Tetra­kis(μ-3,4-dimethoxy­phenyl­acetato)bis­[(3,4-dimethoxy­phenyl­acetato)(1,10-phenanthroline)dysprosium(III)]

Jian-Feng Liu; Xue-Dan Xu; Hua-Qiong Li; Guo-Liang Zhao

doi:10.1107/S1600536810005143

. 2010 Feb 13;66(Pt 3):m291. doi: 10.1107/S1600536810005143

Tetrakis(μ-3,4-dimethoxyphenylacetato)bis[(3,4-dimethoxyphenylacetato)(1,10-phenanthroline)dysprosium(III)]

Jian-Feng Liu ^a, Xue-Dan Xu ^a, Hua-Qiong Li ^a, Guo-Liang Zhao ^a,^*

PMCID: PMC2983715 PMID: 21580236

Abstract

The title centrosymmetric dinuclear dysprosium(III) complex, [Dy₂(C₁₀H₁₁O₄)₆(C₁₂H₈N₂)₂] or [Dy(L)₃phen]₂, is comprised of six 3,4-dimethoxyphenylacetate (L) anions, two 1,10-phenanthroline (phen) molecules and two Dy^III ions. The Dy^III atom is nine-coordinated by seven O atoms from five L ligands and two N atoms from the phen molecules. The L ligands are coordinated to the Dy^III ion in three coordination modes: chelating, bridging and bridging-tridentate. C—H⋯O hydrogen bonding interactions consolidate the crystal packing.

Related literature

For related structures, see: Li et al. (2006 ▶, 2007 ▶).

Experimental

Crystal data

[Dy₂(C₁₀H₁₁O₄)₆(C₁₂H₈N₂)₂]
M _r = 1856.54
Triclinic,
a = 12.3287 (2) Å
b = 12.3843 (3) Å
c = 14.6667 (3) Å
α = 90.968 (1)°
β = 103.461 (1)°
γ = 115.523 (1)°
V = 1947.70 (7) Å³
Z = 1
Mo Kα radiation
μ = 1.99 mm⁻¹
T = 296 K
0.43 × 0.19 × 0.07 mm

Data collection

Bruker APEXII CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T _min = 0.641, T _max = 0.874
26184 measured reflections
6861 independent reflections
5927 reflections with I > 2σ(I)
R _int = 0.035

Refinement

R[F ² > 2σ(F ²)] = 0.028
wR(F ²) = 0.066
S = 1.03
6861 reflections
514 parameters
H-atom parameters constrained
Δρ_max = 0.62 e Å⁻³
Δρ_min = −0.42 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: SHELXTL.

Supplementary Material

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810005143/pv2234sup1.cif

e-66-0m291-sup1.cif^{(41KB, cif)}

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810005143/pv2234Isup2.hkl

e-66-0m291-Isup2.hkl^{(335.7KB, hkl)}

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

Table 1. Hydrogen-bond geometry (Å, °).

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C1—H1A⋯O6ⁱ	0.96	2.54	3.320 (5)	138
C16—H16A⋯O3ⁱⁱ	0.93	2.53	3.425 (4)	161
C18—H18B⋯O3ⁱⁱ	0.96	2.36	3.262 (4)	156
C21—H21A⋯O1ⁱⁱⁱ	0.96	2.49	3.362 (6)	151
C21—H21A⋯O2ⁱⁱⁱ	0.96	2.43	3.214 (5)	139
C33—H33A⋯O7^iv	0.93	2.38	3.231 (4)	153
C31—H31A⋯O4	0.93	2.52	2.977 (4)	111

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

supplementary crystallographic information

Comment

The rare earth complexes with N/O-donors ligands such as 1,10-phenanthroline and carboxylic acid have received considerable attention for many years (Li et al., 2007; Li et al., 2006). The structure of the title compound, [Dy(L)₃phen]₂, (I), is a dinuclear dysprosium complex with Dy—DyA separation of 3.8887 (3) Å. The structure of the complex (Fig. 1) reveals that the molecule contains six 3,4-dimethoxyphenylacetic anions (L) and two 1,10-phenanthroline (phen) molecules and two Dy^III ions. The Dy^III ion is nine-coordinated by two N atoms from one phen and seven O atoms from (L) anions. The Dy—O bond distances range from 2.320 (2) to 2.522 (3) Å and the Dy—N bond distances are 2.536 (3) and 2.612 (3) 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 (Li et al., 2006). The (L) ligands are coordinated to the Dy^III ions in three different modes: chelating, bridging and bridging tridentate. Around each Dy^III, there is one L ligand in chelating mode through two O atoms from the carboxyl group. Two symmetric L ligands bridge the two Dy centers though carboxyl O atoms. One L ligand is coordinated in a bidentate mode with Dy ion with O7 and O8 from carboxyl group and simultaneously bands to DyA ion with O8. 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 1) and weak π···π aromatic interactions from phen molecules and aromatic rings of the L ligands. A packing plot is shown in Fig. 2.

Experimental

A mixture of 3,4-dimethoxyphenylacetic acid (0.5886 g, 3 mmol), Dy₂O₃ (0.1865 g, 0.5 mmol), 1,10-phenanthroline (0.1982 g, 1 mmol) and purified water (20 ml) was sealed in a 25 ml stainless steel reactor and kept at 433 K for 3 d. Then, the reactor was cooled to room temperature at a speed of 5 degrees per hour. Lots of pink single crystals were filtered out of the mixture at high field (80%).