Bis(μ-N,N′,N′′-tri-3-pyridylpyridine-1,3,5-tricarboxamide-κ2 N:N′)bis­[di­chloridomercury(II)] methanol disolvate

Pei Wang; Yufei Wang; Chao Huang; Lixiang Chang; Jie Wu

doi:10.1107/S160053681102040X

. 2011 Jun 4;67(Pt 7):m859. doi: 10.1107/S160053681102040X

Bis(μ-N,N′,N′′-tri-3-pyridylpyridine-1,3,5-tricarboxamide-κ² N:N′)bis[dichloridomercury(II)] methanol disolvate

Pei Wang ^a, Yufei Wang ^b, Chao Huang ^a, Lixiang Chang ^a, Jie Wu ^a,^*

PMCID: PMC3151944 PMID: 21836858

Abstract

The title dinuclear centrosymmetric complex, [Hg₂Cl₄(C₂₄H₁₈N₆O₃)₂]·2CH₃OH, comprises Hg^II atoms coordinated by two Cl atoms and two N atoms from ligands in a distorted tetrahedral geometry. The solvent molecules are linked by hydrogen bonds.

Related literature

For general background, see: Fortner et al. (2005 ▶). For a related structure, see: Qin et al. (2003 ▶).

Experimental

Crystal data

[Hg₂Cl₄(C₂₄H₁₈N₆O₃)₂]·2CH₄O
M _r = 1483.95
Triclinic,
a = 8.6772 (17) Å
b = 12.243 (2) Å
c = 13.530 (3) Å
α = 66.81 (3)°
β = 84.66 (3)°
γ = 86.40 (3)°
V = 1315.0 (4) Å³
Z = 1
Mo Kα radiation
μ = 6.10 mm⁻¹
T = 293 K
0.20 × 0.18 × 0.16 mm

Data collection

Rigaku Saturn724 diffractometer
Absorption correction: numerical (CrystalClear; Rigaku/MSC, 2006 ▶) T _min = 0.738, T _max = 1.000
14489 measured reflections
5170 independent reflections
4461 reflections with I > 2σ(I)
R _int = 0.044

Refinement

R[F ² > 2σ(F ²)] = 0.043
wR(F ²) = 0.074
S = 1.10
5170 reflections
345 parameters
H-atom parameters constrained
Δρ_max = 0.66 e Å⁻³
Δρ_min = −0.65 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: SHELXS97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL.

Supplementary Material

Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S160053681102040X/kp2329sup1.cif

e-67-0m859-sup1.cif^{(24KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S160053681102040X/kp2329Isup2.hkl

e-67-0m859-Isup2.hkl^{(253.2KB, hkl)}

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

Table 1. Selected bond lengths (Å).

Hg1—Cl1	2.3574 (15)
Hg1—Cl2	2.3687 (19)
Hg1—N3ⁱ	2.385 (4)
Hg1—N1	2.400 (4)

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Symmetry code: (i) Inline graphic .

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

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O4—H4⋯N6ⁱⁱ	0.82	1.94	2.740 (6)	167
N5—H5A⋯O1^iv	0.86	2.42	3.141 (6)	142

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Symmetry codes: (ii) Inline graphic ; (iii) ; (iv) .

Acknowledgments

We gratefully acknowledge financial support by the Student Innovative Pilot Project of Zhengzhou University (grant No. 2010cxsy095).

supplementary crystallographic information

Comment

In recent years the rapid progress in supramolecular chemistry has contributed to discovery of special novel structures being of significance for functional materials (Fortner et al. 2005). To control the topology of molecular assemblies, tripodal ligands are proved promising and useful in this area. For example, N,N',N'',-tris(3-pyridinyl)-1,3,5-benzenetricarboxamide (Z (Qin et al. 2003) has been selected as an excellent tripodal ligand and many intriguing complexes have been successfully accomplished with this ligand. In this work, we selected this ligand as linker, generating a new coordination complex, [Hg~2~(C~24~H~18Ñ~6Õ~3~)~2~Cl~4~]2(CH~3ÕH), (I), which is reported here. In the compound, Hg^II atom is four-coordinated by two N atoms from two ligands and two Cl atoms in a distorted tetrahedral coordination sphere (Fig. 1, Table 1). The two Hg^II atoms are bridged with two ligands to form a microporous MOFs with 28-number ring. The Hg(II)—N distances are 2.385 (4) Å and 2.400 (4) Å, respectively. The Hg···Hg distance in the ring is 13.568 (5) Å. In the crystal structure, intermolecular hydrogen bonds N2—H—Cl1, N5—H—O1, and the O4—H—N6 (arising from the CH3OH and ligand) generate the three-dimensional network (Fig. 2, Table 2).

Experimental

The ligand N,N',N''-tris(3-pyridinyl)-1,3,5-benzenetricarboxamide (0.1 mmol, 0.044 g) in DMF (1 mL) was added dropwise to a solution of HgCl₂ (0.05 mmol, 0.014 g) in methanol (5 mL). The precipitate was filtered and the resulting solution was allowed to stand at room temperature in the dark. After one week good quality colourless crystals were obtained, separated from a filtrate and dried in air.