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

Yu-xian Li; Da-wei Li; Dong Zhao

doi:10.1107/S1600536811032442

. 2011 Aug 17;67(Pt 9):m1251. doi: 10.1107/S1600536811032442

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

Yu-xian Li ^a,^*, Da-wei Li ^b, Dong Zhao ^c

PMCID: PMC3200735 PMID: 22058864

Abstract

In the title complex, [Cd(SO₄)(C₉H₈N₆)(H₂O)₄]·2H₂O, the Cd^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 by five O atoms from four water molecules and one monodentate sulfate anion in a distorted octahedral geometry. The sulfate tetrahedron is rotationally disordered over two positions in a 0.651 (12):0.349 (12) ratio. In the crystal, adjacent molecules are linked through O—H⋯O and O—H⋯N hydrogen bonds into a three-dimensional network.

Related literature

For background to complexes based on triazolyl or benzotriazolyl ligands, see: Meng et al. (2009 ▶); Yang et al. (2011 ▶).

Experimental

Crystal data

[Cd(SO₄)(C₉H₈N₆)(H₂O)₄]·2H₂O
M _r = 516.77
Triclinic,
a = 7.7154 (15) Å
b = 8.0667 (16) Å
c = 16.369 (3) Å
α = 100.12 (3)°
β = 91.64 (3)°
γ = 112.38 (3)°
V = 922.3 (3) Å³
Z = 2
Mo Kα radiation
μ = 1.36 mm⁻¹
T = 293 K
0.19 × 0.17 × 0.14 mm

Data collection

Rigaku Saturn CCD diffractometer
Absorption correction: multi-scan (REQAB; Jacobson, 1998 ▶) T _min = 0.782, T _max = 0.832
8812 measured reflections
3608 independent reflections
3361 reflections with I > 2σ(I)
R _int = 0.020

Refinement

R[F ² > 2σ(F ²)] = 0.025
wR(F ²) = 0.057
S = 1.05
3608 reflections
272 parameters
H-atom parameters constrained
Δρ_max = 0.56 e Å⁻³
Δρ_min = −0.32 e Å⁻³

Data collection: CrystalClear (Rigaku/MSC, 2006 ▶); cell refinement: CrystalClear; data reduction: CrystalClear; 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.

Supplementary Material

Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536811032442/pk2337sup1.cif

e-67-m1251-sup1.cif^{(22.3KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811032442/pk2337Isup2.hkl

e-67-m1251-Isup2.hkl^{(176.9KB, 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—H8W⋯O9	0.85	1.89	2.732 (3)	170
O6—H4W⋯O2′	0.85	2.39	2.905 (19)	119
O5—H1W⋯O4ⁱ	0.85	1.91	2.719 (4)	157
O5—H1W⋯O4′ⁱ	0.85	1.84	2.672 (7)	166
O5—H2W⋯O1ⁱⁱ	0.85	1.97	2.817 (3)	172
O8—H7W⋯O3ⁱⁱ	0.85	2.00	2.795 (4)	156
O8—H7W⋯O3′ⁱⁱ	0.85	2.38	3.127 (15)	147
O6—H3W⋯O10ⁱⁱⁱ	0.85	1.83	2.680 (3)	178
O6—H4W⋯N2^iv	0.85	2.27	3.025 (3)	148
O7—H5W⋯O3^v	0.85	1.93	2.730 (4)	157
O9—H9W⋯O4^v	0.85	2.00	2.795 (6)	155
O7—H5W⋯O3′^v	0.85	1.91	2.720 (8)	159
O9—H9W⋯O3′^v	0.85	2.06	2.844 (14)	155
O7—H6W⋯O9^vi	0.85	1.97	2.791 (3)	161
O9—H10W⋯O1^vii	0.85	2.06	2.906 (3)	175
O9—H10W⋯O4′^vii	0.85	2.48	3.030 (11)	123
O10—H11W⋯N6^viii	0.85	2.01	2.861 (3)	177
O10—H12W⋯O2^ix	0.85	2.02	2.809 (8)	155
O10—H12W⋯O4′^ix	0.85	2.19	2.944 (14)	148
O10—H12W⋯O2′^ix	0.85	2.51	3.280 (16)	151

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

supplementary crystallographic information

Comment

Numerous supramolecular complexes based on triazolyl or benzotriazolyl ligands which have abundant N-donor sites have been synthesized. These show a variety of discrete or infinite frameworks of one-, two-, and three-dimensional motifs (Meng et al., 2009; Yang et al., 2011). In order to further explore frameworks with new structures, we used 1H-1,2,3-benzotriazol-1-yl)methyl]-1H-1,2,4-triazole to react with CdSO₄ at room temperature and obtained the title complex [Cd(SO₄) (C₉H₈N₆) (H₂O)₄] (H₂O)₂, which is reported here. As shown in Fig. 1, the Cd^II ion is located in a distorted octahedral coordination environment and is coordinated to five oxygen atoms from four water molecules and one monodentate sulfate anion and one nitrogen atom from the 1H-1,2,3-benzotriazol-1-yl)methyl]-1H-1,2,4-triazole ligand. Atoms O1, O6, O7, O8 and Cd1 are nearly co-planar (the mean deviation from the plane is 0.0473 Å), O5 and N1 atoms are located in the apical positions. The SO₄ tetrahedron is rotationally disordered about its S—O axis passing though O1 and S1 atoms. Intramolecular O—H···O hydrogen bonds stabilize the molecular configuration and O—H···O, O—H···N hydrogen bonds between adjacent molecules consolidate the crystal packing (Fig. 2).

Experimental

The ligand 1H-1,2,3-benzotriazol-1-yl)methyl]-1H-1,2,4-triazole (0.1 mmol) in methanol (4 ml) was added dropwise to an aqueous solution (3 ml) of cadmium sulfate (0.1 mmol). The resulting solution was allowed to stand at room temperature. After three weeks colourless crystals of good quality were obtained from the filtrate and dried in air.