高等学校化学学报

高等学校化学学报 ›› 2001, Vol. 22 ›› Issue (12): 1963.

• 研究论文 •    下一篇

Na2[(VO)12O6B18O39(OH)3]·(11H3O)·4H2O的水热合成和晶体结构

张丽荣, 李光华, 施展, 冯守华   

  1. 吉林大学无机合成与制备化学国家重点实验室, 长春 130023
  • 收稿日期:2000-10-13 出版日期:2001-12-24 发布日期:2001-12-24
  • 通讯作者: 冯守华(1956年出生),男,博士,教授,博士生导师,从事无机合成化学研究.
  • 基金资助:

    国家自然科学基金(批准号:20071013)资助

Hydrothermal Synthesis and Crystal Structure of Na2[(VO)12O6B18O39(OH)3]·(11H3O)·4H2O

ZHANG LiRong, LI GuangHua, SHI Zhan, FENG ShouHua   

  1. State Key Laboratory of Inorganic Synthesis and Preparative Chemistry, Jilin University, Changchun 130023, China
  • Received:2000-10-13 Online:2001-12-24 Published:2001-12-24

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摘要： 以V2O5,Na2B4O7·10H2O,NaH2PO4·2H2O,乙二胺和H2O为原料,按物质的量比0.5:1:1:2.24:111在180℃条件下晶化,得到棕色晶体Na2[(VO)12O6B18O39(OH)3]·(11H3O)·4H2O.单晶结构分析结果表明该化合物属单斜晶系,P21/n空间群,晶胞参数a=1.38970(8)nm,b=1.66159(9)nm,c=1.42748(8)nm,β=95.6910(10)°.Z=4,R=0.0549.该化合物的结构主要由阴离子簇[(VO)12O6B18O39(OH)3]13-构成.该阴离子簇由B18O39(OH)3十八元环夹在两个以共边方式交替相连形成的V6O15簇中间,通过共用氧原子形成三明治式结构新颖的硼-钒-氧阴离子簇,结构中Na+以离子键方式将阴离子簇相互连接,形成二维层状结构.层与层之间通过分子间氢键相互作用.价态计算结果表明,结构中n(VIV):n(VV)=5:1.

关键词: 水热合成, 晶体结构, 金属-氧簇, 硼化合物

Abstract: Ahydrothermal reaction of V2O5, Na2B4O7·10H2O, NaH2PO4·2H2O, en, H2Oin a molar ratio of 0.5:1:1:2.24:111 gives a brown crystal Na2[(VO)12O6B18O39(OH)3] ·(11H3O) · 4H2O. It crystallizes in a monoclinic system with space group P2 1/n and unit cell parameters a=1.38970(8) nm, b=1.66159(9) nm, c=1.42748(8) nm, β=95.6910(10)°, Z=4, R=0.0549. The structure consists of a [(VO)12O6B18O39(OH)3]13- cluster which is connected by Na+ through Na——Oionic bond to form a 2dimensional layered structure. The [(VO)12O6B18O39(OH)3]13- cluster consists of a puckered B18O39(OH)3 ring sandwiched between two triangles of six edgesharing vanadium atoms. The oxidation states of vanadium in the compound are V(Ⅳ) and V(Ⅴ) in a molar ratio of 5:1. Other characterizations are also described.

Key words: Hydrothermal synthesis, Crystal structure, Polyoxovanadium, Borate compound

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