2.361 (16)	N8—C13	1.42 (4)
W4—O26	1.67 (2)	N8—C16	1.50 (4)
W4—O27	1.861 (16)	C9—H9	0.9500
W4—O28	1.876 (17)	C10—C13	1.37 (4)
W4—O29	1.88 (3)	C10—C11	1.54 (4)
W4—O23	1.944 (19)	C14—H14A	0.9800
W4—O10	2.438 (16)	C14—H14B	0.9800
W5—O30	1.65 (2)	C14—H14C	0.9800
W5—O32	1.855 (18)	C15—H15A	0.9800
W5—O27	1.900 (17)	C15—H15B	0.9800
W5—O31	1.93 (2)	C15—H15C	0.9800
W5—O33	1.968 (18)	C16—H16A	0.9800
W5—O11	2.399 (16)	C16—H16B	0.9800
W6—O34	1.698 (14)	C16—H16C	0.9800
W6—O16	1.90 (3)	O5—C19	1.235 (13)
W6—O35	1.905 (18)	O6—C20	1.231 (13)
W6—O31	1.91 (2)	N9—C21	1.24 (4)
W6—O36	1.92 (2)	N9—C17	1.36 (5)
W6—O11	2.393 (15)	N9—H9N	0.8800
W7—O37	1.721 (18)	N10—C17	1.24 (5)
W7—O35	1.838 (18)	N10—C18	1.43 (3)
W7—O15	1.882 (19)	N10—C22	1.500 (19)
W7—O39	1.896 (19)	N11—C23	1.37 (4)
W7—O38	2.019 (19)	N11—C19	1.45 (4)
W7—O12	2.365 (14)	N11—C20	1.50 (4)
W8—O40	1.65 (2)	N12—C20	1.27 (4)
W8—O24	1.83 (2)	N12—C21	1.44 (4)
W8—O20	1.89 (2)	N12—C24	1.45 (4)
W8—O38	1.91 (2)	C17—H17	0.9500
W8—O41	1.922 (17)	C18—C21	1.27 (5)
W8—O12	2.378 (16)	C18—C19	1.46 (4)
W9—O42	1.71 (2)	C22—H22A	0.9800
W9—O32	1.879 (18)	C22—H22B	0.9800
W9—O28	1.881 (17)	C22—H22C	0.9800
W9—O41	1.926 (18)	C23—H23A	0.9800
W9—O39	1.959 (18)	C23—H23B	0.9800
W9—O12	2.396 (17)	C23—H23C	0.9800
W10—O43	1.679 (18)	C24—H24A	0.9800
W10—O45	1.852 (19)	C24—H24B	0.9800
W10—O44	1.88 (2)	C24—H24C	0.9800
W10—O21	1.93 (2)	O7—C27	1.235 (13)
W10—O17	1.980 (19)	O8—C28	1.230 (13)
W10—O9	2.387 (17)	N13—C29	1.35 (5)
W11—O46	1.724 (18)	N13—C25	1.38 (5)
W11—O47	1.855 (15)	N13—H13N	0.8800
W11—O44	1.88 (2)	N14—C25	1.30 (5)
W11—O29	1.91 (3)	N14—C26	1.41 (5)
W11—O25	1.95 (2)	N14—C30	1.500 (19)
W11—O10	2.387 (15)	N15—C28	1.37 (4)
W12—O48	1.68 (2)	N15—C27	1.42 (4)
W12—O47	1.885 (15)	N15—C31	1.57 (4)
W12—O45	1.91 (2)	N16—C29	1.21 (4)
W12—O33	1.917 (18)	N16—C32	1.46 (4)
W12—O36	1.942 (19)	N16—C28	1.51 (3)
W12—O11	2.379 (16)	C25—H25	0.9500
O1—C3	1.233 (13)	C26—C27	1.29 (5)
O2—C4	1.232 (13)	C26—C29	1.41 (5)
N1—C1	1.35 (5)	C30—H30A	0.9800
N1—C5	1.44 (3)	C30—H30B	0.9800
N1—H1N	0.8800	C30—H30C	0.9800
N2—C2	1.31 (4)	C31—H31A	0.9800
N2—C1	1.38 (4)	C31—H31B	0.9800
N2—C6	1.499 (19)	C31—H31C	0.9800
N3—C4	1.26 (4)	C32—H32A	0.9800
N3—C3	1.35 (4)	C32—H32B	0.9800
N3—C7	1.57 (4)	C32—H32C	0.9800
N4—C5	1.29 (4)	O1W—H1W	0.8500
N4—C8	1.46 (4)	O1W—H2W	0.8500
N4—C4	1.53 (4)	O2W—H3W	0.8500
C1—H1	0.9500	O2W—H4W	0.8500
C2—C5	1.36 (4)	O3W—H5W	0.8500
C2—C3	1.45 (5)	O3W—H6W	0.8500
O10—Si1—O11	111.7 (10)	W8—O12—W9	91.6 (6)
O10—Si1—O12	110.4 (9)	W1—O14—W2	121.0 (11)
O11—Si1—O12	110.2 (9)	W1—O15—W7	150.2 (11)
O10—Si1—O9	108.5 (9)	W1—O16—W6	149.2 (13)
O11—Si1—O9	109.4 (9)	W1—O17—W10	122.1 (10)
O12—Si1—O9	106.4 (9)	W2—O19—W3	151.4 (9)
O13—W1—O16	105.5 (12)	W8—O20—W2	147.6 (16)
O13—W1—O15	105.7 (10)	W10—O21—W2	120.8 (10)
O16—W1—O15	87.4 (9)	W4—O23—W3	122.6 (9)
O13—W1—O17	96.0 (10)	W8—O24—W3	151.2 (13)
O16—W1—O17	89.7 (9)	W3—O25—W11	124.8 (14)
O15—W1—O17	158.1 (9)	W4—O27—W5	150.1 (11)
O13—W1—O14	94.2 (10)	W4—O28—W9	148.3 (10)
O16—W1—O14	160.0 (11)	W4—O29—W11	129.3 (16)
O15—W1—O14	90.2 (8)	W6—O31—W5	127.6 (13)
O17—W1—O14	85.1 (8)	W5—O32—W9	152.7 (10)
O13—W1—O9	163.7 (10)	W12—O33—W5	124.4 (10)
O16—W1—O9	87.3 (10)	W7—O35—W6	149.8 (12)
O15—W1—O9	84.6 (8)	W6—O36—W12	124.7 (12)
O17—W1—O9	73.5 (7)	W8—O38—W7	122.3 (10)
O14—W1—O9	72.8 (7)	W7—O39—W9	125.8 (11)
O18—W2—O19	106.2 (9)	W8—O41—W9	125.6 (9)
O18—W2—O20	99.5 (12)	W11—O44—W10	151.3 (11)
O19—W2—O20	86.0 (9)	W10—O45—W12	150.2 (10)
O18—W2—O14	97.0 (10)	W11—O47—W12	152.0 (10)
O19—W2—O14	156.7 (8)	C1—N1—C5	104 (3)
O20—W2—O14	92.3 (10)	C1—N1—H1N	127.8
O18—W2—O21	98.3 (9)	C5—N1—H1N	127.8
O19—W2—O21	90.1 (8)	C2—N2—C1	109 (3)
O20—W2—O21	162.2 (12)	C2—N2—C6	127 (3)
O14—W2—O21	84.3 (8)	C1—N2—C6	124 (3)
O18—W2—O9	166.8 (9)	C4—N3—C3	132 (3)
O19—W2—O9	84.5 (7)	C4—N3—C7	113 (2)
O20—W2—O9	88.8 (11)	C3—N3—C7	115 (3)
O14—W2—O9	72.2 (7)	C5—N4—C8	128 (3)
O21—W2—O9	73.5 (7)	C5—N4—C4	114 (3)
O22—W3—O19	106.2 (12)	C8—N4—C4	119 (3)
O22—W3—O24	103.3 (13)	N1—C1—N2	110 (3)
O19—W3—O24	86.1 (8)	N1—C1—H1	125.2
O22—W3—O25	99.5 (12)	N2—C1—H1	125.2
O19—W3—O25	85.7 (9)	N2—C2—C5	109 (3)
O24—W3—O25	157.2 (11)	N2—C2—C3	133 (3)
O22—W3—O23	97.0 (12)	C5—C2—C3	118 (3)
O19—W3—O23	156.6 (8)	O1—C3—N3	127 (3)
O24—W3—O23	91.8 (9)	O1—C3—C2	121 (3)
O25—W3—O23	87.3 (9)	N3—C3—C2	112 (2)
O22—W3—O10	167.6 (12)	O2—C4—N3	129 (3)
O19—W3—O10	82.4 (7)	O2—C4—N4	115 (3)
O24—W3—O10	86.0 (9)	N3—C4—N4	116 (2)
O25—W3—O10	71.8 (8)	N4—C5—C2	128 (3)
O23—W3—O10	74.2 (7)	N4—C5—N1	124 (3)
O26—W4—O27	107.0 (10)	C2—C5—N1	108 (3)
O26—W4—O28	104.0 (11)	N2—C6—H6A	109.5
O27—W4—O28	88.3 (7)	N2—C6—H6B	109.5
O26—W4—O29	100.9 (13)	H6A—C6—H6B	109.5
O27—W4—O29	84.4 (11)	N2—C6—H6C	109.5
O28—W4—O29	155.2 (12)	H6A—C6—H6C	109.5
O26—W4—O23	95.6 (9)	H6B—C6—H6C	109.5
O27—W4—O23	157.1 (9)	N3—C7—H7A	109.5
O28—W4—O23	89.5 (8)	N3—C7—H7B	109.5
O29—W4—O23	88.1 (10)	H7A—C7—H7B	109.5
O26—W4—O10	164.5 (8)	N3—C7—H7C	109.5
O27—W4—O10	84.7 (8)	H7A—C7—H7C	109.5
O28—W4—O10	86.1 (8)	H7B—C7—H7C	109.5
O29—W4—O10	69.6 (9)	N4—C8—H8A	109.5
O23—W4—O10	72.5 (6)	N4—C8—H8B	109.5
O30—W5—O32	108.9 (11)	H8A—C8—H8B	109.5
O30—W5—O27	106.5 (12)	N4—C8—H8C	109.5
O32—W5—O27	86.5 (8)	H8A—C8—H8C	109.5
O30—W5—O31	99.0 (13)	H8B—C8—H8C	109.5
O32—W5—O31	87.7 (9)	C9—N5—C13	103 (3)
O27—W5—O31	154.4 (10)	C9—N5—H5N	128.7
O30—W5—O33	96.7 (11)	C13—N5—H5N	128.7
O32—W5—O33	154.4 (8)	C9—N6—C10	106 (3)
O27—W5—O33	87.2 (8)	C9—N6—C14	131 (3)
O31—W5—O33	87.3 (8)	C10—N6—C14	123 (3)
O30—W5—O11	163.5 (11)	C11—N7—C12	126 (2)
O32—W5—O11	83.5 (7)	C11—N7—C15	113 (2)
O27—W5—O11	84.5 (8)	C12—N7—C15	121 (3)
O31—W5—O11	70.0 (8)	C12—N8—C13	117 (2)
O33—W5—O11	71.2 (7)	C12—N8—C16	127 (3)
O34—W6—O16	104.4 (13)	C13—N8—C16	117 (3)
O34—W6—O35	105.4 (11)	N6—C9—N5	114 (4)
O16—W6—O35	87.3 (8)	N6—C9—H9	123.0
O34—W6—O31	99.7 (12)	N5—C9—H9	123.0
O16—W6—O31	155.8 (11)	N6—C10—C13	110 (3)
O35—W6—O31	86.6 (9)	N6—C10—C11	133 (3)
O34—W6—O36	98.5 (11)	C13—C10—C11	117 (3)
O16—W6—O36	88.9 (9)	O3—C11—N7	124 (3)
O35—W6—O36	156.0 (9)	O3—C11—C10	123 (3)
O31—W6—O36	87.3 (9)	N7—C11—C10	113 (2)
O34—W6—O11	166.2 (11)	O4—C12—N8	123 (3)
O16—W6—O11	85.6 (10)	O4—C12—N7	114 (3)
O35—W6—O11	84.3 (7)	N8—C12—N7	123 (2)
O31—W6—O11	70.5 (8)	C10—C13—N5	107 (3)
O36—W6—O11	71.7 (7)	C10—C13—N8	125 (3)
O37—W7—O35	107.8 (9)	N5—C13—N8	128 (3)
O37—W7—O15	106.3 (10)	N6—C14—H14A	109.5
O35—W7—O15	88.0 (9)	N6—C14—H14B	109.5
O37—W7—O39	96.7 (10)	H14A—C14—H14B	109.5
O35—W7—O39	90.7 (8)	N6—C14—H14C	109.5
O15—W7—O39	156.2 (8)	H14A—C14—H14C	109.5
O37—W7—O38	94.7 (9)	H14B—C14—H14C	109.5
O35—W7—O38	157.4 (9)	N7—C15—H15A	109.5
O15—W7—O38	87.1 (9)	N7—C15—H15B	109.5
O39—W7—O38	85.0 (8)	H15A—C15—H15B	109.5
O37—W7—O12	162.5 (9)	N7—C15—H15C	109.5
O35—W7—O12	86.0 (8)	H15A—C15—H15C	109.5
O15—W7—O12	84.4 (7)	H15B—C15—H15C	109.5
O39—W7—O12	71.8 (7)	N8—C16—H16A	109.5
O38—W7—O12	71.6 (7)	N8—C16—H16B	109.5
O40—W8—O24	103.7 (12)	H16A—C16—H16B	109.5
O40—W8—O20	98.3 (14)	N8—C16—H16C	109.5
O24—W8—O20	85.3 (9)	H16A—C16—H16C	109.5
O40—W8—O38	97.5 (10)	H16B—C16—H16C	109.5
O24—W8—O38	158.8 (11)	C21—N9—C17	110 (3)
O20—W8—O38	90.5 (11)	C21—N9—H9N	124.8
O40—W8—O41	101.8 (10)	C17—N9—H9N	124.8
O24—W8—O41	89.2 (9)	C17—N10—C18	105 (3)
O20—W8—O41	160.0 (12)	C17—N10—C22	124 (3)
O38—W8—O41	87.7 (8)	C18—N10—C22	131 (3)
O40—W8—O12	168.4 (9)	C23—N11—C19	117 (3)
O24—W8—O12	86.0 (10)	C23—N11—C20	123 (3)
O20—W8—O12	88.7 (12)	C19—N11—C20	120 (2)
O38—W8—O12	73.1 (7)	C20—N12—C21	123 (2)
O41—W8—O12	71.7 (7)	C20—N12—C24	121 (3)
O42—W9—O32	106.6 (9)	C21—N12—C24	117 (3)
O42—W9—O28	104.3 (10)	N10—C17—N9	108 (3)
O32—W9—O28	87.1 (7)	N10—C17—H17	125.9
O42—W9—O41	98.5 (9)	N9—C17—H17	125.9
O32—W9—O41	154.8 (8)	C21—C18—N10	108 (3)
O28—W9—O41	89.4 (8)	C21—C18—C19	129 (3)
O42—W9—O39	98.2 (9)	N10—C18—C19	123 (3)
O32—W9—O39	89.8 (7)	O5—C19—N11	116 (3)
O28—W9—O39	157.3 (10)	O5—C19—C18	133 (3)
O41—W9—O39	84.0 (7)	N11—C19—C18	111 (2)
O42—W9—O12	164.7 (9)	O6—C20—N12	127 (3)
O32—W9—O12	83.7 (7)	O6—C20—N11	113 (3)
O28—W9—O12	87.2 (8)	N12—C20—N11	120 (2)
O41—W9—O12	71.2 (6)	N9—C21—C18	109 (3)
O39—W9—O12	70.1 (7)	N9—C21—N12	134 (3)
O43—W10—O45	104.2 (9)	C18—C21—N12	117 (3)
O43—W10—O44	106.6 (9)	N10—C22—H22A	109.5
O45—W10—O44	88.0 (8)	N10—C22—H22B	109.5
O43—W10—O21	97.6 (9)	H22A—C22—H22B	109.5
O45—W10—O21	157.8 (8)	N10—C22—H22C	109.5
O44—W10—O21	90.2 (9)	H22A—C22—H22C	109.5
O43—W10—O17	97.2 (9)	H22B—C22—H22C	109.5
O45—W10—O17	87.4 (7)	N11—C23—H23A	109.5
O44—W10—O17	156.1 (8)	N11—C23—H23B	109.5
O21—W10—O17	85.4 (8)	H23A—C23—H23B	109.5
O43—W10—O9	166.0 (8)	N11—C23—H23C	109.5
O45—W10—O9	84.0 (7)	H23A—C23—H23C	109.5
O44—W10—O9	84.6 (7)	H23B—C23—H23C	109.5
O21—W10—O9	73.7 (7)	N12—C24—H24A	109.5
O17—W10—O9	71.6 (7)	N12—C24—H24B	109.5
O46—W11—O47	105.3 (10)	H24A—C24—H24B	109.5
O46—W11—O44	106.4 (10)	N12—C24—H24C	109.5
O47—W11—O44	86.7 (8)	H24A—C24—H24C	109.5
O46—W11—O29	101.7 (14)	H24B—C24—H24C	109.5
O47—W11—O29	85.7 (10)	C29—N13—C25	107 (3)
O44—W11—O29	152.0 (13)	C29—N13—H13N	126.4
O46—W11—O25	99.9 (11)	C25—N13—H13N	126.4
O47—W11—O25	154.8 (11)	C25—N14—C26	110 (3)
O44—W11—O25	85.5 (10)	C25—N14—C30	122 (3)
O29—W11—O25	90.1 (10)	C26—N14—C30	128 (3)
O46—W11—O10	167.2 (9)	C28—N15—C27	133 (3)
O47—W11—O10	84.5 (8)	C28—N15—C31	110 (3)
O44—W11—O10	82.1 (7)	C27—N15—C31	117 (3)
O29—W11—O10	70.4 (11)	C29—N16—C32	126 (3)
O25—W11—O10	70.7 (9)	C29—N16—C28	122 (3)
O48—W12—O47	103.4 (9)	C32—N16—C28	111 (2)
O48—W12—O45	107.1 (10)	N14—C25—N13	110 (3)
O47—W12—O45	87.2 (7)	N14—C25—H25	125.0
O48—W12—O33	97.4 (10)	N13—C25—H25	125.0
O47—W12—O33	87.8 (8)	C27—C26—N14	129 (4)
O45—W12—O33	155.6 (8)	C27—C26—C29	126 (4)
O48—W12—O36	100.5 (10)	N14—C26—C29	104 (4)
O47—W12—O36	156.0 (9)	O7—C27—C26	133 (3)
O45—W12—O36	87.5 (8)	O7—C27—N15	118 (3)
O33—W12—O36	87.5 (8)	C26—C27—N15	108 (3)
O48—W12—O11	167.2 (9)	O8—C28—N15	133 (3)
O47—W12—O11	84.3 (7)	O8—C28—N16	120 (3)
O45—W12—O11	83.3 (7)	N15—C28—N16	107 (2)
O33—W12—O11	72.4 (7)	N16—C29—N13	129 (4)
O36—W12—O11	71.8 (8)	N16—C29—C26	122 (4)
Si1—O9—W1	124.4 (9)	N13—C29—C26	109 (3)
Si1—O9—W2	123.9 (8)	N14—C30—H30A	109.5
W1—O9—W2	94.0 (5)	N14—C30—H30B	109.5
Si1—O9—W10	121.3 (8)	H30A—C30—H30B	109.5
W1—O9—W10	92.7 (6)	N14—C30—H30C	109.5
W2—O9—W10	91.8 (6)	H30A—C30—H30C	109.5
Si1—O10—W3	126.2 (9)	H30B—C30—H30C	109.5
Si1—O10—W11	124.9 (10)	N15—C31—H31A	109.5
W3—O10—W11	92.4 (5)	N15—C31—H31B	109.5
Si1—O10—W4	121.9 (8)	H31A—C31—H31B	109.5
W3—O10—W4	90.7 (6)	N15—C31—H31C	109.5
W11—O10—W4	90.4 (5)	H31A—C31—H31C	109.5
Si1—O11—W12	123.9 (9)	H31B—C31—H31C	109.5
Si1—O11—W6	124.8 (9)	N16—C32—H32A	109.5
W12—O11—W6	91.7 (6)	N16—C32—H32B	109.5
Si1—O11—W5	123.1 (9)	H32A—C32—H32B	109.5
W12—O11—W5	92.0 (6)	N16—C32—H32C	109.5
W6—O11—W5	91.8 (5)	H32A—C32—H32C	109.5
Si1—O12—W7	124.3 (8)	H32B—C32—H32C	109.5
Si1—O12—W8	124.7 (8)	H1W—O1W—H2W	108.4
W7—O12—W8	93.0 (5)	H3W—O2W—H4W	108.4
Si1—O12—W9	121.9 (9)	H5W—O3W—H6W	108.4
W7—O12—W9	92.2 (5)
O10—Si1—O9—W1	179.4 (9)	O45—W12—O47—W11	23 (3)
O11—Si1—O9—W1	57.3 (12)	O33—W12—O47—W11	−133 (3)
O12—Si1—O9—W1	−61.7 (11)	O36—W12—O47—W11	−54 (4)
O10—Si1—O9—W2	−56.4 (12)	O11—W12—O47—W11	−60 (3)
O11—Si1—O9—W2	−178.5 (9)	C5—N1—C1—N2	−5 (3)
O12—Si1—O9—W2	62.5 (11)	C2—N2—C1—N1	6 (3)
O10—Si1—O9—W10	60.5 (11)	C6—N2—C1—N1	178 (3)
O11—Si1—O9—W10	−61.6 (12)	C1—N2—C2—C5	−4 (3)
O12—Si1—O9—W10	179.4 (8)	C6—N2—C2—C5	−176 (3)
O11—Si1—O10—W3	−178.7 (9)	C1—N2—C2—C3	177 (3)
O12—Si1—O10—W3	−55.6 (13)	C6—N2—C2—C3	6 (6)
O9—Si1—O10—W3	60.6 (13)	C4—N3—C3—O1	−178 (4)
O11—Si1—O10—W11	56.1 (13)	C7—N3—C3—O1	−4 (5)
O12—Si1—O10—W11	179.2 (9)	C4—N3—C3—C2	7 (5)
O9—Si1—O10—W11	−64.5 (12)	C7—N3—C3—C2	−179 (3)
O11—Si1—O10—W4	−60.3 (13)	N2—C2—C3—O1	−2 (6)
O12—Si1—O10—W4	62.7 (12)	C5—C2—C3—O1	180 (3)
O9—Si1—O10—W4	179.0 (8)	N2—C2—C3—N3	173 (3)
O10—Si1—O11—W12	−57.8 (13)	C5—C2—C3—N3	−5 (4)
O12—Si1—O11—W12	179.0 (9)	C3—N3—C4—O2	−179 (3)
O9—Si1—O11—W12	62.4 (12)	C7—N3—C4—O2	7 (5)
O10—Si1—O11—W6	−178.7 (9)	C3—N3—C4—N4	−5 (5)
O12—Si1—O11—W6	58.1 (13)	C7—N3—C4—N4	−179 (3)
O9—Si1—O11—W6	−58.5 (13)	C5—N4—C4—O2	175 (3)
O10—Si1—O11—W5	61.3 (13)	C8—N4—C4—O2	−1 (4)
O12—Si1—O11—W5	−61.8 (12)	C5—N4—C4—N3	0 (4)
O9—Si1—O11—W5	−178.5 (9)	C8—N4—C4—N3	−177 (3)
O10—Si1—O12—W7	179.3 (9)	C8—N4—C5—C2	177 (3)
O11—Si1—O12—W7	−56.7 (13)	C4—N4—C5—C2	1 (4)
O9—Si1—O12—W7	61.7 (12)	C8—N4—C5—N1	−1 (5)
O10—Si1—O12—W8	56.1 (13)	C4—N4—C5—N1	−177 (2)
O11—Si1—O12—W8	−179.9 (9)	N2—C2—C5—N4	−177 (3)
O9—Si1—O12—W8	−61.5 (12)	C3—C2—C5—N4	1 (5)
O10—Si1—O12—W9	−62.0 (11)	N2—C2—C5—N1	1 (3)
O11—Si1—O12—W9	61.9 (11)	C3—C2—C5—N1	180 (2)
O9—Si1—O12—W9	−179.6 (8)	C1—N1—C5—N4	−179 (3)
O13—W1—O15—W7	132 (2)	C1—N1—C5—C2	2 (3)
O16—W1—O15—W7	27 (2)	C10—N6—C9—N5	0 (4)
O17—W1—O15—W7	−56 (4)	C14—N6—C9—N5	−179 (3)
O14—W1—O15—W7	−133 (2)	C13—N5—C9—N6	−2 (4)
O9—W1—O15—W7	−61 (2)	C9—N6—C10—C13	2 (4)
O37—W7—O15—W1	−133 (2)	C14—N6—C10—C13	−179 (3)
O35—W7—O15—W1	−26 (2)	C9—N6—C10—C11	−175 (3)
O39—W7—O15—W1	62 (3)	C14—N6—C10—C11	4 (5)
O38—W7—O15—W1	132 (2)	C12—N7—C11—O3	179 (3)
O12—W7—O15—W1	61 (2)	C15—N7—C11—O3	3 (5)
O13—W1—O16—W6	−135 (3)	C12—N7—C11—C10	4 (4)
O15—W1—O16—W6	−29 (3)	C15—N7—C11—C10	−172 (3)
O17—W1—O16—W6	129 (3)	N6—C10—C11—O3	3 (6)
O14—W1—O16—W6	54 (5)	C13—C10—C11—O3	−174 (3)
O9—W1—O16—W6	55 (3)	N6—C10—C11—N7	178 (3)
O18—W2—O19—W3	124 (2)	C13—C10—C11—N7	1 (4)
O20—W2—O19—W3	25 (2)	C13—N8—C12—O4	−176 (3)
O14—W2—O19—W3	−62 (3)	C16—N8—C12—O4	2 (5)
O21—W2—O19—W3	−137 (2)	C13—N8—C12—N7	7 (4)
O9—W2—O19—W3	−64 (2)	C16—N8—C12—N7	−175 (3)
O22—W3—O19—W2	−125 (2)	C11—N7—C12—O4	174 (3)
O24—W3—O19—W2	−22 (2)	C15—N7—C12—O4	−11 (4)
O25—W3—O19—W2	137 (2)	C11—N7—C12—N8	−9 (4)
O23—W3—O19—W2	64 (3)	C15—N7—C12—N8	167 (3)
O10—W3—O19—W2	65 (2)	N6—C10—C13—N5	−4 (4)
O40—W8—O20—W2	145 (3)	C11—C10—C13—N5	174 (3)
O24—W8—O20—W2	42 (3)	N6—C10—C13—N8	−180 (3)
O38—W8—O20—W2	−117 (3)	C11—C10—C13—N8	−2 (5)
O41—W8—O20—W2	−33 (5)	C9—N5—C13—C10	3 (4)
O12—W8—O20—W2	−44 (3)	C9—N5—C13—N8	179 (3)
O18—W2—O20—W8	−145 (3)	C12—N8—C13—C10	−2 (4)
O19—W2—O20—W8	−39 (3)	C16—N8—C13—C10	−180 (3)
O14—W2—O20—W8	117 (3)	C12—N8—C13—N5	−177 (3)
O21—W2—O20—W8	39 (6)	C16—N8—C13—N5	5 (5)
O9—W2—O20—W8	45 (3)	C18—N10—C17—N9	−8 (3)
O40—W8—O24—W3	−133 (3)	C22—N10—C17—N9	173 (3)
O20—W8—O24—W3	−35 (3)	C21—N9—C17—N10	9 (4)
O38—W8—O24—W3	44 (5)	C17—N10—C18—C21	4 (3)
O41—W8—O24—W3	125 (3)	C22—N10—C18—C21	−177 (3)
O12—W8—O24—W3	54 (3)	C17—N10—C18—C19	−175 (3)
O26—W4—O27—W5	129 (3)	C22—N10—C18—C19	4 (5)
O28—W4—O27—W5	25 (3)	C23—N11—C19—O5	−2 (5)
O29—W4—O27—W5	−131 (3)	C20—N11—C19—O5	175 (3)
O23—W4—O27—W5	−60 (4)	C23—N11—C19—C18	178 (3)
O10—W4—O27—W5	−61 (3)	C20—N11—C19—C18	−6 (4)
O26—W4—O28—W9	−136 (3)	C21—C18—C19—O5	−179 (4)
O27—W4—O28—W9	−29 (3)	N10—C18—C19—O5	0 (6)
O29—W4—O28—W9	44 (4)	C21—C18—C19—N11	1 (5)
O23—W4—O28—W9	128 (3)	N10—C18—C19—N11	−179 (3)
O10—W4—O28—W9	56 (3)	C21—N12—C20—O6	−180 (2)
O42—W9—O28—W4	134 (3)	C24—N12—C20—O6	5 (5)
O32—W9—O28—W4	28 (3)	C21—N12—C20—N11	−7 (4)
O41—W9—O28—W4	−127 (3)	C24—N12—C20—N11	177 (3)
O39—W9—O28—W4	−54 (4)	C23—N11—C20—O6	−1 (4)
O12—W9—O28—W4	−56 (3)	C19—N11—C20—O6	−177 (3)
O26—W4—O29—W11	−161.8 (19)	C23—N11—C20—N12	−174 (3)
O27—W4—O29—W11	92 (2)	C19—N11—C20—N12	9 (4)
O28—W4—O29—W11	18 (4)	C17—N9—C21—C18	−6 (4)
O23—W4—O29—W11	−66 (2)	C17—N9—C21—N12	174 (3)
O10—W4—O29—W11	5.6 (16)	N10—C18—C21—N9	1 (3)
O30—W5—O32—W9	128 (2)	C19—C18—C21—N9	−179 (3)
O27—W5—O32—W9	22 (2)	N10—C18—C21—N12	−179 (2)
O31—W5—O32—W9	−133 (2)	C19—C18—C21—N12	1 (4)
O33—W5—O32—W9	−54 (3)	C20—N12—C21—N9	−178 (3)
O11—W5—O32—W9	−63 (2)	C24—N12—C21—N9	−2 (4)
O42—W9—O32—W5	−128 (2)	C20—N12—C21—C18	3 (4)
O28—W9—O32—W5	−24 (3)	C24—N12—C21—C18	179 (3)
O41—W9—O32—W5	58 (3)	C26—N14—C25—N13	4 (4)
O39—W9—O32—W5	134 (2)	C30—N14—C25—N13	179 (2)
O12—W9—O32—W5	64 (2)	C29—N13—C25—N14	−2 (4)
O37—W7—O35—W6	131 (2)	C25—N14—C26—C27	−180 (3)
O15—W7—O35—W6	25 (2)	C30—N14—C26—C27	6 (5)
O39—W7—O35—W6	−132 (2)	C25—N14—C26—C29	−4 (3)
O38—W7—O35—W6	−53 (4)	C30—N14—C26—C29	−178 (2)
O12—W7—O35—W6	−60 (2)	N14—C26—C27—O7	−2 (6)
O37—W7—O39—W9	−170.0 (11)	C29—C26—C27—O7	−176 (3)
O35—W7—O39—W9	82.0 (11)	N14—C26—C27—N15	172 (3)
O15—W7—O39—W9	−5 (3)	C29—C26—C27—N15	−3 (4)
O38—W7—O39—W9	−75.7 (11)	C28—N15—C27—O7	−175 (3)
O12—W7—O39—W9	−3.5 (9)	C31—N15—C27—O7	0 (4)
O46—W11—O44—W10	125 (2)	C28—N15—C27—C26	10 (5)
O47—W11—O44—W10	20 (3)	C31—N15—C27—C26	−175 (2)
O29—W11—O44—W10	−54 (4)	C27—N15—C28—O8	176 (3)
O25—W11—O44—W10	−136 (3)	C31—N15—C28—O8	0 (5)
O10—W11—O44—W10	−64 (2)	C27—N15—C28—N16	−11 (5)
O43—W10—O44—W11	−124 (2)	C31—N15—C28—N16	174 (2)
O45—W10—O44—W11	−20 (3)	C29—N16—C28—O8	179 (3)
O21—W10—O44—W11	138 (3)	C32—N16—C28—O8	9 (4)
O17—W10—O44—W11	59 (4)	C29—N16—C28—N15	5 (4)
O9—W10—O44—W11	65 (2)	C32—N16—C28—N15	−166 (2)
O43—W10—O45—W12	125 (2)	C32—N16—C29—N13	−10 (5)
O44—W10—O45—W12	18 (2)	C28—N16—C29—N13	−180 (3)
O21—W10—O45—W12	−67 (3)	C32—N16—C29—C26	170 (3)
O17—W10—O45—W12	−138 (2)	C28—N16—C29—C26	0 (4)
O9—W10—O45—W12	−66 (2)	C25—N13—C29—N16	179 (3)
O46—W11—O47—W12	−129 (3)	C25—N13—C29—C26	−1 (3)
O44—W11—O47—W12	−23 (3)	C27—C26—C29—N16	−2 (5)
O29—W11—O47—W12	130 (3)	N14—C26—C29—N16	−177 (3)
O25—W11—O47—W12	49 (4)	C27—C26—C29—N13	178 (3)
O10—W11—O47—W12	59 (3)	N14—C26—C29—N13	3 (3)
O48—W12—O47—W11	130 (3)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1N···O48^i	0.88	2.04	2.82 (4)	147
N1—H1N···O38	0.88	2.66	3.22 (3)	123
N5—H5N···O1W	0.88	1.78	2.65 (4)	169
N9—H9N···O37^ii	0.88	2.12	2.95 (3)	158
N13—H13N···O2W	0.88	1.74	2.61 (5)	174
O1W—H1W···O40^iii	0.85	2.12	2.84 (4)	142
O1W—H2W···O2	0.85	1.90	2.75 (4)	171
O2W—H3W···O46	0.85	2.02	2.73 (4)	140
O2W—H4W···O6^iv	0.85	1.92	2.76 (3)	169
O3W—H5W···O43	0.85	2.06	2.85 (4)	153
O3W—H6W···O42^v	0.85	2.20	2.98 (4)	153
C9—H9···O5^vi	0.95	2.15	3.10 (5)	176
C17—H17···O29	0.95	2.45	2.98 (5)	116
C25—H25···O1^vii	0.95	2.12	3.07 (4)	175
C6—H6A···O29^viii	0.98	2.57	3.28 (5)	129
C6—H6C···O25^viii	0.98	2.58	3.38 (4)	138
C7—H7C···O4^ix	0.98	2.53	3.49 (5)	166
C8—H8B···O37	0.98	2.53	3.33 (5)	140
C8—H8B···O15	0.98	2.74	3.55 (4)	141
C14—H14B···O22^iii	0.98	2.24	3.08 (4)	143
C14—H14C···O43	0.98	2.40	3.33 (3)	158
C14—H14C···O17	0.98	2.62	3.37 (3)	134
C15—H15B···O26^iii	0.98	2.62	3.34 (5)	130
C16—H16A···O1W	0.98	2.41	3.39 (5)	175
C16—H16B···O42^iii	0.98	2.22	3.08 (4)	146
C16—H16C···O8^x	0.98	2.33	3.20 (5)	147
C22—H22B···O20^vii	0.98	2.73	3.39 (5)	125
C22—H22C···O26	0.98	2.21	3.10 (4)	150
C23—H23B···O17^xi	0.98	2.74	3.57 (5)	143
C23—H23C···O1^xi	0.98	2.67	3.53 (5)	146
C24—H24A···O38^ii	0.98	2.71	3.33 (5)	121
C24—H24A···O48	0.98	2.77	3.50 (4)	132
C24—H24B···O41^ii	0.98	2.54	3.40 (4)	147
C30—H30B···O22	0.98	2.35	3.14 (3)	137
C30—H30C···O42^iv	0.98	2.44	3.26 (3)	140
C30—H30C···O32^iv	0.98	2.60	3.35 (3)	133
C31—H31A···O46^viii	0.98	2.77	3.46 (4)	128
C32—H32A···O43	0.98	2.75	3.21 (3)	109

Symmetry codes: (i) x+1/2, −y+1/2, z+1/2; (ii) x−1/2, −y+1/2, z−1/2; (iii) x−1/2, y−1/2, z; (iv) x−1/2, y+1/2, z; (v) x−1, y, z; (vi) x−1/2, −y+1/2, z+1/2; (vii) x, −y+1, z−1/2; (viii) x, −y+1, z+1/2; (ix) x, −y, z+1/2; (x) x+1/2, y−1/2, z; (xi) x+1/2, −y+1/2, z−1/2.

Tris(3,7-dimethylxanthinium) µ₁₂-phosphato-tetracosa-µ₂-oxido-dodecaoxidododecatungsten ethanol sesquisolvate (2)

Crystal data

(C7H9N4O2)3[PW12O40]·1.5C2H6O	F(000) = 6188
Mr = 3489.82	Dx = 3.867 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
a = 10.8071 (4) Å	Cell parameters from 29521 reflections
b = 23.4412 (13) Å	θ = 2.5–26.1°
c = 23.6644 (10) Å	µ = 23.07 mm^−1
β = 90.720 (3)°	T = 203 K
V = 5994.5 (5) Å^3	Prism, yellow
Z = 4	0.23 × 0.21 × 0.18 mm

Data collection

Stoe Image plate diffraction system diffractometer	7160 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.049
φ oscillation scans	θmax = 26.1°, θmin = 2.5°
Absorption correction: numerical [X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)]	h = −11→13
Tmin = 0.194, Tmax = 0.231	k = −28→28
29521 measured reflections	l = −29→29
11783 independent reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.051	Hydrogen site location: mixed
wR(F^2) = 0.123	H-atom parameters constrained
S = 0.93	w = 1/[σ^2(Fo^2) + (0.0616P)^2] where P = (Fo^2 + 2Fc^2)/3
11783 reflections	(Δ/σ)max = 0.001
889 parameters	Δρmax = 2.13 e Å^−3
18 restraints	Δρmin = −1.84 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
W1	0.48891 (7)	0.03984 (3)	0.32791 (3)	0.04100 (15)
W2	0.48800 (7)	0.11740 (3)	0.45730 (3)	0.04284 (17)
W3	0.76021 (7)	0.11435 (3)	0.37413 (3)	0.04061 (16)
W4	0.49793 (7)	0.11484 (4)	0.19726 (3)	0.04805 (19)
W5	0.22585 (7)	0.11844 (3)	0.27974 (3)	0.04743 (19)
W6	0.22332 (6)	0.19564 (3)	0.40993 (3)	0.04050 (15)
W7	0.49467 (6)	0.26909 (3)	0.45547 (3)	0.04010 (16)
W8	0.76745 (7)	0.26620 (3)	0.37255 (3)	0.04415 (17)
W9	0.76866 (7)	0.18964 (3)	0.24349 (3)	0.04700 (18)
W10	0.50376 (6)	0.26703 (3)	0.19552 (3)	0.03815 (16)
W11	0.23256 (7)	0.27037 (3)	0.27891 (3)	0.04191 (17)
W12	0.50288 (7)	0.34422 (3)	0.32475 (4)	0.04439 (16)
P1	0.4955 (4)	0.19255 (18)	0.32602 (18)	0.0359 (7)
O7A	0.450 (2)	0.1364 (8)	0.2959 (8)	0.032 (4)	0.5
O8A	0.4472 (19)	0.1927 (8)	0.3862 (8)	0.033 (4)	0.5
O9A	0.641 (2)	0.1887 (9)	0.3286 (8)	0.035 (4)	0.5
O10A	0.4498 (17)	0.2451 (8)	0.2947 (8)	0.027 (4)	0.5
O7B	0.537 (2)	0.1419 (9)	0.3566 (8)	0.040 (5)	0.5
O8B	0.351 (2)	0.1963 (9)	0.3269 (9)	0.036 (5)	0.5
O9B	0.543 (2)	0.1945 (9)	0.2667 (9)	0.039 (5)	0.5
O10B	0.542 (2)	0.2493 (10)	0.3568 (8)	0.038 (5)	0.5
O11	0.4880 (16)	−0.0315 (6)	0.3289 (9)	0.082 (5)
O12	0.4577 (14)	0.0609 (8)	0.4028 (7)	0.078 (5)
O13	0.6575 (14)	0.0554 (7)	0.3432 (6)	0.069 (4)
O14	0.5233 (15)	0.0555 (10)	0.2511 (7)	0.099 (7)
O15	0.3233 (15)	0.0588 (10)	0.3112 (6)	0.092 (6)
O16	0.4809 (13)	0.0822 (7)	0.5184 (5)	0.061 (4)
O17	0.6580 (15)	0.1128 (7)	0.4379 (7)	0.073 (4)
O18	0.5166 (13)	0.1933 (6)	0.4797 (9)	0.086 (6)
O19	0.3200 (15)	0.1411 (6)	0.4475 (9)	0.084 (6)
O20	0.8808 (14)	0.0772 (7)	0.3949 (7)	0.074 (4)
O21	0.804 (2)	0.1347 (7)	0.2993 (6)	0.101 (7)
O22	0.801 (2)	0.1904 (6)	0.3936 (5)	0.087 (6)
O23	0.4978 (16)	0.0792 (7)	0.1362 (6)	0.070 (4)
O24	0.3237 (15)	0.1135 (10)	0.2159 (8)	0.098 (7)
O25	0.4742 (12)	0.1911 (7)	0.1720 (9)	0.083 (5)
O26	0.6661 (15)	0.1342 (6)	0.2074 (9)	0.082 (5)
O27	0.0982 (12)	0.0837 (6)	0.2573 (6)	0.057 (3)
O28	0.197 (2)	0.1948 (6)	0.2586 (5)	0.091 (6)
O29	0.187 (2)	0.1412 (6)	0.3550 (5)	0.083 (6)
O30	0.0948 (12)	0.1993 (5)	0.4480 (6)	0.054 (3)
O31	0.3240 (14)	0.2518 (5)	0.4458 (8)	0.071 (5)
O32	0.191 (2)	0.2503 (5)	0.3542 (6)	0.084 (6)
O33	0.4965 (14)	0.3063 (8)	0.5157 (6)	0.074 (4)
O34	0.4707 (14)	0.3288 (9)	0.4019 (8)	0.099 (7)
O35	0.6673 (16)	0.2695 (9)	0.4355 (8)	0.106 (8)
O36	0.8939 (11)	0.3011 (6)	0.3940 (5)	0.057 (3)
O37	0.812 (2)	0.2445 (6)	0.2985 (6)	0.102 (8)
O38	0.6699 (15)	0.3274 (9)	0.3401 (7)	0.091 (6)
O39	0.8957 (13)	0.1885 (6)	0.2053 (6)	0.059 (3)
O40	0.6707 (15)	0.2457 (6)	0.2055 (8)	0.079 (5)
O41	0.5038 (19)	0.3019 (10)	0.1344 (6)	0.109 (8)
O42	0.3332 (15)	0.2721 (7)	0.2140 (7)	0.072 (4)
O43	0.5356 (13)	0.3261 (7)	0.2480 (8)	0.080 (5)
O44	0.1095 (12)	0.3063 (7)	0.2575 (5)	0.061 (4)
O45	0.3330 (14)	0.3294 (7)	0.3092 (7)	0.071 (5)
O46	0.5046 (13)	0.4163 (5)	0.3253 (6)	0.056 (3)
O1	0.4129 (12)	0.4920 (5)	0.4361 (5)	0.046 (3)
O2	0.3852 (14)	0.3926 (5)	0.5997 (5)	0.053 (3)
N1	0.1096 (14)	0.3567 (6)	0.4497 (6)	0.041 (3)
H1N	0.061153	0.330273	0.462798	0.062*
N2	0.1902 (13)	0.4194 (5)	0.3928 (5)	0.036 (3)
N3	0.3954 (13)	0.4403 (6)	0.5160 (6)	0.045 (3)
H3N	0.456189	0.460424	0.529894	0.067*
N4	0.2496 (13)	0.3682 (6)	0.5310 (5)	0.038 (3)
C1	0.0985 (17)	0.3819 (7)	0.3977 (7)	0.046 (4)
H1	0.037075	0.374149	0.370317	0.056*
C2	0.2609 (16)	0.4197 (7)	0.4430 (6)	0.038 (3)
C3	0.3616 (15)	0.4533 (7)	0.4618 (7)	0.039 (4)
C4	0.3479 (18)	0.4001 (7)	0.5521 (8)	0.046 (4)
C5	0.2079 (15)	0.3794 (7)	0.4772 (7)	0.038 (3)
C6	0.2041 (19)	0.4576 (8)	0.3447 (7)	0.049 (4)
H6A	0.277301	0.480998	0.350319	0.073*
H6B	0.212557	0.435315	0.310469	0.073*
H6C	0.131795	0.481929	0.341442	0.073*
C7	0.1990 (19)	0.3187 (7)	0.5629 (8)	0.050 (4)
H7A	0.238113	0.316852	0.599985	0.074*
H7B	0.110356	0.323256	0.567054	0.074*
H7C	0.215578	0.283686	0.542451	0.074*
O3	0.4177 (12)	0.1817 (5)	0.0167 (5)	0.049 (3)
O4	0.3727 (15)	0.3733 (6)	0.0310 (6)	0.061 (4)
N5	0.1054 (14)	0.2487 (6)	0.1272 (6)	0.044 (3)
H5N	0.055427	0.271116	0.145340	0.066*
N6	0.1929 (13)	0.1725 (6)	0.0960 (6)	0.041 (3)
N7	0.3849 (14)	0.2775 (7)	0.0232 (6)	0.047 (3)
H7N	0.442012	0.282726	−0.001862	0.071*
N8	0.2367 (13)	0.3194 (6)	0.0818 (6)	0.040 (3)
C8	0.1033 (16)	0.1904 (7)	0.1268 (7)	0.040 (4)
H8	0.046119	0.167238	0.145753	0.048*
C9	0.2561 (14)	0.2178 (7)	0.0736 (6)	0.035 (3)
C10	0.3586 (15)	0.2217 (9)	0.0346 (6)	0.042 (4)
C11	0.3357 (16)	0.3266 (8)	0.0449 (8)	0.045 (4)
C12	0.1999 (14)	0.2649 (7)	0.0941 (7)	0.037 (4)
C13	0.2136 (19)	0.1107 (8)	0.0830 (8)	0.052 (5)
H13A	0.285684	0.106824	0.059339	0.078*
H13B	0.226831	0.089869	0.117959	0.078*
H13C	0.141542	0.095547	0.063322	0.078*
C14	0.1866 (18)	0.3690 (8)	0.1124 (9)	0.055 (5)
H14A	0.223472	0.403676	0.097960	0.082*
H14B	0.097595	0.370478	0.106981	0.082*
H14C	0.205952	0.365333	0.152393	0.082*
O5	0.8945 (14)	0.4151 (6)	0.3115 (5)	0.060 (3)
O6	0.9017 (12)	0.3149 (5)	0.1470 (5)	0.051 (3)
N9	0.6153 (14)	0.4618 (5)	0.1714 (6)	0.043 (3)
H9N	0.574933	0.462242	0.139363	0.064*
N10	0.6779 (16)	0.4843 (7)	0.2572 (7)	0.055 (4)
N11	0.8876 (14)	0.3638 (6)	0.2297 (7)	0.044 (3)
H11N	0.941866	0.340741	0.244605	0.067*
N12	0.7569 (15)	0.3839 (6)	0.1512 (6)	0.047 (4)
C15	0.5972 (19)	0.4964 (8)	0.2152 (10)	0.058 (5)
H15	0.536647	0.525109	0.216475	0.069*
C16	0.7470 (15)	0.4388 (7)	0.2378 (7)	0.041 (4)
C17	0.846 (2)	0.4088 (8)	0.2654 (8)	0.054 (5)
C18	0.8528 (16)	0.3523 (6)	0.1742 (8)	0.042 (4)
C19	0.7075 (15)	0.4260 (7)	0.1860 (7)	0.040 (4)
C20	0.684 (2)	0.5135 (9)	0.3110 (9)	0.062 (5)
H20A	0.749716	0.497102	0.334087	0.093*
H20B	0.700755	0.553685	0.304839	0.093*
H20C	0.605725	0.509359	0.330166	0.093*
C21	0.722 (2)	0.3781 (8)	0.0913 (8)	0.055 (5)
H21A	0.652799	0.403443	0.082744	0.082*
H21B	0.791351	0.388067	0.067873	0.082*
H21C	0.697027	0.339022	0.083611	0.082*
O47	0.4514 (16)	0.4661 (7)	0.0892 (7)	0.082 (5)*
H1O	0.426758	0.436971	0.070890	0.124*
C22	0.364 (3)	0.5112 (11)	0.0809 (11)	0.100 (9)*
H22A	0.404496	0.547692	0.089502	0.120*
H22B	0.295767	0.506279	0.107205	0.120*
C23	0.314 (4)	0.5126 (19)	0.0220 (14)	0.171 (19)*
H23A	0.255767	0.543716	0.018169	0.256*
H23B	0.381798	0.518181	−0.004095	0.256*
H23C	0.273111	0.476783	0.013601	0.256*
O48	0.891 (5)	0.501 (2)	0.458 (3)	0.166 (19)*	0.5
H2O	0.919711	0.519262	0.429934	0.249*	0.5
C24	0.862 (5)	0.442 (2)	0.439 (4)	0.159 (19)*	0.5
H24A	0.894194	0.436619	0.401230	0.191*	0.5
H24B	0.904689	0.415244	0.464609	0.191*	0.5
C25	0.733 (6)	0.430 (3)	0.439 (3)	0.120 (19)*	0.5
H25A	0.718892	0.391540	0.426732	0.180*	0.5
H25B	0.701139	0.435188	0.477082	0.180*	0.5
H25C	0.690643	0.456563	0.413704	0.180*	0.5

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
W1	0.0420 (4)	0.0382 (3)	0.0428 (3)	0.0024 (3)	0.0017 (3)	0.0015 (3)
W2	0.0446 (4)	0.0497 (4)	0.0341 (4)	0.0023 (3)	−0.0023 (3)	0.0092 (3)
W3	0.0408 (4)	0.0455 (4)	0.0354 (3)	0.0084 (3)	−0.0026 (3)	0.0004 (3)
W4	0.0383 (4)	0.0700 (5)	0.0358 (4)	0.0016 (3)	−0.0033 (3)	−0.0178 (3)
W5	0.0417 (4)	0.0616 (4)	0.0389 (4)	−0.0165 (3)	−0.0045 (3)	−0.0001 (3)
W6	0.0385 (3)	0.0452 (3)	0.0380 (3)	0.0000 (3)	0.0072 (3)	−0.0015 (3)
W7	0.0377 (4)	0.0526 (4)	0.0300 (3)	0.0058 (3)	−0.0039 (3)	−0.0078 (3)
W8	0.0387 (4)	0.0586 (4)	0.0349 (4)	−0.0120 (3)	−0.0076 (3)	0.0000 (3)
W9	0.0408 (4)	0.0576 (4)	0.0428 (4)	−0.0094 (3)	0.0112 (3)	−0.0135 (3)
W10	0.0401 (4)	0.0453 (3)	0.0289 (3)	−0.0024 (3)	−0.0038 (3)	0.0038 (3)
W11	0.0434 (4)	0.0417 (3)	0.0403 (4)	0.0036 (3)	−0.0131 (3)	0.0010 (3)
W12	0.0404 (4)	0.0391 (3)	0.0537 (4)	−0.0006 (3)	−0.0014 (3)	0.0061 (3)
P1	0.0372 (19)	0.0366 (17)	0.0340 (18)	−0.0035 (19)	−0.0018 (15)	−0.0029 (19)
O7A	0.048 (11)	0.034 (7)	0.015 (8)	0.014 (8)	−0.003 (8)	−0.009 (7)
O8A	0.035 (10)	0.033 (9)	0.029 (7)	0.017 (9)	−0.005 (7)	−0.004 (7)
O9A	0.040 (7)	0.038 (10)	0.027 (9)	0.014 (8)	−0.005 (7)	−0.001 (9)
O10A	0.018 (8)	0.042 (7)	0.021 (8)	−0.006 (7)	−0.004 (7)	0.000 (7)
O7B	0.053 (14)	0.046 (12)	0.022 (10)	0.032 (10)	−0.009 (10)	−0.006 (9)
O8B	0.035 (11)	0.042 (11)	0.031 (10)	0.008 (9)	−0.005 (9)	−0.010 (9)
O9B	0.055 (14)	0.029 (9)	0.033 (10)	−0.002 (10)	−0.014 (10)	0.006 (9)
O10B	0.032 (11)	0.064 (14)	0.017 (9)	0.003 (10)	−0.002 (8)	−0.017 (9)
O11	0.072 (10)	0.055 (8)	0.119 (14)	−0.016 (8)	0.036 (10)	−0.030 (9)
O12	0.044 (8)	0.122 (13)	0.067 (10)	−0.008 (9)	0.011 (7)	−0.021 (10)
O13	0.063 (9)	0.100 (11)	0.044 (8)	−0.010 (8)	0.006 (7)	−0.014 (7)
O14	0.050 (9)	0.19 (2)	0.052 (9)	0.035 (11)	0.007 (7)	0.026 (11)
O15	0.054 (9)	0.183 (19)	0.041 (8)	0.035 (11)	0.015 (7)	0.038 (10)
O16	0.058 (8)	0.087 (9)	0.037 (7)	−0.009 (7)	0.002 (6)	0.012 (7)
O17	0.068 (10)	0.087 (10)	0.063 (9)	−0.019 (8)	0.012 (8)	−0.032 (8)
O18	0.039 (8)	0.054 (7)	0.163 (17)	−0.001 (6)	−0.029 (9)	−0.006 (10)
O19	0.061 (10)	0.048 (8)	0.141 (17)	−0.013 (7)	−0.040 (10)	−0.010 (9)
O20	0.064 (10)	0.081 (10)	0.075 (10)	0.032 (8)	−0.026 (8)	−0.017 (9)
O21	0.20 (2)	0.066 (9)	0.037 (8)	−0.045 (12)	0.024 (11)	−0.016 (7)
O22	0.19 (2)	0.048 (7)	0.025 (6)	−0.031 (10)	0.021 (8)	−0.001 (6)
O23	0.087 (12)	0.076 (9)	0.048 (8)	0.000 (9)	−0.003 (7)	−0.023 (8)
O24	0.043 (9)	0.170 (18)	0.081 (12)	0.026 (10)	0.013 (8)	0.043 (12)
O25	0.035 (8)	0.066 (8)	0.147 (16)	0.009 (7)	−0.022 (9)	−0.036 (10)
O26	0.063 (10)	0.038 (7)	0.144 (16)	0.003 (6)	−0.040 (10)	−0.010 (9)
O27	0.034 (6)	0.065 (8)	0.073 (9)	−0.017 (6)	−0.006 (6)	0.008 (7)
O28	0.20 (2)	0.045 (7)	0.025 (6)	−0.032 (10)	−0.006 (9)	0.003 (6)
O29	0.177 (19)	0.046 (7)	0.025 (6)	−0.007 (9)	−0.002 (9)	0.013 (5)
O30	0.049 (7)	0.044 (6)	0.070 (9)	0.011 (5)	0.010 (6)	0.011 (6)
O31	0.054 (9)	0.045 (7)	0.114 (13)	0.006 (6)	−0.035 (8)	0.003 (8)
O32	0.176 (19)	0.037 (7)	0.037 (7)	−0.022 (9)	−0.025 (9)	−0.010 (6)
O33	0.059 (9)	0.108 (11)	0.053 (8)	0.031 (9)	−0.022 (7)	−0.020 (9)
O34	0.047 (9)	0.154 (16)	0.099 (13)	0.046 (10)	0.014 (9)	0.081 (12)
O35	0.062 (10)	0.159 (18)	0.098 (14)	0.032 (11)	0.021 (10)	0.093 (13)
O36	0.036 (6)	0.083 (9)	0.052 (7)	−0.022 (7)	−0.005 (6)	0.011 (7)
O37	0.22 (2)	0.050 (8)	0.037 (8)	−0.034 (11)	0.006 (11)	0.006 (6)
O38	0.056 (10)	0.152 (17)	0.064 (10)	0.025 (10)	0.014 (8)	0.052 (11)
O39	0.048 (7)	0.072 (8)	0.056 (8)	0.009 (7)	0.006 (6)	0.004 (7)
O40	0.064 (10)	0.052 (8)	0.122 (15)	−0.003 (7)	−0.025 (9)	−0.035 (9)
O41	0.117 (15)	0.164 (18)	0.046 (8)	−0.079 (14)	−0.036 (9)	0.054 (11)
O42	0.063 (9)	0.078 (10)	0.077 (10)	−0.013 (7)	0.015 (8)	−0.041 (8)
O43	0.035 (7)	0.106 (12)	0.101 (12)	−0.022 (7)	0.023 (8)	−0.059 (10)
O44	0.043 (7)	0.089 (10)	0.049 (7)	0.023 (7)	−0.007 (6)	0.004 (8)
O45	0.056 (9)	0.090 (10)	0.067 (9)	−0.027 (8)	0.019 (7)	−0.046 (8)
O46	0.050 (7)	0.047 (6)	0.070 (8)	−0.019 (6)	0.005 (6)	−0.013 (7)
O1	0.060 (8)	0.038 (6)	0.039 (6)	−0.008 (5)	−0.011 (6)	0.004 (5)
O2	0.075 (9)	0.046 (6)	0.036 (6)	0.001 (6)	−0.017 (6)	−0.002 (5)
N1	0.044 (8)	0.047 (7)	0.033 (7)	−0.009 (6)	0.002 (6)	−0.002 (6)
N2	0.044 (8)	0.030 (6)	0.034 (6)	−0.004 (5)	−0.016 (6)	−0.001 (5)
N3	0.038 (8)	0.040 (7)	0.056 (9)	−0.007 (6)	−0.004 (7)	0.008 (6)
N4	0.043 (8)	0.052 (7)	0.019 (6)	−0.005 (6)	0.001 (5)	0.008 (6)
C1	0.044 (10)	0.058 (10)	0.036 (9)	−0.003 (8)	−0.013 (8)	0.008 (8)
C2	0.048 (9)	0.041 (8)	0.025 (7)	−0.011 (7)	−0.002 (7)	−0.005 (6)
C3	0.033 (8)	0.046 (9)	0.037 (8)	0.005 (7)	−0.007 (7)	−0.002 (7)
C4	0.052 (11)	0.036 (8)	0.051 (11)	0.007 (7)	−0.004 (8)	−0.004 (7)
C5	0.036 (9)	0.043 (8)	0.034 (8)	0.003 (6)	−0.009 (7)	0.004 (6)
C6	0.058 (12)	0.048 (9)	0.039 (9)	−0.005 (8)	−0.005 (8)	0.004 (8)
C7	0.062 (12)	0.044 (9)	0.044 (9)	−0.009 (8)	0.016 (9)	0.009 (7)
O3	0.045 (7)	0.061 (7)	0.042 (6)	0.016 (6)	0.011 (5)	−0.009 (6)
O4	0.078 (10)	0.050 (7)	0.055 (8)	−0.013 (7)	−0.006 (7)	0.002 (6)
N5	0.041 (8)	0.060 (8)	0.030 (7)	−0.003 (7)	0.008 (6)	−0.011 (6)
N6	0.028 (7)	0.045 (7)	0.049 (8)	0.006 (6)	0.002 (6)	−0.001 (6)
N7	0.037 (8)	0.062 (9)	0.043 (8)	−0.010 (7)	−0.002 (6)	0.007 (7)
N8	0.041 (8)	0.046 (8)	0.034 (7)	−0.005 (6)	−0.008 (6)	0.003 (6)
C8	0.046 (9)	0.037 (8)	0.038 (8)	−0.011 (7)	0.006 (7)	0.016 (7)
C9	0.030 (8)	0.045 (8)	0.031 (8)	0.004 (6)	−0.010 (6)	0.010 (6)
C10	0.028 (8)	0.090 (13)	0.010 (6)	0.001 (8)	−0.004 (6)	0.002 (7)
C11	0.034 (9)	0.064 (11)	0.038 (9)	0.000 (8)	−0.005 (7)	0.006 (8)
C12	0.023 (7)	0.046 (8)	0.041 (9)	0.003 (6)	−0.013 (7)	−0.017 (7)
C13	0.051 (11)	0.063 (11)	0.042 (10)	0.015 (9)	−0.007 (8)	−0.011 (8)
C14	0.043 (10)	0.058 (10)	0.062 (12)	0.006 (8)	0.002 (9)	−0.028 (9)
O5	0.066 (9)	0.070 (8)	0.044 (7)	−0.006 (7)	−0.012 (6)	0.000 (6)
O6	0.046 (7)	0.057 (7)	0.051 (7)	0.007 (6)	0.006 (6)	−0.004 (6)
N9	0.052 (9)	0.035 (7)	0.040 (8)	−0.003 (6)	−0.004 (6)	0.002 (6)
N10	0.051 (9)	0.053 (9)	0.061 (10)	−0.004 (7)	0.008 (8)	−0.005 (8)
N11	0.043 (8)	0.033 (7)	0.056 (9)	−0.007 (6)	−0.019 (7)	0.013 (6)
N12	0.049 (9)	0.046 (8)	0.045 (8)	0.006 (6)	−0.009 (7)	0.008 (6)
C15	0.042 (11)	0.050 (10)	0.081 (15)	0.005 (8)	0.001 (10)	0.002 (10)
C16	0.028 (8)	0.055 (9)	0.039 (9)	0.006 (7)	0.002 (7)	0.016 (8)
C17	0.069 (13)	0.045 (10)	0.048 (11)	−0.014 (9)	−0.004 (10)	0.018 (8)
C18	0.043 (9)	0.031 (7)	0.052 (10)	−0.006 (7)	−0.008 (8)	−0.003 (7)
C19	0.036 (8)	0.034 (8)	0.050 (9)	0.004 (6)	0.002 (7)	0.015 (7)
C20	0.071 (14)	0.056 (11)	0.059 (12)	−0.014 (10)	0.008 (11)	−0.017 (10)
C21	0.064 (13)	0.055 (10)	0.046 (10)	0.007 (9)	−0.016 (9)	0.016 (8)

Geometric parameters (Å, º)

W1—O11	1.673 (14)	P1—O9A	1.58 (2)
W1—O12	1.875 (15)	P1—O10B	1.59 (2)
W1—O15	1.881 (15)	O1—C3	1.23 (2)
W1—O13	1.888 (15)	O2—C4	1.21 (2)
W1—O14	1.896 (16)	N1—C5	1.35 (2)
W1—O7A	2.424 (19)	N1—C1	1.37 (2)
W2—O16	1.668 (13)	N1—H1N	0.8700
W2—O12	1.875 (16)	N2—C1	1.33 (2)
W2—O18	1.881 (15)	N2—C2	1.403 (19)
W2—O17	1.903 (16)	N2—C6	1.46 (2)
W2—O19	1.910 (16)	N3—C3	1.37 (2)
W2—O8A	2.474 (19)	N3—C4	1.37 (2)
W2—O7B	2.51 (2)	N3—H3N	0.8700
W3—O20	1.638 (13)	N4—C5	1.370 (19)
W3—O17	1.881 (15)	N4—C4	1.39 (2)
W3—O22	1.891 (13)	N4—C7	1.49 (2)
W3—O21	1.902 (15)	C1—H1	0.9400
W3—O13	1.912 (15)	C2—C5	1.37 (2)
W3—O9A	2.412 (19)	C2—C3	1.41 (2)
W3—O7B	2.53 (2)	C6—H6A	0.9700
W4—O23	1.668 (13)	C6—H6B	0.9700
W4—O26	1.886 (16)	C6—H6C	0.9700
W4—O25	1.902 (17)	C7—H7A	0.9700
W4—O14	1.904 (19)	C7—H7B	0.9700
W4—O24	1.939 (16)	C7—H7C	0.9700
W4—O7A	2.450 (18)	O3—C10	1.21 (2)
W5—O27	1.683 (12)	O4—C11	1.21 (2)
W5—O24	1.859 (17)	N5—C12	1.35 (2)
W5—O28	1.884 (15)	N5—C8	1.37 (2)
W5—O15	1.897 (17)	N5—H5N	0.8700
W5—O29	1.911 (14)	N6—C8	1.29 (2)
W5—O7A	2.48 (2)	N6—C9	1.37 (2)
W5—O8B	2.52 (2)	N6—C13	1.50 (2)
W6—O30	1.667 (13)	N7—C10	1.37 (2)
W6—O29	1.861 (14)	N7—C11	1.37 (2)
W6—O19	1.868 (16)	N7—H7N	0.8700
W6—O32	1.870 (14)	N8—C12	1.37 (2)
W6—O31	1.901 (14)	N8—C11	1.40 (2)
W6—O8B	2.41 (2)	N8—C14	1.48 (2)
W6—O8A	2.49 (2)	C8—H8	0.9400
W7—O33	1.670 (14)	C9—C12	1.35 (2)
W7—O18	1.882 (16)	C9—C10	1.45 (2)
W7—O31	1.900 (15)	C13—H13A	0.9700
W7—O34	1.904 (15)	C13—H13B	0.9700
W7—O35	1.930 (17)	C13—H13C	0.9700
W7—O10B	2.442 (19)	C14—H14A	0.9700
W7—O8A	2.477 (19)	C14—H14B	0.9700
W8—O36	1.666 (12)	C14—H14C	0.9700
W8—O35	1.854 (18)	O5—C17	1.21 (2)
W8—O22	1.879 (15)	O6—C18	1.21 (2)
W8—O37	1.893 (16)	N9—C15	1.33 (3)
W8—O38	1.933 (17)	N9—C19	1.34 (2)
W8—O9A	2.49 (2)	N9—H9N	0.8700
W8—O10B	2.49 (2)	N10—C15	1.34 (3)
W9—O39	1.654 (14)	N10—C16	1.38 (2)
W9—O21	1.881 (19)	N10—C20	1.45 (3)
W9—O37	1.884 (16)	N11—C18	1.39 (2)
W9—O26	1.904 (14)	N11—C17	1.43 (3)
W9—O40	1.905 (17)	N11—H11N	0.8700
W9—O9A	2.45 (2)	N12—C18	1.38 (2)
W9—O9B	2.50 (2)	N12—C19	1.40 (2)
W10—O41	1.661 (14)	N12—C21	1.47 (2)
W10—O40	1.885 (16)	C15—H15	0.9400
W10—O43	1.888 (14)	C16—C19	1.33 (2)
W10—O25	1.891 (14)	C16—C17	1.43 (3)
W10—O42	1.903 (16)	C20—H20A	0.9700
W10—O9B	2.429 (19)	C20—H20B	0.9700
W10—O10A	2.478 (18)	C20—H20C	0.9700
W11—O44	1.649 (12)	C21—H21A	0.9700
W11—O28	1.873 (13)	C21—H21B	0.9700
W11—O45	1.894 (13)	C21—H21C	0.9700
W11—O42	1.894 (15)	O47—C22	1.427 (10)
W11—O32	1.901 (15)	O47—H1O	0.8500
W11—O8B	2.43 (2)	C22—C23	1.489 (10)
W11—O10A	2.445 (18)	C22—H22A	0.9800
W12—O46	1.689 (12)	C22—H22B	0.9800
W12—O38	1.879 (16)	C23—H23A	0.9700
W12—O34	1.897 (17)	C23—H23B	0.9700
W12—O45	1.900 (15)	C23—H23C	0.9700
W12—O43	1.903 (16)	O48—C24	1.488 (10)
W12—O10B	2.39 (2)	O48—H2O	0.8500
W12—O10A	2.495 (19)	C24—C25	1.426 (10)
P1—O7B	1.46 (2)	C24—H24A	0.9800
P1—O9B	1.50 (2)	C24—H24B	0.9800
P1—O10A	1.518 (19)	C25—H25A	0.9700
P1—O8A	1.52 (2)	C25—H25B	0.9700
P1—O8B	1.57 (2)	C25—H25C	0.9700
P1—O7A	1.57 (2)
O11—W1—O12	104.4 (9)	O45—W12—O10B	93.3 (7)
O11—W1—O15	103.5 (10)	O43—W12—O10B	93.5 (7)
O12—W1—O15	87.4 (7)	O46—W12—O10A	159.4 (7)
O11—W1—O13	101.3 (8)	O38—W12—O10A	94.4 (8)
O12—W1—O13	87.3 (6)	O34—W12—O10A	93.0 (8)
O15—W1—O13	155.1 (9)	O45—W12—O10A	63.6 (6)
O11—W1—O14	102.0 (10)	O43—W12—O10A	64.2 (7)
O12—W1—O14	153.6 (9)	O7B—P1—O9B	112.3 (12)
O15—W1—O14	87.2 (6)	O10A—P1—O8A	110.0 (10)
O13—W1—O14	86.9 (7)	O7B—P1—O8B	109.9 (13)
O11—W1—O7A	159.6 (9)	O9B—P1—O8B	111.5 (12)
O12—W1—O7A	91.0 (7)	O10A—P1—O8B	69.0 (11)
O15—W1—O7A	63.3 (9)	O10A—P1—O7A	110.9 (9)
O13—W1—O7A	92.5 (7)	O8A—P1—O7A	108.4 (11)
O14—W1—O7A	63.6 (8)	O10A—P1—O9A	112.6 (10)
O16—W2—O12	103.7 (8)	O7A—P1—O9A	106.2 (11)
O16—W2—O18	103.4 (8)	O7B—P1—O10B	111.1 (11)
O12—W2—O18	152.8 (9)	O9B—P1—O10B	106.9 (11)
O16—W2—O17	103.7 (7)	O8B—P1—O10B	104.9 (11)
O12—W2—O17	87.4 (6)	P1—O7A—W1	125.8 (10)
O18—W2—O17	88.0 (7)	P1—O7A—W4	122.3 (12)
O16—W2—O19	101.3 (8)	W1—O7A—W4	93.8 (6)
O12—W2—O19	88.0 (7)	P1—O7A—W5	120.9 (10)
O18—W2—O19	84.9 (6)	W1—O7A—W5	93.2 (7)
O17—W2—O19	155.0 (8)	W4—O7A—W5	92.2 (6)
O16—W2—O8A	158.9 (7)	P1—O8A—W2	125.0 (10)
O12—W2—O8A	90.5 (7)	P1—O8A—W7	123.3 (12)
O18—W2—O8A	62.9 (7)	W2—O8A—W7	91.9 (6)
O17—W2—O8A	92.3 (7)	P1—O8A—W6	123.8 (10)
O19—W2—O8A	63.2 (7)	W2—O8A—W6	91.8 (7)
O16—W2—O7B	161.3 (7)	W7—O8A—W6	91.4 (6)
O12—W2—O7B	63.0 (7)	P1—O9A—W3	125.7 (12)
O18—W2—O7B	90.9 (8)	P1—O9A—W9	122.5 (10)
O17—W2—O7B	64.4 (7)	W3—O9A—W9	94.1 (7)
O19—W2—O7B	91.7 (8)	P1—O9A—W8	121.0 (10)
O8A—W2—O7B	39.7 (6)	W3—O9A—W8	93.1 (7)
O20—W3—O17	102.8 (8)	W9—O9A—W8	91.5 (8)
O20—W3—O22	104.3 (9)	P1—O10A—W11	125.3 (10)
O17—W3—O22	87.7 (6)	P1—O10A—W10	123.5 (11)
O20—W3—O21	101.8 (10)	W11—O10A—W10	92.4 (6)
O17—W3—O21	155.4 (10)	P1—O10A—W12	122.9 (10)
O22—W3—O21	86.0 (6)	W11—O10A—W12	92.0 (7)
O20—W3—O13	100.8 (8)	W10—O10A—W12	91.2 (6)
O17—W3—O13	87.1 (6)	P1—O7B—W2	126.0 (11)
O22—W3—O13	154.9 (8)	P1—O7B—W3	125.2 (15)
O21—W3—O13	88.6 (7)	W2—O7B—W3	89.9 (6)
O20—W3—O9A	159.3 (9)	P1—O8B—W6	126.2 (11)
O17—W3—O9A	93.3 (8)	P1—O8B—W11	123.6 (12)
O22—W3—O9A	63.1 (8)	W6—O8B—W11	94.8 (7)
O21—W3—O9A	62.7 (9)	P1—O8B—W5	118.8 (10)
O13—W3—O9A	92.7 (7)	W6—O8B—W5	92.8 (8)
O20—W3—O7B	160.0 (9)	W11—O8B—W5	92.0 (7)
O17—W3—O7B	64.4 (7)	P1—O9B—W10	127.5 (12)
O22—W3—O7B	91.0 (9)	P1—O9B—W9	123.4 (11)
O21—W3—O7B	91.9 (9)	W10—O9B—W9	92.5 (8)
O13—W3—O7B	64.7 (7)	P1—O10B—W12	125.4 (11)
O9A—W3—O7B	40.5 (8)	P1—O10B—W7	121.7 (12)
O23—W4—O26	102.8 (8)	W12—O10B—W7	95.0 (7)
O23—W4—O25	101.5 (8)	P1—O10B—W8	120.3 (11)
O26—W4—O25	86.6 (6)	W12—O10B—W8	93.9 (8)
O23—W4—O14	102.2 (8)	W7—O10B—W8	92.5 (6)
O26—W4—O14	87.7 (8)	W2—O12—W1	143.5 (10)
O25—W4—O14	156.2 (9)	W1—O13—W3	140.1 (9)
O23—W4—O24	101.4 (9)	W1—O14—W4	139.0 (12)
O26—W4—O24	155.8 (9)	W1—O15—W5	141.1 (12)
O25—W4—O24	87.6 (8)	W3—O17—W2	140.4 (10)
O14—W4—O24	88.2 (7)	W2—O18—W7	141.9 (11)
O23—W4—O7A	158.4 (8)	W6—O19—W2	141.4 (11)
O26—W4—O7A	92.6 (8)	W9—O21—W3	140.7 (13)
O25—W4—O7A	94.4 (7)	W8—O22—W3	141.6 (11)
O14—W4—O7A	62.9 (7)	W5—O24—W4	138.4 (11)
O24—W4—O7A	64.4 (8)	W10—O25—W4	140.4 (10)
O27—W5—O24	100.7 (8)	W4—O26—W9	140.9 (10)
O27—W5—O28	104.1 (8)	W11—O28—W5	142.9 (9)
O24—W5—O28	86.4 (8)	W6—O29—W5	142.6 (10)
O27—W5—O15	102.5 (8)	W7—O31—W6	138.6 (9)
O24—W5—O15	87.4 (7)	W6—O32—W11	141.9 (11)
O28—W5—O15	153.4 (9)	W12—O34—W7	139.1 (11)
O27—W5—O29	103.8 (8)	W8—O35—W7	140.6 (12)
O24—W5—O29	155.4 (9)	W9—O37—W8	139.4 (11)
O28—W5—O29	86.8 (6)	W12—O38—W8	138.6 (11)
O15—W5—O29	88.1 (7)	W10—O40—W9	140.1 (11)
O27—W5—O7A	157.7 (6)	W11—O42—W10	138.8 (10)
O24—W5—O7A	64.7 (7)	W10—O43—W12	139.2 (10)
O28—W5—O7A	92.1 (8)	W11—O45—W12	139.0 (9)
O15—W5—O7A	61.9 (7)	C5—N1—C1	108.8 (14)
O29—W5—O7A	92.0 (8)	C5—N1—H1N	125.6
O27—W5—O8B	157.3 (7)	C1—N1—H1N	125.6
O24—W5—O8B	95.6 (9)	C1—N2—C2	109.1 (13)
O28—W5—O8B	61.0 (7)	C1—N2—C6	123.9 (13)
O15—W5—O8B	93.9 (8)	C2—N2—C6	126.6 (13)
O29—W5—O8B	60.6 (7)	C3—N3—C4	129.8 (15)
O7A—W5—O8B	45.0 (6)	C3—N3—H3N	115.1
O30—W6—O29	104.0 (8)	C4—N3—H3N	115.1
O30—W6—O19	104.0 (8)	C5—N4—C4	118.1 (14)
O29—W6—O19	88.6 (7)	C5—N4—C7	120.1 (15)
O30—W6—O32	101.4 (8)	C4—N4—C7	121.4 (14)
O29—W6—O32	86.6 (5)	N2—C1—N1	107.9 (14)
O19—W6—O32	154.5 (9)	N2—C1—H1	126.1
O30—W6—O31	101.5 (7)	N1—C1—H1	126.1
O29—W6—O31	154.5 (8)	C5—C2—N2	105.6 (14)
O19—W6—O31	87.0 (6)	C5—C2—C3	121.5 (14)
O32—W6—O31	86.6 (6)	N2—C2—C3	132.8 (14)
O30—W6—O8B	158.0 (7)	O1—C3—N3	120.9 (15)
O29—W6—O8B	63.5 (7)	O1—C3—C2	127.4 (15)
O19—W6—O8B	94.0 (8)	N3—C3—C2	111.6 (15)
O32—W6—O8B	61.6 (8)	O2—C4—N3	123.9 (18)
O31—W6—O8B	91.7 (8)	O2—C4—N4	120.1 (17)
O30—W6—O8A	160.2 (7)	N3—C4—N4	115.9 (15)
O29—W6—O8A	91.2 (8)	N1—C5—N4	128.3 (15)
O19—W6—O8A	63.2 (7)	N1—C5—C2	108.6 (14)
O32—W6—O8A	91.9 (8)	N4—C5—C2	123.0 (15)
O31—W6—O8A	64.4 (7)	N2—C6—H6A	109.5
O8B—W6—O8A	41.5 (6)	N2—C6—H6B	109.5
O33—W7—O18	103.4 (9)	H6A—C6—H6B	109.5
O33—W7—O31	102.4 (8)	N2—C6—H6C	109.5
O18—W7—O31	87.4 (6)	H6A—C6—H6C	109.5
O33—W7—O34	100.6 (9)	H6B—C6—H6C	109.5
O18—W7—O34	155.9 (9)	N4—C7—H7A	109.5
O31—W7—O34	87.3 (7)	N4—C7—H7B	109.5
O33—W7—O35	101.8 (9)	H7A—C7—H7B	109.5
O18—W7—O35	87.8 (7)	N4—C7—H7C	109.5
O31—W7—O35	155.7 (9)	H7A—C7—H7C	109.5
O34—W7—O35	87.5 (6)	H7B—C7—H7C	109.5
O33—W7—O10B	156.2 (9)	C12—N5—C8	106.8 (14)
O18—W7—O10B	94.9 (9)	C12—N5—H5N	126.6
O31—W7—O10B	93.4 (8)	C8—N5—H5N	126.6
O34—W7—O10B	62.0 (9)	C8—N6—C9	110.3 (13)
O35—W7—O10B	63.3 (8)	C8—N6—C13	123.1 (15)
O33—W7—O8A	160.4 (8)	C9—N6—C13	126.4 (14)
O18—W7—O8A	62.8 (7)	C10—N7—C11	130.3 (15)
O31—W7—O8A	64.8 (7)	C10—N7—H7N	114.8
O34—W7—O8A	93.7 (9)	C11—N7—H7N	114.8
O35—W7—O8A	92.0 (9)	C12—N8—C11	118.1 (14)
O36—W8—O35	102.7 (9)	C12—N8—C14	121.4 (15)
O36—W8—O22	103.3 (8)	C11—N8—C14	119.9 (15)
O35—W8—O22	86.5 (8)	N6—C8—N5	108.5 (14)
O36—W8—O37	101.4 (9)	N6—C8—H8	125.8
O35—W8—O37	155.9 (10)	N5—C8—H8	125.8
O22—W8—O37	86.6 (6)	C12—C9—N6	105.5 (14)
O36—W8—O38	101.4 (8)	C12—C9—C10	121.6 (16)
O35—W8—O38	88.1 (7)	N6—C9—C10	132.9 (15)
O22—W8—O38	155.3 (9)	O3—C10—N7	124.0 (15)
O37—W8—O38	88.6 (8)	O3—C10—C9	125.5 (17)
O36—W8—O9A	158.1 (7)	N7—C10—C9	110.4 (16)
O35—W8—O9A	92.5 (9)	O4—C11—N7	121.7 (17)
O22—W8—O9A	61.5 (7)	O4—C11—N8	122.4 (17)
O37—W8—O9A	64.0 (8)	N7—C11—N8	115.8 (15)
O38—W8—O9A	94.7 (8)	N5—C12—C9	108.9 (15)
O36—W8—O10B	157.0 (7)	N5—C12—N8	127.5 (14)
O35—W8—O10B	63.1 (8)	C9—C12—N8	123.6 (16)
O22—W8—O10B	94.2 (9)	N6—C13—H13A	109.5
O37—W8—O10B	94.4 (9)	N6—C13—H13B	109.5
O38—W8—O10B	62.1 (8)	H13A—C13—H13B	109.5
O9A—W8—O10B	44.9 (7)	N6—C13—H13C	109.5
O39—W9—O21	102.0 (9)	H13A—C13—H13C	109.5
O39—W9—O37	100.9 (9)	H13B—C13—H13C	109.5
O21—W9—O37	86.3 (6)	N8—C14—H14A	109.5
O39—W9—O26	103.0 (8)	N8—C14—H14B	109.5
O21—W9—O26	87.7 (8)	H14A—C14—H14B	109.5
O37—W9—O26	156.1 (10)	N8—C14—H14C	109.5
O39—W9—O40	102.3 (8)	H14A—C14—H14C	109.5
O21—W9—O40	155.7 (9)	H14B—C14—H14C	109.5
O37—W9—O40	89.2 (8)	C15—N9—C19	107.2 (15)
O26—W9—O40	86.7 (6)	C15—N9—H9N	126.4
O39—W9—O9A	158.0 (7)	C19—N9—H9N	126.4
O21—W9—O9A	62.0 (8)	C15—N10—C16	105.4 (16)
O37—W9—O9A	64.9 (8)	C15—N10—C20	125.0 (18)
O26—W9—O9A	91.9 (8)	C16—N10—C20	129.6 (18)
O40—W9—O9A	94.5 (7)	C18—N11—C17	128.4 (15)
O39—W9—O9B	159.5 (7)	C18—N11—H11N	115.8
O21—W9—O9B	93.9 (9)	C17—N11—H11N	115.8
O37—W9—O9B	92.9 (9)	C18—N12—C19	116.0 (14)
O26—W9—O9B	64.4 (7)	C18—N12—C21	121.0 (16)
O40—W9—O9B	62.4 (7)	C19—N12—C21	122.4 (15)
O41—W10—O40	103.2 (10)	N9—C15—N10	110.3 (17)
O41—W10—O43	102.1 (10)	N9—C15—H15	124.8
O40—W10—O43	86.9 (6)	N10—C15—H15	124.8
O41—W10—O25	102.0 (10)	C19—C16—N10	108.1 (15)
O40—W10—O25	86.9 (6)	C19—C16—C17	122.7 (17)
O43—W10—O25	155.9 (9)	N10—C16—C17	129.2 (17)
O41—W10—O42	100.4 (10)	O5—C17—N11	119.1 (19)
O40—W10—O42	156.4 (8)	O5—C17—C16	132 (2)
O43—W10—O42	88.4 (6)	N11—C17—C16	109.4 (16)
O25—W10—O42	88.1 (6)	O6—C18—N12	120.6 (16)
O41—W10—O9B	161.2 (11)	O6—C18—N11	122.0 (16)
O40—W10—O9B	64.3 (8)	N12—C18—N11	117.4 (15)
O43—W10—O9B	91.6 (8)	C16—C19—N9	109.0 (15)
O25—W10—O9B	64.7 (8)	C16—C19—N12	125.6 (15)
O42—W10—O9B	92.7 (8)	N9—C19—N12	125.3 (15)
O41—W10—O10A	158.3 (10)	N10—C20—H20A	109.5
O40—W10—O10A	93.6 (8)	N10—C20—H20B	109.5
O43—W10—O10A	64.7 (7)	H20A—C20—H20B	109.5
O25—W10—O10A	92.5 (8)	N10—C20—H20C	109.5
O42—W10—O10A	63.6 (7)	H20A—C20—H20C	109.5
O44—W11—O28	104.0 (9)	H20B—C20—H20C	109.5
O44—W11—O45	101.5 (8)	N12—C21—H21A	109.5
O28—W11—O45	154.5 (9)	N12—C21—H21B	109.5
O44—W11—O42	102.0 (7)	H21A—C21—H21B	109.5
O28—W11—O42	86.1 (7)	N12—C21—H21C	109.5
O45—W11—O42	87.6 (6)	H21A—C21—H21C	109.5
O44—W11—O32	102.4 (8)	H21B—C21—H21C	109.5
O28—W11—O32	87.5 (5)	C22—O47—H1O	108.8
O45—W11—O32	88.1 (6)	O47—C22—C23	112.1 (11)
O42—W11—O32	155.5 (8)	O47—C22—H22A	109.2
O44—W11—O8B	157.9 (8)	C23—C22—H22A	109.2
O28—W11—O8B	63.2 (8)	O47—C22—H22B	109.2
O45—W11—O8B	92.8 (8)	C23—C22—H22B	109.2
O42—W11—O8B	95.2 (7)	H22A—C22—H22B	107.9
O32—W11—O8B	60.9 (8)	C22—C23—H23A	109.5
O44—W11—O10A	160.0 (7)	C22—C23—H23B	109.5
O28—W11—O10A	90.2 (8)	H23A—C23—H23B	109.5
O45—W11—O10A	64.8 (7)	C22—C23—H23C	109.5
O42—W11—O10A	64.5 (7)	H23A—C23—H23C	109.5
O32—W11—O10A	92.0 (8)	H23B—C23—H23C	109.5
O46—W12—O38	101.4 (8)	C24—O48—H2O	107.5
O46—W12—O34	100.7 (8)	C25—C24—O48	112.5 (11)
O38—W12—O34	87.8 (7)	C25—C24—H24A	109.1
O46—W12—O45	101.3 (7)	O48—C24—H24A	109.1
O38—W12—O45	157.3 (8)	C25—C24—H24B	109.1
O34—W12—O45	87.9 (7)	O48—C24—H24B	108.0
O46—W12—O43	103.2 (7)	H24A—C24—H24B	107.8
O38—W12—O43	87.0 (7)	C24—C25—H25A	109.5
O34—W12—O43	156.1 (8)	C24—C25—H25B	109.5
O45—W12—O43	88.0 (6)	H25A—C25—H25B	109.5
O46—W12—O10B	158.1 (7)	C24—C25—H25C	109.5
O38—W12—O10B	64.9 (8)	H25A—C25—H25C	109.5
O34—W12—O10B	63.3 (7)	H25B—C25—H25C	109.5
O10A—P1—O7A—W1	−178.3 (12)	O29—W5—O28—W11	47 (2)
O8A—P1—O7A—W1	−57.4 (16)	O7A—W5—O28—W11	−45 (2)
O9A—P1—O7A—W1	59.1 (15)	O8B—W5—O28—W11	−10.9 (17)
O10A—P1—O7A—W4	58.1 (14)	O30—W6—O29—W5	152.2 (16)
O8A—P1—O7A—W4	179.0 (11)	O19—W6—O29—W5	−103.7 (18)
O9A—P1—O7A—W4	−64.5 (13)	O32—W6—O29—W5	51.3 (17)
O10A—P1—O7A—W5	−57.4 (14)	O31—W6—O29—W5	−24 (3)
O8A—P1—O7A—W5	63.5 (13)	O8B—W6—O29—W5	−8.5 (15)
O9A—P1—O7A—W5	180.0 (11)	O8A—W6—O29—W5	−40.5 (17)
O10A—P1—O8A—W2	179.0 (11)	O33—W7—O31—W6	−154.3 (14)
O7A—P1—O8A—W2	57.6 (15)	O18—W7—O31—W6	−51.1 (15)
O9A—P1—O8A—W2	−57.4 (16)	O34—W7—O31—W6	105.4 (15)
O10A—P1—O8A—W7	−60.4 (13)	O35—W7—O31—W6	28 (2)
O7A—P1—O8A—W7	178.1 (11)	O10B—W7—O31—W6	43.6 (15)
O9A—P1—O8A—W7	63.2 (13)	O8A—W7—O31—W6	9.9 (12)
O10A—P1—O8A—W6	58.0 (15)	O30—W6—O32—W11	−154.5 (15)
O7A—P1—O8A—W6	−63.5 (14)	O29—W6—O32—W11	−50.9 (16)
O9A—P1—O8A—W6	−178.4 (11)	O19—W6—O32—W11	29 (2)
O10A—P1—O9A—W3	179.4 (11)	O31—W6—O32—W11	104.4 (16)
O8A—P1—O9A—W3	57.4 (15)	O8B—W6—O32—W11	10.7 (14)
O7A—P1—O9A—W3	−59.0 (14)	O8A—W6—O32—W11	40.2 (15)
O10A—P1—O9A—W9	−56.3 (15)	O46—W12—O34—W7	−156.1 (16)
O8A—P1—O9A—W9	−178.3 (11)	O38—W12—O34—W7	−54.9 (17)
O7A—P1—O9A—W9	65.3 (14)	O45—W12—O34—W7	102.9 (17)
O10A—P1—O9A—W8	58.6 (14)	O43—W12—O34—W7	23 (3)
O8A—P1—O9A—W8	−63.4 (14)	O10B—W12—O34—W7	8.1 (14)
O7A—P1—O9A—W8	−179.8 (11)	O10A—W12—O34—W7	39.4 (17)
O8A—P1—O10A—W11	−59.0 (15)	O36—W8—O35—W7	152.6 (18)
O7A—P1—O10A—W11	61.0 (14)	O22—W8—O35—W7	−104.6 (19)
O9A—P1—O10A—W11	179.8 (11)	O37—W8—O35—W7	−31 (3)
O8A—P1—O10A—W10	179.0 (11)	O38—W8—O35—W7	51.3 (19)
O7A—P1—O10A—W10	−61.1 (13)	O9A—W8—O35—W7	−43.3 (19)
O9A—P1—O10A—W10	57.8 (14)	O10B—W8—O35—W7	−8.1 (16)
O8A—P1—O10A—W12	61.6 (14)	O39—W9—O37—W8	−157.3 (19)
O7A—P1—O10A—W12	−178.4 (11)	O21—W9—O37—W8	−55.8 (19)
O9A—P1—O10A—W12	−59.6 (14)	O26—W9—O37—W8	20 (3)
O9B—P1—O7B—W2	179.0 (14)	O40—W9—O37—W8	100 (2)
O8A—P1—O7B—W2	0.1 (14)	O9A—W9—O37—W8	4.9 (17)
O8B—P1—O7B—W2	−56.2 (18)	O9B—W9—O37—W8	38 (2)
O10B—P1—O7B—W2	59.3 (19)	O36—W8—O37—W9	157.9 (18)
O9B—P1—O7B—W3	58.3 (16)	O35—W8—O37—W9	−19 (3)
O8A—P1—O7B—W3	−120.7 (16)	O22—W8—O37—W9	55 (2)
O8B—P1—O7B—W3	−177.0 (11)	O38—W8—O37—W9	−101 (2)
O10B—P1—O7B—W3	−61.4 (15)	O9A—W8—O37—W9	−4.8 (16)
O7B—P1—O8B—W6	55.1 (16)	O10B—W8—O37—W9	−39 (2)
O9B—P1—O8B—W6	−179.7 (12)	O46—W12—O38—W8	154.4 (16)
O10B—P1—O8B—W6	−64.4 (16)	O34—W12—O38—W8	53.9 (17)
O7B—P1—O8B—W11	−177.4 (11)	O45—W12—O38—W8	−25 (3)
O9B—P1—O8B—W11	−52.1 (15)	O43—W12—O38—W8	−102.7 (17)
O10B—P1—O8B—W11	63.2 (14)	O10B—W12—O38—W8	−7.5 (14)
O7B—P1—O8B—W5	−63.0 (14)	O10A—W12—O38—W8	−38.9 (17)
O9B—P1—O8B—W5	62.2 (15)	O41—W10—O40—W9	−155.5 (15)
O10B—P1—O8B—W5	177.6 (11)	O43—W10—O40—W9	102.8 (15)
O7B—P1—O9B—W10	179.1 (14)	O25—W10—O40—W9	−53.9 (14)
O8B—P1—O9B—W10	55.2 (17)	O42—W10—O40—W9	24 (2)
O10B—P1—O9B—W10	−58.9 (17)	O9B—W10—O40—W9	9.5 (12)
O7B—P1—O9B—W9	−56.0 (17)	O10A—W10—O40—W9	38.4 (14)
O10A—P1—O9B—W9	124.8 (15)	O44—W11—O42—W10	155.1 (12)
O8B—P1—O9B—W9	−179.9 (11)	O28—W11—O42—W10	−101.4 (14)
O10B—P1—O9B—W9	66.0 (15)	O45—W11—O42—W10	53.8 (13)
O7B—P1—O10B—W12	179.4 (14)	O32—W11—O42—W10	−26 (2)
O9B—P1—O10B—W12	56.5 (16)	O8B—W11—O42—W10	−38.8 (13)
O8B—P1—O10B—W12	−62.0 (15)	O10A—W11—O42—W10	−9.3 (11)
O7B—P1—O10B—W7	−56.2 (16)	O41—W10—O43—W12	152.1 (16)
O9B—P1—O10B—W7	−179.1 (12)	O40—W10—O43—W12	−105.1 (16)
O8B—P1—O10B—W7	62.4 (15)	O25—W10—O43—W12	−30 (2)
O7B—P1—O10B—W8	58.6 (16)	O42—W10—O43—W12	51.8 (15)
O9B—P1—O10B—W8	−64.3 (15)	O9B—W10—O43—W12	−40.9 (15)
O8B—P1—O10B—W8	177.2 (12)	O10A—W10—O43—W12	−9.6 (13)
O16—W2—O12—W1	−152.1 (16)	O44—W11—O45—W12	−156.5 (14)
O18—W2—O12—W1	32 (3)	O28—W11—O45—W12	21 (3)
O17—W2—O12—W1	−48.6 (16)	O42—W11—O45—W12	−54.7 (15)
O19—W2—O12—W1	106.8 (17)	O32—W11—O45—W12	101.2 (15)
O8A—W2—O12—W1	43.7 (16)	O8B—W11—O45—W12	40.4 (15)
O7B—W2—O12—W1	13.9 (14)	O10A—W11—O45—W12	8.1 (12)
O11—W1—O12—W2	150.0 (16)	O46—W12—O45—W11	157.1 (14)
O15—W1—O12—W2	−106.8 (17)	O38—W12—O45—W11	−23 (3)
O13—W1—O12—W2	48.9 (16)	O34—W12—O45—W11	−102.5 (15)
O14—W1—O12—W2	−28 (3)	O43—W12—O45—W11	54.0 (15)
O7A—W1—O12—W2	−43.5 (17)	O10B—W12—O45—W11	−39.3 (15)
O11—W1—O13—W3	−154.9 (14)	O10A—W12—O45—W11	−8.0 (12)
O12—W1—O13—W3	−50.7 (14)	C2—N2—C1—N1	−1 (2)
O15—W1—O13—W3	27 (2)	C6—N2—C1—N1	−175.5 (15)
O14—W1—O13—W3	103.5 (15)	C5—N1—C1—N2	1 (2)
O7A—W1—O13—W3	40.2 (13)	C1—N2—C2—C5	1.5 (19)
O11—W1—O14—W4	155.1 (17)	C6—N2—C2—C5	175.3 (16)
O12—W1—O14—W4	−26 (3)	C1—N2—C2—C3	−175.1 (19)
O15—W1—O14—W4	51.9 (17)	C6—N2—C2—C3	−1 (3)
O13—W1—O14—W4	−104.0 (17)	C4—N3—C3—O1	178.1 (16)
O7A—W1—O14—W4	−9.6 (15)	C4—N3—C3—C2	1 (3)
O11—W1—O15—W5	−155.9 (16)	C5—C2—C3—O1	−176.7 (17)
O12—W1—O15—W5	99.9 (16)	N2—C2—C3—O1	−1 (3)
O13—W1—O15—W5	22 (3)	C5—C2—C3—N3	0 (2)
O14—W1—O15—W5	−54.2 (17)	N2—C2—C3—N3	175.9 (17)
O7A—W1—O15—W5	7.5 (13)	C3—N3—C4—O2	−179.5 (18)
O27—W5—O15—W1	155.5 (15)	C3—N3—C4—N4	−1 (3)
O24—W5—O15—W1	55.1 (17)	C5—N4—C4—O2	178.0 (16)
O28—W5—O15—W1	−22 (3)	C7—N4—C4—O2	−9 (3)
O29—W5—O15—W1	−100.7 (16)	C5—N4—C4—N3	−1 (2)
O7A—W5—O15—W1	−7.4 (13)	C7—N4—C4—N3	172.7 (15)
O8B—W5—O15—W1	−40.4 (16)	C1—N1—C5—N4	177.3 (17)
O20—W3—O17—W2	−153.1 (14)	C1—N1—C5—C2	0 (2)
O22—W3—O17—W2	102.8 (15)	C4—N4—C5—N1	−175.2 (16)
O21—W3—O17—W2	28 (2)	C7—N4—C5—N1	11 (3)
O13—W3—O17—W2	−52.6 (14)	C4—N4—C5—C2	2 (2)
O9A—W3—O17—W2	39.9 (14)	C7—N4—C5—C2	−171.8 (16)
O7B—W3—O17—W2	10.6 (12)	N2—C2—C5—N1	−0.9 (19)
O16—W2—O18—W7	−154.7 (15)	C3—C2—C5—N1	176.1 (15)
O12—W2—O18—W7	21 (3)	N2—C2—C5—N4	−178.3 (15)
O17—W2—O18—W7	101.7 (16)	C3—C2—C5—N4	−1 (3)
O19—W2—O18—W7	−54.3 (16)	C9—N6—C8—N5	−1.6 (19)
O8A—W2—O18—W7	8.1 (14)	C13—N6—C8—N5	−175.8 (15)
O7B—W2—O18—W7	37.4 (16)	C12—N5—C8—N6	1.1 (19)
O33—W7—O18—W2	156.9 (15)	C8—N6—C9—C12	1.3 (18)
O31—W7—O18—W2	54.8 (16)	C13—N6—C9—C12	175.4 (15)
O34—W7—O18—W2	−23 (3)	C8—N6—C9—C10	−176.4 (16)
O35—W7—O18—W2	−101.5 (17)	C13—N6—C9—C10	−2 (3)
O10B—W7—O18—W2	−38.5 (16)	C11—N7—C10—O3	−172.1 (17)
O8A—W7—O18—W2	−8.1 (14)	C11—N7—C10—C9	4 (2)
O30—W6—O19—W2	−157.0 (15)	C12—C9—C10—O3	176.0 (15)
O29—W6—O19—W2	98.9 (16)	N6—C9—C10—O3	−7 (3)
O32—W6—O19—W2	20 (3)	C12—C9—C10—N7	0 (2)
O31—W6—O19—W2	−55.9 (16)	N6—C9—C10—N7	177.2 (16)
O8B—W6—O19—W2	35.6 (16)	C10—N7—C11—O4	177.9 (17)
O8A—W6—O19—W2	6.8 (14)	C10—N7—C11—N8	−5 (3)
O39—W9—O21—W3	155.7 (17)	C12—N8—C11—O4	178.6 (16)
O37—W9—O21—W3	55.4 (18)	C14—N8—C11—O4	−10 (3)
O26—W9—O21—W3	−101.4 (18)	C12—N8—C11—N7	2 (2)
O40—W9—O21—W3	−25 (3)	C14—N8—C11—N7	173.1 (15)
O9A—W9—O21—W3	−8.1 (15)	C8—N5—C12—C9	−0.3 (18)
O9B—W9—O21—W3	−37.3 (18)	C8—N5—C12—N8	179.7 (15)
O36—W8—O22—W3	−154.0 (15)	N6—C9—C12—N5	−0.6 (17)
O35—W8—O22—W3	103.7 (17)	C10—C9—C12—N5	177.5 (13)
O37—W8—O22—W3	−53.2 (17)	N6—C9—C12—N8	179.4 (14)
O38—W8—O22—W3	26 (3)	C10—C9—C12—N8	−3 (2)
O9A—W8—O22—W3	8.9 (14)	C11—N8—C12—N5	−178.2 (15)
O10B—W8—O22—W3	41.1 (16)	C14—N8—C12—N5	10 (2)
O20—W3—O22—W8	153.4 (16)	C11—N8—C12—C9	2 (2)
O17—W3—O22—W8	−104.0 (17)	C14—N8—C12—C9	−169.6 (15)
O21—W3—O22—W8	52.2 (17)	C19—N9—C15—N10	1 (2)
O13—W3—O22—W8	−26 (3)	C16—N10—C15—N9	−1 (2)
O9A—W3—O22—W8	−9.1 (14)	C20—N10—C15—N9	−179.8 (17)
O7B—W3—O22—W8	−39.7 (16)	C15—N10—C16—C19	1 (2)
O27—W5—O24—W4	−155.0 (17)	C20—N10—C16—C19	179.2 (18)
O28—W5—O24—W4	101.3 (19)	C15—N10—C16—C17	180.0 (18)
O15—W5—O24—W4	−52.8 (19)	C20—N10—C16—C17	−2 (3)
O29—W5—O24—W4	27 (3)	C18—N11—C17—O5	−173.9 (17)
O7A—W5—O24—W4	7.2 (15)	C18—N11—C17—C16	7 (2)
O8B—W5—O24—W4	40.9 (19)	C19—C16—C17—O5	179 (2)
O41—W10—O25—W4	157.1 (15)	N10—C16—C17—O5	0 (3)
O40—W10—O25—W4	54.2 (15)	C19—C16—C17—N11	−2 (2)
O43—W10—O25—W4	−21 (2)	N10—C16—C17—N11	178.7 (16)
O42—W10—O25—W4	−102.7 (15)	C19—N12—C18—O6	−179.6 (15)
O9B—W10—O25—W4	−8.8 (13)	C21—N12—C18—O6	−7 (3)
O10A—W10—O25—W4	−39.2 (14)	C19—N12—C18—N11	2 (2)
O23—W4—O26—W9	154.1 (16)	C21—N12—C18—N11	174.4 (16)
O25—W4—O26—W9	53.0 (17)	C17—N11—C18—O6	174.7 (16)
O14—W4—O26—W9	−103.9 (18)	C17—N11—C18—N12	−7 (3)
O24—W4—O26—W9	−23 (3)	N10—C16—C19—N9	−0.1 (19)
O7A—W4—O26—W9	−41.2 (17)	C17—C16—C19—N9	−179.3 (16)
O44—W11—O28—W5	−149.6 (19)	N10—C16—C19—N12	177.5 (15)
O45—W11—O28—W5	33 (3)	C17—C16—C19—N12	−2 (3)
O42—W11—O28—W5	109 (2)	C15—N9—C19—C16	−1 (2)
O32—W11—O28—W5	−47 (2)	C15—N9—C19—N12	−178.3 (16)
O8B—W11—O28—W5	11.1 (17)	C18—N12—C19—C16	2 (3)
O10A—W11—O28—W5	44.6 (19)	C21—N12—C19—C16	−170.1 (18)
O27—W5—O28—W11	150.5 (19)	C18—N12—C19—N9	179.0 (16)
O24—W5—O28—W11	−109 (2)	C21—N12—C19—N9	7 (3)
O15—W5—O28—W11	−32 (3)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1N···O3^i	0.87	2.04	2.776 (18)	142
N1—H1N···O36^ii	0.87	2.51	2.965 (18)	113
N3—H3N···O1^iii	0.87	1.97	2.835 (18)	177
N5—H5N···O6^ii	0.87	1.95	2.738 (19)	149
N7—H7N···O30^iv	0.87	2.09	2.95 (2)	171
N9—H9N···O47	0.87	1.78	2.62 (2)	161
N11—H11N···O44^v	0.87	2.00	2.822 (19)	156
O47—H1O···O4	0.85	1.86	2.71 (2)	180
O48—H2O···O23^vi	0.85	2.29	3.13 (7)	171
C1—H1···O5^ii	0.94	2.28	3.08 (2)	144
C1—H1···O36^ii	0.94	2.38	2.91 (2)	116
C8—H8···O39^ii	0.94	2.22	2.93 (2)	132
C8—H8···O2^vii	0.94	2.48	3.12 (2)	125
C15—H15···O27^viii	0.94	2.10	3.02 (2)	165
C7—H7B···O3^i	0.97	2.39	3.22 (2)	143
C7—H7C···O31	0.97	2.69	3.47 (2)	138
C13—H13B···O24	0.97	2.59	3.35 (3)	135
C13—H13C···O1^ix	0.97	2.50	3.13 (2)	123
C14—H14B···O6^ii	0.97	2.67	3.44 (2)	136
C14—H14B···O16^vii	0.97	2.67	3.33 (2)	125
C20—H20B···O26^vi	0.97	2.39	3.29 (2)	154
C20—H20C···O46	0.97	2.44	3.01 (2)	117
C21—H21A···O47	0.97	2.63	3.57 (3)	164
C21—H21B···O16^iv	0.97	2.47	3.44 (3)	173
C21—H21C···O41	0.97	2.57	3.14 (3)	117
C22—H22A···O20^vi	0.98	2.44	3.20 (3)	134
C22—H22B···O15^viii	0.98	2.64	3.46 (3)	142
C23—H23A···O19^viii	0.97	2.56	3.43 (4)	148
C23—H23C···O4	0.97	2.68	3.33 (4)	125
C24—H24A···O5	0.98	2.18	3.12 (9)	159
C24—H24B···O3^x	0.98	2.59	3.48 (8)	152
C25—H25A···O38	0.97	2.59	3.43 (6)	145

Symmetry codes: (i) x−1/2, −y+1/2, z+1/2; (ii) x−1, y, z; (iii) −x+1, −y+1, −z+1; (iv) x+1/2, −y+1/2, z−1/2; (v) x+1, y, z; (vi) −x+3/2, y+1/2, −z+1/2; (vii) x−1/2, −y+1/2, z−1/2; (viii) −x+1/2, y+1/2, −z+1/2; (ix) −x+1/2, y−1/2, −z+1/2; (x) x+1/2, −y+1/2, z+1/2.