Chlorido(1,10-phenanthroline)(1H-1,2,4-triazole-3-carboxyl­ato)copper(II)

Jie Zhu; Xian-Hong Yin; Yu Feng; Shan-Shan Zhang; Kai Zhao; Cui-Wu Lin

doi:10.1107/S160053680706299X

. 2007 Dec 6;64(Pt 1):m71. doi: 10.1107/S160053680706299X

Chlorido(1,10-phenanthroline)(1H-1,2,4-triazole-3-carboxylato)copper(II)

Jie Zhu ^a,^b, Xian-Hong Yin ^a,^b,^*, Yu Feng ^a, Shan-Shan Zhang ^a, Kai Zhao ^b, Cui-Wu Lin ^b

PMCID: PMC2914951 PMID: 21200641

Abstract

The title complex, [Cu(C₃H₂N₃O₂)Cl(C₁₂H₈N₂)], crystallizes with two independent molecules in the asymmetric unit. Each Cu^II atom is coordinated by an N atom and an O atom from the bidentate 1H-1,2,4-triazole-3-carboxylate ligand, two N atoms from the 1,10-phenanthroline ligand, and the Cl atom. The coordination geometry is based on a ClN₃O square pyramid. In the crystal structure, the molecules are linked by intermolecular N—H⋯O hydrogen bonds.

Related literature

For related literature, see: Guo & Wang (2005 ▶); Zhao et al. (2008 ▶).

Experimental

Crystal data

[Cu(C₃H₂N₃O₂)Cl(C₁₂H₈N₂)]
M _r = 391.27
Monoclinic,
a = 12.7302 (16) Å
b = 17.562 (3) Å
c = 14.299 (2) Å
β = 113.836 (2)°
V = 2924.2 (7) Å³
Z = 8
Mo Kα radiation
μ = 1.70 mm⁻¹
T = 298 (2) K
0.53 × 0.49 × 0.47 mm

Data collection

Siemens SMART CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.467, T _max = 0.503 (expected range = 0.418–0.451)
14193 measured reflections
5142 independent reflections
3277 reflections with I > 2σ(I)
R _int = 0.038

Refinement

R[F ² > 2σ(F ²)] = 0.034
wR(F ²) = 0.096
S = 1.04
5142 reflections
433 parameters
2 restraints
H-atom parameters constrained
Δρ_max = 0.33 e Å⁻³
Δρ_min = −0.41 e Å⁻³

Data collection: SMART (Siemens, 1996 ▶); cell refinement: SAINT (Siemens, 1996 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a ▶); molecular graphics: SHELXTL (Sheldrick, 1997b ▶); software used to prepare material for publication: SHELXTL.

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S160053680706299X/tk2217sup1.cif

e-64-00m71-sup1.cif^{(29.9KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S160053680706299X/tk2217Isup2.hkl

e-64-00m71-Isup2.hkl^{(251.8KB, 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
N2—H2⋯O4ⁱ	0.86	1.99	2.835 (4)	166
N7—H7⋯O2ⁱⁱ	0.86	1.94	2.797 (4)	172

Open in a new tab

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

Acknowledgments

The authors thank the National Natural Science Foundation of China (grant No. 20761002). This research was sponsored by the Fund of the Talent Highland Research Programme of Guangxi University (grant No. 205121), the Science Foundation of the State Ethnic Affairs Commission (grant No. 07GX05), the Development Foundation of Guangxi Research Institute of Chemical Industry and the Science Foundation of Guangxi University for Nationalities (grant Nos. 0409032, 0409012 and 0509ZD047).

supplementary crystallographic information

Comment

In connection with on-going studies in coordination chemistry (Zhao et al., 2008) and the biological importance of triazole molecules (Guo & Wang, 2005), the crystal structure of a new ternary Cu(II) complex with 1H-1,2,4-triazole-3-carboxylate (TRIA), 1,10-phenanthroline (phen) and Cl is described.

Two independent mononuclear complex molecules, Cu(TRIA)(phen)Cl, comprise the asymmetric unit of (I), Fig. 1. Each Cu atom is chelated by a N atom and a O atom, derived from the TRIA anion, two N atoms from the chelating phen ligand, and the penta-coordinated coordination geometry is completed by a Cl atom. The latter atom occupies an axial position in the approximately square-pyramidal N₃OCl coordination geometry; the angles around the Cu(II) atom range from 81.66 (12) to 166.88 (12)°.

The primary intermolecular contacts in the crystal structure are of the type N—H···O and involve both amines and both of the non-coordinating carbonyls of the TRIA anions (Table 1).

Experimental

CuCl₂.2H₂O (0.5 mmol, 85.2 mg) dissolved in distilled water (15 ml) was added with stirring at 323 K to 1H-1,2,4-triazole-3-carboxylic acid (1 mmol, 113 mg) also dissolved in distilled water (5 ml). The resulting blue solution was allowed to react for 30 min and 1,10-phenanthroline (0.5 mmol, 99.1 mg) dissolved in ethanol (5 ml) was added. Dark-blue crystals suitable for X-ray analysis were obtained by slow evaporation over a period of one month (yield 85%). Analysis. Found: C 46.08, H 2.52, Cl 9.00, Cu 16.29, N 17.83, O 8.23%. C₁₅H₁₀ClCuN₅O₂ requires: C 46.04, H 2.58, Cl 9.06, Cu 16.24, N 17.90, O 8.18%.