catena-Poly[[bis­[1-phenyl-3-(1H-1,2,4-triazol-1-yl)propan-1-one-κN 4]cadmium(II)]-di-μ-azido-κ4 N 1:N 3]

Ying Guo; Hua Cai; Jiangang Li; Guobao Wan

doi:10.1107/S1600536808012609

. 2008 May 7;64(Pt 6):m784. doi: 10.1107/S1600536808012609

catena-Poly[[bis[1-phenyl-3-(1H-1,2,4-triazol-1-yl)propan-1-one-κN ⁴]cadmium(II)]-di-μ-azido-κ⁴ N ¹:N ³]

Ying Guo ^a, Hua Cai ^a,^*, Jiangang Li ^a, Guobao Wan ^a

PMCID: PMC2961553 PMID: 21202473

Abstract

In the crystal structure of the title complex, [Cd(N₃)₂(C₁₁H₁₁N₃₁)₂]_n, there are two crystallographically independent Cd^II atoms. Both exist in an octahedral environment composed of four N atoms of the N₃ ⁻ groups and two N atoms from two monodentate 1-phenyl-3-(1H-1,2,4-triazol-1-yl)propan-1-one ligands that are positioned trans to each other. Adjacent Cd^II centres in the crystal structure are bridged by a pair of N₃ ⁻ anions in a μ-1,3-fashion, forming an infinite one-dimensional array.

Related literature

For related literature, see: Guo & Cai (2007 ▶).

Experimental

Crystal data

[Cd(N₃)₂(C₁₁H₁₁N₃₁)₂]
M _r = 598.92
Monoclinic,
a = 10.1626 (16) Å
b = 17.732 (3) Å
c = 28.124 (4) Å
β = 91.980 (2)°
V = 5064.9 (14) Å³
Z = 8
Mo Kα radiation
μ = 0.91 mm⁻¹
T = 294 (2) K
0.24 × 0.22 × 0.14 mm

Data collection

Bruker SMART CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 2004 ▶) T _min = 0.760, T _max = 1.000 (expected range = 0.670–0.881)
26797 measured reflections
8928 independent reflections
7054 reflections with I > 2σ(I)
R _int = 0.021

Refinement

R[F ² > 2σ(F ²)] = 0.031
wR(F ²) = 0.069
S = 1.09
8928 reflections
667 parameters
H-atom parameters constrained
Δρ_max = 0.67 e Å⁻³
Δρ_min = −0.72 e Å⁻³

Data collection: SMART (Bruker, 2001 ▶); cell refinement: SAINT (Bruker, 2001 ▶); data reduction: SAINT; 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 datablocks I, global. DOI: 10.1107/S1600536808012609/bv2096sup1.cif

e-64-0m784-sup1.cif^{(39.3KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808012609/bv2096Isup2.hkl

e-64-0m784-Isup2.hkl^{(436.7KB, hkl)}

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

supplementary crystallographic information

Comment

Pseudohalide anions N₃^-, NCS^- and NCO^- are known as extremely versatile ligands in coordination chemistry because of their multiple bridging modes. Recently, we initiated a research program involving synthesizing supramolecules based on a pseudohalide and a flexible ligand consisting of a propanone unit substituted with an imidazole and a phenyl group (Cai & Guo, 2007). To further explore this series, we synthesized the title compound, (I), a new Cd^II complex based on the mixed ligands azide and 3-(1H-1,2,4-triazol-1-yl) -1-phenylpropan-1-one (L), which consists of a propanone unit substituted with an triazole and a phenyl group.

The X-ray crystallographic analysis shows that the structure of complex I consists of 1-D Cd^II chains with two Cd^II atoms in the asymmetric unit. Two crystallographically independent Cd^II ions have similar coordination environment, but different bond parameters. In both cases, each Cd^II atom is in a distorted N₆ octahedron environment, consisting of two terminal and two bridging azide N atoms and N atoms from two ligand (L) (arranged in a cis fation). The Cd—N bond distance range from 2.313 (3)Å to 2.369 (3) Å. Cd1 and Cd2 are displaced by 0.2047 and 0.7313Å from the mean basal plane toward the apical nitrogen atoms (N24 and N7). In this structure, the ligand L displays monodentate binding to Cd^II and the triazole and phenyl rings in each of the ligands are not coplanar. The dihedral angels formed by the least-squares planes of the phenyl and triazole rings are 78.1 (1)°, 74.5 (1)° 74.3 (1)° and 77.5 (1)°, respectively. Adjacent Cd^II centers are bridged by two azide anions in an end-to-end (µ-1,3) fashion forming a 1-D chain polymer, as illustrated in Fig.2. The minimum interdinuclear Cd···Cd distance is 5.415 Å.

Experimental

All the starting materials and solvents for syntheses were obtained commercially and used as received. Cd(NO₃)₂.4H₂O (30.8 mg, 0.1 mmol), 3-(1H-1,2,4-triazol-1-yl)-1-phenylpropan-1-one (22.3 mg, 0.1 mmol) and NaN₃ (6.7 mg, 0.1 mmol) were mixed in a CH₃CN–H₂O (20 ml, 1:1 v/v) solution with vigorous stirring for ca 30 min. The resulting solution was filtered and left to stand at room temperature. Colourless prismatic crystals of I suitable for X-ray analysis were obtained in 60% yield by slow evaporation of the solvent over a period of 1 week. Analysis, calculated for CdC₂₂H₂₂N₁₂O₂: C 44.12, H 3.70, N 28.06; found: C 44.15, H 3.83, N 28.10.