{μ-6,6′-Dimeth­oxy-2,2′-[propane-1,3-diylbis(nitrilo­methyl­idyne)]diphenolato}dimethano­ltrinitratonickel(II)samarium(III) methanol disolvate

Fei Liu

doi:10.1107/S1600536808038920

. 2009 Jan 8;65(Pt 2):m126. doi: 10.1107/S1600536808038920

{μ-6,6′-Dimethoxy-2,2′-[propane-1,3-diylbis(nitrilomethylidyne)]diphenolato}dimethanoltrinitratonickel(II)samarium(III) methanol disolvate

Fei Liu ^a,^*

PMCID: PMC2968130 PMID: 21581745

Abstract

In the title complex, [NiSm(C₁₉H₂₀N₂O₄)(NO₃)₃(CH₄O)₂]·2CH₃OH, the Ni^II ion is coordinated by two O atoms and two N atoms of a deprotonated Schiff base ligand and by two O atoms of two methanol ligands in 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 a Schiff base ligand in a distorted bicapped square-antiprismatic environment. In the crystal structure, intermolecular O—H⋯O hydrogen bonds connect complex molecules and methanol solvent molecules, forming (10 Inline graphic ) sheets.

Related literature

For the isostructural Pr(III) complex, see: Liu & Zhang (2008 ▶). For a related Sm(III) complex, see: Wang et al. (2008 ▶).

Experimental

Crystal data

[NiSm(C₁₉H₂₀N₂O₄)(NO₃)₃(CH₄O)₂]·2CH₄O
M _r = 863.63
Monoclinic,
a = 13.066 (3) Å
b = 11.121 (2) Å
c = 22.128 (4) Å
β = 90.60 (3)°
V = 3215.2 (11) Å³
Z = 4
Mo Kα radiation
μ = 2.48 mm⁻¹
T = 291 (2) K
0.21 × 0.20 × 0.18 mm

Data collection

Rigaku R-AXIS RAPID diffractometer
Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T _min = 0.619, T _max = 0.660
22609 measured reflections
7354 independent reflections
6200 reflections with I > 2σ(I)
R _int = 0.035

Refinement

R[F ² > 2σ(F ²)] = 0.027
wR(F ²) = 0.063
S = 1.03
7354 reflections
430 parameters
18 restraints
H-atom parameters constrained
Δρ_max = 0.58 e Å⁻³
Δρ_min = −0.38 e Å⁻³

Data collection: RAPID-AUTO (Rigaku, 1998 ▶); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002 ▶); 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: SHELXL97.

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536808038920/lh2735sup1.cif

e-65-0m126-sup1.cif^{(26.7KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536808038920/lh2735Isup2.hkl

e-65-0m126-Isup2.hkl^{(359.8KB, 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
O17—H17⋯O11	0.82	2.14	2.926 (4)	160
O16—H16⋯O17	0.85	1.89	2.730 (5)	170
O15—H25⋯O16ⁱ	0.85	1.83	2.660 (4)	169
O14—H24⋯O6ⁱⁱ	0.84	2.25	3.090 (4)	173

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

Acknowledgments

The authors gratefully acknowledge financial support from the Education Department of Liaoning Province (2006 B 112) and Liaoning University.

supplementary crystallographic information

Comment

As shown in Fig. 1, the hexadentate Schiff base ligand links Ni and Sm atoms into a dinuclear complex through two phenolate O atoms, which is similar to the bonding reported for other Nickel-Praseodymium and copper-samarium complexes of the same ligand (Liu & Zhang, 2008 and Wang et al., 2008). The Sm^III ion in the title complex is ten-coordinated by four oxygen atoms from the ligand and six oxygen atoms from three nitrate ions. The Ni^II center is six-coordinate by two nitrogen atoms and two oxygen atoms from the ligand and two methanol oxygen atoms. There are two solvent methanol molecules in the asymmetric unit. In the crystal structure, intermolecular O—H—O hydrogen bonds connect complex molecules and methanol solvent molecules to form (10-2) sheets.

Experimental

The title complex was obtained by the treatment of nickel(II) acetate tetrahydrate (0.0622 g, 0.25 mmol) with the Schiff base (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 (0.1115 g, 0.25 mmol). The reaction mixture was cooled and filtered; diethyl ether was allowed to diffuse slowly into the solution of the filtrate. Blue single crystals were obtained after several days. Analysis calculated for C₂₃H₃₆NiN₅O₁₇ Sm: C31.99; H, 4.20; N, 8.11; found: C, 32.01; H, 4.18; N, 8.14