Acta Cryst. (2007). E63, m2034 [ doi:10.1107/S160053680703111X ]
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N1]nickel(II)In the title compound, [Ni(C5H3N6)2(H2O)2], the central Ni atom is located on a centre of inversion and is coordinated by two chelating pyrazinyltetrazolate ligands and two water molecules in a slightly distorted octahedral geometry [Ni-N = 2.082 (2) and 2.125 (2) Å, and Ni-O = 2.068 (2) Å]. These molecules are linked by O-H
N hydrogen bonds into a three-dimensional network.
A 5 ml of NiCl2.6H2O (48 mg, 0.2 mmol) solution in methanol was layered on a 10 ml of 2-(1H-tetrazol-5-yl)pyrazine (60 mg, 0.4 mmol) solution in methanol/water (1:1), and allowed to stand. After two months, purple crystals of (I) were isolated in about 20% yield.
H atoms bound to carbon were included in calculated positions and treated in the subsequent refinement as riding atoms, with C—H = 0.93 Å and Uiso(H) = 1.2 Ueq(C,N). The H atoms of the water molecules were located in Fourier difference maps and refined with isotropic displacement parameters set at 1.5 times those of the parent O atoms.
Data collection: SMART (Bruker, 1998); cell refinement: SMART; data reduction: SAINT (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97; molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL.
![[Figure 1]](./hg2242fig1thm.gif)
| Fig. 1. The molecular structure of (I). Displacement ellipsoids are drawn at the 30% probability level. [symmetry code: (A) -x, 2 - y, 2 - z.] |
![[Figure 2]](./hg2242fig2thm.gif)
| Fig. 2. Three-dimensional hydrogen-bonded network. |
| [Ni(C5H3N6)2(H2O)2] | F(000) = 396 |
| Mr = 389.01 | Dx = 1.812 Mg m−3 |
| Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
| Hall symbol: -P 2yn | Cell parameters from 2310 reflections |
| a = 6.1539 (11) Å | θ = 2.7–26.3° |
| b = 11.3456 (19) Å | µ = 1.40 mm−1 |
| c = 10.6126 (18) Å | T = 294 K |
| β = 105.845 (2)° | Block, purple |
| V = 712.8 (2) Å3 | 0.22 × 0.20 × 0.20 mm |
| Z = 2 |
| Bruker SMART CCD area-detector diffractometer | 1451 independent reflections |
| Radiation source: fine-focus sealed tube | 1223 reflections with I > 2σ(I) |
| graphite | Rint = 0.024 |
| φ and ω scans | θmax = 26.4°, θmin = 2.7° |
| Absorption correction: multi-scan (SADABS; Bruker, 1998) | h = −6→7 |
| Tmin = 0.948, Tmax = 1.000 | k = −11→14 |
| 3871 measured reflections | l = −13→11 |
| Refinement on F2 | Primary atom site location: structure-invariant direct methods |
| Least-squares matrix: full | Secondary atom site location: difference Fourier map |
| R[F2 > 2σ(F2)] = 0.024 | Hydrogen site location: inferred from neighbouring sites |
| wR(F2) = 0.065 | H atoms treated by a mixture of independent and constrained refinement |
| S = 1.06 | w = 1/[σ2(Fo2) + (0.0305P)2 + 0.3065P] where P = (Fo2 + 2Fc2)/3 |
| 1451 reflections | (Δ/σ)max < 0.001 |
| 123 parameters | Δρmax = 0.39 e Å−3 |
| 2 restraints | Δρmin = −0.25 e Å−3 |
| [Ni(C5H3N6)2(H2O)2] | V = 712.8 (2) Å3 |
| Mr = 389.01 | Z = 2 |
| Monoclinic, P21/n | Mo Kα radiation |
| a = 6.1539 (11) Å | µ = 1.40 mm−1 |
| b = 11.3456 (19) Å | T = 294 K |
| c = 10.6126 (18) Å | 0.22 × 0.20 × 0.20 mm |
| β = 105.845 (2)° |
| Bruker SMART CCD area-detector diffractometer | 1451 independent reflections |
| Absorption correction: multi-scan (SADABS; Bruker, 1998) | 1223 reflections with I > 2σ(I) |
| Tmin = 0.948, Tmax = 1.000 | Rint = 0.024 |
| 3871 measured reflections | θmax = 26.4° |
| R[F2 > 2σ(F2)] = 0.024 | H atoms treated by a mixture of independent and constrained refinement |
| wR(F2) = 0.065 | Δρmax = 0.39 e Å−3 |
| S = 1.06 | Δρmin = −0.25 e Å−3 |
| 1451 reflections | Absolute structure: ? |
| 123 parameters | Flack parameter: ? |
| 2 restraints | Rogers parameter: ? |
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. |
| x | y | z | Uiso*/Ueq | ||
| Ni1 | 0.0000 | 1.0000 | 1.0000 | 0.02261 (12) | |
| N1 | 0.1308 (3) | 1.17316 (13) | 0.99873 (14) | 0.0247 (3) | |
| N2 | 0.2383 (3) | 1.41026 (16) | 0.9762 (2) | 0.0456 (5) | |
| N3 | −0.4243 (3) | 1.25269 (15) | 0.79180 (16) | 0.0328 (4) | |
| N4 | −0.5848 (3) | 1.16844 (16) | 0.76264 (17) | 0.0367 (4) | |
| N5 | −0.5029 (3) | 1.06965 (15) | 0.82244 (16) | 0.0333 (4) | |
| N6 | −0.2877 (3) | 1.08776 (14) | 0.89169 (15) | 0.0275 (4) | |
| C1 | 0.3369 (3) | 1.21598 (18) | 1.05560 (19) | 0.0313 (4) | |
| H1C | 0.4478 | 1.1655 | 1.1038 | 0.038* | |
| C2 | 0.3893 (4) | 1.3336 (2) | 1.0445 (2) | 0.0391 (5) | |
| H2A | 0.5343 | 1.3600 | 1.0859 | 0.047* | |
| C3 | 0.0328 (4) | 1.36789 (18) | 0.9198 (2) | 0.0385 (5) | |
| H3A | −0.0775 | 1.4188 | 0.8718 | 0.046* | |
| C4 | −0.0221 (3) | 1.25059 (17) | 0.93032 (17) | 0.0260 (4) | |
| C5 | −0.2457 (3) | 1.20037 (16) | 0.87052 (18) | 0.0255 (4) | |
| O1 | 0.0740 (3) | 0.96615 (14) | 0.82476 (15) | 0.0369 (4) | |
| H1A | 0.204 (2) | 0.985 (2) | 0.819 (3) | 0.055 (8)* | |
| H1B | 0.037 (5) | 0.8993 (14) | 0.789 (3) | 0.070 (9)* |
| U11 | U22 | U33 | U12 | U13 | U23 | |
| Ni1 | 0.02113 (18) | 0.01848 (18) | 0.02574 (18) | −0.00025 (13) | 0.00220 (13) | 0.00169 (13) |
| N1 | 0.0232 (8) | 0.0255 (8) | 0.0244 (8) | −0.0001 (6) | 0.0047 (6) | −0.0001 (6) |
| N2 | 0.0394 (11) | 0.0286 (10) | 0.0617 (12) | −0.0085 (8) | 0.0018 (9) | 0.0004 (9) |
| N3 | 0.0283 (9) | 0.0323 (9) | 0.0348 (9) | 0.0015 (7) | 0.0037 (7) | 0.0064 (7) |
| N4 | 0.0278 (9) | 0.0391 (10) | 0.0382 (9) | −0.0006 (8) | 0.0006 (7) | 0.0055 (8) |
| N5 | 0.0250 (9) | 0.0338 (10) | 0.0376 (9) | −0.0039 (7) | 0.0027 (7) | 0.0004 (8) |
| N6 | 0.0215 (8) | 0.0261 (8) | 0.0321 (8) | −0.0012 (7) | 0.0025 (7) | 0.0012 (7) |
| C1 | 0.0252 (10) | 0.0340 (11) | 0.0311 (10) | 0.0006 (8) | 0.0014 (8) | 0.0000 (8) |
| C2 | 0.0312 (11) | 0.0387 (12) | 0.0427 (12) | −0.0085 (9) | 0.0019 (9) | −0.0061 (10) |
| C3 | 0.0361 (12) | 0.0263 (11) | 0.0485 (13) | −0.0002 (9) | 0.0038 (10) | 0.0043 (9) |
| C4 | 0.0258 (10) | 0.0252 (9) | 0.0263 (9) | 0.0008 (8) | 0.0056 (7) | 0.0012 (8) |
| C5 | 0.0248 (9) | 0.0238 (9) | 0.0276 (9) | 0.0021 (8) | 0.0065 (8) | 0.0022 (7) |
| O1 | 0.0389 (9) | 0.0367 (9) | 0.0376 (8) | −0.0126 (7) | 0.0150 (7) | −0.0101 (7) |
| Ni1—N1 | 2.1245 (16) | N4—N5 | 1.319 (2) |
| Ni1—N6 | 2.0823 (15) | N5—N6 | 1.343 (2) |
| Ni1—O1 | 2.0679 (15) | N6—C5 | 1.335 (2) |
| Ni1—O1i | 2.0679 (15) | C1—C2 | 1.386 (3) |
| Ni1—N6i | 2.0823 (16) | C1—H1C | 0.9300 |
| Ni1—N1i | 2.1245 (16) | C2—H2A | 0.9300 |
| N1—C1 | 1.338 (2) | C3—C4 | 1.385 (3) |
| N1—C4 | 1.346 (2) | C3—H3A | 0.9300 |
| N2—C3 | 1.332 (3) | C4—C5 | 1.464 (3) |
| N2—C2 | 1.333 (3) | O1—H1A | 0.843 (10) |
| N3—C5 | 1.325 (2) | O1—H1B | 0.850 (10) |
| N3—N4 | 1.348 (2) | ||
| O1i—Ni1—O1 | 180.000 (1) | C5—N6—N5 | 105.16 (15) |
| O1i—Ni1—N6 | 92.57 (7) | C5—N6—Ni1 | 112.10 (12) |
| O1—Ni1—N6 | 87.43 (7) | N5—N6—Ni1 | 142.32 (13) |
| O1i—Ni1—N6i | 87.43 (7) | N1—C1—C2 | 121.68 (19) |
| O1—Ni1—N6i | 92.57 (7) | N1—C1—H1C | 119.2 |
| N6—Ni1—N6i | 180.000 (1) | C2—C1—H1C | 119.2 |
| O1i—Ni1—N1 | 90.62 (6) | N2—C2—C1 | 122.0 (2) |
| O1—Ni1—N1 | 89.38 (6) | N2—C2—H2A | 119.0 |
| N6—Ni1—N1 | 79.68 (6) | C1—C2—H2A | 119.0 |
| N6i—Ni1—N1 | 100.32 (6) | N2—C3—C4 | 122.2 (2) |
| O1i—Ni1—N1i | 89.38 (6) | N2—C3—H3A | 118.9 |
| O1—Ni1—N1i | 90.62 (6) | C4—C3—H3A | 118.9 |
| N6—Ni1—N1i | 100.32 (6) | N1—C4—C3 | 121.38 (18) |
| N6i—Ni1—N1i | 79.68 (6) | N1—C4—C5 | 114.57 (17) |
| N1—Ni1—N1i | 180.0 | C3—C4—C5 | 124.06 (18) |
| C1—N1—C4 | 116.31 (17) | N3—C5—N6 | 111.69 (17) |
| C1—N1—Ni1 | 130.31 (13) | N3—C5—C4 | 128.19 (18) |
| C4—N1—Ni1 | 113.38 (12) | N6—C5—C4 | 120.11 (16) |
| C3—N2—C2 | 116.37 (19) | Ni1—O1—H1A | 117.2 (19) |
| C5—N3—N4 | 104.87 (16) | Ni1—O1—H1B | 118 (2) |
| N5—N4—N3 | 109.39 (16) | H1A—O1—H1B | 110 (3) |
| N4—N5—N6 | 108.90 (16) | ||
| O1i—Ni1—N1—C1 | 85.06 (17) | Ni1—N1—C1—C2 | −179.17 (15) |
| O1—Ni1—N1—C1 | −94.94 (17) | C3—N2—C2—C1 | 0.6 (3) |
| N6—Ni1—N1—C1 | 177.56 (18) | N1—C1—C2—N2 | −0.4 (3) |
| N6i—Ni1—N1—C1 | −2.44 (18) | C2—N2—C3—C4 | −0.4 (3) |
| O1i—Ni1—N1—C4 | −94.15 (13) | C1—N1—C4—C3 | 0.1 (3) |
| O1—Ni1—N1—C4 | 85.85 (13) | Ni1—N1—C4—C3 | 179.45 (16) |
| N6—Ni1—N1—C4 | −1.65 (13) | C1—N1—C4—C5 | −179.58 (17) |
| N6i—Ni1—N1—C4 | 178.35 (13) | Ni1—N1—C4—C5 | −0.2 (2) |
| C5—N3—N4—N5 | 0.0 (2) | N2—C3—C4—N1 | 0.1 (3) |
| N3—N4—N5—N6 | 0.1 (2) | N2—C3—C4—C5 | 179.8 (2) |
| N4—N5—N6—C5 | −0.1 (2) | N4—N3—C5—N6 | 0.0 (2) |
| N4—N5—N6—Ni1 | −171.40 (16) | N4—N3—C5—C4 | 178.99 (18) |
| O1i—Ni1—N6—C5 | 93.53 (14) | N5—N6—C5—N3 | 0.1 (2) |
| O1—Ni1—N6—C5 | −86.47 (14) | Ni1—N6—C5—N3 | 174.35 (13) |
| N1—Ni1—N6—C5 | 3.37 (13) | N5—N6—C5—C4 | −179.04 (16) |
| N1i—Ni1—N6—C5 | −176.63 (13) | Ni1—N6—C5—C4 | −4.8 (2) |
| O1i—Ni1—N6—N5 | −95.5 (2) | N1—C4—C5—N3 | −175.51 (19) |
| O1—Ni1—N6—N5 | 84.5 (2) | C3—C4—C5—N3 | 4.8 (3) |
| N1—Ni1—N6—N5 | 174.3 (2) | N1—C4—C5—N6 | 3.4 (3) |
| N1i—Ni1—N6—N5 | −5.7 (2) | C3—C4—C5—N6 | −176.24 (19) |
| C4—N1—C1—C2 | 0.0 (3) |
| Symmetry codes: (i) −x, −y+2, −z+2. |
| D—H···A | D—H | H···A | D···A | D—H···A |
| O1—H1A···N5ii | 0.84 (1) | 2.04 (1) | 2.863 (2) | 166 (2) |
| O1—H1B···N3iii | 0.85 (1) | 1.91 (1) | 2.761 (2) | 175 (3) |
| Symmetry codes: (ii) x+1, y, z; (iii) −x−1/2, y−1/2, −z+3/2. |
| Ni1—N1 | 2.1245 (16) | Ni1—O1 | 2.0679 (15) |
| Ni1—N6 | 2.0823 (15) | ||
| O1i—Ni1—N6 | 92.57 (7) | O1—Ni1—N1 | 89.38 (6) |
| O1—Ni1—N6 | 87.43 (7) | N6—Ni1—N1 | 79.68 (6) |
| O1i—Ni1—N6i | 87.43 (7) | N6i—Ni1—N1 | 100.32 (6) |
| O1i—Ni1—N1 | 90.62 (6) |
| Symmetry codes: (i) −x, −y+2, −z+2. |
| D—H···A | D—H | H···A | D···A | D—H···A |
| O1—H1A···N5ii | 0.84 (1) | 2.04 (1) | 2.863 (2) | 166 (2) |
| O1—H1B···N3iii | 0.85 (1) | 1.91 (1) | 2.761 (2) | 175 (3) |
| Symmetry codes: (ii) x+1, y, z; (iii) −x−1/2, y−1/2, −z+3/2. |
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.
Deng, H., Qiu, Y.-C., Zeng, R.-H. & Sun, F. (2007). Acta Cryst. E63, m450–m451.
Liu, J.-T., Fan, S.-D. & Ng, S. W. (2007a). Acta Cryst. E63, m1651–?.
Liu, J.-T., Fan, S.-D. & Ng, S. W. (2007b). Acta Cryst. E63, m1652–?.
Luo, J., Zhang, X.-R., Cui, L.-L., Dai, W.-Q. & Liu, B.-S. (2006). Acta Cryst. C62, m614–m616.
Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Göttingen, Germany.
Song, W.-D. & Xi, D.-L. (2006). Acta Cryst. E62, m2841–m2842.
Zeng, R.-H., Cui, Y.-C., Liu, Z.-H., Li, Y.-H. & Deng, H. (2007). Acta Cryst. E63, m1591–?.
Recently, we (Liu et al., 2007a, 2007b) and others (Deng et al., 2007; Luo et al., 2006; Song et al., 2006; Zeng et al., 2007) reported the crystal structures of Cu(II), Pb(II), Mn(II), Zn(II), Co(II) and Fe(II) complexes with the 5-(2-pyrazinyl)-5H-tetrazolate ligand. Except for that of the Pb(II) (one dimensional), these complexes adopt a mononuclear structure, being isomorphous with the title compound, C10H10NiN12O2 (I) (Fig. 1). The central Ni atom, located on a center of inversion, is coordinated by two water molecules and two ligand molecules to form a slightly distorted octahedral geometry. Furthermore, a three-dimensional supramolecular framework (Fig. 2) is formed by the intermolecular O—H—N hydrogen-bond interactions. The hydrogen bond parameters are listed in Table 2.