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Hydrothermal Synthesis and Structural Characterization of Two New Three-Dimensional Oxyfluorinated Titanium PhosphatesTi4(HPO4)2(PO4)4F2·C4N2H12·H2O and Ti4(HPO4)2(PO4)4F2·C2N2H10·H2O

✍ Scribed by Yunlong Fu; Yunling Liu; Zhan Shi; Yongcun Zou; Wenqin Pang

Publisher
Elsevier Science
Year
2001
Tongue
English
Weight
416 KB
Volume
162
Category
Article
ISSN
0022-4596

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✦ Synopsis

Two new organo-templated three-dimensional 6uorinated titanium phosphates Ti 4 (HPO 4 ) 2 (PO 4 ) 4 F 2 ' C 4 N 2 H 12 ' H 2 O 1 and Ti 4 (HPO 4 ) 2 (PO 4 ) 4 F 2 ' C 2 N 2 H 10 ' H 2 O 2 have been prepared hydrothermally in the presence of piperazine (C 4 N 2 H 10 ) and ethylenediamine (C 2 N 2 H 8 ) as templates, respectively. The assynthesized products are characterized by powder X-ray di4raction, IR spectroscopy, and thermogravimetric and di4erential thermal analyses (TG-DTA). The structures have been solved by single-crystal X-ray di4raction analysis. The compound 1 crystallized in the monoclinic space group C2/c (no. 15), with M ‫؍‬ 907.61 g/mol, a ‫؍‬ 16.6549(17) A > , b ‫؍‬ 6.3378(6) A > , c ‫؍‬ 22.208(2) A > , ‫؍‬ 94.862(4)3, V ‫؍‬ 2335.7(4) A > 3 , Z ‫؍‬ 4, R 1 [I'2 (I)] ‫؍‬ 0.0393, wR 2 [I'2 (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) A > , b ‫؍‬ 6.3219(6) A > , c ‫؍‬ 11.0725(10) A > , ‫؍‬ 94.362(2)3, V ‫؍‬ 1160.88(18) A > 3 , Z ‫؍‬ 2, R 1 [I'2 (I )] ‫؍‬ 0.0461, wR 2 [I'2 (I)] ‫؍‬ 0.1403. They have similar three-dimensional frameworks built up from TiO 6 , TiO 5 F octahedral, PO 4 , and PO 3 (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.

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