Hydrothermal synthesis and structural characterization of two new three-dimensional oxyfluorinated titanium phosphates Ti4(HPO4)2(PO4)4F2 • C4N2H12 • H2O and Ti4(HPO4)2(PO4)4F2 • C2N2H10 •H2O

被引:21
作者
Fu, YL [1 ]
Liu, YL [1 ]
Shi, Z [1 ]
Zou, YC [1 ]
Pang, WQ [1 ]
机构
[1] Jilin Univ, State Key Lab Inorgan Synth & Preparat Chem, Changchun 130023, Peoples R China
基金
中国国家自然科学基金;
关键词
hydrothermal synthesis; crystal structure; titanium phosphates;
D O I
10.1006/jssc.2001.9360
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
Two new organo-templated three-dimensional fluorinated titanium phosphates Ti-4(HPO4)(2)(PO4)(4)F-2 . C4NH12 . H2O 1 and Ti-4(HPO4)(2)(PO4)(4)F-2 . C2N2H10 . H2O 2 have been prepared hydrothermally in the presence of piperazine (C4N2H10) and ethylenediamine (C2N2H8) as templates, respectively. The assynthesized products are characterized by powder X-ray diffraction, IR spectroscopy, and thermogravimetric and differential thermal analyses (TG-DTA). The structures have been solved by single-crystal X-ray diffraction analysis. The compound I crystallized in the monoclinic space group C2/c (no. 15), with M = 907.61 g/mol, a = 16.6549(17) Angstrom, b = 6.3378(6) A, c = 22.208(2) Angstrom, beta = 94.862(4)degrees, V = 2335.7(4) Angstrom (3), Z = 4, R-1[I > 2 sigma (I)] = 0.0393, wR(2)[I > 2 sigma (I)] = 0.1071 and the compound 2 in the monoclinic space group C2/m (no. 12), with M = 880.56 g/mol, a = 16.6324(14) Angstrom, b = 6.3219(6) Angstrom, c = 11.0725(10) Angstrom, beta = 94.362(2)degrees, V = 1160.88(18) Angstrom (3), Z = 2, R-1[I > 2a(I)] = 0.0461, wR(2)[I > 2 sigma (I)] = 0.1403. They have similar three-dimensional frameworks built up from TiO6, TiO5F octahedral, PO4, and PO3(OH) tetrahedral units. There exist two types of 8-membered ring channels along the b axis in which the diprontonated piperazine or ethylenediamine molecules are entrapped and along the c axis in which water molecules are entrapped. (C) 2001 Academic Press.
引用
收藏
页码:96 / 102
页数:7
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