Acta Cryst. (2008). E64, m1113 [ doi:10.1107/S1600536808023994 ]
![[mu]](/logos/entities/mu_rmgif.gif)
-1H-1,2,4-triazole-3,5-dicarboxylato]In the title compound, [Zn(C4HN3O4)(H2O)3]n, each ZnII atom adopts a distorted octahedral coordination geometry, being surrounded by one chelating and one monodentate 1H-1,2,4-triazole-3,5-dicarboxylate ligand and three water molecules. Adjacent ZnII cations are linked by a 1H-1,2,4-triazole-3,5-dicarboxylate ligand in a 2,![[kappa]](/logos/entities/kappa_rmgif.gif)
3 fashion to form a chain running along the c axis. The crystal packing is stabilized by N-H
O, O-HN and O-HO hydrogen bonds.
A mixture of H3tda (0.0157 g, 0.1 mmol), Zn(NO3)2.6H2O (0.0297 g, 0.1 mmol), and water (10 ml) was stirred for 1 h at room temperature, and then filtered. The filtrate was allowed to evaporate slowly at room temperature. After 3 weeks, colorless block crystals were obtained in 30% yield (0.0082 g) based on ZnII.
H atoms were located in a difference map but refined as riding with N—H = 0.80 Å and O—H = 0.85 Å and with Uiso(H) = 1.2Uiso(N,O).
Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).
![[Figure 1]](./bt2754fig1thm.gif)
| Fig. 1. Local coordination environment of the title compound with 30% thermal ellipsoids. Symmetry code: a: x, -1/2 - y, -1/2 + z. |
![[Figure 2]](./bt2754fig2thm.gif)
| Fig. 2. The one-dimensional chain of the title compound. |
| [Zn(C4HN3O4)(H2O)3] | F000 = 552 |
| Mr = 274.50 | Dx = 2.144 Mg m−3 |
| Monoclinic, P21/c | Mo Kα radiation λ = 0.71073 Å |
| Hall symbol: -P 2ybc | Cell parameters from 805 reflections |
| a = 10.7388 (11) Å | θ = 2.5–28.0º |
| b = 6.6608 (7) Å | µ = 2.92 mm−1 |
| c = 13.7789 (10) Å | T = 293 (2) K |
| β = 120.384 (6)º | Block, colourless |
| V = 850.22 (14) Å3 | 0.13 × 0.12 × 0.12 mm |
| Z = 4 |
| Bruker APEX CCD diffractometer | 1652 independent reflections |
| Radiation source: fine-focus sealed tube | 1501 reflections with I > 2σ(I) |
| Monochromator: graphite | Rint = 0.026 |
| T = 293(2) K | θmax = 26.0º |
| φ and ω scans | θmin = 2.2º |
| Absorption correction: multi-scan (SADABS; Sheldrick, 2000) | h = −12→13 |
| Tmin = 0.703, Tmax = 0.721 | k = −8→7 |
| 4297 measured reflections | l = −16→16 |
| Refinement on F2 | Secondary atom site location: difference Fourier map |
| Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
| R[F2 > 2σ(F2)] = 0.034 | H-atom parameters constrained |
| wR(F2) = 0.090 | w = 1/[σ2(Fo2) + (0.0485P)2 + 1.155P] where P = (Fo2 + 2Fc2)/3 |
| S = 1.06 | (Δ/σ)max < 0.001 |
| 1652 reflections | Δρmax = 0.53 e Å−3 |
| 136 parameters | Δρmin = −0.31 e Å−3 |
| Primary atom site location: structure-invariant direct methods | Extinction correction: none |
| [Zn(C4HN3O4)(H2O)3] | V = 850.22 (14) Å3 |
| Mr = 274.50 | Z = 4 |
| Monoclinic, P21/c | Mo Kα |
| a = 10.7388 (11) Å | µ = 2.92 mm−1 |
| b = 6.6608 (7) Å | T = 293 (2) K |
| c = 13.7789 (10) Å | 0.13 × 0.12 × 0.12 mm |
| β = 120.384 (6)º |
| Bruker APEX CCD diffractometer | 1652 independent reflections |
| Absorption correction: multi-scan (SADABS; Sheldrick, 2000) | 1501 reflections with I > 2σ(I) |
| Tmin = 0.703, Tmax = 0.721 | Rint = 0.026 |
| 4297 measured reflections |
| R[F2 > 2σ(F2)] = 0.034 | 136 parameters |
| wR(F2) = 0.090 | H-atom parameters constrained |
| S = 1.06 | Δρmax = 0.53 e Å−3 |
| 1652 reflections | Δρmin = −0.31 e Å−3 |
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 | ||
| Zn1 | −0.21910 (4) | −0.31001 (6) | −0.54678 (3) | 0.01968 (16) | |
| C1 | −0.5300 (4) | −0.3318 (5) | −0.6300 (2) | 0.0150 (6) | |
| C2 | −0.4615 (3) | −0.2580 (5) | −0.5104 (2) | 0.0138 (6) | |
| C3 | −0.2985 (3) | −0.1691 (5) | −0.3493 (3) | 0.0158 (6) | |
| C4 | −0.1588 (4) | −0.1138 (5) | −0.2453 (3) | 0.0188 (7) | |
| N1 | −0.5320 (3) | −0.2264 (4) | −0.4566 (2) | 0.0164 (6) | |
| N2 | −0.4261 (3) | −0.1687 (4) | −0.3544 (2) | 0.0166 (6) | |
| H2A | −0.4471 | −0.1452 | −0.3071 | 0.020* | |
| N3 | −0.3183 (3) | −0.2244 (4) | −0.4487 (2) | 0.0155 (5) | |
| O1 | −0.4393 (2) | −0.3607 (4) | −0.66272 (18) | 0.0200 (5) | |
| O2 | −0.6604 (3) | −0.3595 (4) | −0.68401 (19) | 0.0258 (6) | |
| O3 | −0.0468 (3) | −0.1174 (5) | −0.2503 (2) | 0.0327 (6) | |
| O4 | −0.1676 (2) | −0.0634 (4) | −0.16134 (18) | 0.0227 (5) | |
| O1W | −0.2327 (3) | −0.0209 (4) | −0.60933 (19) | 0.0305 (6) | |
| H1WA | −0.2626 | 0.0338 | −0.6731 | 0.037* | |
| H1WB | −0.1556 | 0.0484 | −0.5776 | 0.037* | |
| O2W | −0.1842 (2) | −0.6059 (4) | −0.47695 (19) | 0.0231 (5) | |
| H2WA | −0.2630 | −0.6585 | −0.4892 | 0.028* | |
| H2WB | −0.1227 | −0.6151 | −0.4072 | 0.028* | |
| O3W | −0.0099 (2) | −0.2331 (4) | −0.42261 (18) | 0.0199 (5) | |
| H3WA | −0.0169 | −0.1900 | −0.3675 | 0.024* | |
| H3WB | 0.0497 | −0.3301 | −0.3975 | 0.024* |
| U11 | U22 | U33 | U12 | U13 | U23 | |
| Zn1 | 0.0174 (2) | 0.0265 (2) | 0.0153 (2) | −0.00014 (16) | 0.00829 (18) | 0.00025 (15) |
| C1 | 0.0181 (16) | 0.0154 (15) | 0.0108 (15) | −0.0001 (12) | 0.0069 (13) | 0.0002 (12) |
| C2 | 0.0149 (16) | 0.0154 (14) | 0.0108 (14) | 0.0004 (12) | 0.0062 (13) | 0.0004 (12) |
| C3 | 0.0148 (16) | 0.0180 (15) | 0.0142 (15) | −0.0001 (12) | 0.0070 (13) | 0.0000 (12) |
| C4 | 0.0200 (17) | 0.0205 (16) | 0.0114 (15) | −0.0017 (14) | 0.0047 (14) | −0.0023 (12) |
| N1 | 0.0147 (14) | 0.0214 (14) | 0.0127 (13) | −0.0021 (11) | 0.0066 (11) | −0.0020 (10) |
| N2 | 0.0192 (14) | 0.0234 (14) | 0.0097 (13) | 0.0000 (11) | 0.0090 (12) | −0.0015 (10) |
| N3 | 0.0149 (14) | 0.0185 (13) | 0.0117 (13) | −0.0020 (11) | 0.0058 (11) | −0.0016 (10) |
| O1 | 0.0192 (12) | 0.0314 (13) | 0.0105 (11) | −0.0023 (10) | 0.0083 (10) | −0.0029 (9) |
| O2 | 0.0139 (12) | 0.0414 (15) | 0.0172 (12) | −0.0040 (11) | 0.0042 (10) | −0.0087 (11) |
| O3 | 0.0151 (13) | 0.0615 (18) | 0.0201 (13) | −0.0055 (12) | 0.0079 (11) | −0.0142 (12) |
| O4 | 0.0230 (13) | 0.0337 (13) | 0.0122 (11) | −0.0086 (11) | 0.0095 (10) | −0.0049 (10) |
| O1W | 0.0323 (15) | 0.0272 (13) | 0.0200 (12) | −0.0081 (11) | 0.0045 (11) | 0.0055 (10) |
| O2W | 0.0187 (12) | 0.0288 (13) | 0.0187 (12) | −0.0025 (10) | 0.0072 (10) | 0.0037 (10) |
| O3W | 0.0187 (12) | 0.0252 (12) | 0.0170 (11) | 0.0015 (10) | 0.0098 (10) | −0.0006 (10) |
| Zn1—O1W | 2.085 (2) | C3—C4 | 1.505 (5) |
| Zn1—O3W | 2.085 (2) | C4—O3 | 1.241 (4) |
| Zn1—O4i | 2.096 (2) | C4—O4 | 1.252 (4) |
| Zn1—O1 | 2.106 (2) | N1—N2 | 1.342 (4) |
| Zn1—O2W | 2.141 (2) | N2—H2A | 0.8053 |
| Zn1—N3 | 2.177 (3) | O4—Zn1ii | 2.096 (2) |
| C1—O2 | 1.223 (4) | O1W—H1WA | 0.8499 |
| C1—O1 | 1.278 (4) | O1W—H1WB | 0.8500 |
| C1—C2 | 1.508 (4) | O2W—H2WA | 0.8500 |
| C2—N1 | 1.316 (4) | O2W—H2WB | 0.8500 |
| C2—N3 | 1.348 (4) | O3W—H3WA | 0.8500 |
| C3—N3 | 1.328 (4) | O3W—H3WB | 0.8500 |
| C3—N2 | 1.336 (4) | ||
| O1W—Zn1—O3W | 86.17 (10) | N2—C3—C4 | 123.4 (3) |
| O1W—Zn1—O4i | 92.88 (10) | O3—C4—O4 | 125.8 (3) |
| O3W—Zn1—O4i | 97.55 (9) | O3—C4—C3 | 118.0 (3) |
| O1W—Zn1—O1 | 91.02 (10) | O4—C4—C3 | 116.2 (3) |
| O3W—Zn1—O1 | 172.75 (9) | C2—N1—N2 | 102.3 (3) |
| O4i—Zn1—O1 | 89.25 (9) | C3—N2—N1 | 110.9 (3) |
| O1W—Zn1—O2W | 174.71 (10) | C3—N2—H2A | 131.1 |
| O3W—Zn1—O2W | 89.22 (9) | N1—N2—H2A | 118.0 |
| O4i—Zn1—O2W | 85.14 (9) | C3—N3—C2 | 103.4 (3) |
| O1—Zn1—O2W | 93.86 (9) | C3—N3—Zn1 | 147.1 (2) |
| O1W—Zn1—N3 | 93.49 (10) | C2—N3—Zn1 | 109.04 (19) |
| O3W—Zn1—N3 | 95.09 (9) | C1—O1—Zn1 | 118.15 (19) |
| O4i—Zn1—N3 | 166.20 (10) | C4—O4—Zn1ii | 139.4 (2) |
| O1—Zn1—N3 | 78.40 (9) | Zn1—O1W—H1WA | 137.2 |
| O2W—Zn1—N3 | 89.51 (9) | Zn1—O1W—H1WB | 116.3 |
| O2—C1—O1 | 127.2 (3) | H1WA—O1W—H1WB | 93.4 |
| O2—C1—C2 | 119.3 (3) | Zn1—O2W—H2WA | 111.1 |
| O1—C1—C2 | 113.4 (3) | Zn1—O2W—H2WB | 115.7 |
| N1—C2—N3 | 114.6 (3) | H2WA—O2W—H2WB | 108.8 |
| N1—C2—C1 | 124.5 (3) | Zn1—O3W—H3WA | 105.7 |
| N3—C2—C1 | 120.9 (3) | Zn1—O3W—H3WB | 115.1 |
| N3—C3—N2 | 108.8 (3) | H3WA—O3W—H3WB | 106.3 |
| N3—C3—C4 | 127.8 (3) |
| Symmetry codes: (i) x, −y−1/2, z−1/2; (ii) x, −y−1/2, z+1/2. |
| D—H···A | D—H | H···A | D···A | D—H···A |
| N2—H2A···O1ii | 0.81 | 1.95 | 2.723 (3) | 161 |
| O1W—H1WA···O2iii | 0.85 | 1.85 | 2.697 (3) | 176 |
| O1W—H1WB···O3Wiv | 0.85 | 2.16 | 2.946 (3) | 154 |
| O2W—H2WA···N1v | 0.85 | 2.08 | 2.925 (4) | 172 |
| O2W—H2WB···O3vi | 0.85 | 2.01 | 2.848 (3) | 170 |
| O3W—H3WA···O3 | 0.85 | 1.86 | 2.708 (3) | 174 |
| O3W—H3WB···O4vi | 0.85 | 1.91 | 2.753 (3) | 174 |
| Symmetry codes: (ii) x, −y−1/2, z+1/2; (iii) −x−1, y+1/2, −z−3/2; (iv) −x, −y, −z−1; (v) −x−1, −y−1, −z−1; (vi) −x, y−1/2, −z−1/2. |
| D—H···A | D—H | H···A | D···A | D—H···A |
| N2—H2A···O1i | 0.81 | 1.95 | 2.723 (3) | 161 |
| O1W—H1WA···O2ii | 0.85 | 1.85 | 2.697 (3) | 176 |
| O1W—H1WB···O3Wiii | 0.85 | 2.16 | 2.946 (3) | 154 |
| O2W—H2WA···N1iv | 0.85 | 2.08 | 2.925 (4) | 172 |
| O2W—H2WB···O3v | 0.85 | 2.01 | 2.848 (3) | 170 |
| O3W—H3WA···O3 | 0.85 | 1.86 | 2.708 (3) | 174 |
| O3W—H3WB···O4v | 0.85 | 1.91 | 2.753 (3) | 174 |
| Symmetry codes: (i) x, −y−1/2, z+1/2; (ii) −x−1, y+1/2, −z−3/2; (iii) −x, −y, −z−1; (iv) −x−1, −y−1, −z−1; (v) −x, y−1/2, −z−1/2. |
The authors thank the Program for Young Excellent Talents in Southeast University for financial support.
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Tian, J.-L., Yan, S.-P., Liao, D.-Z., Jiang, Z.-H. & Cheng, P. (2003). Inorg. Chem. Commun. 6, 1025–1029.
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Yin, P., Zheng, L.-M., Gao, S. & Xin, X.-Q. (2001). Chem. Commun. pp. 2346–2347.
Synthesis and characterization of coordination polymers is of great interest due to the formation of fascinating structures with interesting applications (Yin et al. 2001; Yang et al. 2004). Among these coordination polymers, one-dimensional chain complexes as important precursors of molecular magnets have attracted wide interest of experimental and theoretical chemists (Tian et al. 2003). Herein, we report a new one-dimensional compound [Zn(Htda)(H2O)3)]n (H3tda = 1H-1,2,4-triazole-3,5-dicarboxylic acid).
The asymmetric unit of the title compound, [Zn(Htda)(H2O)3)]n (H3tda = 1H-1,2,4-triazole-3,5-dicarboxylic acid), contains a ZnII cation, a Htda anion and three coordinated water molecules. In the compound, the ZnII ion displays a slightly distorted octahedral geometry, being surrounded by one chelating and one monodentate Htda ligands, and three H2O molecules. Meanwhile, the adjacent ZnII cations are linked by a µ3-Htda ligand to form a one-dimensional chain. The shortest intrachain Zn···Zn distance is 6.936 (4) Å. The chains are further stabilized by N—H···O and O—H···O hydrogen bonds.