catena-Poly[[[diiodidomercury(II)]-μ-N,N′-di-3-pyridylpyridine-2,6-dicarboxamide] dimethyl­formamide solvate]

Li-Hua Huang; Jie Wu; Fang-Fang Pan

doi:10.1107/S1600536808036581

. 2008 Nov 13;64(Pt 12):m1533. doi: 10.1107/S1600536808036581

catena-Poly[[[diiodidomercury(II)]-μ-N,N′-di-3-pyridylpyridine-2,6-dicarboxamide] dimethylformamide solvate]

Li-Hua Huang ^a, Jie Wu ^a,^*, Fang-Fang Pan ^a

PMCID: PMC2960109 PMID: 21581148

Abstract

In the title complex, {[HgI₂(C₁₇H₁₃N₅O₂)]·C₃H₇NO}_n, the Hg atom is coordinated by two I atoms and two N atoms from two different ligands in a distorted tetrahedral environment. Hg atoms are bridged by N,N′-di-3-pyridylpyridine-2,6-dicarboxamide ligands, forming a helical chain running along the a axis.

Related literature

For binuclear complexes of N,N′-bis(pyridin-3-yl)-2,6-pyridinedicarboxamide, see: Baer et al. (2002 ▶); Huang & Wu (2008 ▶); Qin et al. (2003 ▶).

Experimental

Crystal data

[HgI₂(C₁₇H₁₃N₅O₂)]·C₃H₇NO
M _r = 846.81
Orthorhombic,
a = 21.295 (4) Å
b = 9.7177 (19) Å
c = 24.440 (5) Å
V = 5057.5 (17) Å³
Z = 8
Mo Kα radiation
μ = 8.56 mm⁻¹
T = 293 (2) K
0.20 × 0.18 × 0.08 mm

Data collection

Rigaku Saturn724 diffractometer
Absorption correction: numerical (CrystalClear; Rigaku/MSC, 2006 ▶) T _min = 0.279, T _max = 0.547
48014 measured reflections
4447 independent reflections
4250 reflections with I > 2σ(I)
R _int = 0.073

Refinement

R[F ² > 2σ(F ²)] = 0.062
wR(F ²) = 0.119
S = 1.31
4447 reflections
291 parameters
H-atom parameters constrained
Δρ_max = 1.21 e Å⁻³
Δρ_min = −0.92 e Å⁻³

Data collection: CrystalClear (Rigaku/MSC, 2006 ▶); cell refinement: CrystalClear; data reduction: CrystalClear; 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 global, I. DOI: 10.1107/S1600536808036581/hg2428sup1.cif

e-64-m1533-sup1.cif^{(21.8KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808036581/hg2428Isup2.hkl

e-64-m1533-Isup2.hkl^{(218KB, 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
N4—H4⋯O3	0.86	2.23	3.008 (10)	150
N2—H2⋯O3	0.86	2.26	2.964 (10)	139

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Acknowledgments

The authors thank Professor Hou Hong-Wei of Zhengzhou University for his help.

supplementary crystallographic information

Comment

The expansion of the field of metal-organic frameworks (MOFs) of predetermined structure depends on the judicious choice of new linkers and nodes of appropriate coordination algorithms. Rigid, polydentate N-donor ligands are typical linkers employed in such work. The rigid conjugated clamp-like multi-pyridine ligand N,N'-bis(pyridin-3-yl)-2,6-pyridinedicarboxamide, is a convenient bridging ligand for the synthesis of chain complexes. However, the previous work proved that the ligand also can form binuclear complex with 28-number ring (Huang et al.; 2004, Qin et al. 2003; Baer et al. 2002). We think, among the factors that induce the self-assembly processes with this ligand, the rotation of terminal pyridine groups plays a crucial role in deciding between binuclear versus. extended structures of the metal complexes. In this work, we selected this ligand as linker, generating a new helical chain coordination complex, {[HgI₂(C₁₇N₅O₂)](DMF)}_n, (I), which is reported here. In compound (I) each Hg(II) atom is four-coordinated by two N atoms from two ligands and two I atoms in a distorted tetrahedral coordination sphere (Fig. 1). The Hg(II) atoms are bridged with N,N'-bis(pyridin-3-yl)-2,6-pyridinedicarboxamide ligands to form a helical chain running the a axis (Fig. 2).

In the crystal structure, the intermolecular N—H···N hydrogen bonds and the N—H···O hydrogen bonds arising from the DMF and ligand complete the structure.

Experimental

The ligand N,N'-bis(pyridin-3-yl)-2,6-pyridinedicarboxamide (0.05 mmol, 0.016 g) in DMF (5 ml) was added dropwise to a solution of HgI2 (0.1 mmol, 0.036 g) in methanol (3 ml). The precipitate was filtered and the resulting solution was allowed to stand at room temperature in the dark. After one week good quality colorless crystals were obtained from the filtrate and dried in air.