catena-Poly[[(1,10-phenanthroline-κ2 N,N′)praseodymium(III)]-di-μ-phenoxy­acetato-κ4 O:O′-[(1,10-phenanthroline-κ2 N,N′)praseodymium(III)]-di-μ-phenoxy­acetato-κ4 O:O′-di-μ-phenoxy­acetato-κ3 O,O′:O;κ3 O:O,O′]

H Zhong; X-M Yang; Q-Y Luo; Y-P Xu

doi:10.1107/S1600536807068614

This article has been retracted.

Retraction in: Acta Crystallogr Sect E Struct Rep Online. 2009 Dec 19;66(Pt 1):e11 See also: PMC Retraction Policy

. 2008 Jan 9;64(Pt 2):m317–m318. doi: 10.1107/S1600536807068614

catena-Poly[[(1,10-phenanthroline-κ² N,N′)praseodymium(III)]-di-μ-phenoxyacetato-κ⁴ O:O′-[(1,10-phenanthroline-κ² N,N′)praseodymium(III)]-di-μ-phenoxyacetato-κ⁴ O:O′-di-μ-phenoxyacetato-κ³ O,O′:O;κ³ O:O,O′]

H Zhong ^a,^*, X-M Yang ^b, Q-Y Luo ^a, Y-P Xu ^a

PMCID: PMC2960179 PMID: 21201288

Abstract

The title complex, [Pr₂(C₈H₇O₃)₆(C₁₂H₈N₂)₂]_n, which has an inversion centre midway between the two Pr^III atoms of the structural unit, forms a one-dimensional polymer bridged alternately by either two bidentate, or two bidentate and two terdentate, phenoxyacetate carboxylate groups. Each Pr^III atom is thus nine-coordinated by two N atoms of a 1,10-phenanthroline ligand and seven O atoms from six phenoxyacetate ligands. The coordination geometry at the Pr^III atom is distorted tricapped trigonal prismatic. One phenyl ring is disordered over two positions; the site occupancy factors are ca 0.6 and 0.4.

Related literature

For related literature, see: Allen et al. (1987 ▶); Daiguebonne et al. (2000 ▶); Farrugia et al. (2000 ▶); Kay et al. (1972 ▶); Ma et al. (1999 ▶); Mao et al. (1998 ▶); Starynowicz (1991 ▶, 1993 ▶); Tsukube & Shinoda (2002 ▶); Zhang et al. (2005 ▶); Zeng et al. (2000 ▶); Zhong et al. (2007 ▶).

Experimental

Crystal data

[Pr₂(C₈H₇O₃)₆(C₁₂H₈N₂)₂]
M _r = 1549.04
Monoclinic,
a = 20.204 (4) Å
b = 8.499 (4) Å
c = 20.799 (3) Å
β = 107.198 (6)°
V = 3411.8 (17) Å³
Z = 2
Mo Kα radiation
μ = 1.49 mm⁻¹
T = 273 (2) K
0.33 × 0.12 × 0.08 mm

Data collection

Bruker APEXII area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.642, T _max = 0.890
27763 measured reflections
7712 independent reflections
5037 reflections with I > 2σ(I)
R _int = 0.043

Refinement

R[F ² > 2σ(F ²)] = 0.036
wR(F ²) = 0.097
S = 0.90
7712 reflections
452 parameters
144 restraints
H-atom parameters constrained
Δρ_max = 1.03 e Å⁻³
Δρ_min = −0.64 e Å⁻³

Data collection: SMART (Siemens, 1996 ▶); cell refinement: SAINT (Siemens, 1996 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Siemens, 1996 ▶); software used to prepare material for publication: SHELXTL.

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536807068614/rt2009sup1.cif

e-64-0m317-sup1.cif^{(28.9KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536807068614/rt2009Isup2.hkl

e-64-0m317-Isup2.hkl^{(377.3KB, hkl)}

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

Table 1. Selected geometric parameters (Å, °).

Pr1—O1	2.489 (2)
Pr1—O2ⁱ	2.535 (2)
Pr1—O4	2.565 (2)
Pr1—O5	2.817 (3)
Pr1—O5ⁱ	2.449 (2)
Pr1—O7	2.409 (3)
Pr1—O8ⁱⁱ	2.545 (3)
Pr1—N1	2.753 (3)
Pr1—N2	2.720 (3)

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O1—Pr1—O4	73.62 (8)
O1—Pr1—O5	65.11 (8)
O1—Pr1—O7	145.88 (9)
O4—Pr1—O5	48.17 (8)
O4—Pr1—O7	138.84 (9)
O5—Pr1—O7	139.57 (8)
O1—Pr1—N1	127.55 (9)
O4—Pr1—N1	63.48 (9)
O5—Pr1—N1	102.34 (9)
O7—Pr1—N1	77.09 (9)
O1—Pr1—N2	81.11 (9)
O4—Pr1—N2	74.08 (9)
O5—Pr1—N2	118.22 (8)
O7—Pr1—N2	96.74 (9)
N1—Pr1—N2	59.78 (10)

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

Table 2. Hydrogen-bond geometry (Å, °).

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C1—H1⋯O2ⁱ	0.93	2.46	3.147 (5)	130
C10—H10⋯O4ⁱⁱⁱ	0.93	2.34	3.211 (5)	156
C12—H12⋯O8ⁱⁱ	0.93	2.47	3.063 (5)	122
C22—H22B⋯O7^iv	0.97	2.41	3.353 (5)	166

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

Acknowledgments

This work was supported by the Science and Technology Bureau of Jian, Jiangxi Province, China (grant No. 20052817).

supplementary crystallographic information

Comment

In recent years, there has been great interest in the synthesis of metal organic frameworks (MOFs) with organic ligands and rare earth metals because of their novel structures, fascinating properties and important roles in special materials with potential optical, electronic, magnetic and biological applications (Daiguebonne et al., 2000; Farrugia et al., 2000; Tsukube & Shinoda, 2002; Zhang et al., 2005). These compounds are usually prepared by the reaction of rare-earth metal ions with bi- or multidentate ligands (Starynowicz, 1991, 1993; Kay et al., 1972; Ma et al., 1999; Zeng et al., 2000; Mao et al., 1998). We report herein the crystal structure of the title compound, (I).

In the molecular unit of (I) (Fig. 1), the ligand bond lengths and angles are within normal ranges (Allen et al., 1987). The Pr^III metal centres are bridged alternatively either by two bidentate, or by two terdentate and two bidentate, phenoxyacetato carboxylate groups with an inversion centre between them. Each Pr atom is nine-coordinated by two N atoms of the 1,10-phenanthroline ligand and seven O atoms from six phenoxyacetate ligands (Table 1), and the coordination geometry at the Pr atom forms a tricapped trigonal prism. The Pr—O bond lengths are in the range 2.409 (3) to 2.817 (3) Å. The Pr—N bond lengths are in the range 2.720 (3) to 2.753 (3) Å. Hydrogen bonds between C—H groups and O atoms of neighbouring phenoxyacetate ligands, with C···O distances of 3.063 (5) to 3.353 (5) Å, generate a layered hydrogen-bonded network (Table 2).

Experimental

The title compound was synthesized using the hydrothermal method in a 23 ml Teflon-lined Parr bomb, which was then sealed. Praseodymium(III) chloride hexahydrate (71.1 mg, 0.2 mmol), 1,10-phenanthroline (39.6 mg, 0.2 mmol), phenoxyacetic acid (91.3 mg, 0.6 mmol), sodium hydroxide (24 mg, 0.6 mmol) and distilled water (4 g) were placed into the bomb and sealed. The bomb was then heated under autogenous pressure for 7 d at 413 K and allowed to cool at room temperature for 24 h. Upon opening the bomb, a clear colorless solution was decanted from small green crystals. These crystals were washed with distilled water followed by ethanol, and allowed to air-dry at room temperature (yield: 72.7 mg, 36%).