Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807023306/xu2250sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807023306/xu2250Isup2.hkl |
CCDC reference: 650582
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.009 Å
- R factor = 0.045
- wR factor = 0.134
- Data-to-parameter ratio = 13.6
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 3000 Deg. PLAT341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 9 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 10 H2 O
Alert level G PLAT794_ALERT_5_G Check Predicted Bond Valency for V1 (5) 5.02 PLAT794_ALERT_5_G Check Predicted Bond Valency for V2 (5) 5.01 PLAT794_ALERT_5_G Check Predicted Bond Valency for V3 (5) 5.03 PLAT794_ALERT_5_G Check Predicted Bond Valency for V4 (5) 5.05 PLAT794_ALERT_5_G Check Predicted Bond Valency for V5 (5) 5.00 PLAT794_ALERT_5_G Check Predicted Bond Valency for V6 (5) 5.05 PLAT794_ALERT_5_G Check Predicted Bond Valency for V7 (5) 5.03 PLAT794_ALERT_5_G Check Predicted Bond Valency for V8 (5) 5.03 PLAT794_ALERT_5_G Check Predicted Bond Valency for V9 (5) 5.01 PLAT794_ALERT_5_G Check Predicted Bond Valency for V10 (5) 5.01
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 10 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 10 ALERT type 5 Informative message, check
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.
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%.
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.
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.
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.
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).
3(C5H16N2)2+.[V10O28]6−.6H2O | Z = 2 |
Mr = 1378.09 | F(000) = 1388 |
Triclinic, P1 | Dx = 2.042 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 11.525 (2) Å | Cell parameters from 1736 reflections |
b = 11.743 (2) Å | θ = 3.5–25.1° |
c = 18.709 (4) Å | µ = 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 |
Bruker APEX area-detector diffractometer | 8110 independent reflections |
Radiation source: fine-focus sealed tube | 4858 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.024 |
φ and ω scan | θmax = 25.2°, θmin = 2.0° |
Absorption correction: multi-scan (SADABS; Bruker, 2002) | h = −13→13 |
Tmin = 0.556, Tmax = 0.684 | k = −14→11 |
12138 measured reflections | l = −19→22 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.045 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.134 | H-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 parameters | Δρmax = 1.02 e Å−3 |
0 restraints | Δρmin = −0.71 e Å−3 |
3(C5H16N2)2+.[V10O28]6−.6H2O | γ = 117.29 (3)° |
Mr = 1378.09 | V = 2241.7 (10) Å3 |
Triclinic, P1 | Z = 2 |
a = 11.525 (2) Å | Mo Kα radiation |
b = 11.743 (2) Å | µ = 2.09 mm−1 |
c = 18.709 (4) Å | T = 298 K |
α = 90.45 (3)° | 0.30 × 0.26 × 0.18 mm |
β = 94.21 (3)° |
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 = 0.684 | Rint = 0.024 |
12138 measured reflections |
R[F2 > 2σ(F2)] = 0.045 | 0 restraints |
wR(F2) = 0.134 | H-atom parameters constrained |
S = 1.03 | Δρmax = 1.02 e Å−3 |
8110 reflections | Δρmin = −0.71 e Å−3 |
595 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
C1 | 0.1582 (6) | 0.3274 (6) | 0.3030 (3) | 0.0486 (17) | |
H1A | 0.1923 | 0.3863 | 0.2656 | 0.073* | |
H1B | 0.0723 | 0.3159 | 0.3111 | 0.073* | |
H1C | 0.1532 | 0.2464 | 0.2891 | 0.073* | |
C2 | 0.3772 (6) | 0.3895 (6) | 0.3602 (3) | 0.0495 (17) | |
H2A | 0.3684 | 0.3055 | 0.3500 | 0.074* | |
H2B | 0.4341 | 0.4263 | 0.4032 | 0.074* | |
H2C | 0.4137 | 0.4430 | 0.3210 | 0.074* | |
C3 | 0.2530 (6) | 0.5035 (5) | 0.3935 (3) | 0.0396 (15) | |
H3A | 0.1647 | 0.4905 | 0.3986 | 0.047* | |
H3B | 0.2879 | 0.5636 | 0.3560 | 0.047* | |
C4 | 0.3352 (5) | 0.5634 (5) | 0.4629 (3) | 0.0327 (13) | |
H4A | 0.4273 | 0.5953 | 0.4559 | 0.039* | |
H4B | 0.3124 | 0.5000 | 0.4992 | 0.039* | |
C5 | 0.3097 (6) | 0.6723 (5) | 0.4867 (3) | 0.0383 (15) | |
H5A | 0.3181 | 0.7272 | 0.4468 | 0.046* | |
H5B | 0.2206 | 0.6377 | 0.5001 | 0.046* | |
C6 | 0.1303 (6) | −0.1879 (6) | −0.1992 (3) | 0.0536 (18) | |
H6A | 0.1289 | −0.2671 | −0.2139 | 0.080* | |
H6B | 0.1469 | −0.1334 | −0.2391 | 0.080* | |
H6C | 0.0472 | −0.2053 | −0.1825 | 0.080* | |
C7 | 0.3621 (6) | −0.1187 (6) | −0.1575 (3) | 0.0509 (17) | |
H7A | 0.4284 | −0.0741 | −0.1191 | 0.076* | |
H7B | 0.3885 | −0.0749 | −0.2011 | 0.076* | |
H7C | 0.3505 | −0.2047 | −0.1636 | 0.076* | |
C8 | 0.2499 (6) | 0.0073 (5) | −0.1239 (3) | 0.0402 (15) | |
H8A | 0.1634 | 0.0001 | −0.1197 | 0.048* | |
H8B | 0.2860 | 0.0602 | −0.1641 | 0.048* | |
C9 | 0.3351 (6) | 0.0743 (5) | −0.0567 (3) | 0.0389 (15) | |
H9A | 0.4227 | 0.0840 | −0.0603 | 0.047* | |
H9B | 0.2997 | 0.0234 | −0.0158 | 0.047* | |
C10 | 0.3409 (6) | 0.2042 (6) | −0.0465 (3) | 0.0434 (16) | |
H10A | 0.3871 | 0.2581 | −0.0844 | 0.052* | |
H10B | 0.2525 | 0.1946 | −0.0505 | 0.052* | |
C11 | 0.1445 (6) | 0.6791 (6) | 0.2703 (3) | 0.0394 (15) | |
H11A | 0.2114 | 0.6593 | 0.2555 | 0.059* | |
H11B | 0.0633 | 0.6017 | 0.2700 | 0.059* | |
H11C | 0.1694 | 0.7183 | 0.3179 | 0.059* | |
C12 | 0.2544 (6) | 0.8844 (6) | 0.2121 (3) | 0.0472 (17) | |
H12A | 0.2847 | 0.9338 | 0.2568 | 0.071* | |
H12B | 0.2427 | 0.9359 | 0.1754 | 0.071* | |
H12C | 0.3177 | 0.8579 | 0.1991 | 0.071* | |
C13 | 0.0264 (6) | 0.8086 (6) | 0.2393 (3) | 0.0386 (15) | |
H13A | 0.0626 | 0.8698 | 0.2800 | 0.046* | |
H13B | 0.0076 | 0.8515 | 0.1994 | 0.046* | |
C14 | −0.0993 (6) | 0.6996 (5) | 0.2577 (3) | 0.0334 (14) | |
H14A | −0.0909 | 0.6789 | 0.3073 | 0.040* | |
H14B | −0.1194 | 0.6243 | 0.2274 | 0.040* | |
C15 | −0.2084 (6) | 0.7375 (6) | 0.2464 (3) | 0.0358 (14) | |
H15A | −0.1832 | 0.8179 | 0.2729 | 0.043* | |
H15B | −0.2213 | 0.7506 | 0.1959 | 0.043* | |
N1 | 0.2463 (4) | 0.3797 (4) | 0.3702 (2) | 0.0313 (11) | |
H1 | 0.2109 | 0.3233 | 0.4050 | 0.038* | |
N2 | 0.4011 (4) | 0.7498 (4) | 0.5480 (3) | 0.0403 (12) | |
H2D | 0.3817 | 0.7049 | 0.5873 | 0.060* | |
H2E | 0.3938 | 0.8213 | 0.5547 | 0.060* | |
H2F | 0.4828 | 0.7700 | 0.5389 | 0.060* | |
N3 | 0.2359 (5) | −0.1227 (4) | −0.1401 (2) | 0.0362 (12) | |
H3 | 0.2104 | −0.1688 | −0.1003 | 0.043* | |
N4 | 0.4074 (4) | 0.2680 (4) | 0.0238 (3) | 0.0402 (13) | |
H4C | 0.4890 | 0.2781 | 0.0275 | 0.060* | |
H4D | 0.3640 | 0.2200 | 0.0588 | 0.060* | |
H4E | 0.4091 | 0.3444 | 0.0274 | 0.060* | |
N5 | 0.1280 (5) | 0.7699 (5) | 0.2197 (2) | 0.0374 (12) | |
H5 | 0.1000 | 0.7281 | 0.1758 | 0.045* | |
N6 | −0.3327 (5) | 0.6385 (5) | 0.2705 (3) | 0.0473 (14) | |
H6D | −0.3552 | 0.5642 | 0.2470 | 0.071* | |
H6E | −0.3954 | 0.6621 | 0.2615 | 0.071* | |
H6F | −0.3225 | 0.6296 | 0.3174 | 0.071* | |
O1 | 0.0812 (3) | 0.3762 (3) | 0.55044 (19) | 0.0314 (9) | |
O2 | 0.3306 (3) | 0.3370 (3) | 0.57192 (18) | 0.0278 (8) | |
O3 | −0.3799 (3) | −0.0088 (3) | 0.61327 (19) | 0.0325 (9) | |
O4 | 0.2918 (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) | |
O7 | 0.2912 (3) | 0.1067 (3) | 0.61371 (16) | 0.0210 (8) | |
O8 | 0.0956 (3) | −0.2327 (3) | 0.55729 (17) | 0.0235 (8) | |
O9 | 0.3267 (3) | −0.0501 (3) | 0.52439 (18) | 0.0241 (8) | |
O10 | −0.1539 (3) | −0.0427 (3) | 0.62667 (17) | 0.0220 (8) | |
O11 | 0.0655 (3) | −0.0732 (3) | 0.64332 (16) | 0.0214 (8) | |
O12 | 0.0795 (3) | 0.1475 (3) | 0.59142 (16) | 0.0180 (7) | |
O13 | −0.1227 (3) | −0.2032 (3) | 0.53428 (16) | 0.0180 (7) | |
O14 | 0.1072 (3) | −0.0160 (3) | 0.50820 (15) | 0.0163 (7) | |
O15 | 0.0699 (3) | 0.8761 (3) | 0.03827 (19) | 0.0324 (9) | |
O16 | 0.3277 (3) | 0.8510 (3) | 0.04986 (19) | 0.0312 (9) | |
O17 | −0.3650 (3) | 0.4919 (3) | 0.12861 (19) | 0.0328 (9) | |
O18 | 0.3275 (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) | |
O21 | 0.3096 (3) | 0.6320 (3) | 0.10206 (17) | 0.0222 (8) | |
O22 | 0.1193 (3) | 0.2858 (3) | 0.05863 (17) | 0.0245 (8) | |
O23 | 0.3388 (3) | 0.4694 (3) | 0.01366 (17) | 0.0229 (8) | |
O24 | −0.1333 (3) | 0.4677 (3) | 0.13348 (16) | 0.0226 (8) | |
O25 | 0.0919 (3) | 0.4484 (3) | 0.14297 (16) | 0.0230 (8) | |
O26 | 0.0866 (3) | 0.6587 (3) | 0.08654 (16) | 0.0194 (7) | |
O27 | −0.1086 (3) | 0.3007 (3) | 0.04267 (16) | 0.0194 (7) | |
O28 | 0.1101 (3) | 0.4891 (3) | 0.00524 (15) | 0.0176 (7) | |
O29W | 0.1019 (4) | 0.5780 (4) | 0.6443 (2) | 0.0519 (12) | |
H29B | 0.0787 | 0.6370 | 0.6219 | 0.062* | |
H29A | 0.0678 | 0.5048 | 0.6159 | 0.062* | |
O30W | 0.4552 (4) | 0.8194 (4) | 0.3381 (2) | 0.0510 (12) | |
H30A | 0.4373 | 0.8781 | 0.3504 | 0.061* | |
H30B | 0.5336 | 0.8400 | 0.3569 | 0.061* | |
O31W | 0.5050 (4) | 0.7341 (5) | 0.2138 (2) | 0.0691 (16) | |
H31A | 0.4401 | 0.7063 | 0.1744 | 0.083* | |
H31B | 0.4756 | 0.7602 | 0.2450 | 0.083* | |
O32W | 0.3581 (5) | 0.6211 (4) | 0.6865 (3) | 0.0694 (14) | |
H32A | 0.2789 | 0.6135 | 0.6890 | 0.083* | |
H32B | 0.4049 | 0.6618 | 0.7262 | 0.083* | |
O33W | −0.1878 (5) | 0.8894 (4) | −0.1162 (3) | 0.0828 (18) | |
H33A | −0.1447 | 0.9474 | −0.0819 | 0.099* | |
H33B | −0.1489 | 0.8321 | −0.1110 | 0.099* | |
O34W | 0.4372 (7) | 0.2430 (6) | 0.2017 (4) | 0.134 (3) | |
H34A | 0.4070 | 0.3078 | 0.1972 | 0.161* | |
H34B | 0.3874 | 0.1859 | 0.1747 | 0.161* | |
V1 | −0.00384 (8) | 0.22701 (8) | 0.52518 (4) | 0.0204 (2) | |
V2 | 0.24366 (8) | 0.18796 (8) | 0.54459 (4) | 0.0200 (2) | |
V3 | −0.27039 (8) | 0.00560 (8) | 0.56005 (5) | 0.0229 (2) | |
V4 | 0.22029 (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) | |
V7 | 0.24429 (8) | 0.69956 (8) | 0.03168 (4) | 0.0203 (2) | |
V8 | −0.26351 (8) | 0.50339 (8) | 0.07083 (5) | 0.0236 (2) | |
V9 | 0.24551 (9) | 0.45527 (9) | 0.09123 (5) | 0.0242 (2) | |
V10 | −0.01191 (8) | 0.47419 (8) | 0.08540 (4) | 0.0173 (2) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.054 (4) | 0.046 (4) | 0.028 (3) | 0.008 (3) | 0.004 (3) | 0.007 (3) |
C2 | 0.043 (4) | 0.051 (4) | 0.058 (4) | 0.024 (4) | 0.014 (3) | 0.000 (3) |
C3 | 0.036 (4) | 0.031 (4) | 0.052 (4) | 0.015 (3) | 0.003 (3) | 0.012 (3) |
C4 | 0.030 (3) | 0.028 (3) | 0.042 (4) | 0.014 (3) | 0.003 (3) | 0.004 (3) |
C5 | 0.036 (3) | 0.039 (4) | 0.047 (4) | 0.023 (3) | 0.001 (3) | 0.004 (3) |
C6 | 0.052 (4) | 0.047 (4) | 0.033 (4) | −0.001 (3) | −0.002 (3) | 0.004 (3) |
C7 | 0.062 (5) | 0.049 (4) | 0.045 (4) | 0.027 (4) | 0.014 (3) | 0.007 (3) |
C8 | 0.034 (3) | 0.034 (4) | 0.049 (4) | 0.013 (3) | 0.001 (3) | 0.012 (3) |
C9 | 0.035 (3) | 0.036 (4) | 0.050 (4) | 0.021 (3) | −0.002 (3) | −0.002 (3) |
C10 | 0.045 (4) | 0.038 (4) | 0.053 (4) | 0.026 (3) | −0.006 (3) | 0.003 (3) |
C11 | 0.053 (4) | 0.046 (4) | 0.035 (3) | 0.037 (3) | −0.001 (3) | −0.001 (3) |
C12 | 0.043 (4) | 0.051 (4) | 0.044 (4) | 0.020 (4) | −0.003 (3) | 0.006 (3) |
C13 | 0.049 (4) | 0.034 (4) | 0.037 (3) | 0.024 (3) | −0.008 (3) | −0.009 (3) |
C14 | 0.046 (4) | 0.040 (4) | 0.022 (3) | 0.027 (3) | −0.003 (3) | −0.001 (3) |
C15 | 0.043 (4) | 0.044 (4) | 0.028 (3) | 0.026 (3) | 0.001 (3) | −0.003 (3) |
N1 | 0.032 (3) | 0.027 (3) | 0.027 (3) | 0.007 (2) | 0.007 (2) | 0.008 (2) |
N2 | 0.028 (3) | 0.033 (3) | 0.058 (3) | 0.013 (2) | 0.008 (2) | −0.001 (2) |
N3 | 0.041 (3) | 0.033 (3) | 0.026 (3) | 0.008 (2) | 0.006 (2) | 0.008 (2) |
N4 | 0.025 (3) | 0.031 (3) | 0.065 (4) | 0.014 (2) | 0.004 (2) | 0.003 (3) |
N5 | 0.051 (3) | 0.045 (3) | 0.022 (3) | 0.028 (3) | −0.004 (2) | −0.003 (2) |
N6 | 0.051 (3) | 0.055 (4) | 0.043 (3) | 0.029 (3) | 0.010 (3) | −0.002 (3) |
O1 | 0.033 (2) | 0.021 (2) | 0.041 (2) | 0.0126 (18) | 0.0011 (17) | −0.0058 (17) |
O2 | 0.024 (2) | 0.019 (2) | 0.033 (2) | 0.0046 (17) | −0.0010 (16) | −0.0026 (16) |
O3 | 0.027 (2) | 0.039 (2) | 0.036 (2) | 0.0176 (19) | 0.0104 (17) | −0.0018 (18) |
O4 | 0.031 (2) | 0.042 (2) | 0.030 (2) | 0.022 (2) | −0.0005 (17) | 0.0059 (18) |
O5 | 0.026 (2) | 0.0203 (19) | 0.0259 (19) | 0.0137 (17) | 0.0032 (15) | −0.0038 (15) |
O6 | 0.0183 (18) | 0.0210 (19) | 0.0268 (19) | 0.0071 (16) | 0.0043 (15) | 0.0004 (15) |
O7 | 0.0192 (18) | 0.023 (2) | 0.0215 (18) | 0.0114 (16) | −0.0040 (14) | −0.0034 (15) |
O8 | 0.031 (2) | 0.019 (2) | 0.0261 (19) | 0.0160 (17) | 0.0006 (15) | 0.0019 (15) |
O9 | 0.0201 (19) | 0.023 (2) | 0.032 (2) | 0.0131 (17) | 0.0004 (15) | −0.0002 (16) |
O10 | 0.0252 (19) | 0.022 (2) | 0.0208 (18) | 0.0128 (17) | 0.0034 (15) | 0.0016 (15) |
O11 | 0.0257 (19) | 0.023 (2) | 0.0165 (18) | 0.0126 (17) | 0.0003 (14) | 0.0028 (15) |
O12 | 0.0186 (18) | 0.0155 (18) | 0.0205 (18) | 0.0086 (15) | 0.0013 (14) | −0.0017 (14) |
O13 | 0.0164 (18) | 0.0148 (18) | 0.0210 (18) | 0.0055 (15) | 0.0024 (14) | 0.0025 (14) |
O14 | 0.0178 (18) | 0.0140 (17) | 0.0174 (17) | 0.0074 (15) | 0.0022 (13) | −0.0006 (13) |
O15 | 0.032 (2) | 0.019 (2) | 0.044 (2) | 0.0106 (18) | −0.0005 (18) | −0.0064 (17) |
O16 | 0.028 (2) | 0.023 (2) | 0.037 (2) | 0.0078 (17) | −0.0005 (17) | −0.0008 (17) |
O17 | 0.029 (2) | 0.037 (2) | 0.036 (2) | 0.0176 (19) | 0.0077 (17) | −0.0020 (18) |
O18 | 0.034 (2) | 0.040 (2) | 0.030 (2) | 0.022 (2) | −0.0027 (17) | 0.0022 (18) |
O19 | 0.026 (2) | 0.025 (2) | 0.0250 (19) | 0.0156 (17) | 0.0023 (15) | −0.0033 (15) |
O20 | 0.0198 (19) | 0.026 (2) | 0.0259 (19) | 0.0116 (17) | 0.0052 (15) | 0.0033 (15) |
O21 | 0.0223 (19) | 0.023 (2) | 0.0219 (19) | 0.0121 (17) | −0.0043 (14) | −0.0016 (15) |
O22 | 0.026 (2) | 0.021 (2) | 0.028 (2) | 0.0124 (17) | −0.0002 (15) | 0.0024 (16) |
O23 | 0.0235 (19) | 0.023 (2) | 0.0258 (19) | 0.0136 (17) | 0.0002 (15) | −0.0011 (15) |
O24 | 0.025 (2) | 0.024 (2) | 0.0205 (18) | 0.0125 (17) | 0.0040 (15) | 0.0017 (15) |
O25 | 0.028 (2) | 0.024 (2) | 0.0178 (18) | 0.0122 (17) | 0.0016 (15) | 0.0017 (15) |
O26 | 0.0226 (19) | 0.0164 (19) | 0.0190 (18) | 0.0090 (16) | 0.0007 (14) | −0.0035 (14) |
O27 | 0.0187 (18) | 0.0156 (18) | 0.0223 (18) | 0.0066 (15) | 0.0010 (14) | 0.0009 (14) |
O28 | 0.0197 (18) | 0.0160 (18) | 0.0162 (17) | 0.0076 (15) | 0.0011 (14) | −0.0018 (14) |
O29W | 0.077 (3) | 0.033 (3) | 0.050 (3) | 0.030 (3) | 0.000 (2) | 0.000 (2) |
O30W | 0.030 (2) | 0.053 (3) | 0.069 (3) | 0.021 (2) | −0.014 (2) | −0.023 (2) |
O31W | 0.057 (3) | 0.111 (4) | 0.053 (3) | 0.055 (3) | −0.022 (2) | −0.037 (3) |
O32W | 0.064 (3) | 0.071 (4) | 0.080 (4) | 0.038 (3) | 0.002 (3) | −0.002 (3) |
O33W | 0.124 (5) | 0.042 (3) | 0.083 (4) | 0.045 (3) | −0.038 (3) | −0.009 (3) |
O34W | 0.145 (7) | 0.109 (6) | 0.159 (7) | 0.073 (5) | −0.017 (5) | −0.037 (5) |
V1 | 0.0211 (5) | 0.0155 (5) | 0.0259 (5) | 0.0098 (4) | 0.0010 (4) | −0.0017 (4) |
V2 | 0.0170 (5) | 0.0170 (5) | 0.0244 (5) | 0.0069 (4) | −0.0016 (4) | −0.0023 (4) |
V3 | 0.0201 (5) | 0.0258 (5) | 0.0255 (5) | 0.0126 (4) | 0.0038 (4) | 0.0002 (4) |
V4 | 0.0255 (5) | 0.0280 (5) | 0.0231 (5) | 0.0164 (4) | −0.0005 (4) | 0.0024 (4) |
V5 | 0.0181 (5) | 0.0163 (5) | 0.0160 (4) | 0.0085 (4) | 0.0010 (3) | 0.0001 (3) |
V6 | 0.0216 (5) | 0.0166 (5) | 0.0262 (5) | 0.0103 (4) | 0.0004 (4) | −0.0007 (4) |
V7 | 0.0183 (5) | 0.0183 (5) | 0.0233 (5) | 0.0078 (4) | −0.0001 (4) | −0.0010 (4) |
V8 | 0.0220 (5) | 0.0265 (5) | 0.0245 (5) | 0.0128 (4) | 0.0038 (4) | −0.0007 (4) |
V9 | 0.0252 (5) | 0.0276 (5) | 0.0242 (5) | 0.0164 (4) | −0.0010 (4) | 0.0018 (4) |
V10 | 0.0185 (5) | 0.0172 (5) | 0.0158 (4) | 0.0079 (4) | 0.0005 (3) | −0.0005 (3) |
C1—N1 | 1.489 (6) | V4—O4 | 1.603 (3) |
C1—H1A | 0.9600 | O5—V1 | 1.822 (3) |
C1—H1B | 0.9600 | O5—V3 | 1.845 (3) |
C1—H1C | 0.9600 | O6—V2i | 1.822 (3) |
C2—N1 | 1.486 (7) | O6—V3 | 1.902 (3) |
C2—H2A | 0.9600 | O7—V2 | 1.810 (3) |
C2—H2B | 0.9600 | O7—V4 | 1.883 (3) |
C2—H2C | 0.9600 | O8—V1i | 1.825 (3) |
C3—N1 | 1.480 (6) | O8—V4 | 1.873 (3) |
C3—C4 | 1.507 (7) | O9—V4 | 1.834 (3) |
C3—H3A | 0.9700 | O9—V3i | 1.834 (3) |
C3—H3B | 0.9700 | O10—V5 | 1.693 (3) |
C4—C5 | 1.508 (7) | O10—V3 | 2.035 (3) |
C4—H4A | 0.9700 | O11—V5 | 1.690 (3) |
C4—H4B | 0.9700 | O11—V4 | 2.036 (3) |
C5—N2 | 1.477 (7) | O12—V5 | 1.893 (3) |
C5—H5A | 0.9700 | O12—V1 | 1.999 (3) |
C5—H5B | 0.9700 | O12—V2 | 1.999 (3) |
C6—N3 | 1.491 (7) | O13—V5 | 1.972 (3) |
C6—H6A | 0.9600 | O13—V1i | 2.012 (3) |
C6—H6B | 0.9600 | O13—V2i | 2.021 (3) |
C6—H6C | 0.9600 | O14—V5 | 2.103 (3) |
C7—N3 | 1.494 (7) | O14—V5i | 2.111 (3) |
C7—H7A | 0.9600 | O14—V2 | 2.244 (3) |
C7—H7B | 0.9600 | O14—V1i | 2.260 (3) |
C7—H7C | 0.9600 | O14—V3i | 2.308 (3) |
C8—N3 | 1.485 (7) | O14—V4 | 2.315 (3) |
C8—C9 | 1.502 (7) | V6—O15 | 1.617 (3) |
C8—H8A | 0.9700 | V7—O16 | 1.605 (3) |
C8—H8B | 0.9700 | V8—O17 | 1.612 (4) |
C9—C10 | 1.507 (7) | V9—O18 | 1.602 (3) |
C9—H9A | 0.9700 | O19—V6 | 1.829 (3) |
C9—H9B | 0.9700 | O19—V8 | 1.832 (3) |
C10—N4 | 1.479 (7) | O20—V7ii | 1.814 (3) |
C10—H10A | 0.9700 | O20—V8 | 1.907 (3) |
C10—H10B | 0.9700 | O21—V7 | 1.830 (3) |
C11—N5 | 1.499 (6) | O21—V9 | 1.860 (3) |
C11—H11A | 0.9600 | O22—V6ii | 1.792 (3) |
C11—H11B | 0.9600 | O22—V9 | 1.909 (3) |
C11—H11C | 0.9600 | O23—V9 | 1.832 (3) |
C12—N5 | 1.480 (7) | O23—V8ii | 1.848 (3) |
C12—H12A | 0.9600 | O24—V10 | 1.691 (3) |
C12—H12B | 0.9600 | O24—V8 | 2.032 (3) |
C12—H12C | 0.9600 | O25—V10 | 1.682 (3) |
C13—C14 | 1.495 (8) | O25—V9 | 2.050 (3) |
C13—N5 | 1.503 (7) | O26—V10 | 1.930 (3) |
C13—H13A | 0.9700 | O26—V7 | 2.018 (3) |
C13—H13B | 0.9700 | O26—V6 | 2.032 (3) |
C14—C15 | 1.518 (7) | O27—V10 | 1.948 (3) |
C14—H14A | 0.9700 | O27—V6ii | 1.995 (3) |
C14—H14B | 0.9700 | O27—V7ii | 2.014 (3) |
C15—N6 | 1.477 (7) | O28—V10 | 2.085 (3) |
C15—H15A | 0.9700 | O28—V10ii | 2.126 (3) |
C15—H15B | 0.9700 | O28—V6ii | 2.247 (3) |
N1—H1 | 0.9100 | O28—V7 | 2.260 (3) |
N2—H2D | 0.8900 | O28—V8ii | 2.321 (3) |
N2—H2E | 0.8900 | O28—V9 | 2.322 (3) |
N2—H2F | 0.8900 | O29W—H29B | 0.9411 |
N3—H3 | 0.9100 | O29W—H29A | 0.9099 |
N4—H4C | 0.8900 | O30W—H30A | 0.8405 |
N4—H4D | 0.8900 | O30W—H30B | 0.8660 |
N4—H4E | 0.8900 | O31W—H31A | 0.9488 |
N5—H5 | 0.9100 | O31W—H31B | 0.8181 |
N6—H6D | 0.8900 | O32W—H32A | 0.8804 |
N6—H6E | 0.8900 | O32W—H32B | 0.8766 |
N6—H6F | 0.8900 | O33W—H33A | 0.8700 |
V1—O1 | 1.612 (3) | O33W—H33B | 0.9676 |
V2—O2 | 1.622 (3) | O34W—H34A | 0.9720 |
V3—O3 | 1.614 (3) | O34W—H34B | 0.7962 |
N1—C1—H1A | 109.5 | V6ii—O28—V8ii | 85.28 (11) |
N1—C1—H1B | 109.5 | V7—O28—V8ii | 86.66 (11) |
H1A—C1—H1B | 109.5 | V10—O28—V9 | 88.12 (11) |
N1—C1—H1C | 109.5 | V10ii—O28—V9 | 170.14 (16) |
H1A—C1—H1C | 109.5 | V6ii—O28—V9 | 86.37 (11) |
H1B—C1—H1C | 109.5 | V7—O28—V9 | 84.85 (11) |
N1—C2—H2A | 109.5 | V8ii—O28—V9 | 83.17 (10) |
N1—C2—H2B | 109.5 | H29B—O29W—H29A | 108.4 |
H2A—C2—H2B | 109.5 | H30A—O30W—H30B | 107.1 |
N1—C2—H2C | 109.5 | H31A—O31W—H31B | 105.3 |
H2A—C2—H2C | 109.5 | H32A—O32W—H32B | 107.3 |
H2B—C2—H2C | 109.5 | H33A—O33W—H33B | 102.4 |
N1—C3—C4 | 115.2 (4) | H34A—O34W—H34B | 104.1 |
N1—C3—H3A | 108.5 | O1—V1—O5 | 103.12 (17) |
C4—C3—H3A | 108.5 | O1—V1—O8i | 102.97 (17) |
N1—C3—H3B | 108.5 | O5—V1—O8i | 95.31 (15) |
C4—C3—H3B | 108.5 | O1—V1—O12 | 100.68 (16) |
H3A—C3—H3B | 107.5 | O5—V1—O12 | 89.63 (14) |
C3—C4—C5 | 108.5 (4) | O8i—V1—O12 | 154.03 (14) |
C3—C4—H4A | 110.0 | O1—V1—O13i | 100.41 (16) |
C5—C4—H4A | 110.0 | O5—V1—O13i | 154.35 (14) |
C3—C4—H4B | 110.0 | O8i—V1—O13i | 89.21 (14) |
C5—C4—H4B | 110.0 | O12—V1—O13i | 76.03 (13) |
H4A—C4—H4B | 108.4 | O1—V1—O14i | 175.06 (15) |
N2—C5—C4 | 112.4 (4) | O5—V1—O14i | 79.86 (13) |
N2—C5—H5A | 109.1 | O8i—V1—O14i | 80.52 (13) |
C4—C5—H5A | 109.1 | O12—V1—O14i | 75.27 (12) |
N2—C5—H5B | 109.1 | O13i—V1—O14i | 76.00 (12) |
C4—C5—H5B | 109.1 | O2—V2—O7 | 101.61 (16) |
H5A—C5—H5B | 107.9 | O2—V2—O6i | 103.40 (17) |
N3—C6—H6A | 109.5 | O7—V2—O6i | 95.38 (15) |
N3—C6—H6B | 109.5 | O2—V2—O12 | 99.67 (16) |
H6A—C6—H6B | 109.5 | O7—V2—O12 | 90.05 (14) |
N3—C6—H6C | 109.5 | O6i—V2—O12 | 154.66 (14) |
H6A—C6—H6C | 109.5 | O2—V2—O13i | 100.90 (15) |
H6B—C6—H6C | 109.5 | O7—V2—O13i | 155.12 (14) |
N3—C7—H7A | 109.5 | O6i—V2—O13i | 89.56 (14) |
N3—C7—H7B | 109.5 | O12—V2—O13i | 75.83 (13) |
H7A—C7—H7B | 109.5 | O2—V2—O14 | 174.78 (15) |
N3—C7—H7C | 109.5 | O7—V2—O14 | 80.76 (13) |
H7A—C7—H7C | 109.5 | O6i—V2—O14 | 80.89 (13) |
H7B—C7—H7C | 109.5 | O12—V2—O14 | 75.58 (12) |
N3—C8—C9 | 115.0 (4) | O13i—V2—O14 | 75.97 (12) |
N3—C8—H8A | 108.5 | O3—V3—O9i | 103.59 (16) |
C9—C8—H8A | 108.5 | O3—V3—O5 | 102.92 (17) |
N3—C8—H8B | 108.5 | O9i—V3—O5 | 91.38 (15) |
C9—C8—H8B | 108.5 | O3—V3—O6 | 100.78 (17) |
H8A—C8—H8B | 107.5 | O9i—V3—O6 | 90.14 (15) |
C8—C9—C10 | 109.6 (5) | O5—V3—O6 | 155.18 (14) |
C8—C9—H9A | 109.7 | O3—V3—O10 | 99.79 (16) |
C10—C9—H9A | 109.7 | O9i—V3—O10 | 156.55 (14) |
C8—C9—H9B | 109.7 | O5—V3—O10 | 85.03 (14) |
C10—C9—H9B | 109.7 | O6—V3—O10 | 83.79 (14) |
H9A—C9—H9B | 108.2 | O3—V3—O14i | 174.52 (15) |
N4—C10—C9 | 112.5 (5) | O9i—V3—O14i | 81.70 (13) |
N4—C10—H10A | 109.1 | O5—V3—O14i | 78.12 (13) |
C9—C10—H10A | 109.1 | O6—V3—O14i | 77.59 (13) |
N4—C10—H10B | 109.1 | O10—V3—O14i | 74.88 (12) |
C9—C10—H10B | 109.1 | O4—V4—O9 | 101.91 (17) |
H10A—C10—H10B | 107.8 | O4—V4—O8 | 101.43 (17) |
N5—C11—H11A | 109.5 | O9—V4—O8 | 91.83 (15) |
N5—C11—H11B | 109.5 | O4—V4—O7 | 102.55 (17) |
H11A—C11—H11B | 109.5 | O9—V4—O7 | 91.52 (15) |
N5—C11—H11C | 109.5 | O8—V4—O7 | 154.52 (14) |
H11A—C11—H11C | 109.5 | O4—V4—O11 | 102.08 (16) |
H11B—C11—H11C | 109.5 | O9—V4—O11 | 156.01 (14) |
N5—C12—H12A | 109.5 | O8—V4—O11 | 83.94 (14) |
N5—C12—H12B | 109.5 | O7—V4—O11 | 82.79 (14) |
H12A—C12—H12B | 109.5 | O4—V4—O14 | 176.56 (15) |
N5—C12—H12C | 109.5 | O9—V4—O14 | 81.53 (12) |
H12A—C12—H12C | 109.5 | O8—V4—O14 | 78.11 (12) |
H12B—C12—H12C | 109.5 | O7—V4—O14 | 77.43 (12) |
C14—C13—N5 | 114.3 (5) | O11—V4—O14 | 74.49 (12) |
C14—C13—H13A | 108.7 | O11—V5—O10 | 106.42 (15) |
N5—C13—H13A | 108.7 | O11—V5—O12 | 98.35 (15) |
C14—C13—H13B | 108.7 | O10—V5—O12 | 98.86 (15) |
N5—C13—H13B | 108.7 | O11—V5—O13 | 96.20 (15) |
H13A—C13—H13B | 107.6 | O10—V5—O13 | 94.96 (15) |
C13—C14—C15 | 109.1 (5) | O12—V5—O13 | 156.18 (14) |
C13—C14—H14A | 109.9 | O11—V5—O14 | 87.61 (14) |
C15—C14—H14A | 109.9 | O10—V5—O14 | 165.73 (14) |
C13—C14—H14B | 109.9 | O12—V5—O14 | 81.28 (13) |
C15—C14—H14B | 109.9 | O13—V5—O14 | 80.60 (13) |
H14A—C14—H14B | 108.3 | O11—V5—O14i | 165.84 (14) |
N6—C15—C14 | 111.7 (5) | O10—V5—O14i | 87.58 (14) |
N6—C15—H15A | 109.3 | O12—V5—O14i | 81.15 (13) |
C14—C15—H15A | 109.3 | O13—V5—O14i | 80.15 (12) |
N6—C15—H15B | 109.3 | O14—V5—O14i | 78.32 (13) |
C14—C15—H15B | 109.3 | O15—V6—O22ii | 103.92 (17) |
H15A—C15—H15B | 107.9 | O15—V6—O19 | 102.71 (17) |
C3—N1—C2 | 112.8 (4) | O22ii—V6—O19 | 95.81 (15) |
C3—N1—C1 | 110.3 (4) | O15—V6—O27ii | 99.87 (16) |
C2—N1—C1 | 110.2 (4) | O22ii—V6—O27ii | 91.11 (14) |
C3—N1—H1 | 107.8 | O19—V6—O27ii | 153.99 (14) |
C2—N1—H1 | 107.8 | O15—V6—O26 | 99.51 (16) |
C1—N1—H1 | 107.8 | O22ii—V6—O26 | 154.88 (14) |
C5—N2—H2D | 109.5 | O19—V6—O26 | 87.72 (14) |
C5—N2—H2E | 109.5 | O27ii—V6—O26 | 75.91 (13) |
H2D—N2—H2E | 109.5 | O15—V6—O28ii | 174.18 (15) |
C5—N2—H2F | 109.5 | O22ii—V6—O28ii | 80.73 (13) |
H2D—N2—H2F | 109.5 | O19—V6—O28ii | 80.07 (13) |
H2E—N2—H2F | 109.5 | O27ii—V6—O28ii | 76.34 (12) |
C8—N3—C6 | 109.5 (5) | O26—V6—O28ii | 75.38 (12) |
C8—N3—C7 | 112.2 (5) | O15—V6—V7 | 89.80 (13) |
C6—N3—C7 | 111.6 (5) | O22ii—V6—V7 | 130.60 (11) |
C8—N3—H3 | 107.8 | O19—V6—V7 | 127.54 (11) |
C6—N3—H3 | 107.8 | O27ii—V6—V7 | 39.52 (9) |
C7—N3—H3 | 107.8 | O26—V6—V7 | 39.82 (9) |
C10—N4—H4C | 109.5 | O28ii—V6—V7 | 84.48 (9) |
C10—N4—H4D | 109.5 | O16—V7—O20ii | 103.06 (18) |
H4C—N4—H4D | 109.5 | O16—V7—O21 | 102.41 (17) |
C10—N4—H4E | 109.5 | O20ii—V7—O21 | 95.10 (15) |
H4C—N4—H4E | 109.5 | O16—V7—O27ii | 99.75 (16) |
H4D—N4—H4E | 109.5 | O20ii—V7—O27ii | 89.78 (14) |
C12—N5—C11 | 111.3 (4) | O21—V7—O27ii | 155.56 (14) |
C12—N5—C13 | 110.6 (5) | O16—V7—O26 | 100.63 (16) |
C11—N5—C13 | 113.4 (4) | O20ii—V7—O26 | 154.04 (14) |
C12—N5—H5 | 107.0 | O21—V7—O26 | 90.03 (14) |
C11—N5—H5 | 107.0 | O27ii—V7—O26 | 75.80 (13) |
C13—N5—H5 | 107.0 | O16—V7—O28 | 174.69 (15) |
C15—N6—H6D | 109.5 | O20ii—V7—O28 | 80.36 (13) |
C15—N6—H6E | 109.5 | O21—V7—O28 | 81.17 (13) |
H6D—N6—H6E | 109.5 | O27ii—V7—O28 | 76.05 (12) |
C15—N6—H6F | 109.5 | O26—V7—O28 | 75.31 (12) |
H6D—N6—H6F | 109.5 | O16—V7—V6 | 90.45 (13) |
H6E—N6—H6F | 109.5 | O20ii—V7—V6 | 128.83 (11) |
V1—O5—V3 | 115.52 (17) | O21—V7—V6 | 130.18 (11) |
V2i—O6—V3 | 113.97 (17) | O27ii—V7—V6 | 39.07 (9) |
V2—O7—V4 | 114.64 (16) | O26—V7—V6 | 40.16 (9) |
V1i—O8—V4 | 114.51 (17) | O28—V7—V6 | 84.24 (9) |
V4—O9—V3i | 113.57 (16) | O17—V8—O19 | 103.14 (17) |
V5—O10—V3 | 109.96 (16) | O17—V8—O23ii | 103.42 (17) |
V5—O11—V4 | 110.27 (16) | O19—V8—O23ii | 92.55 (15) |
V5—O12—V1 | 108.38 (15) | O17—V8—O20 | 101.36 (17) |
V5—O12—V2 | 107.56 (15) | O19—V8—O20 | 154.51 (14) |
V1—O12—V2 | 101.07 (14) | O23ii—V8—O20 | 88.51 (14) |
V5—O13—V1i | 106.68 (15) | O17—V8—O24 | 100.17 (16) |
V5—O13—V2i | 106.75 (14) | O19—V8—O24 | 85.36 (14) |
V1i—O13—V2i | 99.88 (14) | O23ii—V8—O24 | 156.17 (14) |
V5—O14—V5i | 101.68 (13) | O20—V8—O24 | 83.53 (14) |
V5—O14—V2 | 92.45 (12) | O17—V8—O28ii | 174.91 (15) |
V5i—O14—V2 | 94.71 (12) | O19—V8—O28ii | 78.03 (13) |
V5—O14—V1i | 94.12 (12) | O23ii—V8—O28ii | 81.41 (13) |
V5i—O14—V1i | 92.41 (12) | O20—V8—O28ii | 76.95 (13) |
V2—O14—V1i | 169.15 (15) | O24—V8—O28ii | 74.92 (12) |
V5—O14—V3i | 170.82 (15) | O18—V9—O23 | 103.17 (17) |
V5i—O14—V3i | 87.50 (11) | O18—V9—O21 | 102.75 (17) |
V2—O14—V3i | 86.63 (11) | O23—V9—O21 | 92.49 (15) |
V1i—O14—V3i | 85.51 (11) | O18—V9—O22 | 101.19 (17) |
V5—O14—V4 | 87.64 (11) | O23—V9—O22 | 90.76 (15) |
V5i—O14—V4 | 170.60 (15) | O21—V9—O22 | 154.41 (14) |
V2—O14—V4 | 85.99 (11) | O18—V9—O25 | 101.39 (16) |
V1i—O14—V4 | 85.66 (11) | O23—V9—O25 | 155.36 (14) |
V3i—O14—V4 | 83.18 (10) | O21—V9—O25 | 84.10 (14) |
V6—O19—V8 | 115.41 (17) | O22—V9—O25 | 82.44 (14) |
V7ii—O20—V8 | 115.26 (18) | O18—V9—O28 | 174.72 (16) |
V7—O21—V9 | 113.80 (16) | O23—V9—O28 | 81.70 (12) |
V6ii—O22—V9 | 115.30 (17) | O21—V9—O28 | 78.89 (13) |
V9—O23—V8ii | 113.72 (16) | O22—V9—O28 | 76.49 (12) |
V10—O24—V8 | 110.52 (16) | O25—V9—O28 | 73.69 (12) |
V10—O25—V9 | 110.27 (16) | O25—V10—O24 | 106.30 (16) |
V10—O26—V7 | 106.79 (15) | O25—V10—O26 | 97.37 (15) |
V10—O26—V6 | 107.81 (15) | O24—V10—O26 | 96.91 (15) |
V7—O26—V6 | 100.02 (14) | O25—V10—O27 | 97.73 (15) |
V10—O27—V6ii | 106.02 (15) | O24—V10—O27 | 96.00 (15) |
V10—O27—V7ii | 107.35 (15) | O26—V10—O27 | 156.51 (13) |
V6ii—O27—V7ii | 101.41 (14) | O25—V10—O28 | 87.90 (14) |
V10—O28—V10ii | 101.68 (13) | O24—V10—O28 | 165.79 (14) |
V10—O28—V6ii | 93.19 (13) | O26—V10—O28 | 81.38 (13) |
V10ii—O28—V6ii | 94.09 (12) | O27—V10—O28 | 81.30 (13) |
V10—O28—V7 | 93.59 (12) | O25—V10—O28ii | 166.22 (14) |
V10ii—O28—V7 | 93.37 (12) | O24—V10—O28ii | 87.48 (14) |
V6ii—O28—V7 | 168.71 (15) | O26—V10—O28ii | 80.38 (13) |
V10—O28—V8ii | 171.23 (15) | O27—V10—O28ii | 80.66 (13) |
V10ii—O28—V8ii | 87.05 (11) | O28—V10—O28ii | 78.32 (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—N4 | 171.8 (5) | V9—O21—V7—O27ii | 31.5 (4) |
N5—C13—C14—C15 | −156.9 (4) | V9—O21—V7—O26 | 85.27 (18) |
C13—C14—C15—N6 | −174.4 (4) | V9—O21—V7—O28 | 10.15 (16) |
C4—C3—N1—C2 | −58.7 (6) | V9—O21—V7—V6 | 84.83 (19) |
C4—C3—N1—C1 | 177.6 (5) | V10—O26—V7—O16 | −169.93 (16) |
C9—C8—N3—C6 | 169.2 (5) | V6—O26—V7—O16 | 77.88 (17) |
C9—C8—N3—C7 | −66.2 (6) | V10—O26—V7—O20ii | 34.5 (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—O1 | 175.06 (18) | V6—O26—V7—O21 | −179.48 (14) |
V3—O5—V1—O8i | 70.40 (19) | V10—O26—V7—O27ii | 92.58 (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—O28 | 13.57 (13) |
V3—O5—V1—O14i | −8.96 (16) | V6—O26—V7—O28 | −98.62 (14) |
V5—O12—V1—O1 | 169.40 (17) | V10—O26—V7—V6 | 112.19 (19) |
V2—O12—V1—O1 | −77.72 (18) | V10—O28—V7—O20ii | 177.09 (14) |
V5—O12—V1—O5 | 66.12 (17) | V10ii—O28—V7—O20ii | −80.97 (13) |
V2—O12—V1—O5 | 179.00 (15) | V6ii—O28—V7—O20ii | 50.3 (8) |
V5—O12—V1—O8i | −35.3 (4) | V8ii—O28—V7—O20ii | 5.88 (12) |
V2—O12—V1—O8i | 77.6 (3) | V9—O28—V7—O20ii | 89.31 (12) |
V5—O12—V1—O13i | −92.40 (16) | V10—O28—V7—O21 | 80.34 (14) |
V2—O12—V1—O13i | 20.48 (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—O14i | 99.39 (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—O12 | 85.12 (18) | V10ii—O28—V7—O27ii | 11.22 (12) |
V4—O7—V2—O13i | 30.6 (4) | V6ii—O28—V7—O27ii | 142.5 (8) |
V4—O7—V2—O14 | 9.74 (16) | V8ii—O28—V7—O27ii | 98.06 (12) |
V5—O12—V2—O2 | −167.99 (16) | V9—O28—V7—O27ii | −178.51 (13) |
V1—O12—V2—O2 | 78.50 (17) | V10—O28—V7—O26 | −12.03 (11) |
V5—O12—V2—O7 | −66.20 (16) | V10ii—O28—V7—O26 | 89.91 (13) |
V1—O12—V2—O7 | −179.71 (14) | V6ii—O28—V7—O26 | −138.8 (8) |
V5—O12—V2—O6i | 36.6 (4) | V8ii—O28—V7—O26 | 176.75 (13) |
V1—O12—V2—O6i | −76.9 (3) | V9—O28—V7—O26 | −99.82 (12) |
V5—O12—V2—O13i | 93.10 (16) | V10—O28—V7—V6 | −51.88 (9) |
V1—O12—V2—O13i | −20.41 (13) | V10ii—O28—V7—V6 | 50.06 (9) |
V5—O12—V2—O14 | 14.25 (13) | V6ii—O28—V7—V6 | −178.7 (8) |
V1—O12—V2—O14 | −99.27 (14) | V8ii—O28—V7—V6 | 136.90 (8) |
V5—O14—V2—O7 | 80.25 (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—O16 | 107.4 (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—O16 | 105.0 (2) |
V5—O14—V2—O6i | 177.28 (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—O6i | 50.0 (8) | O15—V6—V7—O20ii | −108.1 (2) |
V3i—O14—V2—O6i | 6.43 (12) | O22ii—V6—V7—O20ii | 0.2 (2) |
V4—O14—V2—O6i | 89.82 (12) | O19—V6—V7—O20ii | 145.94 (19) |
V5—O14—V2—O12 | −12.20 (11) | O27ii—V6—V7—O20ii | −2.2 (2) |
V5i—O14—V2—O12 | 89.74 (13) | O26—V6—V7—O20ii | 146.7 (2) |
V1i—O14—V2—O12 | −139.4 (8) | O28ii—V6—V7—O20ii | 72.96 (17) |
V3i—O14—V2—O12 | 176.95 (13) | O15—V6—V7—O21 | 105.87 (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—O13i | 11.06 (12) | O27ii—V6—V7—O21 | −148.2 (2) |
V1i—O14—V2—O13i | 141.9 (8) | O26—V6—V7—O21 | 0.68 (19) |
V3i—O14—V2—O13i | 98.27 (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—O27ii | 2.4 (2) |
V1—O5—V3—O9i | −72.40 (19) | O19—V6—V7—O27ii | 148.2 (2) |
V1—O5—V3—O6 | 20.9 (4) | O26—V6—V7—O27ii | 148.9 (2) |
V1—O5—V3—O10 | 84.38 (18) | O28ii—V6—V7—O27ii | 75.19 (17) |
V1—O5—V3—O14i | 8.82 (16) | O15—V6—V7—O26 | 105.19 (19) |
V2i—O6—V3—O3 | 176.95 (18) | O22ii—V6—V7—O26 | −146.5 (2) |
V2i—O6—V3—O9i | 73.09 (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—O28 | 179.19 (16) |
V5—O10—V3—O3 | −178.89 (19) | O22ii—V6—V7—O28 | −72.52 (17) |
V5—O10—V3—O9i | 5.4 (4) | O19—V6—V7—O28 | 73.24 (16) |
V5—O10—V3—O5 | −76.61 (18) | O27ii—V6—V7—O28 | −74.93 (16) |
V5—O10—V3—O6 | 81.19 (18) | O26—V6—V7—O28 | 73.99 (16) |
V5—O10—V3—O14i | 2.41 (15) | O28ii—V6—V7—O28 | 0.26 (15) |
V3i—O9—V4—O4 | 178.96 (19) | V6—O19—V8—O17 | −175.33 (18) |
V3i—O9—V4—O8 | 76.87 (19) | V6—O19—V8—O23ii | −70.92 (19) |
V3i—O9—V4—O7 | −77.87 (18) | V6—O19—V8—O20 | 21.0 (4) |
V3i—O9—V4—O11 | −2.3 (5) | V6—O19—V8—O24 | 85.29 (18) |
V3i—O9—V4—O14 | −0.82 (16) | V6—O19—V8—O28ii | 9.74 (16) |
V1i—O8—V4—O4 | −173.82 (19) | V7ii—O20—V8—O17 | 177.13 (18) |
V1i—O8—V4—O9 | −71.28 (19) | V7ii—O20—V8—O19 | −19.0 (4) |
V1i—O8—V4—O7 | 26.1 (4) | V7ii—O20—V8—O23ii | 73.74 (19) |
V1i—O8—V4—O11 | 85.04 (18) | V7ii—O20—V8—O24 | −83.76 (18) |
V1i—O8—V4—O14 | 9.66 (16) | V7ii—O20—V8—O28ii | −7.79 (16) |
V2—O7—V4—O4 | 173.98 (19) | V10—O24—V8—O17 | −179.79 (19) |
V2—O7—V4—O9 | 71.43 (19) | V10—O24—V8—O19 | −77.24 (19) |
V2—O7—V4—O8 | −26.0 (4) | V10—O24—V8—O23ii | 8.5 (4) |
V2—O7—V4—O11 | −85.19 (18) | V10—O24—V8—O20 | 79.78 (18) |
V2—O7—V4—O14 | −9.55 (16) | V10—O24—V8—O28ii | 1.59 (15) |
V5—O11—V4—O4 | 179.90 (19) | V8ii—O23—V9—O18 | 177.35 (19) |
V5—O11—V4—O9 | 1.2 (4) | V8ii—O23—V9—O21 | −78.94 (19) |
V5—O11—V4—O8 | −79.66 (18) | V8ii—O23—V9—O22 | 75.68 (18) |
V5—O11—V4—O7 | 78.54 (18) | V8ii—O23—V9—O25 | 2.3 (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—O18 | 175.18 (19) |
V2—O14—V4—O9 | −86.47 (13) | V7—O21—V9—O23 | 71.09 (19) |
V1i—O14—V4—O9 | 86.59 (13) | V7—O21—V9—O22 | −25.9 (4) |
V3i—O14—V4—O9 | 0.60 (12) | V7—O21—V9—O25 | −84.44 (18) |
V5—O14—V4—O8 | 87.21 (14) | V7—O21—V9—O28 | −9.95 (16) |
V2—O14—V4—O8 | 179.84 (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—O21 | 25.4 (4) |
V5—O14—V4—O7 | −85.62 (13) | V6ii—O22—V9—O25 | 84.29 (19) |
V2—O14—V4—O7 | 7.00 (12) | V6ii—O22—V9—O28 | 9.32 (16) |
V1i—O14—V4—O7 | −179.94 (13) | V10—O25—V9—O18 | −178.88 (19) |
V3i—O14—V4—O7 | 94.08 (13) | V10—O25—V9—O23 | −3.8 (4) |
V5—O14—V4—O11 | 0.27 (11) | V10—O25—V9—O21 | 79.26 (18) |
V2—O14—V4—O11 | 92.90 (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—O11 | 179.98 (13) | V10—O28—V9—O23 | 179.39 (14) |
V4—O11—V5—O10 | 177.70 (16) | V6ii—O28—V9—O23 | 86.08 (13) |
V4—O11—V5—O12 | −80.44 (17) | V7—O28—V9—O23 | −86.83 (13) |
V4—O11—V5—O13 | 80.66 (17) | V8ii—O28—V9—O23 | 0.40 (12) |
V4—O11—V5—O14 | 0.38 (16) | V10—O28—V9—O21 | −86.40 (14) |
V4—O11—V5—O14i | 6.5 (7) | V6ii—O28—V9—O21 | −179.71 (14) |
V3—O10—V5—O11 | 179.60 (16) | V7—O28—V9—O21 | 7.38 (12) |
V3—O10—V5—O12 | 78.11 (17) | V8ii—O28—V9—O21 | 94.62 (13) |
V3—O10—V5—O13 | −82.44 (17) | V10—O28—V9—O22 | 86.59 (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—O11 | 179.85 (15) | V8ii—O28—V9—O22 | −92.39 (13) |
V2—O12—V5—O11 | 71.35 (17) | V10—O28—V9—O25 | 0.65 (11) |
V1—O12—V5—O10 | −71.96 (17) | V6ii—O28—V9—O25 | −92.67 (13) |
V2—O12—V5—O10 | 179.54 (15) | V7—O28—V9—O25 | 94.42 (13) |
V1—O12—V5—O13 | 52.8 (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—O14 | 93.59 (15) | V9—O25—V10—O26 | −80.11 (17) |
V2—O12—V5—O14 | −14.91 (14) | V9—O25—V10—O27 | 81.84 (18) |
V1—O12—V5—O14i | 14.16 (14) | V9—O25—V10—O28 | 0.91 (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—O25 | 178.10 (16) |
V2i—O13—V5—O11 | −179.11 (15) | V8—O24—V10—O26 | 78.31 (17) |
V1i—O13—V5—O10 | 179.84 (15) | V8—O24—V10—O27 | −82.01 (17) |
V2i—O13—V5—O10 | 73.75 (16) | V8—O24—V10—O28 | −3.8 (7) |
V1i—O13—V5—O12 | 54.4 (4) | V8—O24—V10—O28ii | −1.68 (16) |
V2i—O13—V5—O12 | −51.7 (4) | V7—O26—V10—O25 | 72.32 (17) |
V1i—O13—V5—O14 | 13.52 (13) | V6—O26—V10—O25 | 179.05 (15) |
V2i—O13—V5—O14 | −92.58 (15) | V7—O26—V10—O24 | 179.83 (15) |
V1i—O13—V5—O14i | 93.17 (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—O11 | 178.48 (15) | V6—O26—V10—O27 | 49.4 (4) |
V2—O14—V5—O11 | −86.20 (14) | V7—O26—V10—O28 | −14.41 (14) |
V1i—O14—V5—O11 | 85.16 (14) | V6—O26—V10—O28 | 92.31 (15) |
V4—O14—V5—O11 | −0.32 (13) | V7—O26—V10—O28ii | −93.93 (15) |
V5i—O14—V5—O10 | 9.0 (6) | V6—O26—V10—O28ii | 12.80 (14) |
V2—O14—V5—O10 | 104.3 (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—O24 | 73.01 (17) |
V2—O14—V5—O12 | 12.63 (12) | V6ii—O27—V10—O26 | 57.8 (4) |
V1i—O14—V5—O12 | −176.01 (13) | V7ii—O27—V10—O26 | −50.0 (4) |
V4—O14—V5—O12 | 98.52 (12) | V6ii—O27—V10—O28 | 14.86 (13) |
V5i—O14—V5—O13 | 81.79 (14) | V7ii—O27—V10—O28 | −92.92 (15) |
V2—O14—V5—O13 | 177.12 (13) | V6ii—O27—V10—O28ii | 94.35 (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—O14i | 0.0 | V6ii—O28—V10—O25 | 85.50 (14) |
V2—O14—V5—O14i | 95.33 (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—O24 | 2.2 (6) |
V8—O19—V6—O15 | 175.22 (18) | V6ii—O28—V10—O24 | −92.7 (6) |
V8—O19—V6—O22ii | 69.5 (2) | V7—O28—V10—O24 | 96.4 (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—O26 | 12.31 (12) |
V10—O26—V6—O15 | 170.52 (17) | V9—O28—V10—O26 | 97.02 (12) |
V7—O26—V6—O15 | −78.09 (18) | V10ii—O28—V10—O27 | 82.19 (14) |
V10—O26—V6—O22ii | −30.8 (4) | V6ii—O28—V10—O27 | −12.65 (11) |
V7—O26—V6—O22ii | 80.6 (4) | V7—O28—V10—O27 | 176.38 (13) |
V10—O26—V6—O19 | 68.01 (17) | V9—O28—V10—O27 | −98.91 (12) |
V7—O26—V6—O19 | 179.40 (15) | V10ii—O28—V10—O28ii | 0.0 |
V10—O26—V6—O27ii | −91.60 (16) | V6ii—O28—V10—O28ii | −94.84 (14) |
V7—O26—V6—O27ii | 19.80 (13) | V7—O28—V10—O28ii | 94.19 (14) |
V10—O26—V6—O28ii | −12.32 (13) | V9—O28—V10—O28ii | 178.91 (17) |
V7—O26—V6—O28ii | 99.07 (14) |
Symmetry codes: (i) −x, −y, −z+1; (ii) −x, −y+1, −z. |
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1···O13i | 0.91 | 1.79 | 2.691 (5) | 173 |
N2—H2D···O32W | 0.89 | 2.08 | 2.968 (7) | 172 |
N2—H2E···O9iii | 0.89 | 2.05 | 2.873 (5) | 153 |
N2—H2F···O6iv | 0.89 | 1.89 | 2.772 (6) | 173 |
N3—H3···O27v | 0.91 | 1.87 | 2.736 (6) | 159 |
N4—H4C···O20vi | 0.89 | 1.89 | 2.772 (5) | 171 |
N4—H4D···O33Wii | 0.89 | 2.21 | 3.035 (7) | 154 |
N4—H4E···O23 | 0.89 | 1.99 | 2.820 (5) | 156 |
N5—H5···O26 | 0.91 | 1.82 | 2.709 (5) | 166 |
N6—H6D···O17 | 0.89 | 2.34 | 3.056 (6) | 137 |
N6—H6D···O32Wvii | 0.89 | 2.50 | 3.046 (7) | 120 |
N6—H6E···O31Wviii | 0.89 | 1.89 | 2.745 (6) | 160 |
N6—H6F···O2vii | 0.89 | 2.12 | 2.958 (6) | 156 |
O29W—H29A···O1 | 0.91 | 2.00 | 2.848 (5) | 154 |
O29W—H29B···O8iii | 0.94 | 1.90 | 2.790 (5) | 156 |
O30W—H30A···O3vii | 0.84 | 2.06 | 2.895 (5) | 174 |
O30W—H30B···O7ix | 0.87 | 1.86 | 2.716 (5) | 173 |
O31W—H31A···O21 | 0.95 | 1.83 | 2.770 (5) | 173 |
O31W—H31B···O30W | 0.82 | 1.94 | 2.724 (6) | 160 |
O32W—H32A···O29W | 0.88 | 2.00 | 2.808 (6) | 152 |
O32W—H32B···O34Wix | 0.88 | 2.03 | 2.873 (8) | 160 |
O33W—H33A···O15x | 0.87 | 1.98 | 2.787 (6) | 153 |
O33W—H33B···O22ii | 0.97 | 1.84 | 2.723 (5) | 150 |
O34W—H34A···O18 | 0.97 | 2.11 | 3.055 (7) | 163 |
O34W—H34B···O33Wii | 0.80 | 2.24 | 2.903 (8) | 141 |
Symmetry codes: (i) −x, −y, −z+1; (ii) −x, −y+1, −z; (iii) x, y+1, z; (iv) x+1, y+1, z; (v) −x, −y, −z; (vi) x+1, y, z; (vii) −x, −y+1, −z+1; (viii) x−1, y, z; (ix) −x+1, −y+1, −z+1; (x) −x, −y+2, −z. |
Experimental details
Crystal data | |
Chemical formula | 3(C5H16N2)2+.[V10O28]6−.6H2O |
Mr | 1378.09 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 298 |
a, b, c (Å) | 11.525 (2), 11.743 (2), 18.709 (4) |
α, β, γ (°) | 90.45 (3), 94.21 (3), 117.29 (3) |
V (Å3) | 2241.7 (10) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 2.09 |
Crystal size (mm) | 0.30 × 0.26 × 0.18 |
Data collection | |
Diffractometer | Bruker APEX area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Bruker, 2002) |
Tmin, Tmax | 0.556, 0.684 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 12138, 8110, 4858 |
Rint | 0.024 |
(sin θ/λ)max (Å−1) | 0.600 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.045, 0.134, 1.03 |
No. of reflections | 8110 |
No. of parameters | 595 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.02, −0.71 |
Computer programs: SMART (Bruker, 2002), SAINT (Bruker, 2002), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), XP (Siemens, 1994), WinGX (Farrugia, 1999).
V1—O1 | 1.612 (3) | V6—O15 | 1.617 (3) |
V2—O2 | 1.622 (3) | V7—O16 | 1.605 (3) |
V3—O3 | 1.614 (3) | V8—O17 | 1.612 (4) |
V4—O4 | 1.603 (3) | V9—O18 | 1.602 (3) |
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1···O13i | 0.91 | 1.79 | 2.691 (5) | 173 |
N2—H2D···O32W | 0.89 | 2.08 | 2.968 (7) | 172 |
N2—H2E···O9ii | 0.89 | 2.05 | 2.873 (5) | 153 |
N2—H2F···O6iii | 0.89 | 1.89 | 2.772 (6) | 173 |
N3—H3···O27iv | 0.91 | 1.87 | 2.736 (6) | 159 |
N4—H4C···O20v | 0.89 | 1.89 | 2.772 (5) | 171 |
N4—H4D···O33Wvi | 0.89 | 2.21 | 3.035 (7) | 154 |
N4—H4E···O23 | 0.89 | 1.99 | 2.820 (5) | 156 |
N5—H5···O26 | 0.91 | 1.82 | 2.709 (5) | 166 |
N6—H6D···O17 | 0.89 | 2.34 | 3.056 (6) | 137 |
N6—H6D···O32Wvii | 0.89 | 2.50 | 3.046 (7) | 120 |
N6—H6E···O31Wviii | 0.89 | 1.89 | 2.745 (6) | 160 |
N6—H6F···O2vii | 0.89 | 2.12 | 2.958 (6) | 156 |
O29W—H29A···O1 | 0.91 | 2.00 | 2.848 (5) | 154 |
O29W—H29B···O8ii | 0.94 | 1.90 | 2.790 (5) | 156 |
O30W—H30A···O3vii | 0.84 | 2.06 | 2.895 (5) | 174 |
O30W—H30B···O7ix | 0.87 | 1.86 | 2.716 (5) | 173 |
O31W—H31A···O21 | 0.95 | 1.83 | 2.770 (5) | 173 |
O31W—H31B···O30W | 0.82 | 1.94 | 2.724 (6) | 160 |
O32W—H32A···O29W | 0.88 | 2.00 | 2.808 (6) | 152 |
O32W—H32B···O34Wix | 0.88 | 2.03 | 2.873 (8) | 160 |
O33W—H33A···O15x | 0.87 | 1.98 | 2.787 (6) | 153 |
O33W—H33B···O22vi | 0.97 | 1.84 | 2.723 (5) | 150 |
O34W—H34A···O18 | 0.97 | 2.11 | 3.055 (7) | 163 |
O34W—H34B···O33Wvi | 0.80 | 2.24 | 2.903 (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. |
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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.