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′)praseodymium(III)]

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

doi:10.1107/S1600536811034702

. 2011 Aug 31;67(Pt 9):m1321. doi: 10.1107/S1600536811034702

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′)praseodymium(III)]

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

PMCID: PMC3200949 PMID: 22058896

Abstract

In the centrosymmetric binuclear title complex, [Pr₂(C₉H₉O₃)₆(C₁₂H₈N₂)₂], the two Pr^III ions are linked by four 2-phenoxypropionate (L) groups through their bi- and tridentate bridging modes. Each Pr^III ion is nine-coordinated by one 1,10-phenanthroline molecule, one bidentate carboxylate group and four bridging carboxylate groups in a distorted PrN₂O₇ monocapped square-antiprismatic geometry. The title compound is isotypic with its terbium- and dysprosium-containing analogues.

Related literature

For the isotypic Tb and Dy compounds, see: Shen et al. (2011a ▶,b ▶). For a related structure, see: Li et al. (2008 ▶).

Experimental

Crystal data

[Pr₂(C₉H₉O₃)₆(C₁₂H₈N₂)₂]
M _r = 1633.20
Monoclinic,
a = 11.5142 (2) Å
b = 25.8845 (4) Å
c = 13.9275 (2) Å
β = 120.204 (1)°
V = 3587.41 (10) Å³
Z = 2
Mo Kα radiation
μ = 1.42 mm⁻¹
T = 296 K
0.39 × 0.15 × 0.11 mm

Data collection

Bruker APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.779, T _max = 0.862
48041 measured reflections
6322 independent reflections
5424 reflections with I > 2σ(I)
R _int = 0.033

Refinement

R[F ² > 2σ(F ²)] = 0.022
wR(F ²) = 0.051
S = 1.02
6322 reflections
464 parameters
H-atom parameters constrained
Δρ_max = 0.36 e Å⁻³
Δρ_min = −0.30 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/S1600536811034702/hb6378sup1.cif

e-67-m1321-sup1.cif^{(28.2KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811034702/hb6378Isup2.hkl

e-67-m1321-Isup2.hkl^{(309.5KB, hkl)}

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

Table 1. Selected bond lengths (Å).

Pr1—O5ⁱ	2.4215 (15)
Pr1—O7	2.4320 (15)
Pr1—O8ⁱ	2.4657 (15)
Pr1—O2	2.5117 (17)
Pr1—O1	2.5324 (16)
Pr1—O4	2.5501 (15)
Pr1—N1	2.6199 (18)
Pr1—O5	2.6755 (15)
Pr1—N2	2.6782 (18)

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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., 2011a,b) we now describe the title Pr^III complex.

The structure of the title compound (1) is a dinuclear praseodymium complex with Pr—PrA separation of 4.0785 (2) Å. The structure of the complex (Fig. 1) reveals that the molecule contains six L, two phen molecules and two Pr^III ions. Each Pr(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 Pr^III ions in three different modes: chelating,bridging and bridging tridentate.The analysis of structural features indicates that the central Pr(III) ion adopts a distorted monocapped square antiprism geometry(Fig. 2).The Pr—O distances are all within the range 2.4215 (15)–2.6755 (15) Å, and the Pr—N distances rang from 2.6199 (18)–2.6782 (18) Å, all of which are within the range of those of other nine-coordinated Pr^III complexes with carboxylic donor ligands and 1,10-phenanthroline (Li et al., 2008). 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), Pr(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. The colourless crystal was obtained after several days.