Hydrothermal Synthesis and X-Ray Single Crystal Structure of [Zn(en)2]6[(VO)12O6B18O39(OH)3]·13H2O

✍ Scribed by Lirong Zhang; Zhan Shi; Guoyu Yang; Xiaoming Chen; Shouhua Feng

• Publisher: Elsevier Science
• Year: 1999
• Tongue: English
• Weight: 167 KB
• Volume: 148
• Category: Article
• ISSN: 0022-4596
• DOI: 10.1006/jssc.1999.8478

✦ Synopsis

A hydrothermal reaction of NaVO 3 , H 3 BO 3 , Zn(CH 3 COO) 2 , ethylenediamine, and H 2 O gives a coordination cluster [Zn(en

(denoted on Zn 6 V 12 B 18 ). The Zn 6 V 12 B 18 crystallizes in a rhombohedral system with space group R-3 and unit cell parameters a ‫؍‬ 20.686(3) A s , c ‫؍‬ 20.915(4) A s , V ‫؍‬ 7751(2) A s 3 , Z ‫؍‬ 3, and R ‫؍‬ 0.0689. The structure consists of an 18-membered ring of B 18 O 39 (OH) 3 sandwiched between two alternating edge-sharing vanadium+oxygen clusters V 6 O 15 by six B+( 3 +O)+V 2 bonds and three B 2 +( 3 +O)+V bonds. Each of the six zinc atoms coordinated with two ethylenediamine molecules and connected with the B 18 O 39 (OH) 3 ring by one Zn-( 3 +O)+B bond. A water molecule occupied the center of the Zn 6 V 12 B 18 cluster. The oxidation states of vanadium in the compound are V(IV) and V(V) in a ratio of 3 : 1. Other characterizations by IR spectroscopy, TGA, and DTA are also described.