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Acta Cryst. (2007). E63, m1652    [ doi:10.1107/S1600536807023781 ]

Poly[diaqua-[mu]3-nitrato-[[mu]2-5-(2-pyrazinyl)-5H-tetrazolato]lead(II)]

J.-T. Liu, S.-D. Fan and S. W. Ng

Abstract top

In the crystal structure of the polymeric title compound, [Pb(C5H3N6)(NO3)(H2O)2]n, pyrazinyltetrazolate and nitrate ligands chelate a water-coordinated Pb atom, while the heterocyclic ligand is additionally linked to an adjacent Pb atom and the nitrate ligand is linked to two other neighboring Pb atoms. Bridging by the two ligands leads to the formation of a layer architecture with adjacent layers connected into a three-dimensional network by O-H...N hydrogen bonds. The Pb atom has a bicapped square-antiprismatic coordination geometry.

Comment top

The preceeding paper describes the structure of the copper derivative of 2-(1H-tetrazol-5-yl)pyrazine, which is the first report of a metal derivative (Liu et al., 2007).

Related literature top

See Liu et al., 2007 for a report of the copper(II)pyrazinyltetrazolate derivative.

Experimental top

Lead nitrate (33 mg, 0.1 mmol) and 2-(1H-tetrazol-5-yl)pyrazine (30 mg, 0.2 mmol) were dissolved in 10 ml of 1:1 methanol/water solution. The solution was filtered and set aside for crystals to grow. Colorless crystals were isolated in 50% yield after two weeks.

Refinement top

H atoms were placed at calculated positions [C—H = 0.93, O–H = 0.82 Å; U(H) = 1.2Ueq(C,O)], as were included in the refinement in the riding model approximation. The hydrogen atoms of the water molecules were rotated to fit the electron density. The final difference Fourier map had a large peak at 1 Å and a deep hole at 1 Å from Pb1.

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: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2006).

Figures top
[Figure 1] Fig. 1. Thermal ellipsoid plot of a part of the layer structure of the title compound with ellipsoids are drawn at the 70% probability level.
[Figure 2] Fig. 2. A repesentation of the bicapped square-antiprismatic geometry of Pb1.
Poly[diaqua-µ3-nitrato-[µ2-5-(2-pyrazinyl)-5H-tetrazolato]lead(II)] top
Crystal data top
[Pb(C5H3N6)(NO3)(H2O)2]F(000) = 1664
Mr = 452.37Dx = 2.791 Mg m−3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 4180 reflections
a = 25.2969 (6) Åθ = 2.2–28.3°
b = 5.7523 (2) ŵ = 15.70 mm−1
c = 15.7938 (4) ÅT = 295 K
β = 110.484 (1)°Block, colorless
V = 2152.9 (1) Å30.22 × 0.20 × 0.16 mm
Z = 8
Data collection top
Bruker APEX area-detector
diffractometer		2475 independent reflections
Radiation source: fine-focus sealed tube2011 reflections with I > 2σ(I)
graphiteRint = 0.033
φ and ω scansθmax = 27.5°, θmin = 1.7°
Absorption correction: multi-scan
SADABS (Sheldrick, 1996)		h = −31→32
Tmin = 0.056, Tmax = 0.188k = −7→7
8341 measured reflectionsl = −20→20
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)] = 0.027H-atom parameters constrained
wR(F2) = 0.078 w = 1/[σ2(Fo2) + (0.0495P)2 + 3.9882P]
where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max = 0.001
2475 reflectionsΔρmax = 2.05 e Å−3
166 parametersΔρmin = −1.44 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: 0.00140 (8)
Crystal data top
[Pb(C5H3N6)(NO3)(H2O)2]V = 2152.9 (1) Å3
Mr = 452.37Z = 8
Monoclinic, C2/cMo Kα radiation
a = 25.2969 (6) ŵ = 15.70 mm−1
b = 5.7523 (2) ÅT = 295 K
c = 15.7938 (4) Å0.22 × 0.20 × 0.16 mm
β = 110.484 (1)°
Data collection top
Bruker APEX area-detector
diffractometer		2475 independent reflections
Absorption correction: multi-scan
SADABS (Sheldrick, 1996)		2011 reflections with I > 2σ(I)
Tmin = 0.056, Tmax = 0.188Rint = 0.033
8341 measured reflectionsθmax = 27.5°
Refinement top
R[F2 > 2σ(F2)] = 0.027H-atom parameters constrained
wR(F2) = 0.078Δρmax = 2.05 e Å−3
S = 1.04Δρmin = −1.44 e Å−3
2475 reflectionsAbsolute structure: ?
166 parametersFlack parameter: ?
0 restraintsRogers parameter: ?
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Pb10.64631 (1)0.75580 (3)0.70393 (1)0.0202 (1)
O10.6691 (2)0.2869 (6)0.7253 (3)0.035 (1)
O20.7463 (2)0.4286 (7)0.8195 (3)0.050 (1)
O30.7162 (2)0.0889 (7)0.8421 (3)0.050 (1)
O1w0.5588 (1)0.5188 (6)0.6531 (2)0.028 (1)
O2w0.5674 (1)0.9748 (6)0.7340 (2)0.030 (1)
N10.5892 (1)0.9584 (6)0.5529 (2)0.019 (1)
N20.5576 (2)1.1515 (7)0.5335 (2)0.023 (1)
N30.5363 (2)1.1800 (7)0.4459 (2)0.024 (1)
N40.5536 (1)1.0045 (6)0.4050 (2)0.022 (1)
N50.6433 (2)0.3878 (7)0.3736 (2)0.026 (1)
N60.6472 (1)0.5581 (6)0.5411 (2)0.020 (1)
N70.7111 (2)0.2686 (6)0.7966 (3)0.026 (1)
C10.5856 (2)0.8710 (8)0.4729 (2)0.017 (1)
C20.6164 (2)0.6626 (9)0.4636 (3)0.018 (1)
C30.6142 (2)0.5754 (8)0.3806 (3)0.026 (1)
C40.6739 (2)0.2854 (8)0.4513 (4)0.024 (1)
C50.6757 (2)0.3700 (8)0.5335 (3)0.023 (1)
H110.56080.42190.61630.033*
H120.53150.60360.62960.033*
H210.54070.99070.68650.036*
H220.55720.90130.77000.036*
H30.59160.65010.32820.032*
H40.69460.15300.44950.029*
H50.69770.29300.58580.027*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pb10.0189 (2)0.0236 (2)0.0159 (2)−0.0001 (1)0.0034 (1)0.0014 (1)
O10.028 (2)0.042 (2)0.027 (2)0.009 (2)0.001 (2)0.006 (1)
O20.033 (2)0.044 (3)0.071 (3)−0.013 (2)0.015 (2)−0.012 (2)
O30.059 (3)0.038 (2)0.044 (2)0.002 (2)0.005 (2)0.019 (2)
O1w0.025 (2)0.024 (2)0.028 (2)0.002 (1)0.000 (1)−0.006 (1)
O2w0.030 (2)0.040 (2)0.020 (2)0.006 (2)0.007 (1)0.000 (1)
N10.021 (2)0.016 (2)0.018 (2)0.002 (2)0.003 (1)−0.001 (1)
N20.025 (2)0.022 (2)0.022 (2)−0.003 (2)0.008 (2)0.000 (2)
N30.020 (2)0.022 (2)0.025 (2)−0.001 (2)0.003 (2)0.004 (2)
N40.026 (2)0.019 (2)0.017 (2)0.005 (2)0.003 (1)0.001 (1)
N50.031 (2)0.026 (2)0.021 (2)0.000 (2)0.009 (2)−0.002 (2)
N60.019 (2)0.022 (2)0.018 (2)0.002 (2)0.005 (1)0.001 (1)
N70.024 (2)0.028 (3)0.028 (2)0.002 (2)0.011 (2)0.002 (2)
C10.017 (2)0.019 (2)0.015 (2)−0.001 (2)0.005 (2)0.001 (2)
C20.017 (2)0.019 (2)0.021 (2)−0.001 (2)0.010 (2)0.005 (2)
C30.033 (2)0.028 (3)0.015 (2)0.004 (2)0.005 (2)0.001 (2)
C40.020 (2)0.021 (2)0.032 (3)0.002 (2)0.010 (2)−0.004 (2)
C50.023 (2)0.020 (2)0.022 (2)0.003 (2)0.005 (2)0.003 (2)
Geometric parameters (Å, °) top
Pb1—O12.754 (3)N3—N41.351 (5)
Pb1—O1i3.105 (4)N4—C11.337 (5)
Pb1—O23.169 (4)N5—C31.333 (6)
Pb1—O2ii3.033 (4)N5—C41.337 (6)
Pb1—O3i2.976 (4)N6—C51.330 (5)
Pb1—O1w2.483 (3)N6—C21.341 (5)
Pb1—O2w2.541 (3)C1—C21.466 (7)
Pb1—N12.593 (3)C2—C31.386 (6)
Pb1—N5iii2.830 (3)C4—C51.373 (7)
Pb1—N62.819 (3)O1w—H110.8200
O1—N71.253 (6)O1w—H120.8200
O2—N71.243 (5)O2w—H210.8200
O3—N71.240 (5)O2w—H220.8200
N1—C11.334 (5)C3—H30.9300
N1—N21.340 (5)C4—H40.9300
N2—N31.307 (5)C5—H50.9300
O1w—Pb1—O2w70.3 (1)N5iii—Pb1—O264.0 (1)
O1w—Pb1—N178.6 (1)O3i—Pb1—O279.1 (1)
O2w—Pb1—N174.2 (1)O2ii—Pb1—O272.3 (1)
O1w—Pb1—O168.1 (1)O1i—Pb1—O2116.2 (1)
O2w—Pb1—O1127.4 (1)N7—O1—Pb1105.5 (3)
N1—Pb1—O1125.3 (1)N7—O2—Pb185.7 (3)
O1w—Pb1—N677.0 (1)C1—N1—N2105.0 (3)
O2w—Pb1—N6128.9 (1)C1—N1—Pb1122.3 (3)
N1—Pb1—N661.4 (1)N2—N1—Pb1132.8 (2)
O1—Pb1—N669.4 (1)N3—N2—N1109.8 (4)
O1w—Pb1—N5iii80.2 (1)N2—N3—N4109.2 (4)
O2w—Pb1—N5iii71.6 (1)C1—N4—N3104.6 (3)
N1—Pb1—N5iii144.2 (1)C3—N5—C4116.1 (4)
O1—Pb1—N5iii70.9 (1)C5—N6—C2116.2 (3)
N6—Pb1—N5iii139.2 (1)C5—N6—Pb1126.0 (2)
O1w—Pb1—O3i145.5 (1)C2—N6—Pb1117.7 (3)
O2w—Pb1—O3i81.2 (1)O3—N7—O2122.0 (5)
N1—Pb1—O3i112.5 (1)O3—N7—O1118.3 (4)
O1—Pb1—O3i119.7 (1)O2—N7—O1119.7 (4)
N6—Pb1—O3i137.5 (1)N1—C1—N4111.4 (4)
N5iii—Pb1—O3i72.5 (1)N1—C1—C2122.7 (3)
O1w—Pb1—O2ii151.2 (1)N4—C1—C2125.8 (3)
O2w—Pb1—O2ii131.0 (1)N6—C2—C3121.4 (4)
N1—Pb1—O2ii88.6 (1)N6—C2—C1115.8 (3)
O1—Pb1—O2ii100.2 (1)C3—C2—C1122.9 (4)
N6—Pb1—O2ii74.2 (1)N5—C3—C2122.0 (4)
N5iii—Pb1—O2ii122.2 (1)N5—C4—C5121.9 (4)
O3i—Pb1—O2ii63.3 (1)N6—C5—C4122.3 (4)
O1w—Pb1—O1i133.3 (1)Pb1—O1w—H11109.5
O2w—Pb1—O1i67.7 (1)Pb1—O1w—H12109.5
N1—Pb1—O1i71.4 (1)H11—O1w—H12109.5
O1—Pb1—O1i158.0 (2)Pb1—O2w—H21109.5
N6—Pb1—O1i115.8 (1)Pb1—O2w—H22109.5
N5iii—Pb1—O1i104.5 (1)H21—O2w—H22109.5
O3i—Pb1—O1i41.2 (1)N5—C3—H3119.0
O2ii—Pb1—O1i63.3 (1)C2—C3—H3119.0
O1w—Pb1—O2107.6 (1)N5—C4—H4119.0
O2w—Pb1—O2135.1 (1)C5—C4—H4119.0
N1—Pb1—O2150.7 (1)N6—C5—H5118.8
O1—Pb1—O242.0 (1)C4—C5—H5118.8
N6—Pb1—O291.5 (1)
O1w—Pb1—O1—N7−144.1 (3)N1—Pb1—N6—C5178.1 (4)
O2w—Pb1—O1—N7−104.0 (3)O1—Pb1—N6—C5−26.7 (3)
N1—Pb1—O1—N7159.0 (3)N5iii—Pb1—N6—C5−40.4 (4)
N6—Pb1—O1—N7132.2 (3)O3i—Pb1—N6—C585.2 (4)
N5iii—Pb1—O1—N7−57.3 (3)O2ii—Pb1—N6—C580.9 (3)
O3i—Pb1—O1—N7−1.6 (4)O1i—Pb1—N6—C5130.0 (3)
O2ii—Pb1—O1—N763.4 (3)O2—Pb1—N6—C59.8 (3)
O1i—Pb1—O1—N724.0 (7)O1w—Pb1—N6—C282.6 (3)
O2—Pb1—O1—N714.8 (3)O2w—Pb1—N6—C231.8 (3)
O1w—Pb1—O2—N76.0 (3)N1—Pb1—N6—C2−1.4 (3)
O2w—Pb1—O2—N785.4 (3)O1—Pb1—N6—C2153.8 (3)
N1—Pb1—O2—N7−92.1 (3)N5iii—Pb1—N6—C2140.1 (3)
O1—Pb1—O2—N7−14.4 (3)O3i—Pb1—N6—C2−94.2 (3)
N6—Pb1—O2—N7−70.8 (3)O2ii—Pb1—N6—C2−98.5 (3)
N5iii—Pb1—O2—N775.3 (3)O1i—Pb1—N6—C2−49.5 (3)
O3i—Pb1—O2—N7151.0 (3)O2—Pb1—N6—C2−169.7 (3)
O2ii—Pb1—O2—N7−143.7 (3)Pb1—O2—N7—O3−155.2 (5)
O1i—Pb1—O2—N7169.4 (3)Pb1—O2—N7—O125.0 (4)
O1w—Pb1—N1—C1−78.5 (3)Pb1—O1—N7—O3150.0 (4)
O2w—Pb1—N1—C1−151.0 (3)Pb1—O1—N7—O2−30.2 (5)
O1—Pb1—N1—C1−26.0 (4)N2—N1—C1—N40.8 (4)
N6—Pb1—N1—C12.7 (3)Pb1—N1—C1—N4179.5 (3)
N5iii—Pb1—N1—C1−133.2 (3)N2—N1—C1—C2177.2 (4)
O3i—Pb1—N1—C1135.8 (3)Pb1—N1—C1—C2−4.2 (6)
O2ii—Pb1—N1—C175.5 (3)N3—N4—C1—N1−0.8 (5)
O1i—Pb1—N1—C1137.7 (3)N3—N4—C1—C2−177.1 (4)
O2—Pb1—N1—C127.2 (4)C5—N6—C2—C31.1 (6)
O1w—Pb1—N1—N299.7 (4)Pb1—N6—C2—C3−179.4 (3)
O2w—Pb1—N1—N227.2 (3)C5—N6—C2—C1−179.4 (4)
O1—Pb1—N1—N2152.2 (3)Pb1—N6—C2—C10.1 (5)
N6—Pb1—N1—N2−179.0 (4)N1—C1—C2—N62.6 (6)
N5iii—Pb1—N1—N245.0 (4)N4—C1—C2—N6178.4 (4)
O3i—Pb1—N1—N2−46.0 (4)N1—C1—C2—C3−177.9 (4)
O2ii—Pb1—N1—N2−106.3 (4)N4—C1—C2—C3−2.1 (7)
O1i—Pb1—N1—N2−44.0 (3)C4—N5—C3—C21.4 (7)
O2—Pb1—N1—N2−154.5 (3)N6—C2—C3—N5−1.7 (7)
C1—N1—N2—N3−0.5 (4)C1—C2—C3—N5178.8 (4)
Pb1—N1—N2—N3−178.9 (3)C3—N5—C4—C5−0.6 (7)
N1—N2—N3—N40.0 (5)C2—N6—C5—C4−0.3 (6)
N2—N3—N4—C10.5 (4)Pb1—N6—C5—C4−179.8 (3)
O1w—Pb1—N6—C5−97.9 (3)N5—C4—C5—N60.1 (7)
O2w—Pb1—N6—C5−148.7 (3)
Symmetry codes: (i) x, y+1, z; (ii) −x+3/2, y+1/2, −z+3/2; (iii) x, −y+1, z+1/2.
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O1w—H11···N2iv0.822.022.827 (5)171
O1w—H12···N3v0.822.122.932 (5)173
O2w—H21···N4v0.822.323.081 (4)156
O2w—H22···N4vi0.822.232.846 (4)132
Symmetry codes: (iv) x, y−1, z; (v) −x+1, −y+2, −z+1; (vi) x, −y+2, z+1/2.
Table 1
Selected geometric parameters (Å) top
Pb1—O12.754 (3)Pb1—O1w2.483 (3)
Pb1—O1i3.105 (4)Pb1—O2w2.541 (3)
Pb1—O23.169 (4)Pb1—N12.593 (3)
Pb1—O2ii3.033 (4)Pb1—N5iii2.830 (3)
Pb1—O3i2.976 (4)Pb1—N62.819 (3)
Symmetry codes: (i) x, y+1, z; (ii) −x+3/2, y+1/2, −z+3/2; (iii) x, −y+1, z+1/2.
Table 2
Hydrogen-bond geometry (Å, °) top
D—H···AD—HH···AD···AD—H···A
O1w—H11···N2iv0.822.022.827 (5)171
O1w—H12···N3v0.822.122.932 (5)173
O2w—H21···N4v0.822.323.081 (4)156
O2w—H22···N4vi0.822.232.846 (4)132
Symmetry codes: (iv) x, y−1, z; (v) −x+1, −y+2, −z+1; (vi) x, −y+2, z+1/2.
Acknowledgements top

We thank Dalian Nationalities University and the University of Malaya for supporting this study.

references
References top

Barbour, L. J. (2001). J. Supramol. Chem. 1, 189–191.

Bruker (1998). SMART (Version 5.051) and SAINT (Version 5.05). Bruker AXS Inc, Madison, Wisconsin, USA.

Liu, J.-T., Fan, S.-D. & Ng, S. W. (2007). Acta Cryst. E63. submitted (LH2383).

Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany.

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

Westrip, S. P. (2006). publCIF. In preparation.