Tetra­kis(μ-2-phen­oxy­propionato)-κ3 O,O′:O′;κ3 O:O,O′,κ4 O:O′-bis­[(1,10-phenanthroline-κ2 N,N′)(2-phen­oxy­propionato-κ2 O,O′)dysprosium(III)]

Jin-Bei Shen; Jia-Lu Liu; Guo-Liang Zhao

doi:10.1107/S1600536811034696

. 2011 Aug 31;67(Pt 9):m1320. doi: 10.1107/S1600536811034696

Tetrakis(μ-2-phenoxypropionato)-κ³ O,O′:O′;κ³ O:O,O′,κ⁴ O:O′-bis[(1,10-phenanthroline-κ² N,N′)(2-phenoxypropionato-κ² O,O′)dysprosium(III)]

Jin-Bei Shen ^a, Jia-Lu Liu ^a, Guo-Liang Zhao ^a,^b,^*

PMCID: PMC3200901 PMID: 22058895

Abstract

In the centrosymmetric binuclear title complex, [Dy₂(C₉H₉O₃)₆(C₁₂H₈N₂)₂], the two Dy^III ions are linked by four 2-phenoxypropionate (L) groups through their bi- and tridentate bridging modes. Each Dy^III ion is nine-coordinated by one 1,10-phenanthroline molecule, one bidentate carboxylate group and four bridging carboxylate groups in a distorted DyN₂O₇ monocapped square-antiprismatic geometry. The title compound is isotypic with its terbium-containing analogue.

Related literature

For the terbium analogue of the title compound, see: Shen et al. (2011 ▶). For a related structure, see: Liu et al. (2010 ▶).

Experimental

Crystal data

[Dy₂(C₉H₉O₃)₆(C₁₂H₈N₂)₂]
M _r = 1676.38
Monoclinic,
a = 11.4738 (1) Å
b = 25.8057 (3) Å
c = 13.8525 (2) Å
β = 120.657 (1)°
V = 3528.32 (7) Å³
Z = 2
Mo Kα radiation
μ = 2.18 mm⁻¹
T = 296 K
0.32 × 0.14 × 0.08 mm

Data collection

Bruker APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.710, T _max = 0.840
47810 measured reflections
6224 independent reflections
5057 reflections with I > 2σ(I)
R _int = 0.043

Refinement

R[F ² > 2σ(F ²)] = 0.025
wR(F ²) = 0.053
S = 1.05
6224 reflections
463 parameters
H-atom parameters constrained
Δρ_max = 0.76 e Å⁻³
Δρ_min = −0.49 e Å⁻³

Data collection: APEX2 (Bruker, 2006 ▶); cell refinement: SAINT (Bruker, 2006 ▶); data reduction: SAINT; 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 datablock(s) I, global. DOI: 10.1107/S1600536811034696/hb6365sup1.cif

e-67-m1320-sup1.cif^{(28.1KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811034696/hb6365Isup2.hkl

e-67-m1320-Isup2.hkl^{(304.7KB, hkl)}

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

Table 1. Selected bond lengths (Å).

Dy1—O8ⁱ	2.3252 (18)
Dy1—O4	2.3328 (18)
Dy1—O5ⁱ	2.3731 (19)
Dy1—O1	2.412 (2)
Dy1—O7	2.4421 (19)
Dy1—O2	2.462 (2)
Dy1—N2	2.518 (2)
Dy1—N1	2.594 (2)
Dy1—O8	2.622 (2)

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Symmetry code: (i) Inline graphic .

supplementary crystallographic information

Comment

As part of our ongoing studies of 2-phenoxypropionic acid complexes (Shen et al., 2011) we describe a new Dy^III complex.

The structure of the title compound (1) is a dinuclear dysprosium complex with Dy—Dy separation of 3.9857 (3) Å. The structure of the complex (Fig. 1) reveals that the molecule contains six L, two phen molecules and two Dy^III ions. Each Dy(III) ion is coordinated to nine atoms, of which five oxygen atoms are from the bridging carboxylates, two oxygen atoms from the bidentate chelating carboxylate group, and two nitrogen atoms from a 1,10- phenanthroline molecule. The L ligands are coordinated to the Dy^III ions in three different modes: chelating,bridging and bridging tridentate.The analysis of structural features indicates that the central Dy(III) ion adopts a distorted monocapped square antiprism geometry(Fig. 2).The Dy—O distances are all within the range 2.3252 (18)–2.622 (2) Å, and the Dy—N distances rang from 2.518 (2)–2.594 (2) Å, all of which are within the range of those of other nine-coordinated Dy^III complexes with carboxylic donor ligands and 1,10- phenanthroline (Liu et al., 2010). The selected bond lengths and angles for complex 1 are listed in Table 1. In addition, there are no classical hydrogen bonds in the crystal structure, because good hydrogen bond donors are absent. The most significant intermolecular interactions are C—H···O hydrogen bonds (Table 2) and weak π···π aromatic interactions from phen molecules and aromatic rings of the L ligands.

Experimental

Reagents and solvents used were of commercially available quality and without purified before using. 2-phenoxypropionic acid (1.5 mmol), Dy(NO₃)₃.5H₂O (0.5 mmol) and 1,10-phenanthroline (0.5 mmol) were dissolved in 20 ml e nthanol, then 10 ml water was added to the above solution. The mixed solution was stirred for 12 h at room temperature. At last, deposit was filtered out and the colourless solution was kept in the open air. Colourless blocks of (I) were obtained after several days.