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Acta Crystallogr Sect E Struct Rep Online. 2008 August 1; 64(Pt 8): m1040.
Published online 2008 July 19. doi:  10.1107/S1600536808021703
PMCID: PMC2961960

catena-Poly[[bis­(pyridine-κN)nickel(II)]-μ-oxalato-κ4 O 1,O 2:O 1′,O 2′]

Abstract

The title compound, [Ni(C2O4)(C5H5N)2]n, was synthesized under hydro­(solvo)thermal conditions. The NiII atom, lying on a twofold rotation axis, has an octa­hedral coordination geometry involving two N atoms from two pyridine ligands and four O atoms from two oxalate ligands. The Ni atoms are connected by the tetra­dentate bridging oxalate ligands into a one-dimensional zigzag chain.

Related literature

For related literature, see: Lu et al. (1999 [triangle]); Vaidhyanathan et al. (2002 [triangle]); Wang et al. (2007 [triangle]); Yao et al. (2007 [triangle]).

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Object name is e-64-m1040-scheme1.jpg

Experimental

Crystal data

  • [Ni(C2O4)(C5H5N)2]
  • M r = 304.93
  • Monoclinic, An external file that holds a picture, illustration, etc.
Object name is e-64-m1040-efi2.jpg
  • a = 14.357 (3) Å
  • b = 10.801 (2) Å
  • c = 8.6669 (17) Å
  • β = 91.52 (3)°
  • V = 1343.5 (5) Å3
  • Z = 4
  • Mo Kα radiation
  • μ = 1.45 mm−1
  • T = 293 (2) K
  • 0.26 × 0.24 × 0.22 mm

Data collection

  • Rigaku R-AXIS RAPID diffractometer
  • Absorption correction: multi-scan (ABSCOR; Higashi, 1995 [triangle]) T min = 0.640, T max = 0.726
  • 6433 measured reflections
  • 1519 independent reflections
  • 1297 reflections with I > 2σ(I)
  • R int = 0.041

Refinement

  • R[F 2 > 2σ(F 2)] = 0.042
  • wR(F 2) = 0.103
  • S = 1.04
  • 1519 reflections
  • 87 parameters
  • H-atom parameters constrained
  • Δρmax = 0.73 e Å−3
  • Δρmin = −0.30 e Å−3

Data collection: PROCESS-AUTO (Rigaku, 1998 [triangle]); cell refinement: PROCESS-AUTO; data reduction: PROCESS-AUTO; 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 geometric parameters (Å, °)

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808021703/hy2144sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808021703/hy2144Isup2.hkl

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

Acknowledgments

The authors thank Yanbian University for supporting this work.

supplementary crystallographic information

Comment

Much research work has been done on metal–oxalate compounds, in the context of studies of molecular-based magnets and open framework structures (Lu et al., 1999; Yao et al., 2007). The geometrical coordination mode and strength of this ligand provide both rigidity and preferred coordination specificity for metal centers (Vaidhyanathan et al., 2002; Wang et al., 2007). In this paper, we report the hydro(solvo)thermal synthesis and structure of a new one-dimensional nickelous oxalate coordination polymer.

The title compound consists of one NiII atom lying on a twofold rotation axis, an oxalate ligand and two coordinated pyridine molecules (Fig. 1). The NiII atom exhibits a distorted octahedral geometry, defined by four O atoms of two oxalate ligands and two pyridine N atoms in a cis arrangement. The Ni—O distances are 2.046 (2) and 2.0716 (18) Å, while the O—Ni—O angles show distortions particularly as a result of chelation (Table 1). The tetradentate oxalate ligands link adjacent Ni atoms into a one-dimensional zigzag chain.

Experimental

A mixture of K2C2O4.H2O (0.037 g, 0.2 mmol), H3BO3 (0.013 g, 0.2 mmol), NiCl2.2H2O (0.033 g, 0.2 mmol), KOH (0.012 g, 0.2 mmol), pyridine (4 ml) and water (8 ml) in a 25 ml Teflon-lined stainless steel reactor was heated from 298 to 393 K in 2 h and maintained at 393 K for 72 h. After the mixture was cooled to 298 K, blue crystals of the title compound were obtained.

Refinement

H atoms were positioned geometrically and refined as riding atoms, with C—H = 0.93 Å and Uiso(H) = 1.2Ueq(C).

Figures

Fig. 1.
Part of the polymeric structure of the title compound. Displacement ellipsoids are drawn at the 30% probability level. [Symmetry codes: (i) x, 1-y, 1/2+z; (ii) 1-x, 1-y, -z; (iii) 1-x, y, 1/2-z.]

Crystal data

[Ni(C2O4)(C5H5N)2]F000 = 624
Mr = 304.93Dx = 1.508 Mg m3
Monoclinic, C2/cMo Kα radiation λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 1532 reflections
a = 14.357 (3) Åθ = 3.3–27.5º
b = 10.801 (2) ŵ = 1.45 mm1
c = 8.6669 (17) ÅT = 293 (2) K
β = 91.52 (3)ºBlock, blue
V = 1343.5 (5) Å30.26 × 0.24 × 0.22 mm
Z = 4

Data collection

Rigaku R-AXIS RAPID diffractometer1519 independent reflections
Radiation source: rotating anode1297 reflections with I > 2σ(I)
Monochromator: graphiteRint = 0.041
Detector resolution: 10.0 pixels mm-1θmax = 27.5º
T = 293(2) Kθmin = 3.3º
ω scansh = −18→18
Absorption correction: multi-scan(ABSCOR; Higashi, 1995)k = −13→13
Tmin = 0.640, Tmax = 0.726l = −11→10
6433 measured reflections

Refinement

Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.042H-atom parameters constrained
wR(F2) = 0.103  w = 1/[σ2(Fo2) + (0.0487P)2 + 1.5041P] where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max < 0.001
1519 reflectionsΔρmax = 0.73 e Å3
87 parametersΔρmin = −0.30 e Å3
Primary atom site location: structure-invariant direct methodsExtinction correction: none

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

xyzUiso*/Ueq
Ni10.50000.35667 (4)0.25000.04167 (19)
O10.57949 (11)0.49601 (17)0.1553 (2)0.0468 (4)
O20.57299 (12)0.62481 (16)−0.0453 (2)0.0465 (4)
N10.59041 (14)0.2248 (2)0.1633 (3)0.0491 (5)
C10.5679 (2)0.1569 (3)0.0391 (5)0.0726 (10)
H10.50880.1664−0.00590.090*
C20.6274 (3)0.0743 (4)−0.0251 (6)0.0911 (13)
H20.60850.0290−0.11160.090*
C30.7145 (3)0.0584 (3)0.0378 (5)0.0790 (11)
H30.75580.0019−0.00400.090*
C40.7395 (2)0.1274 (4)0.1630 (5)0.0725 (10)
H40.79860.11900.20830.090*
C50.6764 (2)0.2103 (3)0.2231 (4)0.0592 (8)
H50.69460.25770.30830.090*
C60.54390 (16)0.5345 (2)0.0324 (3)0.0405 (5)

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
Ni10.0290 (2)0.0460 (3)0.0499 (3)0.000−0.00167 (18)0.000
O10.0341 (9)0.0554 (11)0.0503 (11)−0.0087 (7)−0.0082 (8)0.0032 (8)
O20.0358 (9)0.0508 (10)0.0527 (11)−0.0083 (7)−0.0047 (8)0.0002 (8)
N10.0351 (11)0.0486 (12)0.0637 (15)0.0030 (9)0.0034 (10)0.0006 (10)
C10.0480 (17)0.074 (2)0.096 (3)0.0063 (15)−0.0007 (17)−0.0296 (19)
C20.067 (2)0.089 (3)0.118 (3)0.007 (2)0.011 (2)−0.043 (3)
C30.060 (2)0.068 (2)0.110 (3)0.0157 (17)0.025 (2)−0.009 (2)
C40.0438 (16)0.086 (2)0.088 (3)0.0185 (15)0.0097 (16)0.021 (2)
C50.0401 (14)0.070 (2)0.067 (2)0.0114 (13)0.0028 (13)0.0074 (15)
C60.0293 (11)0.0451 (13)0.0470 (14)−0.0015 (10)0.0014 (10)−0.0054 (11)

Geometric parameters (Å, °)

Ni1—O2i2.046 (2)C1—C21.364 (5)
Ni1—O2ii2.046 (2)C1—H10.9300
Ni1—O12.0716 (18)C2—C31.362 (6)
Ni1—O1iii2.0716 (18)C2—H20.9300
Ni1—N12.081 (2)C3—C41.357 (6)
Ni1—N1iii2.081 (2)C3—H30.9300
O1—C61.240 (3)C4—C51.385 (5)
O2—C61.263 (3)C4—H40.9300
O2—Ni1ii2.046 (2)C5—H50.9300
N1—C11.335 (4)C6—C6ii1.556 (4)
N1—C51.336 (3)
O2i—Ni1—O2ii168.78 (10)C5—N1—Ni1121.3 (2)
O2i—Ni1—O189.88 (7)N1—C1—C2123.1 (3)
O2ii—Ni1—O181.96 (7)N1—C1—H1118.4
O2i—Ni1—O1iii81.96 (7)C2—C1—H1118.4
O2ii—Ni1—O1iii89.88 (7)C3—C2—C1119.9 (4)
O1—Ni1—O1iii86.81 (11)C3—C2—H2120.1
O2i—Ni1—N194.02 (8)C1—C2—H2120.1
O2ii—Ni1—N193.66 (9)C4—C3—C2118.1 (3)
O1—Ni1—N189.92 (9)C4—C3—H3121.0
O1iii—Ni1—N1174.81 (8)C2—C3—H3121.0
O2i—Ni1—N1iii93.66 (9)C3—C4—C5119.7 (3)
O2ii—Ni1—N1iii94.02 (8)C3—C4—H4120.2
O1—Ni1—N1iii174.81 (8)C5—C4—H4120.2
O1iii—Ni1—N1iii89.92 (9)N1—C5—C4122.4 (3)
N1—Ni1—N1iii93.61 (13)N1—C5—H5118.8
C6—O1—Ni1111.39 (15)C4—C5—H5118.8
C6—O2—Ni1ii111.64 (15)O1—C6—O2125.6 (2)
C1—N1—C5116.8 (3)O1—C6—C6ii117.5 (3)
C1—N1—Ni1121.8 (2)O2—C6—C6ii116.9 (3)

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

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: HY2144).

References

  • Higashi, T. (1995). ABSCOR Rigaku Corporation, Tokyo, Japan.
  • Lu, J.-Y., Lawandy, M.-A. & Li, J. (1999). Inorg. Chem.38, 2695–2704.
  • Rigaku (1998). PROCESS-AUTO Rigaku Corporation, Tokyo, Japan.
  • Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. [PubMed]
  • Vaidhyanathan, R., Natarajan, S. & Rao, C. N. R. (2002). Inorg. Chem.41, 4496–4501. [PubMed]
  • Wang, G.-H., Li, Z.-G., Xu, J.-W. & Hu, N.-H. (2007). Acta Cryst. E63, m289–m291.
  • Yao, H.-G., Ji, M., Ji, S.-H. & An, Y.-L. (2007). Acta Cryst. E63, m1349–m1350.

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