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

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Bis(μ-methano­lato-κ2O:O)bis­­{[4-bromo-N′-(1-methyl-3-oxidobut-2-en-1-yl­­idene-κO)benzohydrazidato-κ2N′,O]oxido­vanadium(V)}

aDepartment of Chemistry, University of Malaya, 50603 Kuala Lumpur, Malaysia
*Correspondence e-mail: seikweng@um.edu.my

(Received 30 May 2011; accepted 5 June 2011; online 11 June 2011)

The dinuclear compound, [V2(C12H11BrN2O2)2(CH3O)2O2], lies on a center of inversion. The doubly-deprotonated Schiff base O,N,O′-chelates to the VV atom; two metal atoms are bridged by the methoxide units. The coordination geometry is a distorted octa­hedron. Weak inter­molecular C—H⋯N hydrogen bonding is present in the crystal structure. The bromo­phenyl unit is disordered over two positions, with the major component being in a 0.909 (6) proportion.

Related literature

For the isotypic compound that has chlorine in place of bromine, see: Sarkar & Pal (2009[Sarkar, A. & Pal, S. (2009). Inorg. Chim. Acta, 362, 3807-3812.]).

[Scheme 1]

Experimental

Crystal data
  • [V2(C12H11BrN2O2)2(CH3O)2O2]

  • Mr = 786.22

  • Monoclinic, P 21 /c

  • a = 8.7517 (5) Å

  • b = 12.3409 (7) Å

  • c = 13.9952 (8) Å

  • β = 101.8782 (7)°

  • V = 1479.17 (15) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 3.39 mm−1

  • T = 100 K

  • 0.30 × 0.25 × 0.20 mm

Data collection
  • Bruker SMART APEX diffractometer

  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996[Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.]) Tmin = 0.430, Tmax = 0.551

  • 18572 measured reflections

  • 3400 independent reflections

  • 3106 reflections with I > 2σ(I)

  • Rint = 0.027

Refinement
  • R[F2 > 2σ(F2)] = 0.023

  • wR(F2) = 0.060

  • S = 0.99

  • 3400 reflections

  • 221 parameters

  • 44 restraints

  • H-atom parameters constrained

  • Δρmax = 0.96 e Å−3

  • Δρmin = −0.32 e Å−3

Table 1
Selected bond lengths (Å)

V1—O1 1.9314 (13)
V1—O2 1.8607 (13)
V1—O3 1.5896 (14)
V1—O4 2.3459 (13)
V1—O4i 1.8289 (13)
V1—N2 2.0770 (15)
Symmetry code: (i) -x, -y+1, -z+1.

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
C12—H12C⋯N1ii 0.96 2.59 3.541 (5) 169
Symmetry code: (ii) [x, -y+{\script{3\over 2}}, z+{\script{1\over 2}}].

Data collection: APEX2 (Bruker, 2009[Bruker (2009). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2009[Bruker (2009). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: X-SEED (Barbour, 2001[Barbour, L. J. (2001). J. Supramol. Chem. 1, 189-191.]); software used to prepare material for publication: publCIF (Westrip, 2010[Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.]).

Supporting information


Comment top

A recent study detailed the crystal structure of [VO(C12H11ClN2O2)(CH3O)]2 (Sarkar & Pal, 2009). The title bromo analog (Scheme I) is isostructural, the two compounds crystallizing with matching cell dimensions. However, the title compound shows some disorder in the halophenyl portion (Fig. 1). Dinuclear [VO(C12H11BrN2O2)(CH3O)]2 lies on a center of inversion. The doubly-deprotonated Schiff base O,N,O'-chelates to the VV atom; two metal centers are bridged by the methoxide unit. The geometry is an octahedron.

Related literature top

For the isotypic compound that has chlorine in place of bromine, see: Sarkar & Pal (2009).

Experimental top

Bis(acetylacetonato)oxovanadium (0.67 g, 2.5 mmol) was heated with 4-bromobenzoic acid hydrazide (0.54 g, 2.5 mmol) in methanol (50 ml) for 1 h. The solution mixture was then filtered and upon slow cooling of the filtrate, dark brown crystals separated out.

Refinement top

Carbon-bound H-atoms were placed in calculated positions (C–H 0.95 to 0.98 Å) and were included in the refinement in the riding model approximation, with U(H) set to 1.2–1.5U(C).

The bromophenyl portion of the ligand is disordered over two positions. The pair of carbon–bromine distances were restrained to within ±0.01 Å each other. For the ring, the 1,2-related distances were restrained to 1.39±0.01 Å, the 1,3-related distances to 2.41±0.01 Å and the 1,4-related distances to 2.78±0.01 Å. Each seven-atom component was restrained to near planarity. Owing to the low degree of disordered, additional restraints were imposed on the primed bromine atom as well as the primed para-carbon atom. Distance restraints were applied so that the angle at the carbon atoms was approximately 120°. The isotropic temperature factors of the primed atoms were set to the anisotropic temperature factors of the unprimed ones. The disorder refined to 0.909 (1): 0.091.

Computing details top

Data collection: APEX2 (Bruker, 2009); cell refinement: SAINT (Bruker, 2009); data reduction: SAINT (Bruker, 2009); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2010).

Figures top
[Figure 1] Fig. 1. Thermal ellipsoid plot (Barbour, 2001) of [VO(C12H11BrN2O2)(CH3O)]2 at the 70% probability level; hydrogen atoms are drawn as spheres of arbitrary radius. The disorder in bromophenyl ring is not shown.
Bis(µ-methanolato-κ2O:O)bis{[4-bromo-N'-(1- methyl-3-oxidobut-2-en-1-ylidene-κO)benzohydrazidato- κ2N',O]oxidovanadium(V)} top
Crystal data top
[V2(C12H11BrN2O2)2(CH3O)2O2]F(000) = 784
Mr = 786.22Dx = 1.765 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 8361 reflections
a = 8.7517 (5) Åθ = 2.2–28.2°
b = 12.3409 (7) ŵ = 3.39 mm1
c = 13.9952 (8) ÅT = 100 K
β = 101.8782 (7)°Prism, brown
V = 1479.17 (15) Å30.30 × 0.25 × 0.20 mm
Z = 2
Data collection top
Bruker SMART APEX
diffractometer
3400 independent reflections
Radiation source: fine-focus sealed tube3106 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.027
ω scansθmax = 27.5°, θmin = 2.2°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1111
Tmin = 0.430, Tmax = 0.551k = 1616
18572 measured reflectionsl = 1818
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.023Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.060H-atom parameters constrained
S = 0.99 w = 1/[σ2(Fo2) + (0.0308P)2 + 1.3638P]
where P = (Fo2 + 2Fc2)/3
3400 reflections(Δ/σ)max = 0.001
221 parametersΔρmax = 0.96 e Å3
44 restraintsΔρmin = 0.32 e Å3
Crystal data top
[V2(C12H11BrN2O2)2(CH3O)2O2]V = 1479.17 (15) Å3
Mr = 786.22Z = 2
Monoclinic, P21/cMo Kα radiation
a = 8.7517 (5) ŵ = 3.39 mm1
b = 12.3409 (7) ÅT = 100 K
c = 13.9952 (8) Å0.30 × 0.25 × 0.20 mm
β = 101.8782 (7)°
Data collection top
Bruker SMART APEX
diffractometer
3400 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
3106 reflections with I > 2σ(I)
Tmin = 0.430, Tmax = 0.551Rint = 0.027
18572 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.02344 restraints
wR(F2) = 0.060H-atom parameters constrained
S = 0.99Δρmax = 0.96 e Å3
3400 reflectionsΔρmin = 0.32 e Å3
221 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Br10.53762 (15)0.29274 (14)0.06235 (3)0.0224 (2)0.909 (6)
Br1'0.5773 (11)0.3313 (11)0.0656 (3)0.0164 (15)0.091 (6)
V10.11414 (4)0.60960 (2)0.50419 (2)0.01169 (8)
O10.21661 (15)0.52544 (10)0.41937 (9)0.0152 (3)
O20.04425 (16)0.69868 (10)0.52973 (9)0.0149 (3)
O30.25986 (16)0.67280 (11)0.56588 (10)0.0179 (3)
O40.10415 (15)0.51204 (10)0.42270 (9)0.0126 (2)
N10.15083 (18)0.65573 (13)0.30152 (11)0.0142 (3)
N20.08999 (18)0.70085 (12)0.37726 (11)0.0125 (3)
C10.4474 (2)0.3788 (2)0.14888 (15)0.0186 (5)0.909 (6)
C1'0.4680 (11)0.4032 (11)0.1483 (7)0.019*0.091 (6)
C20.4295 (3)0.3360 (2)0.23695 (18)0.0202 (6)0.909 (6)
H20.46590.26500.25580.024*0.909 (6)
C2'0.455 (3)0.3560 (15)0.2361 (13)0.020*0.091 (6)
H2'0.50140.28750.25440.024*0.091 (6)
C30.3573 (3)0.39817 (19)0.29774 (18)0.0181 (5)0.909 (6)
H30.34480.36970.35870.022*0.909 (6)
C3'0.373 (3)0.4097 (14)0.2974 (13)0.018*0.091 (6)
H3'0.36320.37800.35770.022*0.091 (6)
C40.3030 (2)0.50212 (18)0.26988 (16)0.0154 (4)0.909 (6)
C4'0.3054 (10)0.5095 (9)0.2697 (8)0.015*0.091 (6)
C50.3265 (4)0.5453 (2)0.18142 (19)0.0177 (4)0.909 (6)
H50.29270.61680.16280.021*0.909 (6)
C5'0.319 (3)0.5568 (15)0.1819 (13)0.018*0.091 (6)
H5'0.27280.62540.16350.021*0.091 (6)
C60.3994 (3)0.4833 (2)0.12096 (18)0.0194 (5)0.909 (6)
H60.41610.51220.06100.023*0.909 (6)
C6'0.401 (3)0.5032 (15)0.1208 (13)0.019*0.091 (6)
H6'0.41100.53490.06060.023*0.091 (6)
C70.2196 (2)0.56521 (15)0.33309 (13)0.0136 (3)
C80.0615 (2)0.86357 (16)0.27592 (14)0.0179 (4)
H8A0.16880.85590.26640.027*
H8B0.03860.94040.28390.027*
H8C0.01120.83450.21890.027*
C90.0435 (2)0.80226 (14)0.36548 (13)0.0136 (3)
C100.0241 (2)0.85486 (15)0.43769 (13)0.0149 (4)
H100.04070.93090.43190.018*
C110.0663 (2)0.80336 (14)0.51441 (13)0.0138 (3)
C120.1443 (2)0.85908 (15)0.58647 (13)0.0166 (4)
H12A0.23750.81830.59320.025*
H12B0.17450.93250.56350.025*
H12C0.07180.86290.64990.025*
C130.2359 (2)0.56198 (17)0.36097 (15)0.0209 (4)
H13A0.29890.50650.32090.031*
H13B0.19970.61510.31850.031*
H13C0.29940.59860.40130.031*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Br10.0193 (3)0.0288 (5)0.01969 (13)0.0092 (3)0.00564 (12)0.00508 (14)
Br1'0.0125 (19)0.018 (3)0.0200 (12)0.001 (2)0.0061 (10)0.0048 (12)
V10.01496 (16)0.01018 (15)0.01058 (15)0.00098 (11)0.00417 (11)0.00064 (11)
O10.0180 (6)0.0146 (6)0.0144 (6)0.0015 (5)0.0069 (5)0.0018 (5)
O20.0203 (7)0.0113 (6)0.0148 (6)0.0004 (5)0.0073 (5)0.0003 (5)
O30.0210 (7)0.0173 (7)0.0152 (6)0.0046 (5)0.0033 (5)0.0012 (5)
O40.0145 (6)0.0121 (6)0.0114 (6)0.0006 (5)0.0030 (5)0.0018 (5)
N10.0173 (8)0.0144 (7)0.0119 (7)0.0009 (6)0.0056 (6)0.0015 (6)
N20.0140 (7)0.0128 (7)0.0114 (7)0.0009 (6)0.0045 (6)0.0006 (6)
C10.0122 (9)0.0263 (12)0.0180 (10)0.0034 (8)0.0048 (8)0.0065 (9)
C20.0191 (13)0.0208 (12)0.0203 (10)0.0059 (10)0.0031 (9)0.0011 (9)
C30.0184 (12)0.0198 (11)0.0170 (10)0.0021 (9)0.0058 (8)0.0004 (8)
C40.0132 (9)0.0176 (10)0.0160 (9)0.0016 (8)0.0046 (8)0.0020 (8)
C50.0184 (11)0.0178 (11)0.0180 (10)0.0001 (9)0.0061 (8)0.0006 (8)
C60.0174 (10)0.0263 (13)0.0160 (10)0.0001 (10)0.0067 (8)0.0012 (9)
C70.0131 (8)0.0147 (8)0.0135 (8)0.0036 (7)0.0033 (7)0.0018 (7)
C80.0236 (10)0.0159 (9)0.0150 (9)0.0020 (7)0.0058 (7)0.0037 (7)
C90.0126 (8)0.0149 (9)0.0130 (8)0.0012 (7)0.0016 (7)0.0010 (7)
C100.0189 (9)0.0102 (8)0.0154 (9)0.0004 (7)0.0033 (7)0.0002 (7)
C110.0141 (8)0.0124 (8)0.0142 (8)0.0003 (6)0.0011 (7)0.0023 (7)
C120.0204 (9)0.0155 (9)0.0146 (9)0.0019 (7)0.0053 (7)0.0020 (7)
C130.0184 (9)0.0194 (10)0.0218 (10)0.0005 (7)0.0032 (8)0.0065 (8)
Geometric parameters (Å, º) top
Br1—C11.9002 (19)C3'—H3'0.9500
Br1'—C1'1.870 (8)C4—C51.401 (3)
V1—O11.9314 (13)C4—C71.479 (3)
V1—O21.8607 (13)C4'—C5'1.389 (9)
V1—O31.5896 (14)C4'—C71.448 (8)
V1—O42.3459 (13)C5—C61.389 (3)
V1—O4i1.8289 (13)C5—H50.9500
V1—N22.0770 (15)C5'—C6'1.390 (9)
O1—C71.309 (2)C5'—H5'0.9500
O2—C111.317 (2)C6—H60.9500
O4—C131.430 (2)C6'—H6'0.9500
O4—V1i1.8289 (13)C8—C91.500 (2)
N1—C71.302 (2)C8—H8A0.9800
N1—N21.396 (2)C8—H8B0.9800
N2—C91.316 (2)C8—H8C0.9800
C1—C21.380 (3)C9—C101.428 (3)
C1—C61.387 (3)C10—C111.363 (3)
C1'—C6'1.385 (9)C10—H100.9500
C1'—C2'1.386 (9)C11—C121.496 (2)
C2—C31.391 (3)C12—H12A0.9800
C2—H20.9500C12—H12B0.9800
C2'—C3'1.394 (9)C12—H12C0.9800
C2'—H2'0.9500C13—H13A0.9800
C3—C41.395 (3)C13—H13B0.9800
C3—H30.9500C13—H13C0.9800
C3'—C4'1.387 (9)
O3—V1—O4i102.96 (6)C3'—C4'—C7119.7 (7)
O3—V1—O298.74 (7)C5'—C4'—C7119.6 (7)
O4i—V1—O2104.72 (6)C6—C5—C4119.90 (19)
O3—V1—O1100.11 (7)C6—C5—H5120.1
O4i—V1—O189.10 (6)C4—C5—H5120.1
O2—V1—O1153.42 (6)C4'—C5'—C6'119.5 (6)
O3—V1—N297.33 (6)C4'—C5'—H5'120.2
O4i—V1—N2156.26 (6)C6'—C5'—H5'120.2
O2—V1—N283.99 (6)C1—C6—C5119.38 (19)
O1—V1—N275.18 (6)C1—C6—H6120.3
O3—V1—O4176.30 (6)C5—C6—H6120.3
O4i—V1—O473.91 (6)C1'—C6'—C5'119.7 (6)
O2—V1—O480.35 (5)C1'—C6'—H6'120.1
O1—V1—O481.95 (5)C5'—C6'—H6'120.1
N2—V1—O486.17 (5)N1—C7—O1122.62 (16)
C7—O1—V1117.75 (12)N1—C7—C4'117.5 (5)
C11—O2—V1129.67 (12)O1—C7—C4'119.9 (5)
C13—O4—V1i124.48 (12)N1—C7—C4119.95 (17)
C13—O4—V1123.17 (11)O1—C7—C4117.43 (17)
V1i—O4—V1106.09 (6)C9—C8—H8A109.5
C7—N1—N2107.84 (14)C9—C8—H8B109.5
C9—N2—N1116.14 (15)H8A—C8—H8B109.5
C9—N2—V1126.68 (12)C9—C8—H8C109.5
N1—N2—V1116.45 (11)H8A—C8—H8C109.5
C2—C1—C6121.62 (19)H8B—C8—H8C109.5
C2—C1—Br1119.58 (16)N2—C9—C10120.41 (16)
C6—C1—Br1118.79 (16)N2—C9—C8120.12 (17)
C6'—C1'—C2'120.9 (6)C10—C9—C8119.48 (16)
C6'—C1'—Br1'119.5 (6)C11—C10—C9124.39 (17)
C2'—C1'—Br1'119.7 (6)C11—C10—H10117.8
C1—C2—C3118.99 (19)C9—C10—H10117.8
C1—C2—H2120.5O2—C11—C10122.07 (17)
C3—C2—H2120.5O2—C11—C12114.39 (16)
C1'—C2'—C3'119.5 (6)C10—C11—C12123.52 (17)
C1'—C2'—H2'120.3C11—C12—H12A109.5
C3'—C2'—H2'120.3C11—C12—H12B109.5
C2—C3—C4120.53 (19)H12A—C12—H12B109.5
C2—C3—H3119.7C11—C12—H12C109.5
C4—C3—H3119.7H12A—C12—H12C109.5
C4'—C3'—C2'119.6 (6)H12B—C12—H12C109.5
C4'—C3'—H3'120.2O4—C13—H13A109.5
C2'—C3'—H3'120.2O4—C13—H13B109.5
C3—C4—C5119.52 (18)H13A—C13—H13B109.5
C3—C4—C7119.89 (19)O4—C13—H13C109.5
C5—C4—C7120.59 (19)H13A—C13—H13C109.5
C3'—C4'—C5'120.7 (6)H13B—C13—H13C109.5
O3—V1—O1—C794.55 (13)C2'—C3'—C4'—C7179.7 (4)
O4i—V1—O1—C7162.44 (13)C3—C4—C5—C61.9 (3)
O2—V1—O1—C740.0 (2)C7—C4—C5—C6177.37 (19)
N2—V1—O1—C70.43 (12)C3'—C4'—C5'—C6'0.2 (9)
O4—V1—O1—C788.57 (13)C7—C4'—C5'—C6'179.8 (6)
O3—V1—O2—C1156.92 (16)C2—C1—C6—C52.2 (3)
O4i—V1—O2—C11162.88 (15)Br1—C1—C6—C5176.95 (15)
O1—V1—O2—C1177.8 (2)C4—C5—C6—C10.3 (3)
N2—V1—O2—C1139.60 (16)C2'—C1'—C6'—C5'0.2 (7)
O4—V1—O2—C11126.72 (16)Br1'—C1'—C6'—C5'179.7 (5)
O4i—V1—O4—C13153.18 (16)C4'—C5'—C6'—C1'0.0 (9)
O2—V1—O4—C1344.67 (14)N2—N1—C7—O14.5 (2)
O1—V1—O4—C13115.43 (14)N2—N1—C7—C4'173.8 (4)
N2—V1—O4—C1339.87 (14)N2—N1—C7—C4176.61 (16)
O4i—V1—O4—V1i0.0V1—O1—C7—N13.1 (2)
O2—V1—O4—V1i108.51 (7)V1—O1—C7—C4'175.2 (4)
O1—V1—O4—V1i91.39 (6)V1—O1—C7—C4177.94 (13)
N2—V1—O4—V1i166.95 (7)C3'—C4'—C7—N1176.1 (15)
C7—N1—N2—C9167.03 (16)C5'—C4'—C7—N13.8 (16)
C7—N1—N2—V13.84 (18)C3'—C4'—C7—O15.5 (16)
O3—V1—N2—C969.23 (16)C5'—C4'—C7—O1174.6 (15)
O4i—V1—N2—C9142.13 (16)C3'—C4'—C7—C440 (8)
O2—V1—N2—C928.85 (16)C5'—C4'—C7—C4140 (8)
O1—V1—N2—C9167.80 (16)C3—C4—C7—N1170.83 (19)
O4—V1—N2—C9109.53 (15)C5—C4—C7—N18.4 (3)
O3—V1—N2—N1100.55 (13)C3—C4—C7—O18.1 (3)
O4i—V1—N2—N148.1 (2)C5—C4—C7—O1172.6 (2)
O2—V1—N2—N1161.38 (13)C3—C4—C7—C4'144 (8)
O1—V1—N2—N11.97 (11)C5—C4—C7—C4'37 (8)
O4—V1—N2—N180.70 (12)N1—N2—C9—C10178.40 (16)
C6—C1—C2—C31.91 (17)V1—N2—C9—C1011.8 (3)
Br1—C1—C2—C3177.28 (11)N1—N2—C9—C81.7 (2)
C6'—C1'—C2'—C3'0.2 (3)V1—N2—C9—C8168.13 (13)
Br1'—C1'—C2'—C3'179.8 (2)N2—C9—C10—C119.9 (3)
C1—C2—C3—C40.34 (15)C8—C9—C10—C11170.21 (18)
C1'—C2'—C3'—C4'0.0 (3)V1—O2—C11—C1032.7 (3)
C2—C3—C4—C52.2 (2)V1—O2—C11—C12148.61 (13)
C2—C3—C4—C7177.03 (14)C9—C10—C11—O21.7 (3)
C2'—C3'—C4'—C5'0.2 (7)C9—C10—C11—C12176.86 (18)
Symmetry code: (i) x, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C12—H12C···N1ii0.962.593.541 (5)169
Symmetry code: (ii) x, y+3/2, z+1/2.

Experimental details

Crystal data
Chemical formula[V2(C12H11BrN2O2)2(CH3O)2O2]
Mr786.22
Crystal system, space groupMonoclinic, P21/c
Temperature (K)100
a, b, c (Å)8.7517 (5), 12.3409 (7), 13.9952 (8)
β (°) 101.8782 (7)
V3)1479.17 (15)
Z2
Radiation typeMo Kα
µ (mm1)3.39
Crystal size (mm)0.30 × 0.25 × 0.20
Data collection
DiffractometerBruker SMART APEX
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.430, 0.551
No. of measured, independent and
observed [I > 2σ(I)] reflections
18572, 3400, 3106
Rint0.027
(sin θ/λ)max1)0.649
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.023, 0.060, 0.99
No. of reflections3400
No. of parameters221
No. of restraints44
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.96, 0.32

Computer programs: APEX2 (Bruker, 2009), SAINT (Bruker, 2009), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), X-SEED (Barbour, 2001), publCIF (Westrip, 2010).

Selected bond lengths (Å) top
V1—O11.9314 (13)V1—O42.3459 (13)
V1—O21.8607 (13)V1—O4i1.8289 (13)
V1—O31.5896 (14)V1—N22.0770 (15)
Symmetry code: (i) x, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C12—H12C···N1ii0.962.593.541 (5)169
Symmetry code: (ii) x, y+3/2, z+1/2.
 

Acknowledgements

We thank the University of Malaya (RG020/09AFR) for supporting this study.

References

First citationBarbour, L. J. (2001). J. Supramol. Chem. 1, 189–191.  CrossRef CAS Google Scholar
First citationBruker (2009). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.  Google Scholar
First citationSarkar, A. & Pal, S. (2009). Inorg. Chim. Acta, 362, 3807–3812.  Web of Science CSD CrossRef CAS Google Scholar
First citationSheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.  Google Scholar
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals Google Scholar
First citationWestrip, S. P. (2010). J. Appl. Cryst. 43, 920–925.  Web of Science CrossRef CAS IUCr Journals Google Scholar

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