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The title compound, aqua­[bis­(salicyl­idene)­ethyl­enediamin­ato-O,N,N',O']­oxovanadium(V) nitrate, [VO(C16H14N2O2)(H2O)]NO3, crystallizes as two polymorphs in the triclinic and monoclinic crystal systems. In both, the V atom has a distorted octahedral coordination geometry with a long V-Owater bond trans to V=O. The coordinated water mol­ecules are hydrogen bonded to the nitrate ions so that pairs of cations are linked to give neutral centrosymmetric dimers. The V=O and V-Owater distances are 1.598 (2) and 2.257 (2) Å, respectively, in the triclinic form, and 1.588 (3) and 2.230 (3) Å, respectively, in the monoclinic form. In the triclinic form, the dimers pack so that the salen [bis(salicyl­idene)ethylenediaminate] ligands are parallel to each other, whereas in the monoclinic form, which is the denser, there is a herring-bone arrangement.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100019132/gg1035sup1.cif
Contains datablocks global, I, II

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100019132/gg1035Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100019132/gg1035IIsup3.hkl
Contains datablock II

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S0108270100019132/gg1035sup4.pdf
Supplementary material

CCDC references: 162549; 162550

Comment top

Complexes of the type VVO(Schiff base)Y (Y is Cl, ClO4 or NO3) can be prepared by oxidizing VIVO(Schiff base) with (NH4)2Ce(NO3)6 in acetonitrile, followed by the addition of HY (Nakajima et al., 1990). The structure of [VVO(salen)](ClO4) [salen is bis(salicylidene)ethylenediaminato-N,N'] has been studied by X-ray diffraction by Bonadies et al. (1987) and the V shown to have a distorted octahedral coordination, with a long [2.456 (3) Å] V—Operchlorate bond trans to VO. Nakajima et al. (1987) proposed, on the basis of absorption spectra, that their VVO(Schiff base)Y complexes had structures analogous to that of the [VVO(salen)]·ClO4 complex. A structural investigation of [VVO(salen)]NO3 prepared by Nakajima's method showed the product to contain two polymorphs, a triclinic form, (I), and a monoclinic form, (II), which contain the [VVO(salen)(H2O)]+ and NO3- ions. The structures of these two polymorphs are presented here. \sch

In both forms the cations are linked by hydrogen bonds via the nitrates to give centrosymmetric dimers (Fig. 1a and b). The V atoms are coordinated to two N atoms and two O atoms of the salen ligand, to the vanadyl oxygen and to a water molecule which is trans to the VO oxygen. This octahedral arrangement is distorted, in that the V atom is displaced out of the N2O2 plane in the direction of the vanadyl oxygen by 0.255 Å in (I) and 0.260 Å in (II), which is similar to the value of 0.270 Å observed in the cation of [VVO(salen)(H2O)]2·Cu2Cl4, (III) (Banci et al., 1984). The VO distances in compounds (I), (II), and (III) are 1.598 (2), 1.588 (3) and 1.590 (5) Å, respectively, and the V—Owater distances are 2.257 (2), 2.230 (3) and 2.310 (5) Å, respectively. These latter values are much longer than the usual VV—O distance; cf. V—Osalen of 1.823 (2) and 1.838 (2) Å in (I), and 1.835 (3) and 1.805 (3) Å in (II). An indication that the VO distances in (I) and (II) really are different is that the VO absorption in the IR spectrum of the bulk sample is a doublet.

The water molecules are hydrogen bonded to the nitrate ion so that there are two nitrate bridges between pairs of cations; Owater···Onitrate distances are 2.737 (2) and 2.779 (2) Å in (I), and 2.705 (4) and 2.813 (4) in (II). The V···V distance in the dimers is almost identical: 7.846 (1) Å in (I) and 7.850 (2) Å in (II). In both cases, the N—O bond for the non-hydrogen-bonded O atom is the shortest: 1.240 (2) Å in (I) and 1.243 (4) Å in (II), compared with 1.260 (2) and 1.263 (2) Å for the remaining two N—O bonds in (I), and 1.254 (4) and 1.258 (4) Å for the remaining two N—O bonds in (II).

Packing diagrams have been deposited as Fig. 2 and Fig. 3. In the triclinic form, (I), the dimers pack so that the salen groups are parallel to each other, whereas in the monoclinic form, (II), there is a herring-bone arrangement, with an angle of 50° between the planes through the salen ligands. The monoclinic form, (II), is the denser, with ρ = 1.609, cf. 1.582 for (I).

Related literature top

For related literature, see: Banci et al. (1984); Bonadies et al. (1987); Nakajima et al. (1990).

Experimental top

(NH4)2Ce(NO3)6 (2.0 g, 3.6 mmol) in acetonitrile (180 ml) was added to VIVO(salen) (1.0 g, 3 mmol) in acetonitrile (90 ml). The volume was reduced to 90 ml by means of a rotary evaporator. The crude product was filtered and then dissolved in 1.5 M nitric acid (90 ml), from which dark violet crystals of the two polymorphs, (I) and (II), were obtained after 24 h (yield 0.7 g, 1.7 mmol). IR spectra (KBr): ν(VO) 965, 972 cm-1.

Refinement top

The H atoms of the water molecules were obtained from a difference map. For (I), these coordinates and an isotropic displacement parameter were refined; for (II), the H-atom coordinates were kept fixed at the observed positions. For both structures, the H atoms of the ligand were constrained to have C—H = 0.95 Å and Uiso = 1.2Ueq of the parent atom. The weighting scheme employed was w = 1/[σcs(F)]2, where = σcs(F) = [σcs(F2) + 1.03 F2]1/2 - |F|, i.e σcs(F) = σcs(F2)/2 F for large F and small σcs(F2), and σcs(F) = [σcs(F2)]1/2 for small F2.

Computing details top

For both compounds, data collection: SMART (Siemens, 1995); cell refinement: SAINT (Siemens, 1995); data reduction: SAINT; program(s) used to solve structure: SIR97 (Altomare et al., 1997) and KRYSTAL (Hazell, 1995); program(s) used to refine structure: modified ORFLS (Busing et al., 1962) and KRYSTAL; molecular graphics: ORTEPIII (Burnett & Johnson, 1996) and KRYSTAL; software used to prepare material for publication: KRYSTAL.

Figures top
[Figure 1]
[Figure 2]
Fig. 1(a). The molecular view of the [VVO(salen)(H2O)]2(NO3)2 dimer in (I) showing the atom-labelling scheme. Displacement ellipsoids are shown at the 50% probability level and H atoms of the water molecules are shown as small circles of arbitrary radius; other H atoms have been omitted for clarity [symmetry code: (i) 1 - x, -y, 1 - z].

Fig. 1(b). The molecular view of the [VVO(salen)(H2O]2(NO3)2 dimer in (II) showing the atom-labelling scheme. Displacement ellipsoids are shown at the 50% probability level and H atoms of the water molecules are shown as small circles of arbitrary radius; other H atoms have been omitted for clarity [symmetry code: (ii) 3/2 - x, 1/2 - y, -z].

# Figures 2 and 3 are to be deposited in the revised 1035rev1.cif version.

# Fig. 2. Packing diagram for the triclinic form I.

# Fig. 3. Packing diagram for the monoclinic form II.
(I) aqua[bis(salicylidene)ethylenediaminato-O,N,N',O']oxovanadium(V) nitrate top
Crystal data top
[VO(C16H14N2O2)(H2O)]·NO3Z = 2
Mr = 413.28F(000) = 424
Triclinic, P1Dx = 1.582 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 8.663 (2) ÅCell parameters from 4080 reflections
b = 8.956 (2) Åθ = 2.7–29.8°
c = 13.293 (3) ŵ = 0.62 mm1
α = 73.029 (3)°T = 120 K
β = 83.852 (4)°Plate, dark violet
γ = 61.662 (3)°0.40 × 0.23 × 0.10 mm
V = 867.7 (3) Å3
Data collection top
Siemens SMART CCD
diffractometer
4960 independent reflections
Radiation source: X-ray tube3763 reflections with I > 3σ(I)
Graphite monochromatorRint = 0.082
ω rotation scansθmax = 29.8°, θmin = 2.7°
Absorption correction: integration
(XPREP; Siemens, 1995)
h = 1111
Tmin = 0.765, Tmax = 0.943k = 1212
16803 measured reflectionsl = 1819
Refinement top
Refinement on F20 restraints
Least-squares matrix: full0 constraints
R[F2 > 2σ(F2)] = 0.033H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.042Weighting scheme based on measured s.u.'s
S = 1.33(Δ/σ)max < 0.001
3763 reflectionsΔρmax = 0.49 (7) e Å3
252 parametersΔρmin = 0.52 (7) e Å3
Crystal data top
[VO(C16H14N2O2)(H2O)]·NO3γ = 61.662 (3)°
Mr = 413.28V = 867.7 (3) Å3
Triclinic, P1Z = 2
a = 8.663 (2) ÅMo Kα radiation
b = 8.956 (2) ŵ = 0.62 mm1
c = 13.293 (3) ÅT = 120 K
α = 73.029 (3)°0.40 × 0.23 × 0.10 mm
β = 83.852 (4)°
Data collection top
Siemens SMART CCD
diffractometer
4960 independent reflections
Absorption correction: integration
(XPREP; Siemens, 1995)
3763 reflections with I > 3σ(I)
Tmin = 0.765, Tmax = 0.943Rint = 0.082
16803 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0330 restraints
wR(F2) = 0.042H atoms treated by a mixture of independent and constrained refinement
S = 1.33Δρmax = 0.49 (7) e Å3
3763 reflectionsΔρmin = 0.52 (7) e Å3
252 parameters
Special details top

Refinement. Sfls: F calc weight full matrix

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
V0.36830 (4)0.30276 (4)0.21034 (2)0.0165 (2)
O10.3522 (2)0.1617 (2)0.1415 (1)0.0235 (9)
O20.5850 (2)0.2938 (2)0.1859 (1)0.0200 (9)
O30.2470 (2)0.4954 (2)0.1367 (1)0.0241 (9)
O40.5271 (2)0.0478 (2)0.3332 (1)0.0227 (9)
O50.5994 (2)0.1776 (2)0.5547 (1)0.0264 (10)
O60.7903 (2)0.2631 (2)0.4827 (1)0.0346 (12)
O70.7816 (2)0.0478 (2)0.4440 (1)0.0329 (11)
N10.1604 (2)0.2805 (2)0.2995 (1)0.0190 (10)
N20.3586 (2)0.4078 (2)0.3338 (1)0.0171 (10)
N30.7249 (2)0.1628 (2)0.4940 (1)0.0205 (10)
C10.2618 (2)0.0723 (2)0.1466 (1)0.0179 (11)
C20.2916 (2)0.0217 (2)0.0724 (1)0.0205 (12)
C30.2012 (2)0.1169 (2)0.0784 (1)0.0249 (13)
C40.0813 (3)0.1199 (2)0.1567 (2)0.0286 (14)
C50.0482 (2)0.0243 (2)0.2287 (2)0.0253 (13)
C60.1384 (2)0.0734 (2)0.2243 (1)0.0190 (11)
C70.0915 (2)0.1812 (2)0.2966 (1)0.0198 (12)
C80.0885 (2)0.3925 (2)0.3731 (1)0.0237 (13)
C90.2454 (2)0.3836 (2)0.4211 (1)0.0213 (12)
C100.4340 (2)0.5033 (2)0.3317 (1)0.0174 (11)
C110.5546 (2)0.5277 (2)0.2528 (1)0.0168 (11)
C120.6081 (2)0.6554 (2)0.2495 (1)0.0196 (12)
C130.7261 (2)0.6808 (2)0.1771 (1)0.0224 (12)
C140.7979 (2)0.5750 (2)0.1078 (1)0.0226 (12)
C150.7517 (2)0.4446 (2)0.1108 (1)0.0208 (12)
C160.6282 (2)0.4219 (2)0.1819 (1)0.0170 (11)
HO4a0.608 (3)0.044 (3)0.372 (2)0.032 (6)*
HO4b0.490 (4)0.010 (3)0.372 (2)0.055 (8)*
H20.37280.02010.01860.0245*
H30.22150.18100.02850.0299*
H40.02210.18750.16060.0343*
H50.03540.02460.28120.0304*
H70.00380.17870.34550.0238*
H8a0.02660.34860.42650.0284*
H8b0.01180.51070.33610.0284*
H9a0.20740.47470.45490.0255*
H9b0.30740.27230.47080.0255*
H100.40840.56120.38550.0209*
H120.56210.72500.29780.0235*
H130.75830.76960.17430.0269*
H140.87940.59230.05810.0271*
H150.80370.37140.06470.0250*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
V0.0199 (2)0.0205 (2)0.0165 (1)0.0144 (1)0.0041 (1)0.0079 (1)
O10.0295 (7)0.0323 (7)0.0249 (6)0.0245 (6)0.0097 (5)0.0157 (5)
O20.0233 (7)0.0221 (6)0.0231 (6)0.0164 (5)0.0065 (5)0.0098 (5)
O30.0298 (7)0.0255 (7)0.0200 (6)0.0148 (6)0.0003 (5)0.0066 (5)
O40.0258 (7)0.0217 (7)0.0263 (7)0.0164 (6)0.0026 (6)0.0053 (5)
O50.0274 (7)0.0313 (7)0.0276 (7)0.0208 (6)0.0118 (6)0.0093 (6)
O60.0347 (8)0.0397 (8)0.0463 (9)0.0301 (7)0.0136 (7)0.0170 (7)
O70.0281 (8)0.0387 (8)0.0393 (8)0.0144 (7)0.0051 (6)0.0245 (7)
N10.0180 (7)0.0221 (7)0.0207 (7)0.0109 (6)0.0023 (6)0.0090 (6)
N20.0171 (7)0.0207 (7)0.0165 (7)0.0113 (6)0.0024 (5)0.0055 (5)
N30.0207 (8)0.0240 (8)0.0194 (7)0.0129 (6)0.0004 (6)0.0048 (6)
C10.0198 (9)0.0175 (8)0.0199 (8)0.0118 (7)0.0031 (7)0.0030 (6)
C20.0211 (9)0.0214 (8)0.0223 (8)0.0121 (7)0.0004 (7)0.0064 (7)
C30.0266 (10)0.0227 (9)0.0316 (10)0.0137 (8)0.0015 (8)0.0113 (8)
C40.0256 (10)0.0271 (10)0.0445 (12)0.0189 (8)0.0027 (8)0.0144 (9)
C50.0210 (9)0.0247 (9)0.0361 (10)0.0153 (8)0.0053 (8)0.0098 (8)
C60.0171 (8)0.0175 (8)0.0244 (9)0.0095 (7)0.0013 (7)0.0052 (7)
C70.0169 (9)0.0224 (8)0.0228 (8)0.0114 (7)0.0014 (7)0.0062 (7)
C80.0212 (9)0.0305 (10)0.0279 (9)0.0153 (8)0.0082 (7)0.0167 (8)
C90.0246 (9)0.0287 (9)0.0193 (8)0.0182 (8)0.0068 (7)0.0107 (7)
C100.0183 (8)0.0182 (8)0.0186 (8)0.0097 (7)0.0003 (6)0.0066 (6)
C110.0167 (8)0.0177 (8)0.0183 (8)0.0100 (7)0.0005 (6)0.0042 (6)
C120.0205 (9)0.0203 (8)0.0222 (8)0.0119 (7)0.0009 (7)0.0069 (7)
C130.0234 (9)0.0224 (9)0.0262 (9)0.0157 (8)0.0021 (7)0.0032 (7)
C140.0219 (9)0.0286 (9)0.0218 (9)0.0176 (8)0.0026 (7)0.0036 (7)
C150.0219 (9)0.0245 (9)0.0198 (8)0.0139 (8)0.0026 (7)0.0066 (7)
C160.0181 (8)0.0175 (8)0.0186 (8)0.0116 (7)0.0006 (6)0.0031 (6)
Geometric parameters (Å, º) top
V—O11.823 (2)C10—C111.445 (2)
V—O21.838 (2)C11—C121.412 (2)
V—O31.598 (2)C11—C161.418 (2)
V—O42.257 (2)C12—C131.380 (3)
V—N12.106 (2)C13—C141.400 (3)
V—N22.093 (2)C14—C151.393 (2)
O1—C11.345 (2)C15—C161.399 (2)
O2—C161.352 (2)O4—HO4b0.78 (3)
O5—N31.260 (2)O4—HO4a0.89 (2)
O6—N31.240 (2)C2—H20.950
O7—N31.263 (2)C3—H30.950
N1—C71.295 (2)C4—H40.950
N1—C81.483 (2)C5—H50.950
N2—C101.293 (2)C7—H70.950
N2—C91.472 (2)C8—H8a0.950
C1—C61.404 (2)C8—H8b0.950
C1—C21.404 (2)C9—H9a0.950
C2—C31.388 (2)C9—H9b0.950
C3—C41.393 (3)C10—H100.950
C4—C51.385 (3)C12—H120.950
C5—C61.410 (2)C13—H130.950
C6—C71.451 (2)C14—H140.950
C8—C91.521 (3)C15—H150.950
O1—V—O2107.77 (5)C12—C11—C16118.7 (2)
O1—V—O3101.94 (6)C10—C11—C12118.9 (1)
O1—V—O484.82 (6)C10—C11—C16122.4 (1)
O1—V—N185.70 (5)C11—C12—C13121.0 (2)
O1—V—N2159.04 (6)C12—C13—C14119.6 (2)
O2—V—O3100.15 (6)C13—C14—C15120.9 (2)
O2—V—O481.57 (5)C14—C15—C16119.7 (2)
O2—V—N1157.18 (6)O2—C16—C15119.7 (1)
O2—V—N285.82 (5)O2—C16—C11120.1 (1)
O3—V—O4172.02 (6)C11—C16—C15120.1 (1)
O3—V—N194.73 (6)HO4a—O4—HO4b104 (2)
O3—V—N290.90 (6)C3—C2—H2120.3
O4—V—N181.43 (6)C1—C2—H2120.3
O4—V—N281.43 (5)C2—C3—H3119.5
N1—V—N276.69 (5)C4—C3—H3119.5
V—O1—C1138.8 (1)C5—C4—H4120.0
V—O2—C16127.3 (1)C3—C4—H4120.0
V—O4—HO4b126 (2)C4—C5—H5120.0
V—O4—HO4a118 (1)C6—C5—H5120.0
V—N1—C7127.2 (1)N1—C7—H7117.6
V—N1—C8114.7 (1)C6—C7—H7117.6
V—N2—C9116.8 (1)H8a—C8—H8b109.5
V—N2—C10123.1 (1)N1—C8—H8a110.3
C7—N1—C8118.1 (1)C9—C8—H8a110.3
C9—N2—C10119.8 (1)N1—C8—H8b110.3
O5—N3—O6119.7 (1)C9—C8—H8b110.3
O6—N3—O7120.4 (2)H9a—C9—H9b109.5
O5—N3—O7119.9 (1)N2—C9—H9a110.2
O1—C1—C6120.8 (1)C8—C9—H9a110.2
O1—C1—C2119.1 (2)N2—C9—H9b110.2
C2—C1—C6120.1 (1)C8—C9—H9b110.2
C1—C2—C3119.4 (2)N2—C10—H10117.9
C2—C3—C4121.0 (2)C11—C10—H10117.9
C3—C4—C5120.1 (2)C13—C12—H12119.5
C4—C5—C6120.1 (2)C11—C12—H12119.5
C1—C6—C5119.4 (2)C12—C13—H13120.2
C1—C6—C7122.1 (1)C14—C13—H13120.2
C5—C6—C7118.4 (2)C15—C14—H14119.5
N1—C7—C6124.9 (2)C13—C14—H14119.5
N1—C8—C9106.3 (1)C14—C15—H15120.2
N2—C9—C8106.6 (1)C16—C15—H15120.2
N2—C10—C11124.2 (1)
(II) aqua[bis(salicylidene)ethylenediaminato-O,N,N',O']oxovanadium(V) nitrate top
Crystal data top
[VO(C16H14N2O2)(H2O)]·NO3F(000) = 1696
Mr = 413.28Dx = 1.609 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 2493 reflections
a = 16.413 (2) Åθ = 1.6–29.8°
b = 8.1634 (8) ŵ = 0.63 mm1
c = 25.628 (3) ÅT = 120 K
β = 96.619 (2)°Plate, dark violet
V = 3411.1 (6) Å30.41 × 0.19 × 0.12 mm
Z = 8
Data collection top
Siemens SMART CCD
diffractometer
4831 independent reflections
Radiation source: X-ray tube2461 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.135
ω rotation scansθmax = 29.8°, θmin = 1.6°
Absorption correction: integration
(XPREP; Siemens, 1995)
h = 2222
Tmin = 0.820, Tmax = 0.992k = 1111
19982 measured reflectionsl = 3535
Refinement top
Refinement on F0 restraints
Least-squares matrix: full0 constraints
R[F2 > 2σ(F2)] = 0.050H-atom parameters constrained
wR(F2) = 0.047Weighting scheme based on measured s.u.'s
S = 1.06(Δ/σ)max < 0.001
2461 reflectionsΔρmax = 0.33 (5) e Å3
244 parametersΔρmin = 0.39 (5) e Å3
Crystal data top
[VO(C16H14N2O2)(H2O)]·NO3V = 3411.1 (6) Å3
Mr = 413.28Z = 8
Monoclinic, C2/cMo Kα radiation
a = 16.413 (2) ŵ = 0.63 mm1
b = 8.1634 (8) ÅT = 120 K
c = 25.628 (3) Å0.41 × 0.19 × 0.12 mm
β = 96.619 (2)°
Data collection top
Siemens SMART CCD
diffractometer
4831 independent reflections
Absorption correction: integration
(XPREP; Siemens, 1995)
2461 reflections with I > 2σ(I)
Tmin = 0.820, Tmax = 0.992Rint = 0.135
19982 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0500 restraints
wR(F2) = 0.047H-atom parameters constrained
S = 1.06Δρmax = 0.33 (5) e Å3
2461 reflectionsΔρmin = 0.39 (5) e Å3
244 parameters
Special details top

Refinement. Sfls: F calc weight full matrix

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
V0.70238 (4)0.20354 (8)0.14587 (3)0.0163 (3)
O10.7245 (1)0.4190 (3)0.1623 (1)0.019 (1)
O20.7920 (2)0.0862 (3)0.1702 (1)0.022 (2)
O30.6407 (2)0.1654 (3)0.1877 (1)0.021 (1)
O40.7752 (2)0.2674 (3)0.0804 (1)0.022 (2)
O50.7142 (2)0.5151 (3)0.0102 (1)0.027 (2)
O60.5994 (2)0.6487 (3)0.0030 (1)0.031 (2)
O70.6124 (2)0.4360 (3)0.0459 (1)0.024 (2)
N10.6079 (2)0.2906 (4)0.0929 (1)0.017 (2)
N20.6707 (2)0.0000 (3)0.0984 (1)0.016 (2)
N30.6419 (2)0.5339 (4)0.0108 (1)0.020 (2)
C10.6694 (2)0.5335 (4)0.1716 (1)0.016 (2)
C20.6924 (2)0.6554 (4)0.2088 (1)0.020 (2)
C30.6375 (2)0.7748 (4)0.2178 (1)0.022 (2)
C40.5600 (2)0.7823 (5)0.1898 (1)0.024 (2)
C50.5376 (2)0.6658 (4)0.1519 (1)0.019 (2)
C60.5919 (2)0.5389 (4)0.1425 (1)0.017 (2)
C70.5677 (2)0.4228 (4)0.1004 (1)0.018 (2)
C80.5802 (2)0.1849 (5)0.0478 (1)0.021 (2)
C90.5899 (2)0.0122 (5)0.0673 (1)0.023 (2)
C100.7154 (2)0.1270 (4)0.0919 (1)0.019 (2)
C110.7933 (2)0.1611 (4)0.1211 (1)0.016 (2)
C120.8329 (2)0.3081 (5)0.1123 (1)0.023 (2)
C130.9043 (3)0.3507 (5)0.1425 (2)0.027 (2)
C140.9386 (2)0.2473 (5)0.1821 (2)0.026 (2)
C150.9005 (2)0.1006 (5)0.1914 (1)0.020 (2)
C160.8291 (2)0.0565 (4)0.1609 (1)0.017 (2)
HO4a0.75560.34080.05510.030*
HO4b0.80330.21010.05750.030*
H20.74570.65510.22770.024*
H30.65280.85510.24390.026*
H40.52280.86670.19660.029*
H50.48510.67130.13210.023*
H70.51960.44550.07730.021*
H8a0.61290.20270.02010.025*
H8b0.52440.20670.03570.025*
H9a0.54790.01320.08870.027*
H9b0.58680.06150.03850.027*
H100.69510.20370.06570.023*
H120.81010.37940.08520.028*
H130.93050.45140.13620.033*
H140.98810.27720.20280.031*
H150.92350.03040.21880.024*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
V0.0179 (3)0.0118 (3)0.0182 (3)0.0033 (3)0.0027 (3)0.0012 (3)
O10.017 (1)0.012 (1)0.025 (1)0.001 (1)0.002 (1)0.005 (1)
O20.022 (2)0.017 (1)0.025 (2)0.007 (1)0.007 (1)0.004 (1)
O30.024 (2)0.017 (1)0.020 (1)0.003 (1)0.001 (1)0.000 (1)
O40.030 (2)0.015 (1)0.023 (1)0.006 (1)0.007 (1)0.000 (1)
O50.023 (2)0.029 (2)0.026 (2)0.004 (1)0.006 (1)0.000 (1)
O60.036 (2)0.021 (2)0.037 (2)0.016 (1)0.001 (1)0.011 (1)
O70.024 (2)0.020 (1)0.026 (2)0.003 (1)0.002 (1)0.005 (1)
N10.020 (2)0.014 (2)0.016 (2)0.001 (1)0.000 (1)0.000 (1)
N20.018 (2)0.013 (2)0.017 (2)0.001 (1)0.002 (1)0.001 (1)
N30.025 (2)0.018 (2)0.017 (2)0.001 (2)0.002 (1)0.004 (1)
C10.021 (2)0.010 (2)0.019 (2)0.001 (2)0.007 (2)0.004 (2)
C20.024 (2)0.017 (2)0.018 (2)0.001 (2)0.001 (2)0.001 (2)
C30.033 (2)0.011 (2)0.021 (2)0.002 (2)0.006 (2)0.002 (2)
C40.035 (2)0.014 (2)0.025 (2)0.008 (2)0.009 (2)0.004 (2)
C50.019 (2)0.013 (2)0.025 (2)0.003 (2)0.003 (2)0.004 (2)
C60.022 (2)0.009 (2)0.019 (2)0.001 (2)0.004 (2)0.001 (2)
C70.015 (2)0.018 (2)0.019 (2)0.001 (2)0.001 (2)0.004 (2)
C80.026 (2)0.018 (2)0.017 (2)0.004 (2)0.006 (2)0.003 (2)
C90.022 (2)0.019 (2)0.025 (2)0.003 (2)0.004 (2)0.004 (2)
C100.025 (2)0.015 (2)0.018 (2)0.004 (2)0.003 (2)0.003 (2)
C110.015 (2)0.014 (2)0.019 (2)0.000 (1)0.005 (2)0.004 (2)
C120.025 (2)0.016 (2)0.027 (2)0.001 (2)0.001 (2)0.002 (2)
C130.026 (2)0.019 (2)0.037 (3)0.011 (2)0.005 (2)0.002 (2)
C140.021 (2)0.022 (2)0.034 (2)0.009 (2)0.003 (2)0.006 (2)
C150.018 (2)0.023 (2)0.020 (2)0.001 (2)0.001 (2)0.002 (2)
C160.019 (2)0.013 (2)0.020 (2)0.002 (2)0.006 (2)0.004 (2)
Geometric parameters (Å, º) top
V—O11.835 (3)C10—C111.432 (5)
V—O21.805 (3)C11—C121.395 (5)
V—O31.588 (3)C11—C161.406 (5)
V—O42.230 (3)C12—C131.373 (5)
V—N12.066 (3)C13—C141.388 (6)
V—N22.089 (3)C14—C151.385 (5)
O1—C11.341 (4)C15—C161.379 (5)
O2—C161.349 (4)O4—HO4a0.914
O5—N31.254 (4)O4—HO4b0.915
O6—N31.243 (4)C2—H20.950
O7—N31.258 (4)C3—H30.950
N1—C71.291 (5)C4—H40.950
N1—C81.471 (4)C5—H50.950
N2—C101.292 (4)C7—H70.950
N2—C91.470 (5)C8—H8b0.950
C1—C21.400 (5)C8—H8a0.950
C1—C61.401 (5)C9—H9b0.950
C2—C31.363 (5)C9—H9a0.950
C3—C41.389 (5)C10—H100.950
C4—C51.378 (5)C12—H120.950
C5—C61.405 (5)C13—H130.950
C6—C71.455 (5)C14—H140.950
C8—C91.498 (5)C15—H150.950
O1—V—O2107.3 (1)C12—C11—C16118.4 (3)
O1—V—O399.0 (1)C10—C11—C12119.1 (3)
O1—V—O480.8 (1)C10—C11—C16122.4 (3)
O1—V—N186.3 (1)C11—C12—C13120.7 (4)
O1—V—N2157.7 (1)C12—C13—C14120.3 (4)
O2—V—O3102.7 (1)C13—C14—C15120.0 (4)
O2—V—O484.2 (1)C14—C15—C16119.9 (4)
O2—V—N1158.4 (1)O2—C16—C15119.8 (3)
O2—V—N285.3 (1)O2—C16—C11119.5 (3)
O3—V—O4172.8 (1)C11—C16—C15120.7 (3)
O3—V—N191.3 (1)HO4a—O4—HO4b92.4
O3—V—N295.9 (1)C3—C2—H2120.3
O4—V—N181.5 (1)C1—C2—H2120.3
O4—V—N282.3 (1)C2—C3—H3119.0
N1—V—N276.9 (1)C4—C3—H3119.0
V—O1—C1126.2 (2)C5—C4—H4120.4
V—O2—C16139.8 (2)C3—C4—H4120.4
V—O4—HO4a120.8C4—C5—H5119.8
V—O4—HO4b135.7C6—C5—H5119.8
V—N1—C7123.1 (2)N1—C7—H7118.1
V—N1—C8117.1 (2)C6—C7—H7118.1
V—N2—C9114.2 (2)H8a—C8—H8b109.5
V—N2—C10127.3 (3)N1—C8—H8b110.3
C7—N1—C8119.4 (3)C9—C8—H8b110.3
C9—N2—C10118.4 (3)N1—C8—H8a110.3
O5—N3—O6120.3 (3)C9—C8—H8a110.3
O6—N3—O7120.0 (3)H9a—C9—H9b109.5
O5—N3—O7119.8 (3)N2—C9—H9b110.0
O1—C1—C2118.9 (3)C8—C9—H9b110.0
O1—C1—C6121.1 (3)N2—C9—H9a110.0
C2—C1—C6119.9 (3)C8—C9—H9a110.0
C1—C2—C3119.4 (4)N2—C10—H10117.5
C2—C3—C4121.9 (3)C11—C10—H10117.5
C3—C4—C5119.2 (4)C13—C12—H12119.6
C4—C5—C6120.5 (4)C11—C12—H12119.6
C1—C6—C5119.1 (3)C12—C13—H13119.8
C1—C6—C7121.9 (3)C14—C13—H13119.8
C5—C6—C7118.9 (3)C15—C14—H14120.0
N1—C7—C6123.7 (3)C13—C14—H14120.0
N1—C8—C9106.2 (3)C16—C15—H15120.1
N2—C9—C8107.4 (3)C14—C15—H15120.1
N2—C10—C11125.1 (3)

Experimental details

(I)(II)
Crystal data
Chemical formula[VO(C16H14N2O2)(H2O)]·NO3[VO(C16H14N2O2)(H2O)]·NO3
Mr413.28413.28
Crystal system, space groupTriclinic, P1Monoclinic, C2/c
Temperature (K)120120
a, b, c (Å)8.663 (2), 8.956 (2), 13.293 (3)16.413 (2), 8.1634 (8), 25.628 (3)
α, β, γ (°)73.029 (3), 83.852 (4), 61.662 (3)90, 96.619 (2), 90
V3)867.7 (3)3411.1 (6)
Z28
Radiation typeMo KαMo Kα
µ (mm1)0.620.63
Crystal size (mm)0.40 × 0.23 × 0.100.41 × 0.19 × 0.12
Data collection
DiffractometerSiemens SMART CCD
diffractometer
Siemens SMART CCD
diffractometer
Absorption correctionIntegration
(XPREP; Siemens, 1995)
Integration
(XPREP; Siemens, 1995)
Tmin, Tmax0.765, 0.9430.820, 0.992
No. of measured, independent and
observed reflections
16803, 4960, 3763 [I > 3σ(I)]19982, 4831, 2461 [I > 2σ(I)]
Rint0.0820.135
(sin θ/λ)max1)0.6990.699
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.033, 0.042, 1.33 0.050, 0.047, 1.06
No. of reflections37632461
No. of parameters252244
H-atom treatmentH atoms treated by a mixture of independent and constrained refinementH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.49 (7), 0.52 (7)0.33 (5), 0.39 (5)

Computer programs: SMART (Siemens, 1995), SAINT (Siemens, 1995), SAINT, SIR97 (Altomare et al., 1997) and KRYSTAL (Hazell, 1995), modified ORFLS (Busing et al., 1962) and KRYSTAL, ORTEPIII (Burnett & Johnson, 1996) and KRYSTAL, KRYSTAL.

Selected geometric parameters (Å, º) for (I) top
V—O11.823 (2)V—O42.257 (2)
V—O21.838 (2)V—N12.106 (2)
V—O31.598 (2)V—N22.093 (2)
O1—V—N2159.04 (6)O3—V—O4172.02 (6)
O2—V—N1157.18 (6)
Selected geometric parameters (Å, º) for (II) top
V—O11.835 (3)V—O42.230 (3)
V—O21.805 (3)V—N12.066 (3)
V—O31.588 (3)V—N22.089 (3)
O1—V—N2157.7 (1)O3—V—O4172.8 (1)
O2—V—N1158.4 (1)
 

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