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′)terbium(III)]

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

doi:10.1107/S1600536811032041

. 2011 Aug 11;67(Pt 9):m1234. doi: 10.1107/S1600536811032041

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′)terbium(III)]

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

PMCID: PMC3200853 PMID: 22058858

Abstract

In the centrosymmetric binuclear title complex, [Tb₂(C₉H₉O₃)₆(C₁₂H₈N₂)₂], the two Tb^III ions are linked by four 2-phenoxypropionate (L) groups through their bi- and tridentate bridging modes. Each Tb^III ion is nine-coordinated by one 1,10-phenanthroline molecule, one bidentate carboxylate group and four bridging carboxylate groups in a distorted TbN₂O₇ monocapped square-antiprismatic geometry.

Related literature

For background to phenoxyalkanoic acids, see: Markus & Buser (1997 ▶). For a related structure, see: Zhao et al. (2008 ▶).

Experimental

Crystal data

[Tb₂(C₉H₉O₃)₆(C₁₂H₈N₂)₂]
M _r = 1669.24
Monoclinic,
a = 11.4747 (3) Å
b = 25.8130 (8) Å
c = 13.8530 (3) Å
β = 120.585 (2)°
V = 3532.35 (16) Å³
Z = 2
Mo Kα radiation
μ = 2.06 mm⁻¹
T = 296 K
0.21 × 0.16 × 0.09 mm

Data collection

Bruker APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.685, T _max = 0.834
24708 measured reflections
6213 independent reflections
4431 reflections with I > 2σ(I)
R _int = 0.051

Refinement

R[F ² > 2σ(F ²)] = 0.033
wR(F ²) = 0.073
S = 1.01
6213 reflections
464 parameters
H-atom parameters constrained
Δρ_max = 0.72 e Å⁻³
Δρ_min = −0.81 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/S1600536811032041/hb6349sup1.cif

e-67-m1234-sup1.cif^{(36.7KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811032041/hb6349Isup2.hkl

e-67-m1234-Isup2.hkl^{(304.1KB, hkl)}

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

Table 1. Selected bond lengths (Å).

Tb1—O8ⁱ	2.336 (3)
Tb1—O5ⁱ	2.344 (3)
Tb1—O4	2.381 (3)
Tb1—O2	2.422 (3)
Tb1—O7	2.457 (3)
Tb1—O1	2.475 (3)
Tb1—N2	2.525 (3)
Tb1—N1	2.606 (3)
Tb1—O8	2.623 (2)

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Symmetry code: (i) Inline graphic .

supplementary crystallographic information

Comment

The group of phenoxyalkanoic acids includes a considerable number of important herbicides. The desired biological activity is largely dependent on the length of the carbon chain of the alkanoic acid, the nature of the phenoxy group, and the position of its attachment to the carbon chain (Markus et al., 1997). The fascinating structures of 2-phenoxypropionic acid complexes coupled with their special functionality catch our interests.Here,we describe the new title Tb^III complex, (I).

The structure of (I) is shown in Fig.1 and the coordination envi- ronment of Tb^III was shown in Fig. 2. The dimeric title compound(1) is centrosymmetric and is comprised of six L and two phen. The two Tb^III ions are linked together by four L groups through their bi- and tri- dentate bridging modes, form a dimeric unit with crystallographic inversion center, and the distance between two Tb^III ions is 3.9935 (3) Å, which is similar to the analogous complexe (Zhao et al., 2008). Each Tb^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 analysis of structural features indicates that the central Tb^III ion adopts a distorted mono-capped square antiprism geometry(Fig. 2). The Tb—O distances are all within the range 2.336 (3)–2.623 (2) Å, and the Tb—N distances rang from 2.525 (3)–2.606 (3) Å. The selected bond lengths for complex 1 are listed in Table 1.

Experimental

Reagents and solvents used were of commercially available quality and without purified before using. 2-phenoxypropionic acid (1.5 mmol), Tb(NO₃)₃.6H₂O (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 to yield colourless blocks of (I) after several days.