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The VV atom of the title complex, [VOL(CH3O)] [L is 3-methoxy­salicyl­aldehyde (4-methoxy­benzoyl)­hydrazon­ate(2−), C16H14N2O4], has a square pyramidal O4N configuration, with two O atoms and one N atom from the tridentate hydrazone ligand and one O atom from the methoxy group forming the basal plane. The oxo atom is located at the apical position. A layer structure is formed by π–π stacking interactions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804010323/bt6444sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804010323/bt6444Isup2.hkl
Contains datablock I

CCDC reference: 242036

Key indicators

  • Single-crystal X-ray study
  • T = 296 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.036
  • wR factor = 0.093
  • Data-to-parameter ratio = 16.6

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT241_ALERT_2_B Check High U(eq) as Compared to Neighbors .... O4
Alert level C STRVA01_ALERT_4_C Flack test results are ambiguous. From the CIF: _refine_ls_abs_structure_Flack 0.490 From the CIF: _refine_ls_abs_structure_Flack_su 0.020 PLAT033_ALERT_2_C Flack Parameter Value Deviates from Zero ....... 0.49 PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) V1 - O1 .. 5.44 su PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.02
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 27.50 From the CIF: _reflns_number_total 3957 Count of symmetry unique reflns 2314 Completeness (_total/calc) 171.00% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 1643 Fraction of Friedel pairs measured 0.710 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: RAPID-AUTO (Rigaku Corporation, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC & Rigaku Corporation, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

Methoxy[3-methoxysalicylaldehyde (4-methoxybenzoyl)hydrazonato(2-)-κ3O,O',N]oxovanadium(V) top
Crystal data top
[VO(C16H14N2O4)(CH3O)]F(000) = 816
Mr = 396.27Dx = 1.499 Mg m3
Orthorhombic, P212121Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2ac 2abCell parameters from 15303 reflections
a = 7.531 (3) Åθ = 3.4–27.5°
b = 11.787 (4) ŵ = 0.60 mm1
c = 19.786 (6) ÅT = 296 K
V = 1756.4 (11) Å3Prism, red
Z = 40.34 × 0.26 × 0.18 mm
Data collection top
Rigaku R-AXIS RAPID
diffractometer
3957 independent reflections
Radiation source: fine-focus sealed tube3658 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.045
Detector resolution: 10 pixels mm-1θmax = 27.5°, θmin = 3.2°
ω scanh = 99
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
k = 1512
Tmin = 0.823, Tmax = 0.899l = 2525
15391 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.036H-atom parameters constrained
wR(F2) = 0.093 w = 1/[σ2(Fo2) + (0.0592P)2 + 0.3631P]
where P = (Fo2 + 2Fc2)/3
S = 1.00(Δ/σ)max < 0.001
3957 reflectionsΔρmax = 0.40 e Å3
239 parametersΔρmin = 0.22 e Å3
0 restraintsAbsolute structure: Flack (1983), 1643 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.49 (2)
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
V10.17704 (6)0.22978 (3)0.79629 (2)0.0349 (1)
N10.1863 (2)0.3437 (1)0.71472 (8)0.0299 (3)
N20.1285 (3)0.3018 (2)0.65158 (9)0.0347 (4)
O10.0182 (3)0.2660 (2)0.82253 (9)0.0602 (5)
O20.3395 (2)0.3283 (1)0.83444 (8)0.0381 (4)
O30.1369 (2)0.1406 (1)0.71590 (7)0.0345 (3)
O40.2323 (4)0.1046 (2)0.8386 (1)0.0807 (9)
O50.4797 (3)0.4284 (1)0.94272 (9)0.0452 (4)
O60.1355 (2)0.0630 (1)0.43446 (8)0.0404 (4)
C10.3582 (3)0.4410 (2)0.8326 (1)0.0304 (4)
C20.4368 (3)0.4969 (2)0.8893 (1)0.0323 (5)
C30.4614 (3)0.6130 (2)0.8871 (1)0.0393 (5)
C40.4103 (3)0.6750 (2)0.8296 (1)0.0416 (5)
C50.3347 (3)0.6230 (2)0.7743 (1)0.0363 (5)
C60.3065 (3)0.5044 (2)0.7752 (1)0.0301 (4)
C70.2315 (3)0.4493 (2)0.7161 (1)0.0325 (4)
C80.5466 (4)0.4816 (2)1.0033 (1)0.0436 (6)
C90.1042 (3)0.1930 (2)0.6585 (1)0.0290 (4)
C100.0442 (3)0.1248 (2)0.5997 (1)0.0299 (4)
C110.0199 (3)0.1757 (2)0.5405 (1)0.0387 (5)
C120.0784 (3)0.1108 (2)0.4858 (1)0.0388 (5)
C130.0722 (3)0.0070 (2)0.4902 (1)0.0301 (4)
C140.0073 (3)0.0590 (2)0.5487 (1)0.0322 (4)
C150.0499 (3)0.0075 (2)0.6032 (1)0.0326 (5)
C160.1328 (5)0.1838 (2)0.4363 (1)0.0529 (7)
C170.2716 (4)0.0079 (2)0.8282 (2)0.0536 (7)
H30.51210.65020.92370.047*
H40.42780.75310.82890.050*
H50.30250.66550.73660.044*
H70.21520.49240.67720.039*
H8A0.65500.52100.99310.065*
H8B0.56900.42471.03690.065*
H8C0.46040.53461.02000.065*
H110.02340.25440.53750.046*
H120.12110.14580.44690.047*
H140.00210.13770.55150.039*
H150.09220.02750.64220.039*
H16A0.01260.20970.44130.079*
H16B0.18160.21320.39510.079*
H16C0.20230.21000.47390.079*
H17A0.27850.02260.78050.080*
H17B0.18020.05420.84780.080*
H17C0.38340.02550.84890.080*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
V10.0577 (2)0.0245 (2)0.0226 (2)0.0102 (2)0.0002 (2)0.0013 (1)
N10.0386 (8)0.0255 (7)0.0256 (8)0.0038 (7)0.0018 (8)0.0016 (6)
N20.049 (1)0.0283 (8)0.0268 (8)0.0060 (7)0.0037 (8)0.0016 (6)
O10.065 (1)0.069 (1)0.047 (1)0.026 (1)0.0187 (9)0.019 (1)
O20.0558 (9)0.0249 (7)0.0335 (8)0.0050 (7)0.0137 (8)0.0004 (6)
O30.0548 (9)0.0247 (6)0.0239 (7)0.0043 (6)0.0021 (6)0.0016 (5)
O40.177 (3)0.0268 (8)0.0380 (9)0.014 (1)0.035 (1)0.0056 (7)
O50.066 (1)0.0325 (8)0.0373 (9)0.0000 (8)0.0179 (8)0.0025 (7)
O60.059 (1)0.0321 (8)0.0300 (7)0.0009 (7)0.0098 (7)0.0053 (6)
C10.034 (1)0.0241 (9)0.033 (1)0.0011 (8)0.0017 (8)0.0021 (8)
C20.035 (1)0.030 (1)0.032 (1)0.0003 (8)0.0022 (9)0.0024 (9)
C30.045 (1)0.031 (1)0.042 (1)0.007 (1)0.004 (1)0.010 (1)
C40.051 (1)0.025 (1)0.050 (1)0.0061 (9)0.000 (1)0.002 (1)
C50.044 (1)0.0259 (9)0.039 (1)0.0018 (9)0.001 (1)0.0018 (8)
C60.035 (1)0.0261 (9)0.0291 (9)0.0028 (8)0.0028 (8)0.0011 (7)
C70.041 (1)0.0280 (9)0.029 (1)0.0014 (8)0.0003 (8)0.0011 (8)
C80.048 (1)0.047 (1)0.035 (1)0.001 (1)0.011 (1)0.006 (1)
C90.034 (1)0.029 (1)0.0239 (9)0.0029 (7)0.0002 (8)0.0021 (7)
C100.036 (1)0.0282 (9)0.0261 (9)0.0037 (8)0.0012 (8)0.0031 (8)
C110.056 (1)0.028 (1)0.032 (1)0.004 (1)0.007 (1)0.0018 (8)
C120.060 (1)0.030 (1)0.027 (1)0.001 (1)0.0083 (9)0.0014 (9)
C130.036 (1)0.032 (1)0.0231 (9)0.0025 (8)0.0012 (8)0.0032 (8)
C140.043 (1)0.0233 (9)0.030 (1)0.0003 (8)0.0014 (9)0.0014 (7)
C150.044 (1)0.030 (1)0.0237 (9)0.0003 (9)0.0040 (9)0.0021 (8)
C160.084 (2)0.032 (1)0.043 (1)0.006 (1)0.014 (1)0.008 (1)
C170.069 (2)0.036 (1)0.056 (2)0.001 (1)0.008 (1)0.003 (1)
Geometric parameters (Å, º) top
V1—N12.100 (2)C5—H50.9300
V1—O11.616 (2)C6—C71.452 (3)
V1—O21.848 (2)C7—H70.9300
V1—O31.931 (2)C8—H8A0.9600
V1—O41.747 (2)C8—H8B0.9600
N1—C71.291 (3)C8—H8C0.9600
N2—C91.302 (3)C9—C101.484 (3)
N1—N21.412 (2)C10—C111.403 (3)
O2—C11.337 (2)C10—C151.384 (3)
O3—C91.317 (3)C11—C121.397 (3)
O4—C171.374 (3)C11—H110.9300
O5—C21.369 (3)C12—C131.391 (3)
O5—C81.444 (3)C12—H120.9300
O6—C131.371 (3)C13—C141.399 (3)
O6—C161.424 (3)C14—C151.401 (3)
C1—C21.428 (3)C14—H140.9300
C1—C61.415 (3)C15—H150.9300
C2—C31.382 (3)C16—H16A0.9600
C3—C41.406 (4)C16—H16B0.9600
C3—H30.9300C16—H16C0.9600
C4—C51.378 (3)C17—H17A0.9600
C4—H40.9300C17—H17B0.9600
C5—C61.414 (3)C17—H17C0.9600
O1—V1—N196.2 (1)C4—C5—C6119.4 (2)
O1—V1—O2107.76 (9)C4—C5—H5120.3
O1—V1—O3105.42 (9)C5—C4—C3121.6 (2)
O1—V1—O4106.6 (1)C5—C4—H4119.2
O2—V1—N183.71 (7)C5—C6—C7119.3 (2)
O2—V1—O3141.50 (8)C6—C1—C2120.1 (2)
O3—V1—N173.76 (6)C6—C5—H5120.3
O4—V1—N1154.2 (1)C6—C7—H7118.3
O4—V1—O2100.2 (1)C7—N1—V1127.5 (1)
O4—V1—O388.40 (8)C7—N1—N2115.9 (2)
N1—C7—C6123.4 (2)C9—N2—N1107.2 (2)
N1—C7—H7118.3C9—O3—V1119.0 (1)
N2—N1—V1116.5 (1)C10—C11—H11119.3
N2—C9—O3121.8 (2)C10—C15—C14120.7 (2)
N2—C9—C10119.6 (2)C10—C15—H15119.6
O2—C1—C2118.8 (2)C11—C10—C9121.8 (2)
O2—C1—C6121.2 (2)C11—C12—H12120.4
O3—C9—C10118.6 (2)C12—C11—C10121.4 (2)
O4—C17—H17A109.5C12—C11—H11119.3
O4—C17—H17B109.5C12—C13—C14120.1 (2)
O4—C17—H17C109.5C13—O6—C16117.1 (2)
O5—C2—C1115.6 (2)C13—C12—C11119.2 (2)
O5—C2—C3125.2 (2)C13—C12—H12120.4
O5—C8—H8A109.5C13—C14—C15120.0 (2)
O5—C8—H8B109.5C13—C14—H14120.0
O5—C8—H8C109.5C14—C15—H15119.6
O6—C13—C12114.8 (2)C15—C10—C9119.5 (2)
O6—C13—C14125.2 (2)C15—C10—C11118.7 (2)
O6—C16—H16A109.5C15—C14—H14120.0
O6—C16—H16B109.5C17—O4—V1142.6 (2)
O6—C16—H16C109.5H8A—C8—H8B109.5
C1—O2—V1133.1 (1)H8A—C8—H8C109.5
C1—C6—C5119.4 (2)H8B—C8—H8C109.5
C1—C6—C7121.2 (2)H16A—C16—H16B109.5
C2—O5—C8117.8 (2)H16A—C16—H16C109.5
C2—C3—C4120.3 (2)H16B—C16—H16C109.5
C2—C3—H3119.9H17A—C17—H17B109.5
C3—C2—C1119.2 (2)H17A—C17—H17C109.5
C3—C4—H4119.2H17B—C17—H17C109.5
C4—C3—H3119.9
V1—N1—N2—C98.4 (2)O3—C9—C10—C159.8 (3)
V1—N1—C7—C68.1 (3)O4—V1—N1—N259.2 (3)
V1—O2—C1—C2150.3 (2)O4—V1—N1—C7124.1 (3)
V1—O2—C1—C631.6 (3)O4—V1—O2—C1169.4 (2)
V1—O3—C9—N212.2 (3)O4—V1—O3—C9173.2 (2)
V1—O3—C9—C10170.0 (2)O5—C2—C3—C4179.2 (2)
N1—V1—O2—C136.4 (2)O6—C13—C14—C15178.4 (2)
N1—V1—O3—C912.1 (2)C1—C2—C3—C40.2 (4)
N1—V1—O4—C1733.3 (6)C1—C6—C7—N19.0 (3)
N1—N2—C9—O31.7 (3)C2—C1—C6—C50.5 (3)
N1—N2—C9—C10179.4 (2)C2—C1—C6—C7178.0 (2)
N2—N1—C7—C6175.2 (2)C2—C3—C4—C50.1 (4)
N2—C9—C10—C15168.0 (2)C3—C4—C5—C60.4 (4)
N2—C9—C10—C1112.5 (3)C4—C5—C6—C10.7 (3)
O1—V1—N1—N293.1 (2)C4—C5—C6—C7178.3 (2)
O1—V1—N1—C783.6 (2)C5—C6—C7—N1173.4 (2)
O1—V1—O2—C158.2 (2)C6—C1—C2—O5179.1 (2)
O1—V1—O3—C980.0 (2)C6—C1—C2—C30.0 (3)
O1—V1—O4—C17117.9 (4)C7—N1—N2—C9174.5 (2)
O2—V1—N1—N2159.7 (2)C8—O5—C2—C1175.3 (2)
O2—V1—N1—C723.6 (2)C8—O5—C2—C33.8 (4)
O2—V1—O3—C968.7 (2)C9—C10—C11—C12179.0 (2)
O2—V1—O4—C17130.0 (4)C9—C10—C15—C14179.4 (2)
O2—C1—C2—O52.8 (3)C10—C11—C12—C130.3 (4)
O2—C1—C2—C3178.1 (2)C11—C10—C15—C140.1 (4)
O2—C1—C6—C5177.6 (2)C11—C12—C13—O6178.9 (2)
O2—C1—C6—C70.1 (3)C11—C12—C13—C140.2 (4)
O3—V1—N1—N211.2 (1)C12—C13—C14—C150.6 (3)
O3—V1—N1—C7172.1 (2)C13—C14—C15—C100.4 (3)
O3—V1—O2—C190.2 (2)C15—C10—C11—C120.5 (4)
O3—V1—O4—C1712.2 (4)C16—O6—C13—C12179.8 (2)
O3—C9—C10—C11169.7 (2)C16—O6—C13—C140.8 (3)
 

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