Chlorido[2,2′-(oxydimethyl­ene)­dipyridine]copper(II) perchlorate–aqua­chlorido[2,2′-(oxydimethyl­ene)­dipyridine]copper(II) perchlorate (1/1)

Hong Li; Long Miao Xie; Shi Guo Zhang

doi:10.1107/S1600536809027123

. 2009 Jul 18;65(Pt 8):m933. doi: 10.1107/S1600536809027123

Chlorido[2,2′-(oxydimethylene)dipyridine]copper(II) perchlorate–aquachlorido[2,2′-(oxydimethylene)dipyridine]copper(II) perchlorate (1/1)

Hong Li ^a,^*, Long Miao Xie ^b, Shi Guo Zhang ^a

PMCID: PMC2977150 PMID: 21583386

Abstract

The asymmetric unit of the title compound, [CuCl(C₁₂H₁₂N₂O)][CuCl(C₁₂H₁₂N₂O)(H₂O)](ClO₄)₂, contains two different discrete cations. In one cation, the Cu^II ion is coordinated in a slightly distorted square-planar geometry, while in the other the Cu^II ion is in a slightly distorted square-pyramidal environment. In the crystal structure, there are O—H⋯O hydrogen bonds between coordinated water molecules and perchlorate anions. Both types of cations are linked into one-dimensional chains along the b axis by weak electrostatic Cu⋯Cl interactions, with Cu⋯Cl distances of 2.8088 (16) and 3.2074 (17) Å.

Related literature

For related structures, see: Li (2007 ▶, 2008a ▶,b ▶).

Experimental

Crystal data

[CuCl(C₁₂H₁₂N₂O)][CuCl(C₁₂H₁₂N₂O)(H₂O)](ClO₄)₂
M _r = 815.37
Triclinic,
a = 10.997 (2) Å
b = 12.882 (3) Å
c = 12.913 (3) Å
α = 97.174 (3)°
β = 112.031 (3)°
γ = 106.851 (3)°
V = 1565.7 (5) Å³
Z = 2
Mo Kα radiation
μ = 1.76 mm⁻¹
T = 298 K
0.42 × 0.23 × 0.21 mm

Data collection

Bruker SMART APEX CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.525, T _max = 0.709
8530 measured reflections
6009 independent reflections
4063 reflections with I > 2σ(I)
R _int = 0.024

Refinement

R[F ² > 2σ(F ²)] = 0.062
wR(F ²) = 0.185
S = 1.05
6009 reflections
411 parameters
3 restraints
H-atom parameters constrained
Δρ_max = 1.01 e Å⁻³
Δρ_min = −0.60 e Å⁻³

Data collection: SMART (Bruker, 1997 ▶); cell refinement: SAINT (Bruker, 1997 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL and PLATON (Spek, 2009 ▶); software used to prepare material for publication: SHELXTL.

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809027123/lh2860sup1.cif

e-65-0m933-sup1.cif^{(27.2KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809027123/lh2860Isup2.hkl

e-65-0m933-Isup2.hkl^{(294.1KB, hkl)}

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

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

Cl3—Cu2	2.2511 (15)
Cl4—Cu1	2.2067 (14)
Cu1—N3	1.968 (4)
Cu1—O1	1.970 (3)
Cu1—N4	1.973 (4)
Cu2—N2	1.970 (4)
Cu2—N1	1.972 (4)
Cu2—O2	2.005 (4)
Cu2—O11	2.298 (4)

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N3—Cu1—O1	80.97 (17)
N3—Cu1—N4	161.79 (19)
O1—Cu1—N4	81.04 (17)
N3—Cu1—Cl4	98.72 (13)
O1—Cu1—Cl4	173.09 (12)
N4—Cu1—Cl4	98.80 (14)
N2—Cu2—N1	159.85 (19)
N2—Cu2—O2	80.78 (17)
N1—Cu2—O2	80.45 (16)
N2—Cu2—Cl3	98.32 (14)
N1—Cu2—Cl3	98.09 (13)
O2—Cu2—Cl3	165.86 (13)
N2—Cu2—O11	93.89 (17)
N1—Cu2—O11	92.93 (17)
O2—Cu2—O11	88.68 (16)
Cl3—Cu2—O11	105.46 (12)

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Table 2. Hydrogen-bond geometry (Å, °).

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O11—H11A⋯O5ⁱ	0.90	2.05	2.725 (8)	131
O11—H11B⋯O9ⁱⁱ	0.90	1.92	2.787 (10)	163

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

Acknowledgments

The authors thank the Project of Scientific Studies Development of Shandong Provincial Education Department (grant No. J08LC51) and the Natural Science Foundation of Shandong Province (grant No. Y2007B26).

supplementary crystallographic information

Comment

Derivatives of pyridine play an important role in modern coordination chemistry and some complexes using 2,2'-(oxydimethylene)dipyridine as a ligand have already been reported (Li, 2007, 2008a,b). Herein we report the crystal structure of the title compound.

The molecular structure of the title compound is shown in Fig. 1. Atom Cu1 is in a slightly distorted square-planar coordination environment and atom Cu2 is coordinated in a slightly distorted square-pyramidal environment with the O atom of the coordinated H₂O ligand in the apical site. 2,2'-(oxydimethylene)dipyridine acts as a tridentate ligand as in the related Cu^II, Zn^II and Cd^II complexes (Li, 2007, 2008a,b). In the crystal structure, there are O—H···O hydrogen bonds between coordinated water molecule and perchlorate ions and both types of cation are linked into one-dimensional chains along the b axis by weak electrostatic Cu···Cl interactions with Cu···Cl distances of 2.8088 (16) and 3.2074 (17) Å (see Fig. 2).

Experimental

An 8ml methanol solution of 2,2'-(oxydimetheylene)dipyridine (0.0386 g, 0.193 mmol) was added to an 8 ml H₂O solution containing Cu(ClO₄)₂.6H₂O (0.0730 g, 0.197 mmol), and the mixture was stirred for a few minutes. Then, diluted HCl solution was added into the mixed solution in drops until the pH = 4.0. Blue single crystals were obtained after the solution had been allowed to stand at room temperature for three weeks.