catena-Poly[[chloridocopper(II)]bis­(μ-3,3′,5,5′-tetra­methyl-4,4′-methylene­dipyrazole)[chloridocopper(II)]-di-μ-chlorido]

Zhi-Min Wang

doi:10.1107/S1600536808006909

. 2008 Mar 14;64(Pt 4):m561. doi: 10.1107/S1600536808006909

catena-Poly[[chloridocopper(II)]bis(μ-3,3′,5,5′-tetramethyl-4,4′-methylenedipyrazole)[chloridocopper(II)]-di-μ-chlorido]

Zhi-Min Wang ^a,^*

PMCID: PMC2960916 PMID: 21202017

Abstract

In the title compound, [Cu₂Cl₄(C₁₁H₁₆N₄)]_n, the Cu atom is coordinated by two N atoms of two 3,3′,5,5′-tetramethyl-4,4′-methylenedipyrazole (H₂mbdpz) ligands, two bridging Cl atoms and one terminal Cl atom, forming a square-pyramidal geometry. The bridging Cl atoms and the bridging H₂mbdpz ligands connect the Cu atoms to build up an extended one-dimensional chain. The chains are further connected through N—H⋯Cl hydrogen bonds to build up a two-dimensional layer in the (011) plane. An inversion centre lies between every pair of adjacent Cu atoms.

Related literature

For related literature, see: Kaes et al. (1998 ▶); Yaghi et al. (1998 ▶); Yagi et al. (2002 ▶); Nassimbeni (2003 ▶).

Experimental

Crystal data

[Cu₂Cl₄(C₁₁H₁₆N₄)]
M _r = 677.44
Triclinic,
a = 8.759 (3) Å
b = 8.879 (3) Å
c = 9.735 (3) Å
α = 79.269 (6)°
β = 63.584 (5)°
γ = 86.922 (5)°
V = 665.8 (4) Å³
Z = 1
Mo Kα radiation
μ = 2.03 mm⁻¹
T = 298 (2) K
0.26 × 0.23 × 0.19 mm

Data collection

Bruker APEXII area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 2004 ▶) T _min = 0.621, T _max = 0.699
3354 measured reflections
2331 independent reflections
1541 reflections with I > 2σ(I)
R _int = 0.033

Refinement

R[F ² > 2σ(F ²)] = 0.064
wR(F ²) = 0.178
S = 0.99
2331 reflections
167 parameters
H-atom parameters constrained
Δρ_max = 0.79 e Å⁻³
Δρ_min = −1.14 e Å⁻³

Data collection: APEX2 (Bruker, 2004 ▶); cell refinement: SAINT (Bruker, 2004 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: PLATON (Spek, 2003 ▶); software used to prepare material for publication: SHELXL97.

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808006909/dn2323sup1.cif

e-64-0m561-sup1.cif^{(16KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808006909/dn2323Isup2.hkl

e-64-0m561-Isup2.hkl^{(114.7KB, 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⋯Cl1ⁱ	0.86	2.43	3.242 (6)	157
N4—H4⋯Cl1ⁱⁱ	0.86	2.34	3.172 (6)	164

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

Acknowledgments

The author is grateful to Shuren University for financial support.

supplementary crystallographic information

Comment

Considerable research efforts have been devoted to searching for new and better inclusion compounds. One of the main reasons is their potential for eventual applications in a variety of technologically useful processes (Nassimbeni, 2003). In the past performance, the majority of cases in one-dimensional coordination networks was focused on bis-monodentate ligand (Yaghi et al., 1998), while a few examples of bis-bidentate, bis-tridentate ones were documented(Kaes et al., 1998). Here, we reported a 1-D complexes using the bis-bidentate ligand 4,4'-methylene-bis(3,5-dimethylpyrazole) (H₂mbdpz).

In the title compound (I), the copper atom is coordinated by two nitrogen atoms of the H₂mbdpz ligand, two bridging chlorine atom and one terminal chlorine, forming a square-pyramidal geometry (Fig. 1). The average Cu—N bond lengths, 1.999 (3) Å, is longer than those observed in other copper complexes (Yagi et al., 2002). The average Cu—Cl bond lengths is 2.439 (3) Å. the bridging chlorine atoms and the bridging H₂mbdpz ligands connect the copper atoms to build up an extended one dimensionnal chain (Fig. 1). The chains are further connected through N—H···Cl hydrogen bonds to build up a two-dimensionnal layer along the (0 1 1) plane (Table 1).

Experimental

CuCl₂(0.028 g, 0.015 mmol), H₂mbdpz(0.023 g, 0.012 mmol) were added to methanol. The mixture was heated for ten hours under reflux. The resultant was then filtered to give a pure solution. Two weeks later suitable single crystals for X-Ray diffraction analysis were obtained.