Tetra­aqua­{1-[(1H-1,2,3-benzotriazol-1-yl)meth­yl]-1H-1,2,4-triazole}sulfato­zinc(II) dihydrate

Yan-Zhi Wang; Xiao-Kun Li; Huai-Xia Yang; Wan Zhou; Xiang-Ru Meng

doi:10.1107/S160053681004331X

. 2010 Oct 30;66(Pt 11):m1483. doi: 10.1107/S160053681004331X

Tetraaqua{1-[(1H-1,2,3-benzotriazol-1-yl)methyl]-1H-1,2,4-triazole}sulfatozinc(II) dihydrate

Yan-Zhi Wang ^a, Xiao-Kun Li ^a, Huai-Xia Yang ^a,^*, Wan Zhou ^b, Xiang-Ru Meng ^b

PMCID: PMC3008971 PMID: 21588898

Abstract

In the title complex, [Zn(SO₄)(C₉H₈N₆)(H₂O)₄]·2H₂O, the Zn^II ion is six-coordinated by one N atom from a 1-[(1H-1,2,3-benzotriazol-1-yl)methyl]-1H-1,2,4-triazole ligand and five O atoms from one monodentate sulfate anion and four water molecules in a distorted octahedral geometry. The sulfate tetrahedron is rotationally disordered over two positions in a 0.618 (19):0.382 (19) ratio. In the crystal, adjacent molecules are linked through O—H⋯O and O—H⋯N hydrogen bonds involving the cation, the anion, and the coordinated and uncoordinated water molecules into a three-dimensional network.

Related literature

For background to complexes based on symmetrical N-heterocyclic ligands, see: Fan & Hanson (2005 ▶); Zhao et al. (2007 ▶). For background to complexes with Zn^II, see: Lin et al. (2008 ▶); Liu et al. (2010 ▶).

Experimental

Crystal data

[Zn(SO₄)(C₉H₈N₆)(H₂O)₄]·2H₂O
M _r = 469.74
Triclinic,
a = 7.5439 (15) Å
b = 7.9573 (16) Å
c = 16.151 (3) Å
α = 99.60 (3)°
β = 92.16 (3)°
γ = 112.24 (3)°
V = 879.4 (3) Å³
Z = 2
Mo Kα radiation
μ = 1.58 mm⁻¹
T = 293 K
0.24 × 0.23 × 0.21 mm

Data collection

Rigaku Saturn CCD diffractometer
Absorption correction: multi-scan (CrystalClear; Rigaku/MSC, 2006 ▶) T _min = 0.703, T _max = 0.733
7688 measured reflections
3442 independent reflections
3130 reflections with I > 2σ(I)
R _int = 0.018

Refinement

R[F ² > 2σ(F ²)] = 0.028
wR(F ²) = 0.070
S = 1.04
3442 reflections
272 parameters
H-atom parameters constrained
Δρ_max = 0.29 e Å⁻³
Δρ_min = −0.27 e Å⁻³

Data collection: CrystalClear (Rigaku/MSC, 2006 ▶); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXL97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL.

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S160053681004331X/wm2415sup1.cif

e-66-m1483-sup1.cif^{(22.6KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S160053681004331X/wm2415Isup2.hkl

e-66-m1483-Isup2.hkl^{(168.8KB, hkl)}

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

Table 1. Hydrogen-bond geometry (Å, °).

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O8—H8A⋯O3′	0.85	2.29	2.793 (14)	118
O10—H10A⋯O1	0.85	2.09	2.938 (2)	178
O10—H10A⋯O2′	0.85	2.51	3.028 (8)	120
O5—H5B⋯O4ⁱ	0.85	1.94	2.761 (5)	163
O5—H5B⋯O4′ⁱ	0.85	2.19	2.988 (13)	156
O7—H7B⋯O1ⁱ	0.85	1.98	2.823 (2)	170
O5—H5A⋯O10ⁱⁱ	0.85	1.90	2.731 (2)	165
O6—H6A⋯O4ⁱⁱⁱ	0.85	1.94	2.752 (5)	159
O6—H6A⋯O4′ⁱⁱⁱ	0.85	1.94	2.778 (8)	171
O6—H6B⋯O10^iv	0.85	1.96	2.808 (2)	172
O7—H7A⋯O2′^iv	0.85	1.84	2.684 (7)	171
O7—H7A⋯O2^iv	0.85	1.87	2.701 (4)	164
O8—H8B⋯O9^v	0.85	1.82	2.673 (3)	177
O8—H8A⋯N2^vi	0.85	2.37	3.122 (3)	148
O9—H9B⋯O3^vii	0.85	2.03	2.837 (8)	159
O9—H9B⋯O2′^vii	0.85	2.22	2.919 (17)	139
O9—H9B⋯O3′^vii	0.85	2.48	3.266 (17)	154
O9—H9A⋯N6^viii	0.85	2.01	2.854 (3)	174
O10—H10B⋯O2^ix	0.85	1.99	2.806 (10)	159
O10—H10B⋯O4′^ix	0.85	2.08	2.836 (15)	147

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Symmetry codes: (i) Inline graphic ; (ii) ; (iii) ; (iv) ; (v) ; (vi) ; (vii) ; (viii) ; (ix) .

Acknowledgments

The study was supported by the Science and Technology Department of Henan Province (grant No. 082102330003).

supplementary crystallographic information

Comment

Up to now, numerous complexes with one-, two- and three-dimensional structure motifs based on symmetrical N-heterocyclic ligands have been synthesized and reported (Fan & Hanson, 2005; Zhao et al., 2007), whereas complexes based on unsymmetrical N-heterocyclic ligands are relatively scarce. Focused on complexes with Zn^II, this ion is able to coordinate to different donors simultaneously and the final products can exhibit promising luminescent properties (Lin et al., 2008; Liu et al., 2010). In this work, through the reaction of 1-((benzotriazol-1-yl)methyl)-1-H-1,2,4-triazole (bmt) with zinc sulfate at room temperature, we obtained the title complex [Zn(bmt)(SO₄)(H₂O)₄](H₂O)₂, which is reported here.

As shown in Figure 1, the Zn^II ion displays a distorted octahedral coordination defined by five oxygen atoms from four water molecules and one monodentate sulfate anion and by one nitrogen atom from the bmt ligand. Atoms O1, O5, O6, O8 and Zn1 are nearly co-planar (the mean deviation from the plane is 0.0258 Å), and atoms O7 and N1 are located in the apical positions. The SO₄ tetrahedron is rotationally disordered about its S—O axis passing through O1 and S1 atoms. O—H···O and O—H···N hydrogen bonds including coordinated and uncoordinated water molecules, the cations and anions consolidate the crystal packing (Figure 2).

Experimental

The ligand 1-((benzotriazol-1-yl)methyl)-1-H-1,2,4-triazole (0.1 mmol) in methanol (5 ml) was added dropwise to an aqueous solution (2 ml) of zinc sulfate (0.1 mmol). The resulting solution was allowed to stand at room temperature. After three weeks, colorless crystals with good quality were obtained from the filtrate and were dried in air.