Tetra­kis(μ2-2-phen­oxy­propionato)-κ3 O,O′:O′;κ3 O:O,O′;κ4 O:O′-bis­[(1,10-phenanthroline-κ2 N,N′)(2-phen­oxy­propionato-κ2 O,O′)gadolinium(III)]

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

doi:10.1107/S1600536811036130

. 2011 Sep 14;67(Pt 10):m1357. doi: 10.1107/S1600536811036130

Tetrakis(μ₂-2-phenoxypropionato)-κ³ O,O′:O′;κ³ O:O,O′;κ⁴ O:O′-bis[(1,10-phenanthroline-κ² N,N′)(2-phenoxypropionato-κ² O,O′)gadolinium(III)]

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

PMCID: PMC3201527 PMID: 22064805

Abstract

In the centrosymmetric binuclear title complex, [Gd₂(C₉H₉O₃)₆(C₁₂H₈N₂)₂], the two Gd(III) ions are linked by four 2-phenoxypropionate (L) groups in bi- and tridentate bridging modes. Each Gd^III ion is nine-coordinated by one 1,10-phenanthroline molecule, one bidentate chelating carboxylate group and four bridging carboxylate groups in a distorted GdN₂O₇ monocapped square-antiprismatic geometry.

Related literature

For background to phenoxyalkanoic acids, see: Markus & Buser (1997 ▶). For a related Gd complex, see: Yu et al. (2010 ▶). For isotypic structures, see: Shen et al. (2011a ▶) for Tb; Shen et al. (2011b ▶) for Pr; Shen et al. (2011c ▶) for Dy; Shen et al. (2011d ▶) for Ce; Shen et al. (2011e ▶) for Ho; Shen et al. (2011f ▶) for La.

Experimental

Crystal data

[Gd₂(C₉H₉O₃)₆(C₁₂H₈N₂)₂]
M _r = 1665.88
Monoclinic,
a = 11.4876 (2) Å
b = 25.8305 (4) Å
c = 13.8715 (2) Å
β = 120.554 (1)°
V = 3544.58 (10) Å³
Z = 2
Mo Kα radiation
μ = 1.93 mm⁻¹
T = 296 K
0.49 × 0.24 × 0.16 mm

Data collection

Bruker APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.585, T _max = 0.741
47235 measured reflections
6250 independent reflections
5788 reflections with I > 2σ(I)
R _int = 0.022

Refinement

R[F ² > 2σ(F ²)] = 0.021
wR(F ²) = 0.043
S = 1.15
6250 reflections
463 parameters
H-atom parameters constrained
Δρ_max = 0.72 e Å⁻³
Δρ_min = −0.37 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: XP in SHELXTL (Sheldrick, 2008 ▶) and DIAMOND (Brandenburg, 2006 ▶); software used to prepare material for publication: SHELXL97.

Supplementary Material

Crystal structure: contains datablock(s) I. DOI: 10.1107/S1600536811036130/wm2524sup1.cif

e-67-m1357-sup1.cif^{(37.9KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811036130/wm2524Isup2.hkl

e-67-m1357-Isup2.hkl^{(306KB, hkl)}

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

Table 1. Selected bond lengths (Å).

Gd1—O7ⁱ	2.3528 (14)
Gd1—O4	2.3624 (15)
Gd1—O5ⁱ	2.3991 (15)
Gd1—O2	2.4443 (16)
Gd1—O8	2.4742 (15)
Gd1—O1	2.4826 (15)
Gd1—N2	2.5496 (18)
Gd1—N1	2.6184 (18)
Gd1—O7	2.6270 (15)

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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 & Buser, 1997). The structures of 2-phenoxypropionic acid (HL) complexes coupled with their special functionality catched our interest. Here, we describe the Gd^III title complex, (I).

The structure of complex (I) is shown in Fig. 1 and the coordination environment of Gd(III) is shown in Fig. 2. The dimeric title compound (I) is centrosymmetric and is comprised of six L anions and two phenanthroline ligands. The two Gd(III) ions are linked together by four L groups through their bi- and tri-dentate bridging modes, forming a dimeric unit. The distance between two Gd(III) ions in the dimeric unit is 4.0047 (2) Å, which is similar to a related complex (Yu et al., 2010). Each Gd(III) ion is coordinated by nine atoms, five of which are oxygen atoms from the bridging carboxylates, two oxygen atoms from the bidentate chelating carboxylate group, and two nitrogen atoms from a 1,10-phenanthroline molecule. The Gd(III) ion adopts a distorted monocapped square antiprisatic geometry (Fig. 2). The Gd—O distances are all within the range 2.3528 (14)–2.6270 (15) Å, and the Gd—N distances range from 2.5496 (18)–2.6184 (18) Å (Table 1).

For isotypic structures, see: for Tb (Shen et al., 2011a), for Pr (Shen et al., 2011b), for Dy (Shen et al., 2011c), for Ce (Shen et al., 2011d), for Ho (Shen et al., 2011e), for La (Shen et al., 2011f).

Experimental

Reagents and solvents used were of commercially available quality and without purified before use. 2-Phenoxypropionic acid (1.5 mmol), Gd(NO₃)₃^.6H₂O (0.5 mmol) and 1,10-phenanthroline (0.5 mmol) were dissolved in 20 ml enthanol, then 10 ml water were added to the above solution. The mixed solution was stirred for 12 h at room temperature. Finally, the deposit was filtered off and the colourless solution was kept in the open air. Colourless crystals were obtained after several days.