{μ-6,6′-Dimeth­oxy-2,2′-[propane-1,3-diylbis(nitrilo­methanylyl­idene)]di­phenolato}dimethano­ltrinitrato­samarium(III)zinc(II) methanol disolvate

Fei Liu; Fang Zhang

doi:10.1107/S1600536811007641

. 2011 Apr 7;67(Pt 5):m525. doi: 10.1107/S1600536811007641

{μ-6,6′-Dimethoxy-2,2′-[propane-1,3-diylbis(nitrilomethanylylidene)]diphenolato}dimethanoltrinitratosamarium(III)zinc(II) methanol disolvate

Fei Liu ^a,^*, Fang Zhang ^a

PMCID: PMC3089085 PMID: 21754267

Abstract

In the title complex, [SmZn(C₁₉H₂₀N₂O₄)(NO₃)₃(CH₃OH)₂]·2CH₃OH, the Zn^II ion is six-coordinated by two O atoms and two N atoms of the deprotonated Schiff base ligand and by two O atoms from methanol molecules, forming a slightly distorted octahedral geometry. The Sm^III ion is coordinated by six O atoms from three chelating nitrate ligands and four O atoms from the Schiff base ligand, forming a distorted bicapped square-antiprismatic environment. In the crystal, intermolecular O—H⋯O hydrogen bonds connect the complex molecules and the two methanol solvent molecules, forming (10 Inline graphic ) sheets.

Related literature

For the isotypic Pr^III/Ni^II complex, see: Liu & Zhang (2008 ▶) and for the isotypic Sm^III/Ni^II complex, see: Liu (2009 ▶). For a related Sm^III/Cu^II complex, see: Wang et al. (2008 ▶).

Experimental

Crystal data

[SmZn(C₁₉H₂₀N₂O₄)(NO₃)₃(CH₄O)₂]·2CH₄O
M _r = 870.29
Monoclinic,
a = 13.1050 (8) Å
b = 11.1190 (7) Å
c = 22.3240 (13) Å
β = 90.999 (1)°
V = 3252.4 (3) Å³
Z = 4
Mo Kα radiation
μ = 2.61 mm⁻¹
T = 296 K
0.32 × 0.26 × 0.24 mm

Data collection

Rigaku R-AXIS RAPID CCD diffractometer
Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T _min = 0.489, T _max = 0.573
23458 measured reflections
5833 independent reflections
4835 reflections with I > 2σ(I)
R _int = 0.073

Refinement

R[F ² > 2σ(F ²)] = 0.070
wR(F ²) = 0.133
S = 1.46
5833 reflections
433 parameters
28 restraints
H-atom parameters constrained
Δρ_max = 0.92 e Å⁻³
Δρ_min = −1.14 e Å⁻³

Data collection: PROCESS-AUTO (Rigaku, 2006 ▶); cell refinement: PROCESS-AUTO; data reduction: CrystalStructure (Rigaku, 2007 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997 ▶); software used to prepare material for publication: WinGX (Farrugia, 1999 ▶).

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536811007641/zs2088sup1.cif

e-67-0m525-sup1.cif^{(41KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536811007641/zs2088Isup2.hkl

e-67-0m525-Isup2.hkl^{(279.8KB, 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
O5—H501⋯O8ⁱ	0.82	2.38	3.107 (11)	148
O6—H601⋯O17ⁱⁱ	0.82	1.99	2.654 (10)	138
O17—H17A⋯O16	0.82	1.88	2.688 (13)	167

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

Acknowledgments

The authors gratefully acknowledge financial support from the Education Department of Liaoning Province (2009 A 265) and Liaoning University.

supplementary crystallographic information

Comment

The title complex, (I), formed with the Schiff base N,N'-bis(2-hydroxy-3-methoxybenzylidene)-1,3-diaminopropane is dinuclear with the Sm^III and Zn^II atoms linked through two phenolate O atoms from the ligand, and is the same as the bonding in the isostructural Pr^III/Ni^II complex (Liu & Zhang, 2008) and the Sm^III/Ni^II complex (Liu, 2009) with the same ligand as well as a related Sm^III/Cu^II complex (Wang et al., 2008).

In (I) (Fig. 1), the Sm^III ion is ten-coordinate, comprising four O atoms from the deprotonated Schiff base ligand and six O atoms from three chelating nitrate ions, forming a distorted bicapped square-antiprismatic environment. The Zn ^II ion has a slightly distorted six-coordinate stereochemistry comprising two N atoms and two O atoms from the Schiff base ligand and two methanol O atoms. There are two solvent methanol molecules for each complex molecule and in the crystal structure, intermolecular O—H···O hydrogen bonds (Table 1) connect these molecules to the complex molecules to form sheet structures extending along (1 0 -2).

Experimental

The title complex was obtained by the treatment of zinc(II) acetate dihydrate (0.0548 g, 0.25 mmol) with the Schiff base [N,N'-bis(2-hydroxy-3-methoxybenzylidene)-1,3-diaminopropane)] (0.0855 g, 0.25 mmol) in methanol (25 ml) at room temperature. The mixture was refluxed for 3 h after the addition of samarium(III) nitrate hexahydrate (0.1111 g, 0.25 mmol). The reaction mixture was cooled and filtered. Diethyl ether was allowed to diffuse slowly into the solution of the filtrate giving colorless single crystals after several days.