Aqua­chloridobis(1,10-phenanthroline-κ2 N,N′)zinc(II) chloride N,N-dimethyl­formamide solvate

Li-Li Kong; Shan Gao; Li-Hua Huo; Seik Weng Ng

doi:10.1107/S1600536808002237

. 2008 Jan 25;64(Pt 2):m423. doi: 10.1107/S1600536808002237

Aquachloridobis(1,10-phenanthroline-κ² N,N′)zinc(II) chloride N,N-dimethylformamide solvate

Li-Li Kong ^a, Shan Gao ^a, Li-Hua Huo ^a, Seik Weng Ng ^b,^*

PMCID: PMC2960305 PMID: 21201367

Abstract

The Zn atom in the title salt, [ZnCl(C₁₂H₈N₂)₂(H₂O)]Cl·C₃H₇NO, is chelated by two phenanthroline molecules and is bonded to one chloride ion and one water molecule, resulting in a ZnN₄ClO octahedral coordination environment with the Cl and O atoms in a cis conformation. The cations and anions are linked by O—H⋯Cl hydrogen bonds across a center of inversion, forming a hydrogen-bonded dimeric association. The dimethylformamide solvent molecule is disordered over two orientations in a 0.56 (1):0.44 (1) ratio.

Related literature

The title compound is isostructural with the cobalt and nickel analogs: see Liu, Gao, Huo & Ng (2004 ▶); Liu, Liu & Zhong (2004 ▶).

Experimental

Crystal data

[ZnCl(C₁₂H₈N₂)₂(H₂O)]Cl·C₃H₇NO
M _r = 587.79
Triclinic,
a = 9.6743 (3) Å
b = 11.6096 (5) Å
c = 12.7486 (5) Å
α = 67.004 (1)°
β = 85.995 (1)°
γ = 80.025 (1)°
V = 1298.14 (9) Å³
Z = 2
Mo Kα radiation
μ = 1.19 mm⁻¹
T = 295 (2) K
0.30 × 0.24 × 0.18 mm

Data collection

Rigaku R-AXIS RAPID diffractometer
Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T _min = 0.660, T _max = 0.815
12819 measured reflections
5884 independent reflections
4602 reflections with I > 2σ(I)
R _int = 0.022

Refinement

R[F ² > 2σ(F ²)] = 0.033
wR(F ²) = 0.103
S = 1.11
5884 reflections
383 parameters
61 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.43 e Å⁻³
Δρ_min = −0.36 e Å⁻³

Data collection: RAPID-AUTO (Rigaku, 1998 ▶); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002 ▶); method used to solve structure: atomic coordinates taken from the iostructural Co compound (Liu et al., 2004 ▶ ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: X-SEED (Barbour, 2001 ▶); software used to prepare material for publication: publCIF (Westrip, 2008 ▶).

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808002237/hb2689sup1.cif

e-64-0m423-sup1.cif^{(27KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808002237/hb2689Isup2.hkl

e-64-0m423-Isup2.hkl^{(288KB, hkl)}

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

Table 1. Selected bond lengths (Å).

Zn1—N1	2.190 (2)
Zn1—N2	2.198 (2)
Zn1—N3	2.157 (2)
Zn1—N4	2.275 (2)
Zn1—O1w	2.090 (2)
Zn1—Cl1	2.3520 (6)

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

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1w—H1w1⋯Cl2	0.85 (3)	2.29 (3)	3.112 (2)	163 (3)
O1w—H1w2⋯Cl2ⁱ	0.84 (3)	2.24 (3)	3.079 (2)	172 (3)

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Symmetry code: (i) Inline graphic .

Acknowledgments

We thank the Heilongjiang Province Natural Science Foundation (No. B200501), the Scientific Fund for Remarkable Teachers of Heilongjiang Province (No. 1054 G036), Heilongjiang University and the University of Malaya for supporting this work.

supplementary crystallographic information

Comment

The title compound, (I), is isostructural with its cobalt (Liu, Gao, Huo & Ng, 2004) and nickel analogs (Liu, Liu & Zhong, 2004).

The Zn atom in (I) is chelated by two phenanthroline molecules and bonded to one chloride ion and one water molecule, resulting in a ZnN₄ClO octahedral coordination environment with the Cl and O atoms in a cis conformation (Table 1, Fig. 1). The cations and anions are linked by O–H···Cl hydrogen bonds across a center of inversion forming a hydrogen-bonded dimeric association. Details of the hydrogen bonds are given in Table 2.

Experimental

Zinc diacetate dihydrate (1 mmol) and 1,10-phenanthroline (2 mmol) were dissolved in a DMF-water mixture. Several drops of hydrochloric acid were added, and the mixture set aside for the growth of crystals.. The mixture was filtered and colorless blocks of (I) were isolated after several days.