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Acta Cryst. (2007). E63, m2912
https://doi.org/10.1107/S1600536807054529
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Retracted: Tetra­kis(pyridine-κN)bis­(thio­cyanato-κN)vanadium(II)

T. Liu and J. Y. Zhu
In the mol­ecule of the title complex, [V(NCS)2(C5H5N)4], the VII atom, located on a centre of inversion, is coordinated in a distorted octa­hedral arrangement by two N atoms of two SCN− and four N atoms of four pyridine ligands. In the crystal structure, C—H...N hydrogen bonds result in the formation of a supra­molecular network.
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Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807054529/at2459sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807054529/at2459Isup2.hkl
Contains datablock I

CCDC reference: 1176495

checkCIF report

Key indicators

  • Single-crystal X-ray study
  • T = 273 K
  • Mean [sigma](C-C) = 0.007 Å
  • R factor = 0.051
  • wR factor = 0.177
  • Data-to-parameter ratio = 16.3

checkCIF/PLATON results

No syntax errors found




Alert level B
PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low .......       0.95
PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X)  V1     -   N1      ..      11.19 su
PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X)  V1     -   N2      ..      10.29 su
PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X)  V1     -   N3      ..      10.60 su


Alert level C
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       2.29
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for         N3
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for         V1
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for        C11
PLAT341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ...          7


Alert level G
PLAT794_ALERT_5_G Check Predicted Bond Valency for V1          (3)       2.56


   0 ALERT level A = In general: serious problem
   4 ALERT level B = Potentially serious problem
   5 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
   7 ALERT type 2 Indicator that the structure model may be wrong or deficient
   2 ALERT type 3 Indicator that the structure quality may be low
   0 ALERT type 4 Improvement, methodology, query or suggestion
   1 ALERT type 5 Informative message, check
Comment top

The crystal structure of tetrakis(pyridine-κN)bis(thiocyanato- κN)chromium(II), (II), has previously been reported (Liu & Zhu, 2007). The crystal structure determination of the title compound, (I), has been carried out in order to elucidate the molecular conformation and to compare it with that of (II). We report herein the crystal structure of (I).

In the molecule of (I) (Fig. 1), the ligand bond lengths and angles (Table 1) are within normal ranges (Allen et al., 1987). The two N atoms of two SCN- and four N atoms of four pyridine ligands are coordinated to the V atom, in a distorted octahedral arrangement (Table 1). The V—N distances for the SCN- and pyridine ligand are 2.066 (3)Å and in the range of [2.153 (3)–2.173 (3) Å], respectively (Table 1), as in (II).

In the crystal structure, the C—H···N hydrogen bonds (Table 2, Fig. 2) result in the formation of a supramolecular network structure, as in (II). The both compounds, (I) and (II), are isostructural.

Related literature top

For a related structure, see: Liu & Zhu (2007). For bond-length data, see: Allen et al. (1987).

Experimental top

Crystals of the title compound were synthesized using hydrothermal method in a Teflon-lined Parr bomb (23 ml), which was then sealed. Lanthanum (III) nitrate hexahydrate (432.4 mg, 1 mmol), vanadium dichloride (243.6 mg, 2 mmol), potassium thiocyanate (194.2 mg, 2 mmol), pyridine (6 ml), and distilled water (10 g) were placed into the bomb and sealed. The bomb was heated under autogenous pressure for 7 d at 453 K and allowed to cool at room temperature for 24 h. Upon opening the bomb, a clear colourless solution was decanted from small colourless crystals. These crystals were washed with distilled water followed by ethanol, and allowed to air-dry at room temperature.

Refinement top

H atoms were positioned geometrically, with C—H = 0.93 Å for aromatic H and constrained to ride on their parent atoms, with Uiso(H) = 1.2Ueq(C).

Computing details top

Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT (Siemens, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Siemens, 1996); software used to prepare material for publication: SHELXTL (Siemens, 1996).

Figures top
[Figure 1] Fig. 1. The molecular structure of the title molecule, with the atom-numbering scheme. Displacement ellipsoids are drawn at the 30% probability level [symmetry code (A): -x + 3/2, -y + 3/2, -z + 1].
[Figure 2] Fig. 2. A packing diagram for (I).
Tetrakis(pyridine-κN)bis(thiocyanato-κN)vanadium(II) top
Crystal data top
[V(NCS)2(C5H5N)4]F(000) = 996
Mr = 483.50Dx = 1.377 Mg m−3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 4483 reflections
a = 12.5011 (13) Åθ = 2.5–27.9°
b = 13.003 (3) ŵ = 0.63 mm−1
c = 14.999 (3) ÅT = 273 K
β = 106.981 (5)°Block, colourless
V = 2331.8 (8) Å30.31 × 0.29 × 0.16 mm
Z = 4
Data collection top
Bruker APEX-II area-detector
diffractometer		2332 independent reflections
Radiation source: fine-focus sealed tube1933 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.020
ϕ and ω scansθmax = 26.6°, θmin = 2.4°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		h = −15→15
Tmin = 0.827, Tmax = 0.904k = −16→16
7623 measured reflectionsl = −18→18
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)] = 0.051H-atom parameters constrained
wR(F2) = 0.178 w = 1/[σ2(Fo2) + (0.1448P)2 + 1.8328P]
where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max < 0.001
2332 reflectionsΔρmax = 1.34 e Å−3
143 parametersΔρmin = −0.58 e Å−3
0 restraintsExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.018 (3)
Crystal data top
[V(NCS)2(C5H5N)4]V = 2331.8 (8) Å3
Mr = 483.50Z = 4
Monoclinic, C2/cMo Kα radiation
a = 12.5011 (13) ŵ = 0.63 mm−1
b = 13.003 (3) ÅT = 273 K
c = 14.999 (3) Å0.31 × 0.29 × 0.16 mm
β = 106.981 (5)°
Data collection top
Bruker APEX-II area-detector
diffractometer		2332 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)		1933 reflections with I > 2σ(I)
Tmin = 0.827, Tmax = 0.904Rint = 0.020
7623 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0510 restraints
wR(F2) = 0.178H-atom parameters constrained
S = 1.04Δρmax = 1.34 e Å−3
2332 reflectionsΔρmin = −0.58 e Å−3
143 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.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
V10.75000.75000.50000.0357 (3)
S11.07294 (10)0.64360 (9)0.41903 (9)0.0802 (4)
N10.7867 (2)0.6901 (2)0.6395 (2)0.0585 (7)
N20.6400 (2)0.6220 (2)0.4417 (2)0.0585 (7)
N30.8866 (2)0.6723 (3)0.4824 (2)0.0632 (8)
C10.8412 (3)0.6005 (3)0.6643 (3)0.0694 (10)
H10.86580.56570.61980.083*
C20.8626 (4)0.5573 (4)0.7514 (3)0.0814 (12)
H20.89900.49430.76500.098*
C30.8289 (4)0.6092 (5)0.8170 (3)0.0901 (14)
H30.84250.58290.87690.108*
C40.7734 (5)0.7029 (5)0.7927 (3)0.0888 (14)
H40.75160.74050.83720.107*
C50.7515 (4)0.7387 (3)0.7051 (3)0.0727 (11)
H50.71070.79920.68920.087*
C60.6742 (4)0.5249 (3)0.4540 (3)0.0719 (10)
H60.74890.51260.48570.086*
C70.6049 (5)0.4401 (4)0.4223 (4)0.0889 (14)
H70.63160.37320.43460.107*
C80.4944 (5)0.4594 (4)0.3717 (4)0.0958 (16)
H80.44580.40540.34720.115*
C90.4584 (5)0.5595 (4)0.3586 (4)0.0929 (14)
H90.38420.57420.32690.112*
C100.5322 (3)0.6369 (3)0.3925 (3)0.0737 (11)
H100.50680.70420.38100.088*
C110.9642 (3)0.6595 (2)0.4562 (2)0.0542 (8)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
V10.0328 (4)0.0368 (4)0.0389 (4)0.0019 (2)0.0126 (3)−0.0020 (2)
S10.0761 (7)0.0787 (7)0.1010 (9)0.0089 (5)0.0497 (6)−0.0007 (5)
N10.0552 (15)0.0657 (17)0.0553 (16)−0.0015 (13)0.0173 (13)−0.0020 (13)
N20.0554 (15)0.0578 (16)0.0627 (17)−0.0035 (13)0.0179 (13)−0.0034 (13)
N30.0551 (16)0.0685 (18)0.0692 (18)0.0064 (14)0.0228 (14)−0.0023 (14)
C10.071 (2)0.072 (2)0.065 (2)0.0113 (19)0.0213 (18)0.0083 (18)
C20.074 (3)0.093 (3)0.076 (3)0.008 (2)0.020 (2)0.020 (2)
C30.078 (3)0.126 (4)0.064 (2)−0.004 (3)0.018 (2)0.024 (3)
C40.089 (3)0.117 (4)0.067 (3)−0.003 (3)0.034 (2)−0.009 (3)
C50.074 (3)0.083 (3)0.061 (2)−0.0019 (19)0.020 (2)−0.0114 (18)
C60.072 (2)0.061 (2)0.085 (3)−0.0012 (18)0.028 (2)−0.0099 (18)
C70.101 (4)0.063 (2)0.109 (4)−0.011 (2)0.041 (3)−0.013 (2)
C80.102 (4)0.087 (3)0.105 (4)−0.040 (3)0.042 (3)−0.026 (3)
C90.077 (3)0.095 (4)0.099 (3)−0.019 (2)0.014 (3)−0.018 (3)
C100.060 (2)0.076 (2)0.081 (3)−0.0013 (18)0.0147 (19)−0.004 (2)
C110.0569 (18)0.0493 (16)0.0559 (18)0.0040 (14)0.0156 (15)−0.0010 (13)
Geometric parameters (Å, º) top
V1—N12.153 (3)C2—H20.9300
V1—N22.173 (3)C3—C41.396 (8)
V1—N32.066 (3)C3—H30.9300
V1—N3i2.066 (3)C4—C51.345 (7)
V1—N1i2.153 (3)C4—H40.9300
V1—N2i2.173 (3)C5—H50.9300
S1—C111.626 (4)C6—C71.397 (6)
N1—C51.346 (5)C6—H60.9300
N1—C11.347 (5)C7—C81.391 (9)
N2—C61.329 (5)C7—H70.9300
N2—C101.348 (5)C8—C91.372 (7)
N3—C111.160 (4)C8—H80.9300
C1—C21.375 (6)C9—C101.360 (6)
C1—H10.9300C9—H90.9300
C2—C31.357 (8)C10—H100.9300
N1—V1—N1i179.998 (1)C1—C2—H2121.0
N1—V1—N292.54 (11)C2—C3—C4118.8 (4)
N1i—V1—N287.46 (11)C2—C3—H3120.6
N1—V1—N389.89 (12)C4—C3—H3120.6
N1i—V1—N390.11 (12)C5—C4—C3120.0 (5)
N2—V1—N2i180.0C5—C4—H4120.0
N2i—V1—N388.64 (12)C3—C4—H4120.0
N2—V1—N391.36 (12)C4—C5—N1122.3 (5)
N3i—V1—N3180.00 (17)C4—C5—H5118.9
N3i—V1—N1i89.89 (12)N1—C5—H5118.9
N3—V1—N1i90.11 (12)N2—C6—C7124.1 (5)
N3i—V1—N2i91.36 (12)N2—C6—H6117.9
N3—V1—N2i88.64 (12)C7—C6—H6117.9
N1—V1—N2i87.46 (11)C8—C7—C6117.5 (5)
N1i—V1—N2i92.54 (11)C8—C7—H7121.3
C5—N1—C1116.8 (3)C6—C7—H7121.3
C5—N1—V1121.2 (3)C9—C8—C7118.8 (4)
C1—N1—V1121.9 (2)C9—C8—H8120.6
C6—N2—C10116.2 (3)C7—C8—H8120.6
C6—N2—V1122.2 (3)C10—C9—C8119.3 (5)
C10—N2—V1121.6 (3)C10—C9—H9120.3
C11—N3—V1156.6 (3)C8—C9—H9120.3
N1—C1—C2124.0 (4)N2—C10—C9124.0 (4)
N1—C1—H1118.0N2—C10—H10118.0
C2—C1—H1118.0C9—C10—H10118.0
C3—C2—C1118.0 (4)N3—C11—S1179.0 (3)
C3—C2—H2121.0
Symmetry code: (i) −x+3/2, −y+3/2, −z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C5—H5···N3i0.932.533.064 (6)118
C1—H1···N30.932.563.090 (5)117
Symmetry code: (i) −x+3/2, −y+3/2, −z+1.

Experimental details

Crystal data
Chemical formula[V(NCS)2(C5H5N)4]
Mr483.50
Crystal system, space groupMonoclinic, C2/c
Temperature (K)273
a, b, c (Å)12.5011 (13), 13.003 (3), 14.999 (3)
β (°) 106.981 (5)
V (Å3)2331.8 (8)
Z4
Radiation typeMo Kα
µ (mm−1)0.63
Crystal size (mm)0.31 × 0.29 × 0.16
Data collection
DiffractometerBruker APEX-II area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.827, 0.904
No. of measured, independent and
observed [I > 2σ(I)] reflections		7623, 2332, 1933
Rint0.020
(sin θ/λ)max (Å−1)0.630
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.051, 0.178, 1.04
No. of reflections2332
No. of parameters143
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å−3)1.34, −0.58

Computer programs: APEX2 (Bruker, 2005), SAINT (Siemens, 1996), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Siemens, 1996).

Selected geometric parameters (Å, º) top
V1—N12.153 (3)V1—N32.066 (3)
V1—N22.173 (3)
N1—V1—N1i179.998 (1)N2—V1—N2i180.0
N1—V1—N292.54 (11)N2i—V1—N388.64 (12)
N1i—V1—N287.46 (11)N2—V1—N391.36 (12)
N1—V1—N389.89 (12)N3i—V1—N3180.00 (17)
N1i—V1—N390.11 (12)
Symmetry code: (i) −x+3/2, −y+3/2, −z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C5—H5···N3i0.932.533.064 (6)118
C1—H1···N30.932.563.090 (5)117
Symmetry code: (i) −x+3/2, −y+3/2, −z+1.
 

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