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Acta Crystallogr Sect E Struct Rep Online. 2010 December 1; 66(Pt 12): m1587.
Published online 2010 November 17. doi:  10.1107/S1600536810046647
PMCID: PMC3011802

Bis[2-(pyridin-2-yl)ethanol-κ2 N,O]bis­(thio­cyanato-κN)nickel(II)

Abstract

In the title complex, [Ni(NCS)2(C7H9NO)2], the NiII atom is in a distorted octa­hedral coordination environment defined by two N atoms of the two thio­cyanate ions and by the N and O atoms of the two chelating 2-(pyridin-2-yl)ethanol ligands. The complex mol­ecule is located around a crystallographic inversion center. In the crystal, mol­ecules are connected into a two-dimensional polymeric structure parallel to (100) by O—H(...)S hydrogen bonds.

Related literature

For related structures, see: Pan et al. (2007 [triangle]); Yu et al. (2010 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-66-m1587-scheme1.jpg

Experimental

Crystal data

  • [Ni(NCS)2(C7H9NO)2]
  • M r = 421.17
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-66-m1587-efi1.jpg
  • a = 8.7197 (9) Å
  • b = 13.8634 (15) Å
  • c = 7.8655 (7) Å
  • β = 105.496 (2)°
  • V = 916.26 (16) Å3
  • Z = 2
  • Mo Kα radiation
  • μ = 1.30 mm−1
  • T = 298 K
  • 0.42 × 0.41 × 0.40 mm

Data collection

  • Bruker SMART 1000 CCD diffractometer
  • Absorption correction: multi-scan (SADABS; Sheldrick, 1996 [triangle]) T min = 0.611, T max = 0.624
  • 4493 measured reflections
  • 1616 independent reflections
  • 1408 reflections with I > 2σ(I)
  • R int = 0.020

Refinement

  • R[F 2 > 2σ(F 2)] = 0.027
  • wR(F 2) = 0.076
  • S = 1.07
  • 1616 reflections
  • 115 parameters
  • 5 restraints
  • H-atom parameters constrained
  • Δρmax = 0.41 e Å−3
  • Δρmin = −0.55 e Å−3

Data collection: SMART (Siemens, 1996 [triangle]); cell refinement: SAINT (Siemens, 1996 [triangle]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: SHELXTL (Sheldrick, 2008 [triangle]); software used to prepare material for publication: SHELXTL.

Table 1
Selected bond lengths (Å)
Table 2
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810046647/gk2318sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810046647/gk2318Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

This work was supported by the Natural Science Foundation of China (grant No. 20671048, 21041002).

supplementary crystallographic information

Comment

Molecular materials with porous coordination frameworks have recently drawn considerable interest because of their attractive properties. The importance of the work in this area is the construction of porous materials from metal ions and organic ligands as building blocks. As a flexible ligand, 2-(hydroxyethyl)pyridine (hepH) can adopt a variety of possible binding modes. As a contribution to this field, we report here the synthesis and structure of the title compound.

In the title complex molecule, [Ni(SCN)2(C7H9NO)2], the nickel(II) atom displays a distorted octahedral coordination geometry, provided by two N atoms of two thiocyanate ions and by the N and O atoms of two 2-(hydroxyethyl)pyridine ligands. Bond lengths and angles involving the metal centre are typical and comparable with those observed in related Co(II) complexes (Pan et al., 2007; Yu et al., 2010). In the crystal structure, molecules are linked through intermolecular O—H···S hydrogen bonds (Table 1).

Experimental

To a stirred methanol (10 ml) and acetonitrile (10 ml) solution of NiCl2.6H2O (1 mmol, 238 mg) was added 2-(pyridyn-2-yl)ethanol (2 mmol, 246 mg) in 5 ml me thanol and tetramethylammonium hydroxide(0.4 mmol, 165 mg, 25% solution in water). After 30 min to the above solution was added KSCN (2 mmol, 194 mg) and the solution was stirred for additional 6 h. The resulting red solution was filtered and was allowed to stand at room temperature for about one week, whereupon blue block crystal, suitable for X-ray diffraction analysis, was obtained.

Refinement

All H atoms were placed in geometrically idealized positions (O–H= 0.93, C—H = 0.93-0.97 Å) and treated as riding on their parent atoms, with Uiso(H) = 1.2Ueq(C). A rigid bond restraints were applied to the Uij values of Ni1, N2, S1 and C8 atoms via DELU instruction of SHELXL97 (Sheldrick, 2008).

Figures

Fig. 1.
The molecular structure of the title compound, with atom labels and 30% probability displacement ellipsoids. Atoms labelled with the suffix A are generated by the symmetry operation -x + 2,-y,-z.

Crystal data

[Ni(NCS)2(C7H9NO)2]F(000) = 436
Mr = 421.17Dx = 1.527 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 2904 reflections
a = 8.7197 (9) Åθ = 2.4–28.0°
b = 13.8634 (15) ŵ = 1.30 mm1
c = 7.8655 (7) ÅT = 298 K
β = 105.496 (2)°Block, blue
V = 916.26 (16) Å30.42 × 0.41 × 0.40 mm
Z = 2

Data collection

Bruker SMART 1000 CCD diffractometer1616 independent reflections
Radiation source: fine-focus sealed tube1408 reflections with I > 2σ(I)
graphiteRint = 0.020
phi and ω scansθmax = 25.0°, θmin = 2.4°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)h = −10→8
Tmin = 0.611, Tmax = 0.624k = −16→15
4493 measured reflectionsl = −7→9

Refinement

Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.027Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.076H-atom parameters constrained
S = 1.07w = 1/[σ2(Fo2) + (0.0356P)2 + 0.5792P] where P = (Fo2 + 2Fc2)/3
1616 reflections(Δ/σ)max = 0.001
115 parametersΔρmax = 0.41 e Å3
5 restraintsΔρmin = −0.55 e Å3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

xyzUiso*/Ueq
Ni11.00000.50000.00000.03039 (15)
S11.22010 (9)0.69823 (5)0.50929 (9)0.0528 (2)
N10.7906 (2)0.54485 (14)0.0607 (2)0.0341 (4)
N21.1214 (2)0.57961 (15)0.2136 (3)0.0409 (5)
O10.9851 (2)0.62603 (12)−0.1523 (2)0.0415 (4)
H11.07930.6489−0.17170.050*
C10.8438 (3)0.6798 (2)−0.2289 (4)0.0498 (7)
H1A0.84090.6968−0.34930.060*
H1B0.84480.7391−0.16300.060*
C20.6971 (3)0.62185 (19)−0.2278 (3)0.0452 (6)
H2A0.60390.6570−0.29360.054*
H2B0.70050.5613−0.28860.054*
C30.6788 (3)0.60033 (17)−0.0472 (3)0.0373 (5)
C40.5510 (3)0.6363 (2)0.0063 (4)0.0484 (6)
H40.47620.6754−0.06920.058*
C50.5344 (3)0.6142 (2)0.1710 (4)0.0535 (7)
H50.44840.63740.20770.064*
C60.6478 (3)0.5570 (2)0.2799 (4)0.0499 (7)
H60.63970.54090.39200.060*
C70.7733 (3)0.52394 (19)0.2214 (3)0.0415 (6)
H70.84960.48540.29630.050*
C81.1618 (3)0.62905 (16)0.3352 (3)0.0320 (5)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Ni10.0355 (2)0.0261 (2)0.0306 (2)0.00073 (16)0.01065 (17)−0.00126 (16)
S10.0696 (5)0.0394 (4)0.0428 (4)−0.0032 (3)0.0034 (3)−0.0099 (3)
N10.0367 (10)0.0311 (10)0.0352 (10)0.0005 (8)0.0107 (8)−0.0025 (8)
N20.0445 (11)0.0363 (11)0.0409 (10)−0.0004 (9)0.0100 (9)−0.0065 (8)
O10.0447 (9)0.0338 (9)0.0486 (10)0.0025 (7)0.0170 (8)0.0102 (7)
C10.0591 (17)0.0436 (15)0.0482 (15)0.0122 (12)0.0168 (13)0.0162 (12)
C20.0467 (15)0.0452 (15)0.0402 (13)0.0105 (12)0.0057 (11)0.0042 (11)
C30.0365 (12)0.0326 (12)0.0409 (13)−0.0014 (10)0.0070 (10)−0.0048 (10)
C40.0398 (13)0.0425 (15)0.0630 (17)0.0045 (12)0.0137 (12)−0.0034 (12)
C50.0480 (15)0.0498 (16)0.0713 (19)−0.0007 (13)0.0310 (14)−0.0105 (14)
C60.0558 (16)0.0530 (16)0.0485 (15)−0.0084 (13)0.0271 (13)−0.0068 (13)
C70.0453 (14)0.0429 (14)0.0393 (13)−0.0025 (11)0.0163 (11)0.0006 (11)
C80.0324 (12)0.0273 (11)0.0361 (11)0.0002 (9)0.0087 (9)0.0011 (7)

Geometric parameters (Å, °)

Ni1—N22.052 (2)C2—C31.501 (3)
Ni1—N12.1011 (19)C2—H2A0.9700
Ni1—O12.1030 (15)C2—H2B0.9700
S1—C81.637 (2)C3—C41.386 (4)
N1—C71.344 (3)C4—C51.375 (4)
N1—C31.349 (3)C4—H40.9300
N2—C81.153 (3)C5—C61.374 (4)
O1—C11.428 (3)C5—H50.9300
O1—H10.9300C6—C71.375 (4)
C1—C21.513 (4)C6—H60.9300
C1—H1A0.9700C7—H70.9300
C1—H1B0.9700
N2i—Ni1—N2180.00 (9)O1—C1—H1B109.5
N2i—Ni1—N1i86.82 (8)C2—C1—H1B109.5
N2—Ni1—N1i93.18 (8)H1A—C1—H1B108.1
N2i—Ni1—N193.18 (8)C3—C2—C1114.5 (2)
N2—Ni1—N186.82 (8)C3—C2—H2A108.6
N1i—Ni1—N1180.0C1—C2—H2A108.6
N2i—Ni1—O192.32 (7)C3—C2—H2B108.6
N2—Ni1—O187.68 (7)C1—C2—H2B108.6
N1i—Ni1—O192.38 (7)H2A—C2—H2B107.6
N1—Ni1—O187.62 (7)N1—C3—C4121.2 (2)
N2i—Ni1—O1i87.68 (7)N1—C3—C2117.8 (2)
N2—Ni1—O1i92.32 (7)C4—C3—C2120.9 (2)
N1i—Ni1—O1i87.62 (7)C5—C4—C3120.1 (3)
N1—Ni1—O1i92.38 (7)C5—C4—H4119.9
O1—Ni1—O1i180.00 (5)C3—C4—H4119.9
C7—N1—C3118.1 (2)C6—C5—C4118.5 (3)
C7—N1—Ni1118.18 (16)C6—C5—H5120.8
C3—N1—Ni1123.47 (16)C4—C5—H5120.8
C8—N2—Ni1167.28 (19)C5—C6—C7119.2 (3)
C1—O1—Ni1126.06 (15)C5—C6—H6120.4
C1—O1—H1117.0C7—C6—H6120.4
Ni1—O1—H1117.0N1—C7—C6122.8 (3)
O1—C1—C2110.9 (2)N1—C7—H7118.6
O1—C1—H1A109.5C6—C7—H7118.6
C2—C1—H1A109.5N2—C8—S1179.3 (2)
N2i—Ni1—N1—C7121.90 (18)N1—Ni1—O1—C1−23.9 (2)
N2—Ni1—N1—C7−58.10 (18)O1—C1—C2—C365.5 (3)
O1—Ni1—N1—C7−145.91 (18)C7—N1—C3—C41.0 (3)
O1i—Ni1—N1—C734.09 (18)Ni1—N1—C3—C4−173.23 (18)
N2i—Ni1—N1—C3−63.84 (19)C7—N1—C3—C2−178.9 (2)
N2—Ni1—N1—C3116.16 (19)Ni1—N1—C3—C26.9 (3)
O1—Ni1—N1—C328.35 (18)C1—C2—C3—N1−63.6 (3)
O1i—Ni1—N1—C3−151.65 (18)C1—C2—C3—C4116.5 (3)
N1i—Ni1—N2—C8176.2 (9)N1—C3—C4—C5−1.2 (4)
N1—Ni1—N2—C8−3.8 (9)C2—C3—C4—C5178.7 (2)
O1—Ni1—N2—C884.0 (9)C3—C4—C5—C60.7 (4)
O1i—Ni1—N2—C8−96.0 (9)C4—C5—C6—C70.0 (4)
N2i—Ni1—O1—C169.2 (2)C3—N1—C7—C6−0.4 (4)
N2—Ni1—O1—C1−110.8 (2)Ni1—N1—C7—C6174.2 (2)
N1i—Ni1—O1—C1156.1 (2)C5—C6—C7—N1−0.1 (4)

Symmetry codes: (i) −x+2, −y+1, −z.

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
O1—H1···S1ii0.932.663.2183 (19)119

Symmetry codes: (ii) x, −y+3/2, z−1/2.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: GK2318).

References

  • Pan, Y.-P., Li, D.-C. & Wang, D.-Q. (2007). Acta Cryst. E63, m3034.
  • Sheldrick, G. M. (1996). SADABS University of Göttingen, Germany.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
  • Siemens (1996). SMART and SAINT Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA.
  • Yu, Y., Guo, Y., Wang, D. & Li, D. (2010). Acta Cryst. E66, m753. [PMC free article] [PubMed]

Articles from Acta Crystallographica Section E: Structure Reports Online are provided here courtesy of International Union of Crystallography