Bis(1H-benzotriazole-4-sulfonato-κ2 N 3,O)(2,2′-bipyridyl-κ2 N,N′)cadmium

Xiao-Hong Zhu; Xiao-Chun Cheng

doi:10.1107/S160053681104596X

. 2011 Nov 5;67(Pt 12):m1699. doi: 10.1107/S160053681104596X

Bis(1H-benzotriazole-4-sulfonato-κ² N ³,O)(2,2′-bipyridyl-κ² N,N′)cadmium

Xiao-Hong Zhu ^a,^*, Xiao-Chun Cheng ^a

PMCID: PMC3238624 PMID: 22199515

Abstract

In the title complex, [Cd(C₆H₄N₃O₃S)₂(C₁₀H₈N₂)], the Cd²⁺ cation is located on a twofold rotation axis and is coordinated by two N and two O atoms from two symmetry-related benzotriazole-4-sulfonate anions and two N atoms from a 2,2-bipyridyl ligand, displaying a distorted CdN₄O₂ octahedral geometry. The crystal structure is stabilized by N—H⋯O and C—H⋯O hydrogen-bonding interactions.

Related literature

For a related structure, see: Xia et al. (2010 ▶).

Experimental

Crystal data

[Cd(C₆H₄N₃O₃S)₂(C₁₀H₈N₂)]
M _r = 664.95
Monoclinic,
a = 8.148 (4) Å
b = 17.207 (7) Å
c = 17.720 (8) Å
β = 103.29 (1)°
V = 2417.8 (19) Å³
Z = 4
Mo Kα radiation
μ = 1.14 mm⁻¹
T = 293 K
0.20 × 0.20 × 0.20 mm

Data collection

Bruker SMART APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.805, T _max = 0.805
8519 measured reflections
3009 independent reflections
2866 reflections with I > 2σ(I)
R _int = 0.073

Refinement

R[F ² > 2σ(F ²)] = 0.028
wR(F ²) = 0.075
S = 1.05
3009 reflections
177 parameters
H-atom parameters constrained
Δρ_max = 0.82 e Å⁻³
Δρ_min = −0.64 e Å⁻³

Data collection: APEX2 (Bruker, 2008 ▶); cell refinement: SAINT (Bruker, 2008 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg, 2000 ▶); software used to prepare material for publication: SHELXTL (Sheldrick, 2008 ▶).

Supplementary Material

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S160053681104596X/pv2474sup1.cif

e-67-m1699-sup1.cif^{(18.8KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S160053681104596X/pv2474Isup2.hkl

e-67-m1699-Isup2.hkl^{(147.8KB, hkl)}

Supplementary material file. DOI: 10.1107/S160053681104596X/pv2474Isup3.cdx

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
N3—H3N⋯O2ⁱ	0.93	1.86	2.776 (3)	167
C3—H3⋯O3ⁱⁱ	0.93	2.55	3.255 (3)	133
C7—H7⋯O2ⁱⁱⁱ	0.93	2.56	3.204 (3)	127

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Symmetry codes: (i) Inline graphic ; (ii) ; (iii) .

Acknowledgments

The authors gratefully acknowledge the Natural Science Foundation of Jiangsu Province of China (BK2008195) for financial support of this work.

supplementary crystallographic information

Comment

Benzotriazole-4-sulfonic acid is often used as a ligand to synthesize complexes for its variable coordination modes. Herein, we report the crystal structure of title complex. The asymmetric unit consists of half of a cadmium ion, half of a 2,2-bipyridyl molecule, and a benzotriazole-4-sulfonate anion. The Cd ion is located on a two fold axis and coordinated by two N atoms from two different benzotriazole-4-sulfonate anions, two N atoms from 2,2-bipyridyl molecule, and two sulfonate O atoms from two different benzotriazole-4-sulfonate anions, displaying a distorted CdN₄O₂ octahedral geometry (Fig. 1). Both benzotriazole-4-sulfonate and 2,2-bipyridyl display bidentate chelating coordinating mode. In the crystal structure, there exist O—H···N and C—H···O hydrogen bonds (Table 1). Sulfonate O atoms as hydrogen bonding acceptor play a very important role in the formation of these hydrogen bonding interactions.

Experimental

A mixture of cadmium perchlorate hexahydrate (83.9 mg, 0.2 mmol), benzotriazole-4-sulfonic acid (39.8 mg, 0.2 mmol), 2,2-bipyridyl (31.2 mg, 0.2 mmol) and potassium hydroxide (11.2 mg, 0.2 mmol) in 12 ml H₂O was sealed in a 16 ml Teflon-lined stainless steel container and heated to 393 K for 3 days. After cooling to room temperature, colorless block crystals of the title complex were obtained.