supplementary materials


HTML versionpdf versioncif file3d viewstructure factorssupplementary materialsCIF check reportsimilar papers buy article online

Acta Cryst. (2007). E63, m1777-m1778    [ doi:10.1107/S1600536807023306 ]

Tris[(3-aminopropyl)dimethylammonium] decavanadate(V) hexahydrate

C.-Y. Zhu, Y.-T. Li, J.-D. Wu, Z.-Y. Wu and X. Wu

Abstract top

The title compound, 3(C5H16N2)2+·[V10O28]6-·6H2O, consists of decavanadate polyanions, doubly protonated N,N-dimethylpropane-1,3-diammonium cations (H2dmpn2+) and uncoordinated water molecules. Two crystallographically independent decavanadate anions are located across inversion centers. The terminal V=O bond distances are much shorter than the bridging V-O bond distances. The structural components are linked by extensive hydrogen bonding, forming a three-dimension supramolecular architecture.

Comment top

Decavanadate has shown high affinity for selected kinases, phosphorylase and reverse transcriptase and has been used to facilitate crystallization of proteins (Boyd et al., 1985; Csermely et al., 1985; DeMaster & Mitchell, 1973; Pai et al., 1977; Soman et al., 1983). Herein, we report the structure of a three-dimensional supramolecular assembly based on decavanadate, N,N-dimethylpropane-1,3-diammonium (H2dmpn2+) and lattice water molecule building blocks, formulated as 3(C5H16N2)2+.(V10O28)6-.6H2O, (I).

The molecular structure of (I) comprises decavanadate polyanions, H2dmpn2+ cations and lattice water molecules in a stoichiometric ratio of 1:3:6 (Fig. 1). There are two halves of independent [V10O28]6- ions, located on different inversion centers and exhibit the usual structure consisting in a stacking of ten octahedra (Correia et al., 2004; Fratzky et al., 2000; Gong et al., 2006). The terminal O—V bond distances are much shorter than bridging O—V bond distances (Table 1). All the H2dmpn2+ cations adopt anti-anti conformations, with N···N separations of 4.992 (7) Å (N1···N2), 4.994 (7) Å (N3···N4) and 4.973 (7) Å (N5···N6), respectively.

The most noticeable feature of the title compound is its extensive hydrogen bond network between the structural components (Table 2). Viewed along c axis, the H2dmpn2+ cations containing atoms N1 and N2, the decavanadate ions incorporating atoms V1 to V5, O29W and O30W are involved in two-dimensional hydrogen-bonding networks (Fig. 2), which interleave with other parallel networks formed by the H2dmpn2+ cations containing atoms N3 and N4, the other kind decavanadate ions, O33W and O34W (Fig. 3). Then these two kinds of decavanadate anions are both further connected by the H2dmpn2+ cations containing atoms N5 and N6, O31W and O32W (Fig. 4), resulting in a three-dimensional supramolecular architecture.

Related literature top

For general background, see Boyd et al., 1985; Csermely et al., 1985; DeMaster & Mitchell, 1973; Pai et al., 1977; Soman et al., 1983. For related structures, see Correia et al., 2004; Fratzky et al., 2000; Gong et al., 2006. For synthesis, see Sathyanarayana & Patel, 1965.

Experimental top

A solution of oxovanadium(IV) oxalate dihydrate (0.095 g, 0.5 mmol), prepared according to the literature procedure (Sathyanarayana & Patel, 1965), in 95% methanol (12 ml) was added successively to a solution of N,N-dimethylpropane-1,3-diamine (0.051 g, 0.5 mmol) in methanol (5 ml). The mixture was stirred continuously at 333 K for 6 h and a lot of brown precipitate formed. The precipitate was filtered, washed sequentially with methanol and diethyl ether, and then dissolved in water. Orange single crystals of (I) (55% yield based on vanadium) suitable for X-ray analysis were obtained from the aqueous solution by slow evaporation at room temperature. Elemental analysis calculated: C 13.07, H 4.39, N 6.10%; found: C 13.36, H 4.51, N 5.87%.

Refinement top

H atoms of water molecules were located in a difference Fourier map and were refined in riding mode, with Uiso(H) = 1.2Ueq(O). Other H atoms were placed in calculated positions, with C—H = 0.97 Å (methylene) or 0.96 Å (methyl) and N—H = 0.89 Å (protonated primary ammonium) or 0.91 Å (protonated tertiary ammonium), and included in the final cycles of refinement in riding mode, with Uiso(H) = 1.5Ueq(C,N) for methyl and protonated primary ammonium and 1.2Ueq(C,N) for others.

Computing details top

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP (Siemens, 1994); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figures top
[Figure 1] Fig. 1. A view of (I) with the atomic numbering scheme. Full displacement ellipsoids (for the independent moiety) and open ellipsoids (for the symmetry-related part) are drawn at the 30% probability level. C-bound H atoms have been omitted for clarity. Dashed lines indicate hydrogen bonds. [Symmetry codes: (i) -x, -y, -z + 1; (ii) -x, -y + 1, -z.]
[Figure 2] Fig. 2. The two-dimensional hydrogen-bonded network formed by the H2dmpn2+ cations containing atoms N1 and N2, the decavanadate ions incorporating atoms V1 to V5 and water molecules, viewed along c axis. [Symmetry codes: (i) -x, -y, -z + 1; (iii) x, y + 1, z; (iv) x + 1, y + 1, z; (vii) -x, -y + 1, -z + 1; (ix) -x + 1, -y + 1, -z + 1.]
[Figure 3] Fig. 3. The two-dimensional hydrogen-bonded network formed by the H2dmpn2+ cations containing atoms N3 and N4, the decavanadate ions incorporating atoms V6 to V10 and water molecules, viewed along c axis. [Symmetry codes: (ii) -x, -y + 1, -z; (v) -x, -y, -z; (vi) x + 1, y, z; (ix) -x + 1, -y + 1, -z + 1; (xi) x, y - 1, z.]
[Figure 4] Fig. 4. The intermolecular hydrogen bonds between the H2dmpn2+ cations containing atoms N5 and N6, both two kinds of decavanadate anions and water molecules. [Symmetry codes: (vii) -x, -y + 1, -z + 1; (viii) x - 1, y, z.]
Tris[(3-aminopropyl)dimethylammonium] decavanadate(V) hexahydrate top
Crystal data top
3(C5H16N2)2+.[V10O28]6−.6H2OZ = 2
Mr = 1378.09F(000) = 1388
Triclinic, P1Dx = 2.042 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 11.525 (2) ÅCell parameters from 1736 reflections
b = 11.743 (2) Åθ = 3.5–25.1°
c = 18.709 (4) ŵ = 2.09 mm−1
α = 90.45 (3)°T = 298 K
β = 94.21 (3)°Block, orange
γ = 117.29 (3)°0.30 × 0.26 × 0.18 mm
V = 2241.7 (10) Å3
Data collection top
Bruker APEX area-detector
diffractometer		8110 independent reflections
Radiation source: fine-focus sealed tube4858 reflections with I > 2σ(I)
graphiteRint = 0.024
φ and ω scanθmax = 25.2°, θmin = 2.0°
Absorption correction: multi-scan
(SADABS; Bruker, 2002)		h = −13→13
Tmin = 0.556, Tmax = 0.684k = −14→11
12138 measured reflectionsl = −19→22
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)] = 0.045Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.134H-atom parameters constrained
S = 1.03 w = 1/[σ2(Fo2) + (0.0576P)2 + 1.1434P]
where P = (Fo2 + 2Fc2)/3
8110 reflections(Δ/σ)max = 0.001
595 parametersΔρmax = 1.02 e Å−3
0 restraintsΔρmin = −0.71 e Å−3
Crystal data top
3(C5H16N2)2+.[V10O28]6−.6H2Oγ = 117.29 (3)°
Mr = 1378.09V = 2241.7 (10) Å3
Triclinic, P1Z = 2
a = 11.525 (2) ÅMo Kα radiation
b = 11.743 (2) ŵ = 2.09 mm−1
c = 18.709 (4) ÅT = 298 K
α = 90.45 (3)°0.30 × 0.26 × 0.18 mm
β = 94.21 (3)°
Data collection top
Bruker APEX area-detector
diffractometer		8110 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2002)		4858 reflections with I > 2σ(I)
Tmin = 0.556, Tmax = 0.684Rint = 0.024
12138 measured reflectionsθmax = 25.2°
Refinement top
R[F2 > 2σ(F2)] = 0.045H-atom parameters constrained
wR(F2) = 0.134Δρmax = 1.02 e Å−3
S = 1.03Δρmin = −0.71 e Å−3
8110 reflectionsAbsolute structure: ?
595 parametersFlack parameter: ?
0 restraintsRogers parameter: ?
Special details top

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

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C10.1582 (6)0.3274 (6)0.3030 (3)0.0486 (17)
H1A0.19230.38630.26560.073*
H1B0.07230.31590.31110.073*
H1C0.15320.24640.28910.073*
C20.3772 (6)0.3895 (6)0.3602 (3)0.0495 (17)
H2A0.36840.30550.35000.074*
H2B0.43410.42630.40320.074*
H2C0.41370.44300.32100.074*
C30.2530 (6)0.5035 (5)0.3935 (3)0.0396 (15)
H3A0.16470.49050.39860.047*
H3B0.28790.56360.35600.047*
C40.3352 (5)0.5634 (5)0.4629 (3)0.0327 (13)
H4A0.42730.59530.45590.039*
H4B0.31240.50000.49920.039*
C50.3097 (6)0.6723 (5)0.4867 (3)0.0383 (15)
H5A0.31810.72720.44680.046*
H5B0.22060.63770.50010.046*
C60.1303 (6)−0.1879 (6)−0.1992 (3)0.0536 (18)
H6A0.1289−0.2671−0.21390.080*
H6B0.1469−0.1334−0.23910.080*
H6C0.0472−0.2053−0.18250.080*
C70.3621 (6)−0.1187 (6)−0.1575 (3)0.0509 (17)
H7A0.4284−0.0741−0.11910.076*
H7B0.3885−0.0749−0.20110.076*
H7C0.3505−0.2047−0.16360.076*
C80.2499 (6)0.0073 (5)−0.1239 (3)0.0402 (15)
H8A0.16340.0001−0.11970.048*
H8B0.28600.0602−0.16410.048*
C90.3351 (6)0.0743 (5)−0.0567 (3)0.0389 (15)
H9A0.42270.0840−0.06030.047*
H9B0.29970.0234−0.01580.047*
C100.3409 (6)0.2042 (6)−0.0465 (3)0.0434 (16)
H10A0.38710.2581−0.08440.052*
H10B0.25250.1946−0.05050.052*
C110.1445 (6)0.6791 (6)0.2703 (3)0.0394 (15)
H11A0.21140.65930.25550.059*
H11B0.06330.60170.27000.059*
H11C0.16940.71830.31790.059*
C120.2544 (6)0.8844 (6)0.2121 (3)0.0472 (17)
H12A0.28470.93380.25680.071*
H12B0.24270.93590.17540.071*
H12C0.31770.85790.19910.071*
C130.0264 (6)0.8086 (6)0.2393 (3)0.0386 (15)
H13A0.06260.86980.28000.046*
H13B0.00760.85150.19940.046*
C14−0.0993 (6)0.6996 (5)0.2577 (3)0.0334 (14)
H14A−0.09090.67890.30730.040*
H14B−0.11940.62430.22740.040*
C15−0.2084 (6)0.7375 (6)0.2464 (3)0.0358 (14)
H15A−0.18320.81790.27290.043*
H15B−0.22130.75060.19590.043*
N10.2463 (4)0.3797 (4)0.3702 (2)0.0313 (11)
H10.21090.32330.40500.038*
N20.4011 (4)0.7498 (4)0.5480 (3)0.0403 (12)
H2D0.38170.70490.58730.060*
H2E0.39380.82130.55470.060*
H2F0.48280.77000.53890.060*
N30.2359 (5)−0.1227 (4)−0.1401 (2)0.0362 (12)
H30.2104−0.1688−0.10030.043*
N40.4074 (4)0.2680 (4)0.0238 (3)0.0402 (13)
H4C0.48900.27810.02750.060*
H4D0.36400.22000.05880.060*
H4E0.40910.34440.02740.060*
N50.1280 (5)0.7699 (5)0.2197 (2)0.0374 (12)
H50.10000.72810.17580.045*
N6−0.3327 (5)0.6385 (5)0.2705 (3)0.0473 (14)
H6D−0.35520.56420.24700.071*
H6E−0.39540.66210.26150.071*
H6F−0.32250.62960.31740.071*
O10.0812 (3)0.3762 (3)0.55044 (19)0.0314 (9)
O20.3306 (3)0.3370 (3)0.57192 (18)0.0278 (8)
O3−0.3799 (3)−0.0088 (3)0.61327 (19)0.0325 (9)
O40.2918 (3)−0.1119 (4)0.66114 (18)0.0327 (9)
O5−0.1423 (3)0.1722 (3)0.57991 (17)0.0229 (8)
O6−0.3388 (3)−0.1664 (3)0.52301 (17)0.0226 (8)
O70.2912 (3)0.1067 (3)0.61371 (16)0.0210 (8)
O80.0956 (3)−0.2327 (3)0.55729 (17)0.0235 (8)
O90.3267 (3)−0.0501 (3)0.52439 (18)0.0241 (8)
O10−0.1539 (3)−0.0427 (3)0.62667 (17)0.0220 (8)
O110.0655 (3)−0.0732 (3)0.64332 (16)0.0214 (8)
O120.0795 (3)0.1475 (3)0.59142 (16)0.0180 (7)
O13−0.1227 (3)−0.2032 (3)0.53428 (16)0.0180 (7)
O140.1072 (3)−0.0160 (3)0.50820 (15)0.0163 (7)
O150.0699 (3)0.8761 (3)0.03827 (19)0.0324 (9)
O160.3277 (3)0.8510 (3)0.04986 (19)0.0312 (9)
O17−0.3650 (3)0.4919 (3)0.12861 (19)0.0328 (9)
O180.3275 (3)0.4259 (3)0.15481 (18)0.0328 (9)
O19−0.1398 (3)0.6720 (3)0.08191 (17)0.0236 (8)
O20−0.3294 (3)0.3285 (3)0.03886 (17)0.0232 (8)
O210.3096 (3)0.6320 (3)0.10206 (17)0.0222 (8)
O220.1193 (3)0.2858 (3)0.05863 (17)0.0245 (8)
O230.3388 (3)0.4694 (3)0.01366 (17)0.0229 (8)
O24−0.1333 (3)0.4677 (3)0.13348 (16)0.0226 (8)
O250.0919 (3)0.4484 (3)0.14297 (16)0.0230 (8)
O260.0866 (3)0.6587 (3)0.08654 (16)0.0194 (7)
O27−0.1086 (3)0.3007 (3)0.04267 (16)0.0194 (7)
O280.1101 (3)0.4891 (3)0.00524 (15)0.0176 (7)
O29W0.1019 (4)0.5780 (4)0.6443 (2)0.0519 (12)
H29B0.07870.63700.62190.062*
H29A0.06780.50480.61590.062*
O30W0.4552 (4)0.8194 (4)0.3381 (2)0.0510 (12)
H30A0.43730.87810.35040.061*
H30B0.53360.84000.35690.061*
O31W0.5050 (4)0.7341 (5)0.2138 (2)0.0691 (16)
H31A0.44010.70630.17440.083*
H31B0.47560.76020.24500.083*
O32W0.3581 (5)0.6211 (4)0.6865 (3)0.0694 (14)
H32A0.27890.61350.68900.083*
H32B0.40490.66180.72620.083*
O33W−0.1878 (5)0.8894 (4)−0.1162 (3)0.0828 (18)
H33A−0.14470.9474−0.08190.099*
H33B−0.14890.8321−0.11100.099*
O34W0.4372 (7)0.2430 (6)0.2017 (4)0.134 (3)
H34A0.40700.30780.19720.161*
H34B0.38740.18590.17470.161*
V1−0.00384 (8)0.22701 (8)0.52518 (4)0.0204 (2)
V20.24366 (8)0.18796 (8)0.54459 (4)0.0200 (2)
V3−0.27039 (8)0.00560 (8)0.56005 (5)0.0229 (2)
V40.22029 (9)−0.07189 (9)0.59676 (4)0.0241 (2)
V5−0.02534 (8)−0.03266 (8)0.58388 (4)0.0166 (2)
V6−0.01327 (8)0.72388 (8)0.01871 (4)0.0210 (2)
V70.24429 (8)0.69956 (8)0.03168 (4)0.0203 (2)
V8−0.26351 (8)0.50339 (8)0.07083 (5)0.0236 (2)
V90.24551 (9)0.45527 (9)0.09123 (5)0.0242 (2)
V10−0.01191 (8)0.47419 (8)0.08540 (4)0.0173 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.054 (4)0.046 (4)0.028 (3)0.008 (3)0.004 (3)0.007 (3)
C20.043 (4)0.051 (4)0.058 (4)0.024 (4)0.014 (3)0.000 (3)
C30.036 (4)0.031 (4)0.052 (4)0.015 (3)0.003 (3)0.012 (3)
C40.030 (3)0.028 (3)0.042 (4)0.014 (3)0.003 (3)0.004 (3)
C50.036 (3)0.039 (4)0.047 (4)0.023 (3)0.001 (3)0.004 (3)
C60.052 (4)0.047 (4)0.033 (4)−0.001 (3)−0.002 (3)0.004 (3)
C70.062 (5)0.049 (4)0.045 (4)0.027 (4)0.014 (3)0.007 (3)
C80.034 (3)0.034 (4)0.049 (4)0.013 (3)0.001 (3)0.012 (3)
C90.035 (3)0.036 (4)0.050 (4)0.021 (3)−0.002 (3)−0.002 (3)
C100.045 (4)0.038 (4)0.053 (4)0.026 (3)−0.006 (3)0.003 (3)
C110.053 (4)0.046 (4)0.035 (3)0.037 (3)−0.001 (3)−0.001 (3)
C120.043 (4)0.051 (4)0.044 (4)0.020 (4)−0.003 (3)0.006 (3)
C130.049 (4)0.034 (4)0.037 (3)0.024 (3)−0.008 (3)−0.009 (3)
C140.046 (4)0.040 (4)0.022 (3)0.027 (3)−0.003 (3)−0.001 (3)
C150.043 (4)0.044 (4)0.028 (3)0.026 (3)0.001 (3)−0.003 (3)
N10.032 (3)0.027 (3)0.027 (3)0.007 (2)0.007 (2)0.008 (2)
N20.028 (3)0.033 (3)0.058 (3)0.013 (2)0.008 (2)−0.001 (2)
N30.041 (3)0.033 (3)0.026 (3)0.008 (2)0.006 (2)0.008 (2)
N40.025 (3)0.031 (3)0.065 (4)0.014 (2)0.004 (2)0.003 (3)
N50.051 (3)0.045 (3)0.022 (3)0.028 (3)−0.004 (2)−0.003 (2)
N60.051 (3)0.055 (4)0.043 (3)0.029 (3)0.010 (3)−0.002 (3)
O10.033 (2)0.021 (2)0.041 (2)0.0126 (18)0.0011 (17)−0.0058 (17)
O20.024 (2)0.019 (2)0.033 (2)0.0046 (17)−0.0010 (16)−0.0026 (16)
O30.027 (2)0.039 (2)0.036 (2)0.0176 (19)0.0104 (17)−0.0018 (18)
O40.031 (2)0.042 (2)0.030 (2)0.022 (2)−0.0005 (17)0.0059 (18)
O50.026 (2)0.0203 (19)0.0259 (19)0.0137 (17)0.0032 (15)−0.0038 (15)
O60.0183 (18)0.0210 (19)0.0268 (19)0.0071 (16)0.0043 (15)0.0004 (15)
O70.0192 (18)0.023 (2)0.0215 (18)0.0114 (16)−0.0040 (14)−0.0034 (15)
O80.031 (2)0.019 (2)0.0261 (19)0.0160 (17)0.0006 (15)0.0019 (15)
O90.0201 (19)0.023 (2)0.032 (2)0.0131 (17)0.0004 (15)−0.0002 (16)
O100.0252 (19)0.022 (2)0.0208 (18)0.0128 (17)0.0034 (15)0.0016 (15)
O110.0257 (19)0.023 (2)0.0165 (18)0.0126 (17)0.0003 (14)0.0028 (15)
O120.0186 (18)0.0155 (18)0.0205 (18)0.0086 (15)0.0013 (14)−0.0017 (14)
O130.0164 (18)0.0148 (18)0.0210 (18)0.0055 (15)0.0024 (14)0.0025 (14)
O140.0178 (18)0.0140 (17)0.0174 (17)0.0074 (15)0.0022 (13)−0.0006 (13)
O150.032 (2)0.019 (2)0.044 (2)0.0106 (18)−0.0005 (18)−0.0064 (17)
O160.028 (2)0.023 (2)0.037 (2)0.0078 (17)−0.0005 (17)−0.0008 (17)
O170.029 (2)0.037 (2)0.036 (2)0.0176 (19)0.0077 (17)−0.0020 (18)
O180.034 (2)0.040 (2)0.030 (2)0.022 (2)−0.0027 (17)0.0022 (18)
O190.026 (2)0.025 (2)0.0250 (19)0.0156 (17)0.0023 (15)−0.0033 (15)
O200.0198 (19)0.026 (2)0.0259 (19)0.0116 (17)0.0052 (15)0.0033 (15)
O210.0223 (19)0.023 (2)0.0219 (19)0.0121 (17)−0.0043 (14)−0.0016 (15)
O220.026 (2)0.021 (2)0.028 (2)0.0124 (17)−0.0002 (15)0.0024 (16)
O230.0235 (19)0.023 (2)0.0258 (19)0.0136 (17)0.0002 (15)−0.0011 (15)
O240.025 (2)0.024 (2)0.0205 (18)0.0125 (17)0.0040 (15)0.0017 (15)
O250.028 (2)0.024 (2)0.0178 (18)0.0122 (17)0.0016 (15)0.0017 (15)
O260.0226 (19)0.0164 (19)0.0190 (18)0.0090 (16)0.0007 (14)−0.0035 (14)
O270.0187 (18)0.0156 (18)0.0223 (18)0.0066 (15)0.0010 (14)0.0009 (14)
O280.0197 (18)0.0160 (18)0.0162 (17)0.0076 (15)0.0011 (14)−0.0018 (14)
O29W0.077 (3)0.033 (3)0.050 (3)0.030 (3)0.000 (2)0.000 (2)
O30W0.030 (2)0.053 (3)0.069 (3)0.021 (2)−0.014 (2)−0.023 (2)
O31W0.057 (3)0.111 (4)0.053 (3)0.055 (3)−0.022 (2)−0.037 (3)
O32W0.064 (3)0.071 (4)0.080 (4)0.038 (3)0.002 (3)−0.002 (3)
O33W0.124 (5)0.042 (3)0.083 (4)0.045 (3)−0.038 (3)−0.009 (3)
O34W0.145 (7)0.109 (6)0.159 (7)0.073 (5)−0.017 (5)−0.037 (5)
V10.0211 (5)0.0155 (5)0.0259 (5)0.0098 (4)0.0010 (4)−0.0017 (4)
V20.0170 (5)0.0170 (5)0.0244 (5)0.0069 (4)−0.0016 (4)−0.0023 (4)
V30.0201 (5)0.0258 (5)0.0255 (5)0.0126 (4)0.0038 (4)0.0002 (4)
V40.0255 (5)0.0280 (5)0.0231 (5)0.0164 (4)−0.0005 (4)0.0024 (4)
V50.0181 (5)0.0163 (5)0.0160 (4)0.0085 (4)0.0010 (3)0.0001 (3)
V60.0216 (5)0.0166 (5)0.0262 (5)0.0103 (4)0.0004 (4)−0.0007 (4)
V70.0183 (5)0.0183 (5)0.0233 (5)0.0078 (4)−0.0001 (4)−0.0010 (4)
V80.0220 (5)0.0265 (5)0.0245 (5)0.0128 (4)0.0038 (4)−0.0007 (4)
V90.0252 (5)0.0276 (5)0.0242 (5)0.0164 (4)−0.0010 (4)0.0018 (4)
V100.0185 (5)0.0172 (5)0.0158 (4)0.0079 (4)0.0005 (3)−0.0005 (3)
Geometric parameters (Å, °) top
C1—N11.489 (6)V4—O41.603 (3)
C1—H1A0.9600O5—V11.822 (3)
C1—H1B0.9600O5—V31.845 (3)
C1—H1C0.9600O6—V2i1.822 (3)
C2—N11.486 (7)O6—V31.902 (3)
C2—H2A0.9600O7—V21.810 (3)
C2—H2B0.9600O7—V41.883 (3)
C2—H2C0.9600O8—V1i1.825 (3)
C3—N11.480 (6)O8—V41.873 (3)
C3—C41.507 (7)O9—V41.834 (3)
C3—H3A0.9700O9—V3i1.834 (3)
C3—H3B0.9700O10—V51.693 (3)
C4—C51.508 (7)O10—V32.035 (3)
C4—H4A0.9700O11—V51.690 (3)
C4—H4B0.9700O11—V42.036 (3)
C5—N21.477 (7)O12—V51.893 (3)
C5—H5A0.9700O12—V11.999 (3)
C5—H5B0.9700O12—V21.999 (3)
C6—N31.491 (7)O13—V51.972 (3)
C6—H6A0.9600O13—V1i2.012 (3)
C6—H6B0.9600O13—V2i2.021 (3)
C6—H6C0.9600O14—V52.103 (3)
C7—N31.494 (7)O14—V5i2.111 (3)
C7—H7A0.9600O14—V22.244 (3)
C7—H7B0.9600O14—V1i2.260 (3)
C7—H7C0.9600O14—V3i2.308 (3)
C8—N31.485 (7)O14—V42.315 (3)
C8—C91.502 (7)V6—O151.617 (3)
C8—H8A0.9700V7—O161.605 (3)
C8—H8B0.9700V8—O171.612 (4)
C9—C101.507 (7)V9—O181.602 (3)
C9—H9A0.9700O19—V61.829 (3)
C9—H9B0.9700O19—V81.832 (3)
C10—N41.479 (7)O20—V7ii1.814 (3)
C10—H10A0.9700O20—V81.907 (3)
C10—H10B0.9700O21—V71.830 (3)
C11—N51.499 (6)O21—V91.860 (3)
C11—H11A0.9600O22—V6ii1.792 (3)
C11—H11B0.9600O22—V91.909 (3)
C11—H11C0.9600O23—V91.832 (3)
C12—N51.480 (7)O23—V8ii1.848 (3)
C12—H12A0.9600O24—V101.691 (3)
C12—H12B0.9600O24—V82.032 (3)
C12—H12C0.9600O25—V101.682 (3)
C13—C141.495 (8)O25—V92.050 (3)
C13—N51.503 (7)O26—V101.930 (3)
C13—H13A0.9700O26—V72.018 (3)
C13—H13B0.9700O26—V62.032 (3)
C14—C151.518 (7)O27—V101.948 (3)
C14—H14A0.9700O27—V6ii1.995 (3)
C14—H14B0.9700O27—V7ii2.014 (3)
C15—N61.477 (7)O28—V102.085 (3)
C15—H15A0.9700O28—V10ii2.126 (3)
C15—H15B0.9700O28—V6ii2.247 (3)
N1—H10.9100O28—V72.260 (3)
N2—H2D0.8900O28—V8ii2.321 (3)
N2—H2E0.8900O28—V92.322 (3)
N2—H2F0.8900O29W—H29B0.9411
N3—H30.9100O29W—H29A0.9099
N4—H4C0.8900O30W—H30A0.8405
N4—H4D0.8900O30W—H30B0.8660
N4—H4E0.8900O31W—H31A0.9488
N5—H50.9100O31W—H31B0.8181
N6—H6D0.8900O32W—H32A0.8804
N6—H6E0.8900O32W—H32B0.8766
N6—H6F0.8900O33W—H33A0.8700
V1—O11.612 (3)O33W—H33B0.9676
V2—O21.622 (3)O34W—H34A0.9720
V3—O31.614 (3)O34W—H34B0.7962
N1—C1—H1A109.5V6ii—O28—V8ii85.28 (11)
N1—C1—H1B109.5V7—O28—V8ii86.66 (11)
H1A—C1—H1B109.5V10—O28—V988.12 (11)
N1—C1—H1C109.5V10ii—O28—V9170.14 (16)
H1A—C1—H1C109.5V6ii—O28—V986.37 (11)
H1B—C1—H1C109.5V7—O28—V984.85 (11)
N1—C2—H2A109.5V8ii—O28—V983.17 (10)
N1—C2—H2B109.5H29B—O29W—H29A108.4
H2A—C2—H2B109.5H30A—O30W—H30B107.1
N1—C2—H2C109.5H31A—O31W—H31B105.3
H2A—C2—H2C109.5H32A—O32W—H32B107.3
H2B—C2—H2C109.5H33A—O33W—H33B102.4
N1—C3—C4115.2 (4)H34A—O34W—H34B104.1
N1—C3—H3A108.5O1—V1—O5103.12 (17)
C4—C3—H3A108.5O1—V1—O8i102.97 (17)
N1—C3—H3B108.5O5—V1—O8i95.31 (15)
C4—C3—H3B108.5O1—V1—O12100.68 (16)
H3A—C3—H3B107.5O5—V1—O1289.63 (14)
C3—C4—C5108.5 (4)O8i—V1—O12154.03 (14)
C3—C4—H4A110.0O1—V1—O13i100.41 (16)
C5—C4—H4A110.0O5—V1—O13i154.35 (14)
C3—C4—H4B110.0O8i—V1—O13i89.21 (14)
C5—C4—H4B110.0O12—V1—O13i76.03 (13)
H4A—C4—H4B108.4O1—V1—O14i175.06 (15)
N2—C5—C4112.4 (4)O5—V1—O14i79.86 (13)
N2—C5—H5A109.1O8i—V1—O14i80.52 (13)
C4—C5—H5A109.1O12—V1—O14i75.27 (12)
N2—C5—H5B109.1O13i—V1—O14i76.00 (12)
C4—C5—H5B109.1O2—V2—O7101.61 (16)
H5A—C5—H5B107.9O2—V2—O6i103.40 (17)
N3—C6—H6A109.5O7—V2—O6i95.38 (15)
N3—C6—H6B109.5O2—V2—O1299.67 (16)
H6A—C6—H6B109.5O7—V2—O1290.05 (14)
N3—C6—H6C109.5O6i—V2—O12154.66 (14)
H6A—C6—H6C109.5O2—V2—O13i100.90 (15)
H6B—C6—H6C109.5O7—V2—O13i155.12 (14)
N3—C7—H7A109.5O6i—V2—O13i89.56 (14)
N3—C7—H7B109.5O12—V2—O13i75.83 (13)
H7A—C7—H7B109.5O2—V2—O14174.78 (15)
N3—C7—H7C109.5O7—V2—O1480.76 (13)
H7A—C7—H7C109.5O6i—V2—O1480.89 (13)
H7B—C7—H7C109.5O12—V2—O1475.58 (12)
N3—C8—C9115.0 (4)O13i—V2—O1475.97 (12)
N3—C8—H8A108.5O3—V3—O9i103.59 (16)
C9—C8—H8A108.5O3—V3—O5102.92 (17)
N3—C8—H8B108.5O9i—V3—O591.38 (15)
C9—C8—H8B108.5O3—V3—O6100.78 (17)
H8A—C8—H8B107.5O9i—V3—O690.14 (15)
C8—C9—C10109.6 (5)O5—V3—O6155.18 (14)
C8—C9—H9A109.7O3—V3—O1099.79 (16)
C10—C9—H9A109.7O9i—V3—O10156.55 (14)
C8—C9—H9B109.7O5—V3—O1085.03 (14)
C10—C9—H9B109.7O6—V3—O1083.79 (14)
H9A—C9—H9B108.2O3—V3—O14i174.52 (15)
N4—C10—C9112.5 (5)O9i—V3—O14i81.70 (13)
N4—C10—H10A109.1O5—V3—O14i78.12 (13)
C9—C10—H10A109.1O6—V3—O14i77.59 (13)
N4—C10—H10B109.1O10—V3—O14i74.88 (12)
C9—C10—H10B109.1O4—V4—O9101.91 (17)
H10A—C10—H10B107.8O4—V4—O8101.43 (17)
N5—C11—H11A109.5O9—V4—O891.83 (15)
N5—C11—H11B109.5O4—V4—O7102.55 (17)
H11A—C11—H11B109.5O9—V4—O791.52 (15)
N5—C11—H11C109.5O8—V4—O7154.52 (14)
H11A—C11—H11C109.5O4—V4—O11102.08 (16)
H11B—C11—H11C109.5O9—V4—O11156.01 (14)
N5—C12—H12A109.5O8—V4—O1183.94 (14)
N5—C12—H12B109.5O7—V4—O1182.79 (14)
H12A—C12—H12B109.5O4—V4—O14176.56 (15)
N5—C12—H12C109.5O9—V4—O1481.53 (12)
H12A—C12—H12C109.5O8—V4—O1478.11 (12)
H12B—C12—H12C109.5O7—V4—O1477.43 (12)
C14—C13—N5114.3 (5)O11—V4—O1474.49 (12)
C14—C13—H13A108.7O11—V5—O10106.42 (15)
N5—C13—H13A108.7O11—V5—O1298.35 (15)
C14—C13—H13B108.7O10—V5—O1298.86 (15)
N5—C13—H13B108.7O11—V5—O1396.20 (15)
H13A—C13—H13B107.6O10—V5—O1394.96 (15)
C13—C14—C15109.1 (5)O12—V5—O13156.18 (14)
C13—C14—H14A109.9O11—V5—O1487.61 (14)
C15—C14—H14A109.9O10—V5—O14165.73 (14)
C13—C14—H14B109.9O12—V5—O1481.28 (13)
C15—C14—H14B109.9O13—V5—O1480.60 (13)
H14A—C14—H14B108.3O11—V5—O14i165.84 (14)
N6—C15—C14111.7 (5)O10—V5—O14i87.58 (14)
N6—C15—H15A109.3O12—V5—O14i81.15 (13)
C14—C15—H15A109.3O13—V5—O14i80.15 (12)
N6—C15—H15B109.3O14—V5—O14i78.32 (13)
C14—C15—H15B109.3O15—V6—O22ii103.92 (17)
H15A—C15—H15B107.9O15—V6—O19102.71 (17)
C3—N1—C2112.8 (4)O22ii—V6—O1995.81 (15)
C3—N1—C1110.3 (4)O15—V6—O27ii99.87 (16)
C2—N1—C1110.2 (4)O22ii—V6—O27ii91.11 (14)
C3—N1—H1107.8O19—V6—O27ii153.99 (14)
C2—N1—H1107.8O15—V6—O2699.51 (16)
C1—N1—H1107.8O22ii—V6—O26154.88 (14)
C5—N2—H2D109.5O19—V6—O2687.72 (14)
C5—N2—H2E109.5O27ii—V6—O2675.91 (13)
H2D—N2—H2E109.5O15—V6—O28ii174.18 (15)
C5—N2—H2F109.5O22ii—V6—O28ii80.73 (13)
H2D—N2—H2F109.5O19—V6—O28ii80.07 (13)
H2E—N2—H2F109.5O27ii—V6—O28ii76.34 (12)
C8—N3—C6109.5 (5)O26—V6—O28ii75.38 (12)
C8—N3—C7112.2 (5)O15—V6—V789.80 (13)
C6—N3—C7111.6 (5)O22ii—V6—V7130.60 (11)
C8—N3—H3107.8O19—V6—V7127.54 (11)
C6—N3—H3107.8O27ii—V6—V739.52 (9)
C7—N3—H3107.8O26—V6—V739.82 (9)
C10—N4—H4C109.5O28ii—V6—V784.48 (9)
C10—N4—H4D109.5O16—V7—O20ii103.06 (18)
H4C—N4—H4D109.5O16—V7—O21102.41 (17)
C10—N4—H4E109.5O20ii—V7—O2195.10 (15)
H4C—N4—H4E109.5O16—V7—O27ii99.75 (16)
H4D—N4—H4E109.5O20ii—V7—O27ii89.78 (14)
C12—N5—C11111.3 (4)O21—V7—O27ii155.56 (14)
C12—N5—C13110.6 (5)O16—V7—O26100.63 (16)
C11—N5—C13113.4 (4)O20ii—V7—O26154.04 (14)
C12—N5—H5107.0O21—V7—O2690.03 (14)
C11—N5—H5107.0O27ii—V7—O2675.80 (13)
C13—N5—H5107.0O16—V7—O28174.69 (15)
C15—N6—H6D109.5O20ii—V7—O2880.36 (13)
C15—N6—H6E109.5O21—V7—O2881.17 (13)
H6D—N6—H6E109.5O27ii—V7—O2876.05 (12)
C15—N6—H6F109.5O26—V7—O2875.31 (12)
H6D—N6—H6F109.5O16—V7—V690.45 (13)
H6E—N6—H6F109.5O20ii—V7—V6128.83 (11)
V1—O5—V3115.52 (17)O21—V7—V6130.18 (11)
V2i—O6—V3113.97 (17)O27ii—V7—V639.07 (9)
V2—O7—V4114.64 (16)O26—V7—V640.16 (9)
V1i—O8—V4114.51 (17)O28—V7—V684.24 (9)
V4—O9—V3i113.57 (16)O17—V8—O19103.14 (17)
V5—O10—V3109.96 (16)O17—V8—O23ii103.42 (17)
V5—O11—V4110.27 (16)O19—V8—O23ii92.55 (15)
V5—O12—V1108.38 (15)O17—V8—O20101.36 (17)
V5—O12—V2107.56 (15)O19—V8—O20154.51 (14)
V1—O12—V2101.07 (14)O23ii—V8—O2088.51 (14)
V5—O13—V1i106.68 (15)O17—V8—O24100.17 (16)
V5—O13—V2i106.75 (14)O19—V8—O2485.36 (14)
V1i—O13—V2i99.88 (14)O23ii—V8—O24156.17 (14)
V5—O14—V5i101.68 (13)O20—V8—O2483.53 (14)
V5—O14—V292.45 (12)O17—V8—O28ii174.91 (15)
V5i—O14—V294.71 (12)O19—V8—O28ii78.03 (13)
V5—O14—V1i94.12 (12)O23ii—V8—O28ii81.41 (13)
V5i—O14—V1i92.41 (12)O20—V8—O28ii76.95 (13)
V2—O14—V1i169.15 (15)O24—V8—O28ii74.92 (12)
V5—O14—V3i170.82 (15)O18—V9—O23103.17 (17)
V5i—O14—V3i87.50 (11)O18—V9—O21102.75 (17)
V2—O14—V3i86.63 (11)O23—V9—O2192.49 (15)
V1i—O14—V3i85.51 (11)O18—V9—O22101.19 (17)
V5—O14—V487.64 (11)O23—V9—O2290.76 (15)
V5i—O14—V4170.60 (15)O21—V9—O22154.41 (14)
V2—O14—V485.99 (11)O18—V9—O25101.39 (16)
V1i—O14—V485.66 (11)O23—V9—O25155.36 (14)
V3i—O14—V483.18 (10)O21—V9—O2584.10 (14)
V6—O19—V8115.41 (17)O22—V9—O2582.44 (14)
V7ii—O20—V8115.26 (18)O18—V9—O28174.72 (16)
V7—O21—V9113.80 (16)O23—V9—O2881.70 (12)
V6ii—O22—V9115.30 (17)O21—V9—O2878.89 (13)
V9—O23—V8ii113.72 (16)O22—V9—O2876.49 (12)
V10—O24—V8110.52 (16)O25—V9—O2873.69 (12)
V10—O25—V9110.27 (16)O25—V10—O24106.30 (16)
V10—O26—V7106.79 (15)O25—V10—O2697.37 (15)
V10—O26—V6107.81 (15)O24—V10—O2696.91 (15)
V7—O26—V6100.02 (14)O25—V10—O2797.73 (15)
V10—O27—V6ii106.02 (15)O24—V10—O2796.00 (15)
V10—O27—V7ii107.35 (15)O26—V10—O27156.51 (13)
V6ii—O27—V7ii101.41 (14)O25—V10—O2887.90 (14)
V10—O28—V10ii101.68 (13)O24—V10—O28165.79 (14)
V10—O28—V6ii93.19 (13)O26—V10—O2881.38 (13)
V10ii—O28—V6ii94.09 (12)O27—V10—O2881.30 (13)
V10—O28—V793.59 (12)O25—V10—O28ii166.22 (14)
V10ii—O28—V793.37 (12)O24—V10—O28ii87.48 (14)
V6ii—O28—V7168.71 (15)O26—V10—O28ii80.38 (13)
V10—O28—V8ii171.23 (15)O27—V10—O28ii80.66 (13)
V10ii—O28—V8ii87.05 (11)O28—V10—O28ii78.32 (13)
N1—C3—C4—C5−168.4 (5)V10—O26—V6—V7−111.39 (19)
C3—C4—C5—N2−171.0 (5)V9—O21—V7—O16−173.84 (19)
N3—C8—C9—C10−179.9 (5)V9—O21—V7—O20ii−69.24 (19)
C8—C9—C10—N4171.8 (5)V9—O21—V7—O27ii31.5 (4)
N5—C13—C14—C15−156.9 (4)V9—O21—V7—O2685.27 (18)
C13—C14—C15—N6−174.4 (4)V9—O21—V7—O2810.15 (16)
C4—C3—N1—C2−58.7 (6)V9—O21—V7—V684.83 (19)
C4—C3—N1—C1177.6 (5)V10—O26—V7—O16−169.93 (16)
C9—C8—N3—C6169.2 (5)V6—O26—V7—O1677.88 (17)
C9—C8—N3—C7−66.2 (6)V10—O26—V7—O20ii34.5 (4)
C14—C13—N5—C12−172.2 (5)V6—O26—V7—O20ii−77.7 (3)
C14—C13—N5—C11−46.3 (6)V10—O26—V7—O21−67.29 (16)
V3—O5—V1—O1175.06 (18)V6—O26—V7—O21−179.48 (14)
V3—O5—V1—O8i70.40 (19)V10—O26—V7—O27ii92.58 (16)
V3—O5—V1—O12−84.06 (18)V6—O26—V7—O27ii−19.61 (12)
V3—O5—V1—O13i−28.9 (4)V10—O26—V7—O2813.57 (13)
V3—O5—V1—O14i−8.96 (16)V6—O26—V7—O28−98.62 (14)
V5—O12—V1—O1169.40 (17)V10—O26—V7—V6112.19 (19)
V2—O12—V1—O1−77.72 (18)V10—O28—V7—O20ii177.09 (14)
V5—O12—V1—O566.12 (17)V10ii—O28—V7—O20ii−80.97 (13)
V2—O12—V1—O5179.00 (15)V6ii—O28—V7—O20ii50.3 (8)
V5—O12—V1—O8i−35.3 (4)V8ii—O28—V7—O20ii5.88 (12)
V2—O12—V1—O8i77.6 (3)V9—O28—V7—O20ii89.31 (12)
V5—O12—V1—O13i−92.40 (16)V10—O28—V7—O2180.34 (14)
V2—O12—V1—O13i20.48 (13)V10ii—O28—V7—O21−177.73 (14)
V5—O12—V1—O14i−13.50 (13)V6ii—O28—V7—O21−46.5 (8)
V2—O12—V1—O14i99.39 (14)V8ii—O28—V7—O21−90.88 (13)
V4—O7—V2—O2−174.99 (18)V9—O28—V7—O21−7.45 (12)
V4—O7—V2—O6i−70.09 (19)V10—O28—V7—O27ii−90.72 (13)
V4—O7—V2—O1285.12 (18)V10ii—O28—V7—O27ii11.22 (12)
V4—O7—V2—O13i30.6 (4)V6ii—O28—V7—O27ii142.5 (8)
V4—O7—V2—O149.74 (16)V8ii—O28—V7—O27ii98.06 (12)
V5—O12—V2—O2−167.99 (16)V9—O28—V7—O27ii−178.51 (13)
V1—O12—V2—O278.50 (17)V10—O28—V7—O26−12.03 (11)
V5—O12—V2—O7−66.20 (16)V10ii—O28—V7—O2689.91 (13)
V1—O12—V2—O7−179.71 (14)V6ii—O28—V7—O26−138.8 (8)
V5—O12—V2—O6i36.6 (4)V8ii—O28—V7—O26176.75 (13)
V1—O12—V2—O6i−76.9 (3)V9—O28—V7—O26−99.82 (12)
V5—O12—V2—O13i93.10 (16)V10—O28—V7—V6−51.88 (9)
V1—O12—V2—O13i−20.41 (13)V10ii—O28—V7—V650.06 (9)
V5—O12—V2—O1414.25 (13)V6ii—O28—V7—V6−178.7 (8)
V1—O12—V2—O14−99.27 (14)V8ii—O28—V7—V6136.90 (8)
V5—O14—V2—O780.25 (13)V9—O28—V7—V6−139.67 (8)
V5i—O14—V2—O7−177.81 (14)O15—V6—V7—O16−0.87 (19)
V1i—O14—V2—O7−47.0 (8)O22ii—V6—V7—O16107.4 (2)
V3i—O14—V2—O7−90.60 (13)O19—V6—V7—O16−106.82 (19)
V4—O14—V2—O7−7.21 (12)O27ii—V6—V7—O16105.0 (2)
V5—O14—V2—O6i177.28 (14)O26—V6—V7—O16−106.06 (19)
V5i—O14—V2—O6i−80.78 (14)O28ii—V6—V7—O16−179.80 (15)
V1i—O14—V2—O6i50.0 (8)O15—V6—V7—O20ii−108.1 (2)
V3i—O14—V2—O6i6.43 (12)O22ii—V6—V7—O20ii0.2 (2)
V4—O14—V2—O6i89.82 (12)O19—V6—V7—O20ii145.94 (19)
V5—O14—V2—O12−12.20 (11)O27ii—V6—V7—O20ii−2.2 (2)
V5i—O14—V2—O1289.74 (13)O26—V6—V7—O20ii146.7 (2)
V1i—O14—V2—O12−139.4 (8)O28ii—V6—V7—O20ii72.96 (17)
V3i—O14—V2—O12176.95 (13)O15—V6—V7—O21105.87 (19)
V4—O14—V2—O12−99.66 (12)O22ii—V6—V7—O21−145.84 (19)
V5—O14—V2—O13i−90.88 (13)O19—V6—V7—O21−0.08 (19)
V5i—O14—V2—O13i11.06 (12)O27ii—V6—V7—O21−148.2 (2)
V1i—O14—V2—O13i141.9 (8)O26—V6—V7—O210.68 (19)
V3i—O14—V2—O13i98.27 (12)O28ii—V6—V7—O21−73.06 (16)
V4—O14—V2—O13i−178.34 (13)O15—V6—V7—O27ii−105.9 (2)
V1—O5—V3—O3−176.69 (19)O22ii—V6—V7—O27ii2.4 (2)
V1—O5—V3—O9i−72.40 (19)O19—V6—V7—O27ii148.2 (2)
V1—O5—V3—O620.9 (4)O26—V6—V7—O27ii148.9 (2)
V1—O5—V3—O1084.38 (18)O28ii—V6—V7—O27ii75.19 (17)
V1—O5—V3—O14i8.82 (16)O15—V6—V7—O26105.19 (19)
V2i—O6—V3—O3176.95 (18)O22ii—V6—V7—O26−146.5 (2)
V2i—O6—V3—O9i73.09 (19)O19—V6—V7—O26−0.76 (19)
V2i—O6—V3—O5−20.5 (4)O27ii—V6—V7—O26−148.9 (2)
V2i—O6—V3—O10−84.22 (18)O28ii—V6—V7—O26−73.73 (16)
V2i—O6—V3—O14i−8.39 (15)O15—V6—V7—O28179.19 (16)
V5—O10—V3—O3−178.89 (19)O22ii—V6—V7—O28−72.52 (17)
V5—O10—V3—O9i5.4 (4)O19—V6—V7—O2873.24 (16)
V5—O10—V3—O5−76.61 (18)O27ii—V6—V7—O28−74.93 (16)
V5—O10—V3—O681.19 (18)O26—V6—V7—O2873.99 (16)
V5—O10—V3—O14i2.41 (15)O28ii—V6—V7—O280.26 (15)
V3i—O9—V4—O4178.96 (19)V6—O19—V8—O17−175.33 (18)
V3i—O9—V4—O876.87 (19)V6—O19—V8—O23ii−70.92 (19)
V3i—O9—V4—O7−77.87 (18)V6—O19—V8—O2021.0 (4)
V3i—O9—V4—O11−2.3 (5)V6—O19—V8—O2485.29 (18)
V3i—O9—V4—O14−0.82 (16)V6—O19—V8—O28ii9.74 (16)
V1i—O8—V4—O4−173.82 (19)V7ii—O20—V8—O17177.13 (18)
V1i—O8—V4—O9−71.28 (19)V7ii—O20—V8—O19−19.0 (4)
V1i—O8—V4—O726.1 (4)V7ii—O20—V8—O23ii73.74 (19)
V1i—O8—V4—O1185.04 (18)V7ii—O20—V8—O24−83.76 (18)
V1i—O8—V4—O149.66 (16)V7ii—O20—V8—O28ii−7.79 (16)
V2—O7—V4—O4173.98 (19)V10—O24—V8—O17−179.79 (19)
V2—O7—V4—O971.43 (19)V10—O24—V8—O19−77.24 (19)
V2—O7—V4—O8−26.0 (4)V10—O24—V8—O23ii8.5 (4)
V2—O7—V4—O11−85.19 (18)V10—O24—V8—O2079.78 (18)
V2—O7—V4—O14−9.55 (16)V10—O24—V8—O28ii1.59 (15)
V5—O11—V4—O4179.90 (19)V8ii—O23—V9—O18177.35 (19)
V5—O11—V4—O91.2 (4)V8ii—O23—V9—O21−78.94 (19)
V5—O11—V4—O8−79.66 (18)V8ii—O23—V9—O2275.68 (18)
V5—O11—V4—O778.54 (18)V8ii—O23—V9—O252.3 (5)
V5—O11—V4—O14−0.36 (15)V8ii—O23—V9—O28−0.55 (16)
V5—O14—V4—O9−179.10 (14)V7—O21—V9—O18175.18 (19)
V2—O14—V4—O9−86.47 (13)V7—O21—V9—O2371.09 (19)
V1i—O14—V4—O986.59 (13)V7—O21—V9—O22−25.9 (4)
V3i—O14—V4—O90.60 (12)V7—O21—V9—O25−84.44 (18)
V5—O14—V4—O887.21 (14)V7—O21—V9—O28−9.95 (16)
V2—O14—V4—O8179.84 (14)V6ii—O22—V9—O18−175.5 (2)
V1i—O14—V4—O8−7.10 (12)V6ii—O22—V9—O23−71.9 (2)
V3i—O14—V4—O8−93.09 (13)V6ii—O22—V9—O2125.4 (4)
V5—O14—V4—O7−85.62 (13)V6ii—O22—V9—O2584.29 (19)
V2—O14—V4—O77.00 (12)V6ii—O22—V9—O289.32 (16)
V1i—O14—V4—O7−179.94 (13)V10—O25—V9—O18−178.88 (19)
V3i—O14—V4—O794.08 (13)V10—O25—V9—O23−3.8 (4)
V5—O14—V4—O110.27 (11)V10—O25—V9—O2179.26 (18)
V2—O14—V4—O1192.90 (13)V10—O25—V9—O22−78.92 (18)
V1i—O14—V4—O11−94.04 (13)V10—O25—V9—O28−0.85 (15)
V3i—O14—V4—O11179.98 (13)V10—O28—V9—O23179.39 (14)
V4—O11—V5—O10177.70 (16)V6ii—O28—V9—O2386.08 (13)
V4—O11—V5—O12−80.44 (17)V7—O28—V9—O23−86.83 (13)
V4—O11—V5—O1380.66 (17)V8ii—O28—V9—O230.40 (12)
V4—O11—V5—O140.38 (16)V10—O28—V9—O21−86.40 (14)
V4—O11—V5—O14i6.5 (7)V6ii—O28—V9—O21−179.71 (14)
V3—O10—V5—O11179.60 (16)V7—O28—V9—O217.38 (12)
V3—O10—V5—O1278.11 (17)V8ii—O28—V9—O2194.62 (13)
V3—O10—V5—O13−82.44 (17)V10—O28—V9—O2286.59 (14)
V3—O10—V5—O14−11.3 (7)V6ii—O28—V9—O22−6.72 (12)
V3—O10—V5—O14i−2.54 (16)V7—O28—V9—O22−179.63 (14)
V1—O12—V5—O11179.85 (15)V8ii—O28—V9—O22−92.39 (13)
V2—O12—V5—O1171.35 (17)V10—O28—V9—O250.65 (11)
V1—O12—V5—O10−71.96 (17)V6ii—O28—V9—O25−92.67 (13)
V2—O12—V5—O10179.54 (15)V7—O28—V9—O2594.42 (13)
V1—O12—V5—O1352.8 (4)V8ii—O28—V9—O25−178.34 (13)
V2—O12—V5—O13−55.7 (4)V9—O25—V10—O24−179.56 (16)
V1—O12—V5—O1493.59 (15)V9—O25—V10—O26−80.11 (17)
V2—O12—V5—O14−14.91 (14)V9—O25—V10—O2781.84 (18)
V1—O12—V5—O14i14.16 (14)V9—O25—V10—O280.91 (16)
V2—O12—V5—O14i−94.34 (15)V9—O25—V10—O28ii−0.5 (7)
V1i—O13—V5—O11−73.01 (17)V8—O24—V10—O25178.10 (16)
V2i—O13—V5—O11−179.11 (15)V8—O24—V10—O2678.31 (17)
V1i—O13—V5—O10179.84 (15)V8—O24—V10—O27−82.01 (17)
V2i—O13—V5—O1073.75 (16)V8—O24—V10—O28−3.8 (7)
V1i—O13—V5—O1254.4 (4)V8—O24—V10—O28ii−1.68 (16)
V2i—O13—V5—O12−51.7 (4)V7—O26—V10—O2572.32 (17)
V1i—O13—V5—O1413.52 (13)V6—O26—V10—O25179.05 (15)
V2i—O13—V5—O14−92.58 (15)V7—O26—V10—O24179.83 (15)
V1i—O13—V5—O14i93.17 (15)V6—O26—V10—O24−73.45 (17)
V2i—O13—V5—O14i−12.92 (14)V7—O26—V10—O27−57.3 (4)
V5i—O14—V5—O11178.48 (15)V6—O26—V10—O2749.4 (4)
V2—O14—V5—O11−86.20 (14)V7—O26—V10—O28−14.41 (14)
V1i—O14—V5—O1185.16 (14)V6—O26—V10—O2892.31 (15)
V4—O14—V5—O11−0.32 (13)V7—O26—V10—O28ii−93.93 (15)
V5i—O14—V5—O109.0 (6)V6—O26—V10—O28ii12.80 (14)
V2—O14—V5—O10104.3 (6)V6ii—O27—V10—O25−71.81 (17)
V1i—O14—V5—O10−84.3 (6)V7ii—O27—V10—O25−179.59 (16)
V4—O14—V5—O10−169.8 (5)V6ii—O27—V10—O24−179.21 (15)
V5i—O14—V5—O12−82.69 (14)V7ii—O27—V10—O2473.01 (17)
V2—O14—V5—O1212.63 (12)V6ii—O27—V10—O2657.8 (4)
V1i—O14—V5—O12−176.01 (13)V7ii—O27—V10—O26−50.0 (4)
V4—O14—V5—O1298.52 (12)V6ii—O27—V10—O2814.86 (13)
V5i—O14—V5—O1381.79 (14)V7ii—O27—V10—O28−92.92 (15)
V2—O14—V5—O13177.12 (13)V6ii—O27—V10—O28ii94.35 (15)
V1i—O14—V5—O13−11.53 (11)V7ii—O27—V10—O28ii−13.43 (14)
V4—O14—V5—O13−97.00 (12)V10ii—O28—V10—O25−179.66 (16)
V5i—O14—V5—O14i0.0V6ii—O28—V10—O2585.50 (14)
V2—O14—V5—O14i95.33 (14)V7—O28—V10—O25−85.47 (14)
V1i—O14—V5—O14i−93.32 (14)V9—O28—V10—O25−0.76 (13)
V4—O14—V5—O14i−178.79 (17)V10ii—O28—V10—O242.2 (6)
V8—O19—V6—O15175.22 (18)V6ii—O28—V10—O24−92.7 (6)
V8—O19—V6—O22ii69.5 (2)V7—O28—V10—O2496.4 (6)
V8—O19—V6—O27ii−35.1 (4)V9—O28—V10—O24−178.9 (5)
V8—O19—V6—O26−85.55 (18)V10ii—O28—V10—O26−81.88 (14)
V8—O19—V6—O28ii−9.99 (16)V6ii—O28—V10—O26−176.72 (13)
V8—O19—V6—V7−85.06 (19)V7—O28—V10—O2612.31 (12)
V10—O26—V6—O15170.52 (17)V9—O28—V10—O2697.02 (12)
V7—O26—V6—O15−78.09 (18)V10ii—O28—V10—O2782.19 (14)
V10—O26—V6—O22ii−30.8 (4)V6ii—O28—V10—O27−12.65 (11)
V7—O26—V6—O22ii80.6 (4)V7—O28—V10—O27176.38 (13)
V10—O26—V6—O1968.01 (17)V9—O28—V10—O27−98.91 (12)
V7—O26—V6—O19179.40 (15)V10ii—O28—V10—O28ii0.0
V10—O26—V6—O27ii−91.60 (16)V6ii—O28—V10—O28ii−94.84 (14)
V7—O26—V6—O27ii19.80 (13)V7—O28—V10—O28ii94.19 (14)
V10—O26—V6—O28ii−12.32 (13)V9—O28—V10—O28ii178.91 (17)
V7—O26—V6—O28ii99.07 (14)
Symmetry codes: (i) −x, −y, −z+1; (ii) −x, −y+1, −z.
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
N1—H1···O13i0.911.792.691 (5)173
N2—H2D···O32W0.892.082.968 (7)172
N2—H2E···O9iii0.892.052.873 (5)153
N2—H2F···O6iv0.891.892.772 (6)173
N3—H3···O27v0.911.872.736 (6)159
N4—H4C···O20vi0.891.892.772 (5)171
N4—H4D···O33Wii0.892.213.035 (7)154
N4—H4E···O230.891.992.820 (5)156
N5—H5···O260.911.822.709 (5)166
N6—H6D···O170.892.343.056 (6)137
N6—H6D···O32Wvii0.892.503.046 (7)120
N6—H6E···O31Wviii0.891.892.745 (6)160
N6—H6F···O2vii0.892.122.958 (6)156
O29W—H29A···O10.912.002.848 (5)154
O29W—H29B···O8iii0.941.902.790 (5)156
O30W—H30A···O3vii0.842.062.895 (5)174
O30W—H30B···O7ix0.871.862.716 (5)173
O31W—H31A···O210.951.832.770 (5)173
O31W—H31B···O30W0.821.942.724 (6)160
O32W—H32A···O29W0.882.002.808 (6)152
O32W—H32B···O34Wix0.882.032.873 (8)160
O33W—H33A···O15x0.871.982.787 (6)153
O33W—H33B···O22ii0.971.842.723 (5)150
O34W—H34A···O180.972.113.055 (7)163
O34W—H34B···O33Wii0.802.242.903 (8)141
Symmetry codes: (i) −x, −y, −z+1; (iii) x, y+1, z; (iv) x+1, y+1, z; (v) −x, −y, −z; (vi) x+1, y, z; (ii) −x, −y+1, −z; (vii) −x, −y+1, −z+1; (viii) x−1, y, z; (ix) −x+1, −y+1, −z+1; (x) −x, −y+2, −z.
Table 1
Selected geometric parameters (Å) top
V1—O11.612 (3)V6—O151.617 (3)
V2—O21.622 (3)V7—O161.605 (3)
V3—O31.614 (3)V8—O171.612 (4)
V4—O41.603 (3)V9—O181.602 (3)
Table 2
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
N1—H1···O13i0.911.792.691 (5)173
N2—H2D···O32W0.892.082.968 (7)172
N2—H2E···O9ii0.892.052.873 (5)153
N2—H2F···O6iii0.891.892.772 (6)173
N3—H3···O27iv0.911.872.736 (6)159
N4—H4C···O20v0.891.892.772 (5)171
N4—H4D···O33Wvi0.892.213.035 (7)154
N4—H4E···O230.891.992.820 (5)156
N5—H5···O260.911.822.709 (5)166
N6—H6D···O170.892.343.056 (6)137
N6—H6D···O32Wvii0.892.503.046 (7)120
N6—H6E···O31Wviii0.891.892.745 (6)160
N6—H6F···O2vii0.892.122.958 (6)156
O29W—H29A···O10.912.002.848 (5)154
O29W—H29B···O8ii0.941.902.790 (5)156
O30W—H30A···O3vii0.842.062.895 (5)174
O30W—H30B···O7ix0.871.862.716 (5)173
O31W—H31A···O210.951.832.770 (5)173
O31W—H31B···O30W0.821.942.724 (6)160
O32W—H32A···O29W0.882.002.808 (6)152
O32W—H32B···O34Wix0.882.032.873 (8)160
O33W—H33A···O15x0.871.982.787 (6)153
O33W—H33B···O22vi0.971.842.723 (5)150
O34W—H34A···O180.972.113.055 (7)163
O34W—H34B···O33Wvi0.802.242.903 (8)141
Symmetry codes: (i) −x, −y, −z+1; (ii) x, y+1, z; (iii) x+1, y+1, z; (iv) −x, −y, −z; (v) x+1, y, z; (vi) −x, −y+1, −z; (vii) −x, −y+1, −z+1; (viii) x−1, y, z; (ix) −x+1, −y+1, −z+1; (x) −x, −y+2, −z.
Acknowledgements top

This project was supported by the National Natural Science Foundation of China (No. 30672515) and a grant from the PhD Program Foundation of Ministry of China (No. 20060423005).

references
References top

Boyd, D. W., Kustin, K. & Niwa, M. (1985). Biochim. Biophys. Acta, 827, 472–475.

Bruker (2002). SADABS, SAINT and SMART. Bruker AXS Inc., Madison, Wisconsin, USA.

Correia, I., Avecilla, F., Marcão, S. & Pessoa, J. C. (2004). Inorg. Chim. Acta, 357, 4476–4487.

Csermely, P., Martonosi, A., Levy, G. C. & Ejchart, A. J. (1985). Biochem. J. 230, 807–815.

DeMaster, E. G. & Mitchell, R. A. (1973). Biochemistry, 12, 3616–3621.

Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837–838.

Fratzky, D., Schneider, M., Rabe, S. & Meisel, M. (2000). Acta Cryst. C56, 740–741.

Gong, Y., Hu, C. W., Li, H., Tang, W., Huang, K. L. & Hou, W. B. (2006). J. Mol. Struct. 784, 228–238.

Pai, E. F., Sachsenheimer, W., Schirmer, R. H. & Schulz, G. E. (1977). J. Mol. Biol. 114, 37–45.

Sathyanarayana, D. N. & Patel, C. C. (1965). J. Inorg. Nucl. Chem. 27, 297–302.

Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Göttingen, Germany.

Siemens (1994). XP. Version 5.03. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA.

Soman, G., Chang, Y. C. & Graves, D. J. (1983). Biochemistry, 22, 4994–5000.