A new coordination tetra­mer of copper(I) iodide and benzyl­dimethyl­amine: tetra-μ3-iodido-tetra­kis[(benzyl­dimethyl­amine-κN)copper(I)]

Shuying Yang; Yuebao Li; Yujie Cui; Jianguo Pan

doi:10.1107/S1600536809026208

. 2009 Jul 11;65(Pt 8):m906. doi: 10.1107/S1600536809026208

A new coordination tetramer of copper(I) iodide and benzyldimethylamine: tetra-μ₃-iodido-tetrakis[(benzyldimethylamine-κN)copper(I)]

Shuying Yang ^a, Yuebao Li ^a, Yujie Cui ^a, Jianguo Pan ^a,^*

PMCID: PMC2977424 PMID: 21583366

Abstract

The title compound, [Cu₄I₄(C₉H₁₃N)₄], has a distorted cubane-like [Cu₄I₄] core structure. Each Cu^I atom is tetrahedrally coordinated by three I atoms and one N atom of an benzyldimethylamine ligand. Each I atom acts as a μ₃-ligand, linking three Cu^I atoms. The Cu—I bond distances vary between 2.6328 (7) and 2.7121 (6) Å, while the Cu—N bond distances vary between 2.107 (3) and 2.122 (3) Å.

Related literature

For the synthesis and structures of copper iodide coordination polymers, see: Bi et al. (2007a ▶,b ▶); Chen et al. (2008 ▶).

Experimental

Crystal data

[Cu₄I₄(C₉H₁₃N)₄]
M _r = 1302.58
Monoclinic,
a = 17.758 (4) Å
b = 11.544 (2) Å
c = 21.540 (4) Å
β = 100.16 (3)°
V = 4346.3 (15) Å³
Z = 4
Mo Kα radiation
μ = 4.80 mm⁻¹
T = 298 K
0.38 × 0.29 × 0.27 mm

Data collection

Rigaku R-AXIS RAPID diffractometer
Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T _min = 0.719, T _max = 1.000 (expected range = 0.197–0.274)
40151 measured reflections
9884 independent reflections
8944 reflections with I > 2σ(I)
R _int = 0.063

Refinement

R[F ² > 2σ(F ²)] = 0.031
wR(F ²) = 0.059
S = 1.08
9884 reflections
434 parameters
6 restraints
H-atom parameters constrained
Δρ_max = 1.77 e Å⁻³
Δρ_min = −0.94 e Å⁻³

Data collection: RAPID-AUTO (Rigaku, 1998 ▶); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEPII (Johnson, 1976 ▶); software used to prepare material for publication: SHELXL97.

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809026208/fj2223sup1.cif

e-65-0m906-sup1.cif^{(30.7KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809026208/fj2223Isup2.hkl

e-65-0m906-Isup2.hkl^{(483.4KB, hkl)}

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

Table 1. Selected geometric parameters (Å, °).

Cu1—N1	2.107 (3)
Cu1—I4	2.6711 (8)
Cu1—I1	2.6892 (6)
Cu1—I2	2.6953 (8)
Cu2—N2	2.108 (3)
Cu2—I3	2.6609 (6)
Cu2—I4	2.6750 (6)
Cu2—I1	2.6819 (9)
Cu3—N3	2.122 (3)
Cu3—I4	2.6611 (6)
Cu3—I2	2.6947 (8)
Cu3—I3	2.7121 (6)
Cu4—N4	2.112 (3)
Cu4—I1	2.6328 (7)
Cu4—I2	2.6788 (6)
Cu4—I3	2.7090 (10)

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Acknowledgments

This work was partially supported by the Zhejiang Provincial Natural Science Foundation (No.Y406277), the Ningbo Municipal Natural Science Foundation (No. 2005 A620023) and the K. C. Wang Magna Fund in Ningbo University.

supplementary crystallographic information

Comment

Copper halides have been widely investigated due to their rich photoluminescent properties and intriguing topology. In recent years, great efforts have been taken to synthesize and characterize copper iodide coordination polymers which have special crystal structure and properties. By now several classes of copper iodide coordination polymers have been successfully synthesized and investigated (Bi et al., 2007a,b; Chen et al., 2008). Herein, we report the synthesis and crystal structure of the title complex.

The title compound (Fig.1) has a distorted cubanelike [Cu₄I₄] core structure. Each copper(I) atom is tetrahedrally coordinated by three iodide atoms and one N atom of n-benzyldimethylamine. Each iodide atom acting as µ₃-I links three copper(I) atoms. The Cu—I bond distances vary between 2.6328 (7) and 2.7121 (6) Å, while the Cu—N bond distances vary between 2.107 (3) and 2.122 (3) Å. The Cu—I and Cu—N bond distances correspond well with that found in the literatures listed in the comment. Finally, Cu₄I₄(C₉H₁₃N)₄ forms the supramolecular structure via intermolecular forces.

Experimental

Cuprous iodide (0.3881 g) and n-benzyldimethylamine (1 ml) were sealed in a glass vial, which was heated at 353 K for two days. Then, the solution (0.5 ml) was put in another glass vial. One day later colorless and transparent crystals were obtained by slow evaporation of the solution at 353 K.