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Acta Cryst. (2007). E63, m1632    [ doi:10.1107/S1600536807021976 ]

Poly[bis[[mu]2-5-(pyrimidin-2-yl)tetrazolato]nickel(II)]

J.-T. Liu and S.-D. Fan

Abstract top

In the title compound, [Ni(C5H3N6)2]n, the NiII atom is located on an inversion centre and exhibits a distorted octahedral geometry. The crystal structure features a two-dimensional square-grid-like network. The compound is isostructural with the iron(II) and cobalt(II) analogues, whose structures and magnetic properties have been reported [Rodríguez, Kivekäsb & Colacio (2005). Chem. Commun. pp. 5228-5230].

Comment top

Poly[5-(pyrimidin-2-yl)tetrazolato]nickel(II)], (I) (Fig. 1), is isostructural with the iron(II) and cobalt(II) analogs (Rodríguez et al., 2005). The three structures feature a two-dimensional square-grid-like network, in which each metal atom is located on an inversion centre and exhibits a distorted octahedral geometry. Each metal atom bonds to four ligands, and each ligand is coordinated to two metal atoms through one of the pyrimidyl nitrogen atoms and the 1-positon tetrazole nitrogen atom in cis position for one, and one 3-position tetrazole nitrogen atom for the other.

Related literature top

For compound preparation, see: Demko & Sharpless (2001). For related literature, see: Rodríguez et al. (2005).

Experimental top

The ligand, 2-(1H-tetrazol-5-yl)pyrimidine (L), was synthesized according to the literature method (Demko & Sharpless, 2001). A mixture of NiCl2.6H2O (48 mg, 0.2 mmol) and ligand L (60 mg, 0.4 mmol) in water (10 ml) was placed in a Teflon-lined stainless-steel Parr bomb that was heated at 413 K for 72 h. The bomb was then cooled to room temperature. Pink crystals were isolated in about 20% yield.

Refinement top

H atoms bound to C atoms were placed in calculated positions (C—H = 0.93 Å) and refined in the riding-model approximation, with Uiso(H) = 1.2Ueq(C).

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL.

Figures top
[Figure 1] Fig. 1. Part of the two-dimensional network structure of (I). Displacement ellipsoids are drawn at the 40% probability level. [symmetry codes: (A) -x, 1 - y, 1 - z; (B) 1/2 + x, 1/2 - y, 1 - z.]
Poly[bis[µ2-5-(pyrimidin-2-yl)tetrazolato]nickel(II)] top
Crystal data top
[Ni(C5H3N6)2]F(000) = 712
Mr = 352.98Dx = 1.745 Mg m−3
Orthorhombic, PbcaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2abCell parameters from 3035 reflections
a = 8.2054 (16) Åθ = 2.5–26.4°
b = 9.1736 (18) ŵ = 1.47 mm−1
c = 17.846 (4) ÅT = 293 K
V = 1343.3 (5) Å3Block, pink
Z = 40.18 × 0.16 × 0.16 mm
Data collection top
Bruker SMART CCD area-detector
diffractometer		1598 independent reflections
Radiation source: fine-focus sealed tube1396 reflections with I > 2σ(I)
graphiteRint = 0.058
φ and ω scansθmax = 27.9°, θmin = 2.3°
Absorption correction: multi-scan
(SADABS; Bruker, 1998)		h = −10→9
Tmin = 0.974, Tmax = 1.000k = −12→10
9528 measured reflectionsl = −23→22
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)] = 0.053Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.105H-atom parameters constrained
S = 1.20 w = 1/[σ2(Fo2) + (0.032P)2 + 2.6446P]
where P = (Fo2 + 2Fc2)/3
1598 reflections(Δ/σ)max = 0.001
106 parametersΔρmax = 0.56 e Å−3
0 restraintsΔρmin = −0.40 e Å−3
Crystal data top
[Ni(C5H3N6)2]V = 1343.3 (5) Å3
Mr = 352.98Z = 4
Orthorhombic, PbcaMo Kα radiation
a = 8.2054 (16) ŵ = 1.47 mm−1
b = 9.1736 (18) ÅT = 293 K
c = 17.846 (4) Å0.18 × 0.16 × 0.16 mm
Data collection top
Bruker SMART CCD area-detector
diffractometer		1598 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 1998)		1396 reflections with I > 2σ(I)
Tmin = 0.974, Tmax = 1.000Rint = 0.058
9528 measured reflectionsθmax = 27.9°
Refinement top
R[F2 > 2σ(F2)] = 0.053H-atom parameters constrained
wR(F2) = 0.105Δρmax = 0.56 e Å−3
S = 1.20Δρmin = −0.40 e Å−3
1598 reflectionsAbsolute structure: ?
106 parametersFlack parameter: ?
0 restraintsRogers parameter: ?
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
Ni10.00000.50000.50000.00927 (16)
N1−0.1491 (3)0.3232 (3)0.48286 (15)0.0130 (6)
C2−0.0291 (4)0.3372 (3)0.35937 (19)0.0142 (6)
N60.0456 (3)0.4562 (3)0.38656 (15)0.0116 (5)
N5−0.0129 (3)0.2818 (3)0.29133 (16)0.0196 (6)
C50.1446 (4)0.5280 (3)0.3397 (2)0.0175 (7)
H50.19930.61050.35650.021*
C1−0.1385 (4)0.2677 (3)0.41376 (17)0.0121 (6)
C40.1666 (4)0.4812 (4)0.2669 (2)0.0213 (7)
H40.23340.53200.23380.026*
N2−0.2581 (3)0.2430 (3)0.51904 (14)0.0128 (5)
N4−0.2388 (3)0.1549 (3)0.40478 (15)0.0148 (6)
C30.0857 (4)0.3563 (4)0.2450 (2)0.0236 (8)
H30.10000.32250.19630.028*
N3−0.3114 (3)0.1428 (3)0.47178 (16)0.0126 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0094 (3)0.0073 (3)0.0111 (3)0.0006 (2)−0.0003 (2)−0.0005 (2)
N10.0116 (12)0.0106 (11)0.0169 (15)0.0001 (10)0.0008 (10)−0.0004 (10)
C20.0143 (14)0.0136 (14)0.0148 (16)−0.0025 (12)0.0006 (12)0.0005 (12)
N60.0129 (12)0.0080 (11)0.0139 (14)0.0016 (9)−0.0010 (10)0.0007 (9)
N50.0216 (15)0.0220 (14)0.0153 (15)−0.0032 (12)0.0039 (12)−0.0051 (11)
C50.0191 (16)0.0108 (14)0.0227 (18)0.0004 (12)0.0033 (13)0.0008 (12)
C10.0129 (14)0.0127 (14)0.0106 (16)−0.0006 (12)0.0002 (12)−0.0003 (11)
C40.0224 (17)0.0219 (16)0.0195 (18)0.0017 (14)0.0079 (14)0.0040 (14)
N20.0118 (12)0.0114 (12)0.0152 (14)−0.0031 (10)0.0012 (11)−0.0004 (10)
N40.0157 (13)0.0153 (12)0.0134 (14)−0.0015 (11)0.0024 (11)−0.0015 (10)
C30.0272 (18)0.0290 (18)0.0146 (18)−0.0029 (16)0.0060 (14)−0.0019 (15)
N30.0138 (12)0.0095 (11)0.0144 (14)−0.0033 (10)0.0018 (10)−0.0013 (10)
Geometric parameters (Å, °) top
Ni1—N1i2.054 (3)N6—C51.338 (4)
Ni1—N12.054 (3)N5—C31.344 (4)
Ni1—N3ii2.089 (2)C5—C41.382 (5)
Ni1—N3iii2.089 (2)C5—H50.93
Ni1—N6i2.098 (3)C1—N41.332 (4)
Ni1—N62.098 (3)C4—C31.381 (5)
N1—N21.326 (3)C4—H40.93
N1—C11.337 (4)N2—N31.322 (4)
C2—N51.323 (4)N4—N31.340 (4)
C2—N61.343 (4)C3—H30.93
C2—C11.468 (4)N3—Ni1iv2.089 (2)
N1i—Ni1—N1180C5—N6—C2116.8 (3)
N1i—Ni1—N3ii88.98 (10)C5—N6—Ni1128.1 (2)
N1—Ni1—N3ii91.02 (10)C2—N6—Ni1115.0 (2)
N1i—Ni1—N3iii91.02 (10)C2—N5—C3115.5 (3)
N1—Ni1—N3iii88.98 (10)N6—C5—C4121.0 (3)
N3ii—Ni1—N3iii180N6—C5—H5119.5
N1i—Ni1—N6i79.12 (10)C4—C5—H5119.5
N1—Ni1—N6i100.88 (10)N4—C1—N1111.5 (3)
N3ii—Ni1—N6i88.87 (10)N4—C1—C2129.5 (3)
N3iii—Ni1—N6i91.13 (10)N1—C1—C2119.0 (3)
N1i—Ni1—N6100.88 (10)C3—C4—C5117.4 (3)
N1—Ni1—N679.12 (10)C3—C4—H4121.3
N3ii—Ni1—N691.13 (10)C5—C4—H4121.3
N3iii—Ni1—N688.87 (10)N3—N2—N1107.4 (2)
N6i—Ni1—N6180C1—N4—N3103.4 (2)
N2—N1—C1106.4 (2)N5—C3—C4122.5 (3)
N2—N1—Ni1140.1 (2)N5—C3—H3118.7
C1—N1—Ni1113.5 (2)C4—C3—H3118.7
N5—C2—N6126.7 (3)N2—N3—N4111.4 (2)
N5—C2—C1120.1 (3)N2—N3—Ni1iv121.8 (2)
N6—C2—C1113.2 (3)N4—N3—Ni1iv126.6 (2)
N3ii—Ni1—N1—N2−85.7 (3)C2—N6—C5—C40.5 (5)
N3iii—Ni1—N1—N294.3 (3)Ni1—N6—C5—C4177.2 (2)
N6i—Ni1—N1—N23.4 (3)N2—N1—C1—N40.5 (3)
N6—Ni1—N1—N2−176.6 (3)Ni1—N1—C1—N4−179.06 (19)
N3ii—Ni1—N1—C193.6 (2)N2—N1—C1—C2178.4 (3)
N3iii—Ni1—N1—C1−86.4 (2)Ni1—N1—C1—C2−1.2 (3)
N6i—Ni1—N1—C1−177.3 (2)N5—C2—C1—N4−4.5 (5)
N6—Ni1—N1—C12.7 (2)N6—C2—C1—N4175.3 (3)
N5—C2—N6—C51.3 (5)N5—C2—C1—N1178.0 (3)
C1—C2—N6—C5−178.4 (3)N6—C2—C1—N1−2.2 (4)
N5—C2—N6—Ni1−175.8 (3)N6—C5—C4—C3−1.4 (5)
C1—C2—N6—Ni14.4 (3)C1—N1—N2—N3−0.4 (3)
N1i—Ni1—N6—C5−0.8 (3)Ni1—N1—N2—N3178.9 (2)
N1—Ni1—N6—C5179.2 (3)N1—C1—N4—N3−0.3 (3)
N3ii—Ni1—N6—C588.4 (3)C2—C1—N4—N3−177.9 (3)
N3iii—Ni1—N6—C5−91.6 (3)C2—N5—C3—C40.8 (5)
N1i—Ni1—N6—C2176.0 (2)C5—C4—C3—N50.7 (5)
N1—Ni1—N6—C2−4.0 (2)N1—N2—N3—N40.2 (3)
N3ii—Ni1—N6—C2−94.8 (2)N1—N2—N3—Ni1iv−174.80 (18)
N3iii—Ni1—N6—C285.2 (2)C1—N4—N3—N20.0 (3)
N6—C2—N5—C3−2.0 (5)C1—N4—N3—Ni1iv174.8 (2)
C1—C2—N5—C3177.8 (3)
Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x−1/2, y+1/2, z; (iii) x+1/2, −y+1/2, −z+1; (iv) x−1/2, −y+1/2, −z+1.
Table 1
Selected geometric parameters (Å, °) top
Ni1—N12.054 (3)Ni1—N62.098 (3)
Ni1—N3i2.089 (2)
N1—Ni1—N3ii91.02 (10)N1—Ni1—N679.12 (10)
N1—Ni1—N3i88.98 (10)N3ii—Ni1—N691.13 (10)
N1—Ni1—N6iii100.88 (10)N3i—Ni1—N688.87 (10)
Symmetry codes: (i) x+1/2, −y+1/2, −z+1; (ii) −x−1/2, y+1/2, z; (iii) −x, −y+1, −z+1.
Acknowledgements top

The authors thank Dalian Nationalities University for supporting this work.

references
References top

Bruker (1998). SMART (Version 5.051), SAINT (Version 5.01), SADABS (Version 2.03) and SHELXTL (Version 6.1). Bruker AXS Inc., Madison, Wisconsin, USA.

Demko, Z. P. & Sharpless, K. B. (2001). J. Org. Chem. 66, 7945–7950.

Rodríguez, A., Kivekäsb, R. & Colacio, E. (2005). Chem. Commun. pp. 5228–5230.

Sheldrick, G. M. (1997). SHELXL97 and SHELXS97. University of Göttingen, Germany.