Download citation
Download citation
link to html
The synthesis and characterization of the title VIV complex of a salicyl­ald­imine, [V(C20H14N2O4)O]·2C2H6OS·2H2O, is described. The reaction of 2,4-di­hydroxy­benz­aldehyde and 1,2-phenyl­enedi­amine with vanadyl sulfate produces a monomeric VIV complex. Its structure reveals that the vanadium(IV) ion is pentacoordinated and situated in a distorted square-pyramidal environment.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680402210X/dn6157sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680402210X/dn6157Isup2.hkl
Contains datablock I

CCDC reference: 252952

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.061
  • wR factor = 0.136
  • Data-to-parameter ratio = 16.0

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors for S1 PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors for S2
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 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 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: SMART (Bruker, 1994); cell refinement: SAINT (Bruker, 1994); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPIII (Burnett & Johnson, 1996); software used to prepare material for publication: SHELXL97.

[N,N'-bis(4-hydroxysalicylidene)-o-phenylenediamine]oxovanadium(IV) bis(dimethyl sulfoxide) dihydrate top
Crystal data top
[V(C20H14N2O4)O]·2C2H6OS·2H2OZ = 2
Mr = 605.56F(000) = 630
Triclinic, P1Dx = 1.465 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.325 (3) ÅCell parameters from 729 reflections
b = 12.312 (4) Åθ = 2.6–22.8°
c = 12.829 (4) ŵ = 0.57 mm1
α = 78.464 (5)°T = 293 K
β = 72.067 (6)°Block, green
γ = 85.072 (6)°0.20 × 0.16 × 0.12 mm
V = 1372.6 (8) Å3
Data collection top
Bruker SMART CCD area-detector
diffractometer
5595 independent reflections
Radiation source: fine-focus sealed tube3146 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.035
φ and ω scansθmax = 26.5°, θmin = 2.2°
Absorption correction: multi-scan
(Blessing, 1995)
h = 811
Tmin = 0.872, Tmax = 0.934k = 1515
8035 measured reflectionsl = 1613
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)] = 0.061Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.136H-atom parameters constrained
S = 1.00 w = 1/[σ2(Fo2) + (0.0557P)2 + 0.0346P]
where P = (Fo2 + 2Fc2)/3
5595 reflections(Δ/σ)max = 0.001
349 parametersΔρmax = 0.56 e Å3
0 restraintsΔρmin = 0.35 e Å3
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
V10.41273 (7)0.27497 (5)0.46389 (6)0.0297 (2)
N10.6179 (3)0.1959 (2)0.4135 (2)0.0293 (7)
N20.5357 (3)0.3418 (2)0.5416 (3)0.0298 (7)
O10.3207 (3)0.14420 (19)0.4552 (2)0.0349 (6)
O20.2358 (3)0.1511 (2)0.2977 (2)0.0411 (7)
H20.14800.13330.32690.062*
O30.2401 (3)0.2824 (2)0.5907 (2)0.0379 (7)
O40.1192 (3)0.4324 (3)0.8778 (3)0.0634 (9)
H40.17570.40030.85680.095*
O50.4019 (3)0.3700 (2)0.3620 (2)0.0430 (7)
C10.3757 (4)0.0670 (3)0.3949 (3)0.0287 (9)
C20.2760 (4)0.0007 (3)0.3769 (3)0.0300 (9)
H2A0.17260.01070.40610.036*
C30.3289 (4)0.0841 (3)0.3165 (3)0.0312 (9)
C40.4842 (4)0.1027 (3)0.2710 (3)0.0374 (10)
H4A0.51970.15770.22830.045*
C50.5812 (4)0.0394 (3)0.2903 (3)0.0367 (10)
H50.68410.05350.26230.044*
C60.5326 (4)0.0470 (3)0.3508 (3)0.0297 (9)
C70.6427 (4)0.1078 (3)0.3689 (3)0.0335 (9)
H70.74210.08200.34660.040*
C80.7390 (4)0.2495 (3)0.4268 (3)0.0341 (9)
C90.8916 (4)0.2272 (3)0.3796 (4)0.0458 (11)
H90.92190.17370.33480.055*
C100.9976 (5)0.2849 (3)0.3999 (4)0.0509 (12)
H101.09960.26870.37020.061*
C110.9535 (4)0.3662 (3)0.4637 (4)0.0476 (12)
H111.02620.40540.47550.057*
C120.8034 (4)0.3902 (3)0.5103 (3)0.0399 (10)
H120.77450.44600.55250.048*
C130.6951 (4)0.3300 (3)0.4937 (3)0.0324 (9)
C140.4798 (4)0.3915 (3)0.6267 (3)0.0363 (10)
H140.54790.42360.65070.044*
C150.3249 (4)0.4011 (3)0.6861 (3)0.0352 (9)
C160.2817 (5)0.4640 (3)0.7721 (4)0.0499 (12)
H160.35570.49950.78650.060*
C170.1365 (5)0.4744 (4)0.8345 (4)0.0531 (12)
H170.11180.51630.89070.064*
C180.0237 (5)0.4212 (3)0.8134 (4)0.0440 (11)
C190.0627 (4)0.3573 (3)0.7304 (3)0.0401 (10)
H190.01240.32150.71760.048*
C200.2103 (4)0.3459 (3)0.6667 (3)0.0310 (9)
O60.4682 (4)0.2176 (3)0.0022 (3)0.0922 (12)
S10.44643 (16)0.23776 (12)0.11374 (12)0.0769 (4)
C210.6205 (6)0.2772 (5)0.1186 (4)0.0816 (17)
H21A0.69250.21680.10740.122*
H21B0.60840.29590.19000.122*
H21C0.65570.34030.06110.122*
C220.3578 (9)0.3660 (5)0.1141 (6)0.144 (3)
H22A0.40980.41650.04850.217*
H22B0.35870.39290.17910.217*
H22C0.25550.36010.11490.217*
O70.0348 (3)0.0336 (3)0.1533 (3)0.0744 (10)
S20.11483 (14)0.09007 (11)0.10524 (11)0.0621 (4)
C230.2433 (5)0.0021 (4)0.0319 (4)0.0773 (16)
H23A0.25640.06790.08310.116*
H23B0.33860.03290.00400.116*
H23C0.20490.02140.02310.116*
C240.0980 (6)0.1878 (4)0.0124 (5)0.097 (2)
H24A0.06860.15080.06150.145*
H24B0.19320.22210.05100.145*
H24C0.02310.24350.01150.145*
O80.9568 (3)0.9151 (2)0.3611 (2)0.0548 (8)
H8A0.88580.87240.40110.082*
H8B0.94330.94230.29850.082*
O90.6776 (3)0.3301 (2)0.8221 (3)0.0638 (9)
H9A0.71060.28210.78050.096*
H9B0.60500.30450.87820.096*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
V10.0253 (4)0.0304 (4)0.0357 (4)0.0024 (3)0.0100 (3)0.0093 (3)
N10.0238 (17)0.0310 (17)0.0342 (19)0.0042 (13)0.0104 (14)0.0043 (15)
N20.0294 (18)0.0261 (16)0.034 (2)0.0063 (13)0.0091 (14)0.0049 (15)
O10.0228 (14)0.0359 (15)0.0489 (18)0.0032 (11)0.0069 (12)0.0196 (13)
O20.0312 (16)0.0456 (16)0.053 (2)0.0068 (13)0.0110 (14)0.0249 (14)
O30.0255 (15)0.0491 (17)0.0433 (18)0.0057 (12)0.0054 (12)0.0233 (14)
O40.043 (2)0.080 (2)0.066 (2)0.0028 (17)0.0058 (17)0.0435 (19)
O50.0422 (17)0.0399 (16)0.0486 (19)0.0030 (12)0.0198 (14)0.0016 (14)
C10.030 (2)0.029 (2)0.027 (2)0.0030 (16)0.0085 (17)0.0040 (17)
C20.023 (2)0.035 (2)0.032 (2)0.0017 (16)0.0068 (16)0.0076 (18)
C30.030 (2)0.033 (2)0.033 (2)0.0065 (17)0.0146 (18)0.0022 (18)
C40.037 (3)0.033 (2)0.046 (3)0.0018 (18)0.012 (2)0.0174 (19)
C50.025 (2)0.039 (2)0.047 (3)0.0022 (17)0.0100 (18)0.013 (2)
C60.026 (2)0.029 (2)0.037 (2)0.0027 (16)0.0138 (17)0.0050 (18)
C70.026 (2)0.031 (2)0.044 (3)0.0038 (16)0.0113 (18)0.0088 (19)
C80.031 (2)0.032 (2)0.042 (3)0.0047 (17)0.0161 (19)0.0052 (19)
C90.028 (2)0.046 (3)0.066 (3)0.0002 (19)0.013 (2)0.018 (2)
C100.028 (2)0.048 (3)0.080 (4)0.003 (2)0.016 (2)0.018 (3)
C110.031 (3)0.043 (3)0.074 (3)0.011 (2)0.023 (2)0.009 (2)
C120.039 (3)0.033 (2)0.051 (3)0.0082 (18)0.015 (2)0.008 (2)
C130.026 (2)0.031 (2)0.040 (3)0.0086 (17)0.0133 (18)0.0019 (18)
C140.038 (3)0.028 (2)0.047 (3)0.0107 (17)0.017 (2)0.0049 (19)
C150.037 (2)0.032 (2)0.038 (3)0.0054 (17)0.0112 (19)0.0082 (19)
C160.056 (3)0.047 (3)0.054 (3)0.012 (2)0.015 (2)0.023 (2)
C170.053 (3)0.056 (3)0.052 (3)0.003 (2)0.003 (2)0.034 (2)
C180.043 (3)0.040 (2)0.045 (3)0.0020 (19)0.004 (2)0.012 (2)
C190.036 (3)0.040 (2)0.044 (3)0.0036 (18)0.009 (2)0.012 (2)
C200.033 (2)0.030 (2)0.030 (2)0.0014 (16)0.0079 (18)0.0069 (18)
O60.086 (3)0.118 (3)0.074 (3)0.030 (2)0.001 (2)0.045 (2)
S10.0719 (10)0.0838 (10)0.0610 (10)0.0101 (8)0.0048 (7)0.0019 (8)
C210.078 (4)0.096 (4)0.064 (4)0.021 (3)0.008 (3)0.015 (3)
C220.206 (8)0.127 (6)0.154 (7)0.092 (6)0.129 (7)0.071 (5)
O70.050 (2)0.106 (3)0.059 (2)0.0168 (19)0.0133 (17)0.007 (2)
S20.0534 (8)0.0753 (9)0.0552 (9)0.0079 (6)0.0148 (6)0.0059 (7)
C230.065 (4)0.087 (4)0.070 (4)0.002 (3)0.013 (3)0.006 (3)
C240.091 (5)0.080 (4)0.105 (5)0.009 (3)0.037 (4)0.034 (4)
O80.0341 (17)0.066 (2)0.057 (2)0.0123 (14)0.0079 (14)0.0018 (16)
O90.057 (2)0.070 (2)0.067 (2)0.0029 (16)0.0081 (17)0.0346 (18)
Geometric parameters (Å, º) top
V1—O51.592 (3)C12—H120.9300
V1—O31.915 (3)C14—C151.418 (5)
V1—O11.926 (2)C14—H140.9300
V1—N22.045 (3)C15—C161.412 (5)
V1—N12.049 (3)C15—C201.422 (5)
N1—C71.296 (4)C16—C171.354 (5)
N1—C81.426 (4)C16—H160.9300
N2—C141.304 (5)C17—C181.404 (6)
N2—C131.430 (4)C17—H170.9300
O1—C11.315 (4)C18—C191.390 (5)
O2—C31.351 (4)C19—C201.379 (5)
O2—H20.8200C19—H190.9300
O3—C201.319 (4)O6—S11.506 (4)
O4—C181.347 (5)S1—C221.718 (6)
O4—H40.8200S1—C211.756 (5)
C1—C21.399 (5)C21—H21A0.9600
C1—C61.416 (5)C21—H21B0.9600
C2—C31.376 (5)C21—H21C0.9600
C2—H2A0.9300C22—H22A0.9600
C3—C41.402 (5)C22—H22B0.9600
C4—C51.350 (5)C22—H22C0.9600
C4—H4A0.9300O7—S21.509 (3)
C5—C61.404 (5)S2—C231.762 (5)
C5—H50.9300S2—C241.771 (5)
C6—C71.420 (5)C23—H23A0.9600
C7—H70.9300C23—H23B0.9600
C8—C91.391 (5)C23—H23C0.9600
C8—C131.393 (5)C24—H24A0.9600
C9—C101.380 (5)C24—H24B0.9600
C9—H90.9300C24—H24C0.9600
C10—C111.375 (6)O8—H8A0.8493
C10—H100.9300O8—H8B0.8494
C11—C121.374 (5)O9—H9A0.8496
C11—H110.9300O9—H9B0.8493
C12—C131.392 (5)
O5—V1—O3110.44 (13)C12—C13—C8120.1 (4)
O5—V1—O1108.63 (12)C12—C13—N2125.4 (4)
O3—V1—O184.26 (11)C8—C13—N2114.5 (3)
O5—V1—N2104.61 (12)N2—C14—C15126.0 (3)
O3—V1—N288.37 (12)N2—C14—H14117.0
O1—V1—N2146.46 (11)C15—C14—H14117.0
O5—V1—N1106.62 (13)C16—C15—C14119.0 (3)
O3—V1—N1142.71 (12)C16—C15—C20117.9 (4)
O1—V1—N187.97 (11)C14—C15—C20123.0 (4)
N2—V1—N178.35 (12)C17—C16—C15122.4 (4)
C7—N1—C8120.7 (3)C17—C16—H16118.8
C7—N1—V1125.4 (2)C15—C16—H16118.8
C8—N1—V1113.8 (2)C16—C17—C18119.3 (4)
C14—N2—C13120.9 (3)C16—C17—H17120.3
C14—N2—V1125.4 (3)C18—C17—H17120.3
C13—N2—V1113.6 (2)O4—C18—C19122.6 (4)
C1—O1—V1130.1 (2)O4—C18—C17117.6 (4)
C3—O2—H2109.5C19—C18—C17119.7 (4)
C20—O3—V1130.6 (2)C20—C19—C18121.4 (4)
C18—O4—H4109.5C20—C19—H19119.3
O1—C1—C2119.0 (3)C18—C19—H19119.3
O1—C1—C6122.5 (3)O3—C20—C19118.4 (3)
C2—C1—C6118.5 (3)O3—C20—C15122.4 (3)
C3—C2—C1120.8 (3)C19—C20—C15119.2 (4)
C3—C2—H2A119.6O6—S1—C22103.7 (3)
C1—C2—H2A119.6O6—S1—C21107.5 (2)
O2—C3—C2122.3 (3)C22—S1—C2197.3 (3)
O2—C3—C4116.9 (3)S1—C21—H21A109.5
C2—C3—C4120.8 (3)S1—C21—H21B109.5
C5—C4—C3118.7 (4)H21A—C21—H21B109.5
C5—C4—H4A120.6S1—C21—H21C109.5
C3—C4—H4A120.6H21A—C21—H21C109.5
C4—C5—C6122.6 (4)H21B—C21—H21C109.5
C4—C5—H5118.7S1—C22—H22A109.5
C6—C5—H5118.7S1—C22—H22B109.5
C5—C6—C1118.6 (3)H22A—C22—H22B109.5
C5—C6—C7118.7 (3)S1—C22—H22C109.5
C1—C6—C7122.7 (3)H22A—C22—H22C109.5
N1—C7—C6126.3 (3)H22B—C22—H22C109.5
N1—C7—H7116.9O7—S2—C23107.0 (2)
C6—C7—H7116.9O7—S2—C24105.3 (2)
C9—C8—C13119.7 (3)C23—S2—C2497.2 (3)
C9—C8—N1125.5 (4)S2—C23—H23A109.5
C13—C8—N1114.9 (3)S2—C23—H23B109.5
C10—C9—C8119.5 (4)H23A—C23—H23B109.5
C10—C9—H9120.2S2—C23—H23C109.5
C8—C9—H9120.2H23A—C23—H23C109.5
C11—C10—C9120.5 (4)H23B—C23—H23C109.5
C11—C10—H10119.8S2—C24—H24A109.5
C9—C10—H10119.8S2—C24—H24B109.5
C12—C11—C10120.9 (4)H24A—C24—H24B109.5
C12—C11—H11119.6S2—C24—H24C109.5
C10—C11—H11119.6H24A—C24—H24C109.5
C11—C12—C13119.3 (4)H24B—C24—H24C109.5
C11—C12—H12120.3H8A—O8—H8B110.7
C13—C12—H12120.3H9A—O9—H9B110.5
O5—V1—N1—C793.4 (3)C5—C6—C7—N1173.0 (4)
O3—V1—N1—C793.2 (3)C1—C6—C7—N19.4 (6)
O1—V1—N1—C715.5 (3)C7—N1—C8—C911.0 (6)
N2—V1—N1—C7164.7 (3)V1—N1—C8—C9166.3 (3)
O5—V1—N1—C883.8 (3)C7—N1—C8—C13168.7 (3)
O3—V1—N1—C889.5 (3)V1—N1—C8—C1314.0 (4)
O1—V1—N1—C8167.3 (2)C13—C8—C9—C100.1 (6)
N2—V1—N1—C818.1 (2)N1—C8—C9—C10179.5 (4)
O5—V1—N2—C1495.0 (3)C8—C9—C10—C111.8 (6)
O3—V1—N2—C1415.7 (3)C9—C10—C11—C121.3 (7)
O1—V1—N2—C1492.8 (3)C10—C11—C12—C130.9 (6)
N1—V1—N2—C14160.7 (3)C11—C12—C13—C82.6 (6)
O5—V1—N2—C1384.9 (2)C11—C12—C13—N2176.6 (4)
O3—V1—N2—C13164.4 (2)C9—C8—C13—C122.1 (6)
O1—V1—N2—C1387.3 (3)N1—C8—C13—C12178.2 (3)
N1—V1—N2—C1319.5 (2)C9—C8—C13—N2177.2 (3)
O5—V1—O1—C181.6 (3)N1—C8—C13—N22.5 (5)
O3—V1—O1—C1168.8 (3)C14—N2—C13—C1217.0 (5)
N2—V1—O1—C190.5 (4)V1—N2—C13—C12162.9 (3)
N1—V1—O1—C125.3 (3)C14—N2—C13—C8162.2 (3)
O5—V1—O3—C2081.7 (3)V1—N2—C13—C817.9 (4)
O1—V1—O3—C20170.5 (3)C13—N2—C14—C15175.1 (3)
N2—V1—O3—C2023.3 (3)V1—N2—C14—C155.0 (5)
N1—V1—O3—C2091.5 (3)N2—C14—C15—C16175.9 (4)
V1—O1—C1—C2160.8 (2)N2—C14—C15—C207.2 (6)
V1—O1—C1—C621.6 (5)C14—C15—C16—C17178.1 (4)
O1—C1—C2—C3178.5 (3)C20—C15—C16—C171.1 (6)
C6—C1—C2—C30.8 (5)C15—C16—C17—C180.1 (7)
C1—C2—C3—O2179.9 (3)C16—C17—C18—O4179.3 (4)
C1—C2—C3—C40.4 (5)C16—C17—C18—C191.1 (7)
O2—C3—C4—C5178.4 (3)O4—C18—C19—C20179.0 (4)
C2—C3—C4—C51.9 (5)C17—C18—C19—C200.9 (6)
C3—C4—C5—C62.3 (6)V1—O3—C20—C19161.9 (3)
C4—C5—C6—C11.1 (6)V1—O3—C20—C1519.1 (5)
C4—C5—C6—C7178.7 (4)C18—C19—C20—O3178.8 (3)
O1—C1—C6—C5178.1 (3)C18—C19—C20—C150.3 (6)
C2—C1—C6—C50.5 (5)C16—C15—C20—O3177.8 (3)
O1—C1—C6—C70.5 (5)C14—C15—C20—O30.8 (6)
C2—C1—C6—C7177.1 (3)C16—C15—C20—C191.2 (5)
C8—N1—C7—C6179.9 (3)C14—C15—C20—C19178.2 (4)
V1—N1—C7—C62.9 (5)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O9—H9B···O6i0.851.872.705 (5)167
O9—H9A···O2ii0.852.012.856 (4)170
O8—H8B···O7iii0.851.932.753 (4)161
O8—H8A···O3iv0.852.293.022 (4)144
O8—H8A···O1iv0.852.212.944 (4)145
O4—H4···O9v0.821.882.701 (4)174
O2—H2···O8vi0.821.782.587 (4)168
Symmetry codes: (i) x, y, z+1; (ii) x+1, y, z+1; (iii) x+1, y+1, z; (iv) x+1, y+1, z+1; (v) x1, y, z; (vi) x1, y1, z.
 

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds