catena-Poly[[[(1,10-phenanthroline-κ2 N,N′)praseodymium(III)]-di-μ-4-hydroxy­benzoato-κ4 O 1:O 1′-μ-nitrato-κ3 O,O′:O] bis­(1,10-phenanthroline)]

Panfeng Wang; Dingding Xu; Xinqing Wang

doi:10.1107/S1600536812029911

. 2012 Aug 4;68(Pt 9):m1148. doi: 10.1107/S1600536812029911

catena-Poly[[[(1,10-phenanthroline-κ² N,N′)praseodymium(III)]-di-μ-4-hydroxybenzoato-κ⁴ O ¹:O ^1′-μ-nitrato-κ³ O,O′:O] bis(1,10-phenanthroline)]

Panfeng Wang ^a, Dingding Xu ^a, Xinqing Wang ^a,^*

PMCID: PMC3435577 PMID: 22969450

Abstract

The title complex, [Pr(C₇H₅O₃)₂(NO₃)(C₁₂H₈N₂)]·2C₁₂H₈N₂, has a polymeric chain structure, with two uncoordinated 1,10-phenanthroline molecules in the lattice. The Pr^III centre has a monocapped square-antiprismatic coordination geometry, comprised of two N atoms from one chelating 1,10-phenanthroline ligand, four carboxylate O atoms from four 4-hydroxybenzoate anions and three O atoms from two nitrate anions. The 4-hydroxybenzoate and nitrate anions function as μ₂-bridging ligands and link the Pr^III ions into a one-dimensional chain structure along the c axis. Intermolecular O—H⋯N hydrogen bonds are observed between the 4-hydroxybenzoate anions and the uncoordinated 1,10-phenanthroline molecules.

Related literature

For related structures, see: Zhou et al. (2008 ▶); Zhu et al. (2010 ▶)

Experimental

Crystal data

[Pr(C₇H₅O₃)₂(NO₃)(C₁₂H₈N₂)]·2C₁₂H₈N₂
M _r = 1017.75
Monoclinic,
a = 21.5625 (2) Å
b = 23.4621 (2) Å
c = 8.6030 (1) Å
β = 98.899 (1)°
V = 4299.88 (7) Å³
Z = 4
Cu Kα radiation
μ = 9.27 mm⁻¹
T = 291 K
0.40 × 0.33 × 0.30 mm

Data collection

Oxford Diffraction Gemini S Ultra diffractometer
Absorption correction: multi-scan (CrysAlis PRO; Oxford Diffraction, 2006 ▶) T _min = 0.119, T _max = 0.167
13264 measured reflections
7308 independent reflections
6794 reflections with I > 2σ(I)
R _int = 0.029

Refinement

R[F ² > 2σ(F ²)] = 0.035
wR(F ²) = 0.092
S = 1.06
7308 reflections
606 parameters
H-atom parameters constrained
Δρ_max = 0.74 e Å⁻³
Δρ_min = −1.31 e Å⁻³

Data collection: CrysAlis CCD (Oxford Diffraction, 2006 ▶); cell refinement: CrysAlis RED (Oxford Diffraction, 2006 ▶); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 (Farrugia, 1997 ▶); software used to prepare material for publication: SHELXL97.

Supplementary Material

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812029911/fj2550sup1.cif

e-68-m1148-sup1.cif^{(51.9KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812029911/fj2550Isup2.hkl

e-68-m1148-Isup2.hkl^{(357.6KB, 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
O6—H6⋯N4ⁱ	0.82	2.07	2.851 (4)	158
O3—H3⋯N6ⁱⁱ	0.82	2.04	2.782 (5)	150

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

Acknowledgments

The authors thank Dr H. P. Xiao for help with the experiments.

supplementary crystallographic information

Experimental

Each reagent was commercially available and of analytical grade. Pr(NO₃)₃^.6H₂O (0.217 g, 0.5 mmol), p-Hydroxybenzoic acid (0.069 g 0.5 mmol), 1, 10-phenanthroline (0.090 g, 0.5 mmol) and NaHCO₃ (0.042 g, 0.5 mmol) were dissolved in water-ethanol solution (10 ml, 5:5). The solution was refluxed for 4 h, and filtered after cooling to room temperature. White single crystals were obtained from the filtrate after 7 days.