metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 66| Part 3| March 2010| Pages m323-m324

Tris[4,4′-(ethene-1,2-di­yl)dipyridinium] deca­vanadate dihydrate

aDpto de Mineralogía y Petrología, Facultad de Ciencia y Tecnología, Universidad del País Vasco/E.H.U., PO Box 644, 48080 Bilbao, Spain, and bDpto Química Inorgánica, Facultad de Ciencia y Tecnología, Universidad del País Vasco/E.H.U., PO Box 644, 48080 Bilbao, Spain
*Correspondence e-mail: karmele.urtiaga@ehu.es

(Received 14 December 2009; accepted 16 February 2010; online 24 February 2010)

The asymmetric unit of the title compound, (C12H12N2)3[V10O28]·2H2O, contains one half of a deca­vanadate anion, one and a half trans-1,2-bis­(4-pyridinio)ethene cations and one water mol­ecule. The V10O28 groups are involved in a three-dimensional hydrogen-bonding network through Ow—H⋯O, N—H⋯O and C—H⋯O inter­actions.

Related literature

For general background to inorganic–organic vanadates, see: Zavalij & Whittingham (1999[Zavalij, P. Y. & Whittingham, M. S. (1999). Acta Cryst. B55, 627-663.]); Fernández de Luis et al. (2009a[Fernández de Luis, R., Mesa, J. L., Urtiaga, M. K., Rojo, T. & Arriortua, M. I. (2009a). Eur. J. Inorg. Chem. pp. 4786-4794.]). For inorganic–organic vanadates constructed from pyridyl ligands, see: Fernández de Luis et al. (2009b[Fernández de Luis, R., Urtiaga, M. K., Mesa, J. L., Rojo, T. & Arriortua, M. I. (2009b). J. Alloys Compd, 480, 54-56.]); Khan et al. (2004[Khan, M. I., Nome, R. C., Ayesh, S., Golub, V. O., O'Connor, C. J. & Doedens, R. J. (2004). Chem. Mater. 16, 5273-5279.]); Zheng et al. (2001[Zheng, L.-M., Wang, X., Wang, Y. & Jacobson, A. J. (2001). J. Mater. Chem. 11, 1100-1105.]). For general background to deca­vanadates, see: Pope & Müller (1991[Pope, M. T. & Müller, A. (1991). Angew. Chem. Int. Ed. Engl. 30, 34-48.], 1994[Pope, M. T. & Müller, A. (1994). Polyoxometalates: From Platonic Solids to Anti-retroviral Activity. Drodrecht, The Netherlands: Kluwer.]); Rhule et al. (1998[Rhule, J. T., Hill, C. L., Judd, D. A. & Schinazi, R. F. (1998). Chem. Rev. 98, 327-358.]). For hydrogen bonding, see: Steiner (2002[Steiner, T. (2002). Angew. Chem. Int. Ed. 41, 48-76.]).

[Scheme 1]

Experimental

Crystal data
  • (C12H12N2)3[V10O28]·2H2O

  • Mr = 1546.14

  • Triclinic, [P \overline 1]

  • a = 9.7343 (4) Å

  • b = 11.7754 (5) Å

  • c = 12.2311 (5) Å

  • α = 113.072 (4)°

  • β = 105.396 (4)°

  • γ = 93.171 (3)°

  • V = 1223.33 (9) Å3

  • Z = 1

  • Mo Kα radiation

  • μ = 1.92 mm−1

  • T = 293 K

  • 0.18 × 0.14 × 0.08 mm

Data collection
  • Oxford Xcalibur2 diffractometer

  • Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2008[Oxford Diffraction (2008). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.]) Tmin = 0.780, Tmax = 0.887

  • 10137 measured reflections

  • 5498 independent reflections

  • 3829 reflections with I > 2σ(I)

  • Rint = 0.029

  • 3 standard reflections every 50 reflections intensity decay: none

Refinement
  • R[F2 > 2σ(F2)] = 0.032

  • wR(F2) = 0.076

  • S = 0.90

  • 5498 reflections

  • 378 parameters

  • 2 restraints

  • H atoms treated by a mixture of independent and constrained refinement

  • Δρmax = 0.64 e Å−3

  • Δρmin = −0.39 e Å−3

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
O1w—H19⋯O11i 0.92 (3) 2.01 (4) 2.919 (3) 168 (4)
O1w—H20⋯O12 0.92 (3) 2.15 (3) 3.028 (3) 160 (3)
N1—H21⋯O9 0.86 1.88 2.721 (3) 164
N2—H22⋯O2ii 0.86 1.75 2.568 (3) 159
N3—H23⋯O5 0.86 1.71 2.564 (3) 172
C2—H2⋯O1iii 0.93 2.50 3.126 (4) 124
C4—H4⋯O1iv 0.93 2.32 3.107 (4) 143
C8—H8⋯O10 0.93 2.57 3.162 (4) 122
C11—H11⋯O3iv 0.93 2.33 3.254 (4) 173
C12—H12⋯O1w 0.93 2.57 3.230 (4) 128
C14—H14⋯O6v 0.93 2.54 3.202 (3) 128
C14—H14⋯O12v 0.93 2.39 3.293 (3) 162
C16—H16⋯O13iv 0.93 2.58 3.401 (4) 147
C17—H17⋯O13 0.93 2.60 3.187 (4) 122
Symmetry codes: (i) -x+1, -y+1, -z; (ii) -x, -y+1, -z+1; (iii) x-1, y+1, z; (iv) -x+1, -y+1, -z+1; (v) x-1, y, z.

Data collection: CrysAlis CCD (Oxford Diffraction, 2008[Oxford Diffraction (2008). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.]); cell refinement: CrysAlis RED (Oxford Diffraction, 2008[Oxford Diffraction (2008). CrysAlis CCD and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England.]); data reduction: CrysAlis RED; program(s) used to solve structure: SIR92 (Altomare et al., 1993[Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993). J. Appl. Cryst. 26, 343-350.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: PLATON (Spek, 2009[Spek, A. L. (2009). Acta Cryst. D65, 148-155.]); software used to prepare material for publication: TOPOS (Blatov, 2006[Blatov, A. V. (2006). IUCr CompComm. Newslett. 7, 4-6.]).

Supporting information


Comment top

The title compound was synthesized as part of our studies focused on the construction of new inorganic-organic vanadates (Zavalij & Whittingham, 1999) with first row transition metal centres (Fernández et al., 2009b). The pyridyl ligands have very often used since they have two nitrogen atoms that can bridge metal atoms to form polymeric compounds (Fernández et al., 2009a), (Khan et al., 2004), (Zheng et al., 2001). However, the hydrothermal synthesis of the Co/Bpe/VxOy system give rise to the crystallization of the title compound as a minor product of the reaction.

The polyoxovanadates exhibit interesting physical and chemical properties with relevance to catalysis, biochemical processes (enzyme inhibitor or activator), medicine, and material science (Pope & Muller, 1991, 1994; Rhule et al., 1998).

The asymmetric unit of (I) consists of one-half decavanadate anion, one and a half pyridinium cations and one water molecule. The decavanadate anion is composed of ten VO6 octahedra combined via shared edges and corners. Six octahedra are arranged in a 2 x 3 equatorial plane sharing edges; the other four octahedra are distributed above and below the equatorial plane, connected by shared sloping edges with the central six octahedra (Fig. 1).

The V—O bond lengths are classified according to the coordinative conditions of the oxygen atoms: terminal O atoms (VO, 1.597 (2) - 1.608 (2) Å); double-bridging O atoms (V—O, 1.684 (2) - 2.083 (2) Å), triply bridging O atoms located on the surface of the [V10O28]6- cluster (V—O, 1.968 (2) - 2.061 (2) Å), and one six-coordinate O atom (V—O 2.085 (2) - 2.344 (2) Å).

The supramolecular structure is formed by Ow—H···O, N—H···O and C—H···O hydrogen bonds, between the anion and the water molecules, between the cation and the anion, and between cation and water molecule (Steiner, 2002).

The decavanadate anions are hydrogen bonded through two water molecules (Fig.2) forming chains in the [010] direction (Fig. 1). The N—H groups of the organic cations interact with the surface oxygen atoms of the decavanadate anion (N1—H21···O9, N2—H22···O2, N3—H23···O5). Each V10O28 anion is linked trough three organic cations to other two V10O28 anion (Fig. 2). The hydrogen bonding trough the water molecules (O—H···O) and organic cations (N—H···O) of the [V10O28] clusters, generates the layers shown in the figure 2. The layers are stacked along the [101] direction via C—H···O hydrogen bonds, establishing the three dimensional supramolecular network (Fig. 3).

Related literature top

For general background to inorganic–organic vanadates, see: Zavalij & Whittingham (1999); Fernández et al. (2009a). For inorganic–organic vanadates constructed from pyridyl ligands, see: Fernández et al. (2009b); Khan et al. (2004); Zheng et al. (2001). For general background to decavanadates, see: Pope & Muller (1991, 1994); Rhule et al. (1998). For hydrogen bonding, see: Steiner (2002).

Experimental top

A mixture consisting of NaVO3 (0.135 mmol), 1,2-di(4-pyridyl)ethylene (0.135 mmol), Co(NO3)2.6H2O (0.135 mmol), and H2O (30 ml) in the molar ratio 1:1:1 was placed in a 50-ml Parr Teflon-lined autoclave. The initial pH value was adjusted to 4.0 with a 1M HNO3 solution under a vigorous stirring. The autoclave was sealed and heated for 3 days at 120°C. After the reaction a mixture of dark brown polycrystalline powder with a minor percentage of the title compound orange single crystals were obtained. In order to obtain the title compound as a single phase, the Co(NO3)2.6H2O was suppressed from the initial reactants. However, all attempts to obtain the title compound as a single phase after the hydrothermal reaction have been unsuccessful.

Refinement top

The H atoms belonging to the organic ligand were placed at geometrically idealized positions (C—H = 0.93 Å and N—H = 0.86 Å) and constrained to ride on their parent atoms [Uiso(H)= 1.2Ueq(C,N)]. H atoms of the water molecule were located in a difference map and refined with O—H inter-atomic distances restrained to 0.93 Å, with the standard deviation set at 0.01 Å.

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2008); cell refinement: CrysAlis RED (Oxford Diffraction, 2008); data reduction: CrysAlis RED (Oxford Diffraction, 2008); program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: PLATON (Spek, 2009); software used to prepare material for publication: TOPOS (Blatov, 2006).

Figures top
[Figure 1] Fig. 1. The molecular structure of the title compound showing the atom-labeling scheme.Displacement ellipsoids are shown at the 50% probability level.
[Figure 2] Fig. 2. [V10O28]6- anions hydrogen bonded trough the water molecules and organic cations giving rise to sheets.
[Figure 3] Fig. 3. The crystal packing of (I). The sheets are stacked along the [101] direction.
tris[4,4'-(ethene-1,2-diyl)dipyridinium] decavanadate dihydrate top
Crystal data top
(C12H12N2)3[V10O28]·2H2OZ = 1
Mr = 1546.14F(000) = 768
Triclinic, P1Dx = 2.099 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.7343 (4) ÅCell parameters from 4312 reflections
b = 11.7754 (5) Åθ = 2.6–28.9°
c = 12.2311 (5) ŵ = 1.92 mm1
α = 113.072 (4)°T = 293 K
β = 105.396 (4)°Plate, orange
γ = 93.171 (3)°0.18 × 0.14 × 0.08 mm
V = 1223.33 (9) Å3
Data collection top
Oxford Xcalibur2
diffractometer
3829 reflections with I > 2σ(I)
Radiation source: fine-focus sealed X-ray tubeRint = 0.029
Graphite monochromatorθmax = 29.0°, θmin = 2.7°
profile data from q/2q scansh = 912
Absorption correction: analytical
(CrysAlis RED; Oxford Diffraction, 2008)
k = 1412
Tmin = 0.780, Tmax = 0.887l = 1515
10137 measured reflections3 standard reflections every 50 reflections
5498 independent reflections intensity decay: none
Refinement top
Refinement on F22 restraints
Least-squares matrix: fullH atoms treated by a mixture of independent and constrained refinement
R[F2 > 2σ(F2)] = 0.032 w = 1/[σ2(Fo2) + (0.0377P)2]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.076(Δ/σ)max < 0.001
S = 0.90Δρmax = 0.64 e Å3
5498 reflectionsΔρmin = 0.39 e Å3
378 parameters
Crystal data top
(C12H12N2)3[V10O28]·2H2Oγ = 93.171 (3)°
Mr = 1546.14V = 1223.33 (9) Å3
Triclinic, P1Z = 1
a = 9.7343 (4) ÅMo Kα radiation
b = 11.7754 (5) ŵ = 1.92 mm1
c = 12.2311 (5) ÅT = 293 K
α = 113.072 (4)°0.18 × 0.14 × 0.08 mm
β = 105.396 (4)°
Data collection top
Oxford Xcalibur2
diffractometer
3829 reflections with I > 2σ(I)
Absorption correction: analytical
(CrysAlis RED; Oxford Diffraction, 2008)
Rint = 0.029
Tmin = 0.780, Tmax = 0.8873 standard reflections every 50 reflections
10137 measured reflections intensity decay: none
5498 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0322 restraints
wR(F2) = 0.076H atoms treated by a mixture of independent and constrained refinement
S = 0.90Δρmax = 0.64 e Å3
5498 reflectionsΔρmin = 0.39 e Å3
378 parameters
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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
O1W0.6206 (3)0.5760 (2)0.2406 (2)0.0481 (6)
V10.56372 (4)0.24085 (4)0.17922 (4)0.01678 (11)
V40.67454 (4)0.01106 (4)0.01759 (4)0.01442 (10)
V50.55805 (4)0.00281 (4)0.23104 (4)0.01684 (11)
V20.66272 (5)0.24385 (4)0.04145 (4)0.01972 (11)
V30.34102 (5)0.22893 (4)0.06201 (4)0.02019 (11)
O60.78126 (17)0.11594 (15)0.00005 (15)0.0193 (4)
O30.58831 (19)0.08980 (17)0.37727 (15)0.0251 (4)
O80.77818 (17)0.09058 (15)0.04656 (15)0.0187 (4)
O130.59849 (19)0.32733 (16)0.32570 (15)0.0259 (4)
O90.40551 (18)0.30068 (15)0.10994 (15)0.0198 (4)
O50.41516 (17)0.09802 (15)0.16167 (14)0.0152 (4)
O100.2165 (2)0.30576 (18)0.09039 (17)0.0311 (5)
O120.68888 (18)0.31452 (15)0.13329 (15)0.0203 (4)
O20.39991 (18)0.11428 (15)0.20214 (15)0.0192 (4)
O110.50190 (19)0.31199 (16)0.07012 (15)0.0219 (4)
O70.50263 (17)0.10133 (14)0.02292 (14)0.0156 (4)
O40.67716 (17)0.10895 (15)0.18500 (14)0.0162 (4)
O10.68157 (18)0.10149 (16)0.22455 (15)0.0203 (4)
O140.7885 (2)0.32950 (18)0.05078 (17)0.0311 (5)
N30.2433 (2)0.2213 (2)0.2692 (2)0.0243 (5)
H230.29590.17350.23230.029*
N10.2556 (3)0.4870 (2)0.1955 (2)0.0313 (6)
H210.30680.43580.16040.038*
N20.2323 (3)1.0304 (2)0.6653 (2)0.0301 (6)
H220.28721.07320.70400.036*
C90.0305 (3)0.5473 (3)0.1930 (2)0.0310 (7)
H90.06820.53390.15200.037*
C30.0588 (3)0.8902 (2)0.5429 (2)0.0230 (6)
C150.0758 (3)0.3752 (2)0.3866 (2)0.0230 (6)
C70.0022 (3)0.7264 (3)0.3679 (3)0.0299 (7)
H70.09790.71370.31930.036*
C170.3018 (3)0.3073 (3)0.3866 (2)0.0316 (7)
H170.39920.31410.42770.038*
C20.2037 (3)0.8813 (3)0.4807 (3)0.0317 (7)
H20.24380.82750.39630.038*
C140.0182 (3)0.2840 (3)0.2653 (2)0.0301 (7)
H140.07920.27350.22180.036*
C100.0919 (3)0.6475 (2)0.3090 (2)0.0252 (6)
C60.0367 (3)0.8142 (3)0.4839 (2)0.0273 (6)
H60.13300.82870.53190.033*
C80.1146 (3)0.4683 (3)0.1390 (3)0.0324 (7)
H80.07250.40060.06160.039*
C40.0052 (3)0.9733 (3)0.6680 (3)0.0330 (7)
H40.09140.98190.71240.040*
C160.2216 (3)0.3861 (3)0.4479 (3)0.0325 (7)
H160.26430.44620.52960.039*
C110.2410 (3)0.6652 (3)0.3648 (3)0.0383 (8)
H110.28630.73230.44190.046*
C180.0196 (3)0.4549 (2)0.4436 (2)0.0280 (6)
H180.11590.44000.39530.034*
C130.1052 (3)0.2090 (3)0.2092 (3)0.0308 (7)
H130.06600.14830.12730.037*
C50.0935 (3)1.0428 (3)0.7266 (3)0.0369 (8)
H50.05601.09940.81030.044*
C10.2869 (3)0.9529 (3)0.5454 (3)0.0346 (7)
H10.38400.94670.50390.041*
C120.3201 (3)0.5841 (3)0.3063 (3)0.0427 (8)
H120.41950.59630.34360.051*
H190.580 (4)0.600 (4)0.178 (3)0.103 (17)*
H200.629 (4)0.4968 (18)0.190 (3)0.090 (15)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
O1W0.0659 (17)0.0344 (15)0.0435 (14)0.0091 (12)0.0161 (13)0.0166 (12)
V10.0169 (2)0.0135 (2)0.0151 (2)0.00251 (18)0.00647 (17)0.00015 (18)
V40.0112 (2)0.0148 (2)0.0138 (2)0.00369 (17)0.00515 (17)0.00151 (17)
V50.0167 (2)0.0183 (2)0.0130 (2)0.00517 (18)0.00559 (17)0.00319 (18)
V20.0200 (2)0.0171 (2)0.0202 (2)0.00216 (18)0.00929 (18)0.00423 (19)
V30.0209 (2)0.0195 (2)0.0203 (2)0.00956 (19)0.00864 (19)0.00638 (19)
O60.0153 (9)0.0184 (10)0.0199 (9)0.0014 (7)0.0075 (7)0.0025 (8)
O30.0279 (11)0.0268 (11)0.0150 (9)0.0061 (8)0.0077 (8)0.0024 (8)
O80.0152 (9)0.0212 (10)0.0185 (9)0.0071 (7)0.0073 (7)0.0053 (8)
O130.0291 (11)0.0213 (10)0.0185 (9)0.0018 (8)0.0088 (8)0.0010 (8)
O90.0214 (10)0.0160 (9)0.0201 (9)0.0079 (7)0.0103 (7)0.0028 (7)
O50.0137 (9)0.0160 (9)0.0130 (8)0.0049 (7)0.0058 (7)0.0017 (7)
O100.0307 (11)0.0334 (11)0.0321 (11)0.0184 (9)0.0125 (9)0.0135 (9)
O120.0199 (10)0.0152 (9)0.0212 (9)0.0014 (7)0.0083 (7)0.0022 (7)
O20.0190 (10)0.0189 (10)0.0187 (9)0.0036 (7)0.0099 (7)0.0044 (8)
O110.0265 (10)0.0174 (10)0.0221 (9)0.0071 (8)0.0106 (8)0.0063 (8)
O70.0148 (9)0.0151 (9)0.0151 (8)0.0056 (7)0.0065 (7)0.0032 (7)
O40.0130 (9)0.0172 (9)0.0135 (8)0.0028 (7)0.0045 (7)0.0013 (7)
O10.0183 (9)0.0248 (10)0.0170 (9)0.0085 (8)0.0062 (7)0.0072 (8)
O140.0305 (11)0.0286 (11)0.0342 (11)0.0003 (9)0.0147 (9)0.0112 (9)
N30.0236 (13)0.0232 (13)0.0283 (12)0.0121 (10)0.0176 (10)0.0060 (10)
N10.0354 (15)0.0297 (14)0.0306 (13)0.0178 (12)0.0192 (11)0.0073 (11)
N20.0366 (15)0.0277 (14)0.0374 (14)0.0163 (11)0.0273 (12)0.0138 (12)
C90.0291 (17)0.0326 (17)0.0265 (15)0.0109 (13)0.0093 (13)0.0067 (13)
C30.0256 (15)0.0204 (15)0.0289 (14)0.0084 (12)0.0169 (12)0.0105 (12)
C150.0249 (15)0.0190 (14)0.0272 (14)0.0080 (12)0.0154 (12)0.0066 (12)
C70.0281 (16)0.0325 (17)0.0281 (15)0.0130 (13)0.0112 (12)0.0094 (13)
C170.0208 (15)0.0371 (18)0.0294 (15)0.0103 (13)0.0096 (12)0.0049 (14)
C20.0335 (17)0.0391 (18)0.0236 (14)0.0163 (14)0.0119 (13)0.0109 (13)
C140.0203 (15)0.0336 (17)0.0288 (15)0.0092 (13)0.0101 (12)0.0033 (13)
C100.0311 (16)0.0218 (15)0.0253 (14)0.0114 (12)0.0142 (12)0.0079 (12)
C60.0236 (15)0.0274 (16)0.0297 (15)0.0081 (12)0.0126 (12)0.0077 (13)
C80.0383 (19)0.0277 (17)0.0251 (15)0.0087 (14)0.0138 (13)0.0022 (13)
C40.0213 (16)0.0331 (18)0.0340 (16)0.0001 (13)0.0114 (13)0.0023 (14)
C160.0281 (17)0.0321 (17)0.0241 (15)0.0065 (13)0.0098 (13)0.0027 (13)
C110.0320 (18)0.0323 (18)0.0323 (16)0.0081 (14)0.0097 (14)0.0049 (14)
C180.0229 (15)0.0273 (17)0.0313 (15)0.0090 (13)0.0116 (12)0.0072 (12)
C130.0266 (16)0.0290 (17)0.0267 (15)0.0065 (13)0.0116 (13)0.0009 (13)
C50.0349 (18)0.0322 (18)0.0351 (17)0.0040 (14)0.0216 (14)0.0009 (14)
C10.0306 (17)0.049 (2)0.0322 (16)0.0216 (15)0.0148 (13)0.0206 (15)
C120.0265 (17)0.048 (2)0.0385 (18)0.0100 (15)0.0107 (14)0.0020 (16)
Geometric parameters (Å, º) top
O1W—H190.92 (3)N1—H210.8600
O1W—H200.92 (3)N2—C11.323 (4)
V1—O131.6035 (16)N2—C51.328 (4)
V1—O121.7835 (17)N2—H220.8600
V1—O91.8657 (17)C9—C81.365 (4)
V1—O41.9675 (16)C9—C101.386 (4)
V1—O52.0614 (17)C9—H90.9300
V1—O72.2568 (15)C3—C41.385 (4)
V4—O61.6836 (17)C3—C21.389 (4)
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O1—V5—O492.10 (7)C5—N2—H22119.7
O2—V5—O4154.88 (7)C8—C9—C10120.1 (3)
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O2—V5—V3i84.31 (5)N3—C17—C16121.4 (3)
O4—V5—V3i88.21 (5)N3—C17—H17119.3
O5—V5—V3i123.19 (4)C16—C17—H17119.3
O7i—V5—V3i48.20 (4)C1—C2—C3119.2 (3)
O3—V5—V189.79 (7)C1—C2—H2120.4
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O2—V5—V1129.48 (6)C13—C14—C15119.8 (3)
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O14—V2—O2i101.51 (8)C7—C6—C3125.5 (3)
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O14—V2—O12102.49 (9)C3—C6—H6117.3
O11—V2—O1291.08 (7)N1—C8—C9120.7 (3)
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V2—V1—V4—O631.26 (6)V2—V1—V3—O8i135.20 (5)
V3—V1—V4—O684.82 (6)O13—V1—V3—O7171.35 (11)
O13—V1—V4—O811.85 (13)O12—V1—V3—O784.76 (8)
O12—V1—V4—O8110.91 (10)O9—V1—V3—O7166.13 (12)
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O4—V1—V4—O81.42 (11)O5—V1—V3—O774.25 (7)
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V3—V1—V5—O1108.92 (7)O3—V5—O5—V180.85 (9)
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O7i—V4—V2—O113.21 (9)O7—V3—O11—V20.99 (8)
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O8—V4—V2—O2i92.20 (11)V1—V3—O11—V245.85 (8)
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O7i—V4—V2—O6177.29 (10)O6—V4—O7—V185.89 (7)
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O7i—V4—V2—O71.28 (10)V2—V4—O7—V184.98 (5)
V1—V4—V2—O756.50 (5)O6—V4—O7—V20.91 (6)
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O8—V4—V2—V3177.52 (10)O4—V4—O7—V298.65 (6)
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O7—V4—V2—V31.75 (5)V3i—V4—O7—V2176.95 (2)
O7i—V4—V2—V33.03 (5)V1—V4—O7—V284.98 (5)
V1—V4—V2—V354.750 (15)O12—V1—O7—V482.12 (7)
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O7—V4—V2—V156.50 (5)V2—V1—O7—V488.43 (6)
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V3—V1—V2—O14131.71 (10)O12—V1—O7—V5i47.1 (4)
O13—V1—V2—O1196.00 (12)O9—V1—O7—V5i49.2 (4)
O12—V1—V2—O11104.95 (11)O4—V1—O7—V5i142.7 (4)
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V3—V1—V2—O1127.02 (6)O9—V1—O7—V37.54 (7)
O13—V1—V2—O2i176.06 (12)O4—V1—O7—V3175.61 (7)
O12—V1—V2—O2i167.11 (12)O5—V1—O7—V396.75 (6)
O9—V1—V2—O2i84.06 (8)V5—V1—O7—V3137.24 (4)
O4—V1—V2—O2i70.39 (8)V4—V1—O7—V3170.89 (8)
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V4—V1—V2—O2i49.32 (7)O4—V1—O7—V2101.93 (6)
V3—V1—V2—O2i60.92 (7)O5—V1—O7—V2179.20 (6)
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O9—V1—V2—O12108.84 (11)V4—V1—O7—V288.43 (6)
O4—V1—V2—O1296.72 (11)V3—V1—O7—V282.46 (5)
O5—V1—V2—O12169.61 (12)O9—V3—O7—V4i88.20 (7)
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O12—V1—V2—V3131.97 (10)O1i—V3—O7—V291.78 (6)
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O14—V2—V3—O1i101.28 (12)O8—V4—O4—V1178.99 (8)
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O11—V2—V3—V1125.30 (10)O5—V5—O4—V120.26 (6)
O2i—V2—V3—V1133.26 (6)O7i—V5—O4—V197.86 (7)
O12—V2—V3—V122.91 (5)V3i—V5—O4—V1145.23 (6)
O6—V2—V3—V154.24 (5)O3—V5—O1—V3i174.03 (10)
O7—V2—V3—V156.00 (5)O2—V5—O1—V3i72.23 (10)
V4—V2—V3—V154.430 (14)O4—V5—O1—V3i83.60 (10)
O13—V1—V3—O100.30 (15)O5—V5—O1—V3i24.6 (2)
O12—V1—V3—O10103.59 (12)O7i—V5—O1—V3i7.14 (9)
O9—V1—V3—O105.53 (14)V1—V5—O1—V3i82.57 (11)
O4—V1—V3—O10166.49 (12)C13—N3—C17—C160.7 (5)
O5—V1—V3—O1097.40 (12)C4—C3—C2—C11.0 (4)
O7—V1—V3—O10171.65 (12)C6—C3—C2—C1177.3 (3)
V5—V1—V3—O10121.58 (11)C16—C15—C14—C130.6 (5)
V4—V1—V3—O10177.75 (11)C18—C15—C14—C13179.3 (3)
V2—V1—V3—O10128.10 (11)C8—C9—C10—C111.7 (4)
O13—V1—V3—O95.23 (13)C8—C9—C10—C7176.6 (3)
O12—V1—V3—O9109.11 (12)C6—C7—C10—C9170.6 (3)
O4—V1—V3—O9160.96 (12)C6—C7—C10—C117.6 (5)
O5—V1—V3—O991.88 (11)C10—C7—C6—C3178.3 (3)
O7—V1—V3—O9166.13 (12)C4—C3—C6—C7175.9 (3)
V5—V1—V3—O9116.06 (10)C2—C3—C6—C72.3 (5)
V4—V1—V3—O9172.22 (10)C12—N1—C8—C90.6 (5)
V2—V1—V3—O9133.62 (10)C10—C9—C8—N10.8 (5)
O13—V1—V3—O11101.87 (11)C2—C3—C4—C50.3 (5)
O12—V1—V3—O112.02 (7)C6—C3—C4—C5178.0 (3)
O9—V1—V3—O11107.10 (12)N3—C17—C16—C150.6 (5)
O4—V1—V3—O1191.94 (8)C14—C15—C16—C170.1 (5)
O5—V1—V3—O11161.03 (7)C18—C15—C16—C17179.8 (3)
O7—V1—V3—O1186.77 (8)C9—C10—C11—C121.2 (5)
V5—V1—V3—O11136.84 (5)C7—C10—C11—C12177.0 (3)
V4—V1—V3—O1180.68 (5)C14—C15—C18—C18ii179.5 (4)
V2—V1—V3—O1126.52 (5)C16—C15—C18—C18ii0.5 (6)
O13—V1—V3—O1i174.42 (11)C17—N3—C13—C140.1 (5)
O12—V1—V3—O1i81.69 (8)C15—C14—C13—N30.6 (5)
O9—V1—V3—O1i169.20 (12)C1—N2—C5—C41.8 (5)
O4—V1—V3—O1i8.24 (9)C3—C4—C5—N21.1 (5)
O5—V1—V3—O1i77.32 (8)C5—N2—C1—C21.1 (5)
O7—V1—V3—O1i3.07 (8)C3—C2—C1—N20.3 (5)
V5—V1—V3—O1i53.14 (7)C8—N1—C12—C111.2 (5)
V4—V1—V3—O1i3.03 (7)C8—N1—C12—C111.2 (5)
V2—V1—V3—O1i57.18 (7)C10—C11—C12—N10.2 (5)
O13—V1—V3—O8i96.40 (10)
Symmetry codes: (i) x+1, y, z; (ii) x, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1w—H19···O11iii0.92 (3)2.01 (4)2.919 (3)168 (4)
O1w—H20···O120.92 (3)2.15 (3)3.028 (3)160 (3)
N1—H21···O90.861.882.721 (3)164
N2—H22···O2ii0.861.752.568 (3)159
N3—H23···O50.861.712.564 (3)172
C2—H2···O1iv0.932.503.126 (4)124
C4—H4···O1v0.932.323.107 (4)143
C8—H8···O100.932.573.162 (4)122
C11—H11···O3v0.932.333.254 (4)173
C12—H12···O1w0.932.573.230 (4)128
C14—H14···O6vi0.932.543.202 (3)128
C14—H14···O12vi0.932.393.293 (3)162
C16—H16···O13v0.932.583.401 (4)147
C17—H17···O130.932.603.187 (4)122
Symmetry codes: (ii) x, y+1, z+1; (iii) x+1, y+1, z; (iv) x1, y+1, z; (v) x+1, y+1, z+1; (vi) x1, y, z.

Experimental details

Crystal data
Chemical formula(C12H12N2)3[V10O28]·2H2O
Mr1546.14
Crystal system, space groupTriclinic, P1
Temperature (K)293
a, b, c (Å)9.7343 (4), 11.7754 (5), 12.2311 (5)
α, β, γ (°)113.072 (4), 105.396 (4), 93.171 (3)
V3)1223.33 (9)
Z1
Radiation typeMo Kα
µ (mm1)1.92
Crystal size (mm)0.18 × 0.14 × 0.08
Data collection
DiffractometerOxford Xcalibur2
diffractometer
Absorption correctionAnalytical
(CrysAlis RED; Oxford Diffraction, 2008)
Tmin, Tmax0.780, 0.887
No. of measured, independent and
observed [I > 2σ(I)] reflections
10137, 5498, 3829
Rint0.029
(sin θ/λ)max1)0.682
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.032, 0.076, 0.90
No. of reflections5498
No. of parameters378
No. of restraints2
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.64, 0.39

Computer programs: CrysAlis CCD (Oxford Diffraction, 2008), CrysAlis RED (Oxford Diffraction, 2008), SIR92 (Altomare et al., 1993), SHELXL97 (Sheldrick, 2008), PLATON (Spek, 2009), TOPOS (Blatov, 2006).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1w—H19···O11i0.92 (3)2.01 (4)2.919 (3)168 (4)
O1w—H20···O120.92 (3)2.15 (3)3.028 (3)160 (3)
N1—H21···O90.861.882.721 (3)164
N2—H22···O2ii0.861.752.568 (3)159
N3—H23···O50.861.712.564 (3)172
C2—H2···O1iii0.932.503.126 (4)124
C4—H4···O1iv0.932.323.107 (4)143
C8—H8···O100.932.573.162 (4)122
C11—H11···O3iv0.932.333.254 (4)173
C12—H12···O1w0.932.573.230 (4)128
C14—H14···O6v0.932.543.202 (3)128
C14—H14···O12v0.932.393.293 (3)162
C16—H16···O13iv0.932.583.401 (4)147
C17—H17···O130.932.603.187 (4)122
Symmetry codes: (i) x+1, y+1, z; (ii) x, y+1, z+1; (iii) x1, y+1, z; (iv) x+1, y+1, z+1; (v) x1, y, z.
 

Acknowledgements

We gratefully acknowledge financial support of this work by the Ministerio de Educación y Ciencia (MAT2007–60400/66737-C02–01) and the Gobierno Vasco (IT-177–07 and GI07/126-IT-312–07). The authors also thank the technicians of SGIker, Drs J. Sangüesa, I. Orue, P. Vitoria and A. Larrañaga, financed by the National Program for the Promotion of Human Resources within the National Plan of Scientific Research, Development and Innovation, Ministerio de Ciencia y Tecnología and Fondo Social Europeo (FSE), for the X-ray diffraction and magnetic measurements, respectively. RFdeL thanks the MEC (Madrid, España) for funding (BES-2005–10322).

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Volume 66| Part 3| March 2010| Pages m323-m324
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