Synthesis and crystal structures of (NH3CH2CH 2NH3)1.5[(VO)2(HPO4) 2(PO4)] and (C4H12N 2)2[V4O6H(HPO4) 2(PO4)2], two layered vanadium phosphates templated with organic diamines

Vítězslav Zima, Kwang Hwa Lii

Research output: Contribution to journalArticlepeer-review

13 Scopus citations

Abstract

Two new layered vanadium phosphates templated by ethylenediamine, (NH 3CH2CH2NH3)1.5[(VO) 2(HPO4)2(PO4)] (1), and piperazine, (C4H12N2)2[V4O 6H(HPO4)2(PO4)2] (2), have been synthesized hydrothermally and their structures determined by single-crystal X-ray diffraction. Compound 1 crystallizes in the monoclinic space group C2/c (no. 15) with a=18.6051(5), b=7.1193(1), c=23.4597(7)Å, β=96.558(2)°, V=3087.03Å3, Z=8, and R1=0.0583. The structure consists of infinite chains of trans-corner-shared VO6 octahedra, which are bridged by phosphate groups. The infinite chains are connected by VO5 square pyramids via V-O-P bonds to form layers with 10-sided windows. Adjacent layers are aligned such that infinite tunnels along the [001] direction are generated. Ethylenediammonium cations are located at sites both in the interlayer space and in the windows within the layers. Crystal data for 2: orthorhombic, space group Pna21 (no. 33), a=13.1812(6), b=15.2918(8), c=6.2821(3) Å, V=1266.25Å3, Z=2, and R1=0.0367. Compound 2 is a mixed-valence VIV/VV vanadium phosphate as was confirmed by magnetic susceptibility measurements. VIVO6 octahedra connected via HPO4 groups form a double chain, which alternates with a chain of trans-corner-shared square pyramids containing an infinite VIV-O-VV-O motif. Both chains are connected through phosphate groups to form a layer, which contains 14-membered empty windows. Piperazinium dications are anchored in the interlayer space.

Original languageEnglish
Pages (from-to)424-430
Number of pages7
JournalJournal of Solid State Chemistry
Volume172
Issue number2
DOIs
StatePublished - May 2003

Keywords

  • Ethylenediamine
  • Hydrothermal synthesis
  • Piperazine
  • Structure
  • Vanadium phosphate

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