Synthesis and Characterization of Zirconogermanates
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- 作者：Jacques Plé ; vert ; Rebeca Sanchez-Smith ; Travis M. Gentz ; Hailian Li ; Thomas L. Groy ; Omar M. Yaghi ; and Michael O'Keeffe
- 刊名：Inorganic Chemistry
- 出版年：2003
- 出版时间：September 22, 2003
- 年：2003
- 卷：42
- 期：19
- 页码：5954 - 5959
- 全文大小：279K
- 年卷期：v.42,no.19(September 22, 2003)
- ISSN：1520-510X
文摘
Six new zirconogermanates have been prepared under hydrothermal conditions using amines as bases. There arefour new structure types (ASU-n) with a common motif of ZrGe5. ASU-23 is a layered structure: ZrGe3O8(OH)F·[C10H26N4]·H2O, space group P21/n, a = 6.7957(8) Å, b = 12.700(1) Å, c = 24.293(3) Å, 
= 97.936(2)
, V =2076.4(4) Å3. ASU-24 is a pillared layered structure: Zr3Ge6O18(OH2,F)4F2·[C6H18N2]·[C6H17N2]2·2H2O, space groupP21/n, a = 7.4249(3) Å, b = 25.198(1) Å, c = 11.3483(5) Å, = 90.995(1), V = 2122.9(2) Å3. This materialhas the lowest framework density (FD) of any oxide material that we are aware of (FD = 8.48 metal atoms/nm3).Two other materials form three-dimensional open-frameworks, ASU-25: ZrGe3O9·[C3H12N2], space group P1121/a,a = 13.1994(4) Å, b = 7.6828(2) Å, c = 11.2373(3) Å, 
= 91.233(3), V = 1139.29(5) Å3. The other is ASU-26:ZrGe3O9·[C2H10N2], space group Pn, a = 13.7611(3) Å, b = 7.7294(2) Å, c = 11.2331(3) Å, = 104.793(1), V= 1155.21(4) Å3. ASU-25 is related to the mineral umbite K2ZrSi3O9·H2O. The germanium equivalent has beenprepared through the inorganic route: K2ZrGe3O9·H2O, space group P212121, a = 13.6432(6) Å, b = 7.4256(3) Å,c = 10.3973(4) Å, V = 1053.33(8) Å3. The structural relationships between ASU-25 and its inorganic counterpartare described. The thermal decomposition of the germanium umbite generated the cyclic trigermanate K2ZrGe3O9,analogue of the mineral wadeite, crystallizing in the orthorhombic system, a = 7.076 Å, b = 12.123 Å, c = 10.451Å, V = 904.5 Å3.
= 97.936(2), V =2076.4(4) Å3. ASU-24 is a pillared layered structure: Zr3Ge6O18(OH2,F)4F2·[C6H18N2]·[C6H17N2]2·2H2O, space groupP21/n, a = 7.4249(3) Å, b = 25.198(1) Å, c = 11.3483(5) Å, = 90.995(1), V = 2122.9(2) Å3. This materialhas the lowest framework density (FD) of any oxide material that we are aware of (FD = 8.48 metal atoms/nm3).Two other materials form three-dimensional open-frameworks, ASU-25: ZrGe3O9·[C3H12N2], space group P1121/a,a = 13.1994(4) Å, b = 7.6828(2) Å, c = 11.2373(3) Å, = 91.233(3), V = 1139.29(5) Å3. The other is ASU-26:ZrGe3O9·[C2H10N2], space group Pn, a = 13.7611(3) Å, b = 7.7294(2) Å, c = 11.2331(3) Å, = 104.793(1), V= 1155.21(4) Å3. ASU-25 is related to the mineral umbite K2ZrSi3O9·H2O. The germanium equivalent has beenprepared through the inorganic route: K2ZrGe3O9·H2O, space group P212121, a = 13.6432(6) Å, b = 7.4256(3) Å,c = 10.3973(4) Å, V = 1053.33(8) Å3. The structural relationships between ASU-25 and its inorganic counterpartare described. The thermal decomposition of the germanium umbite generated the cyclic trigermanate K2ZrGe3O9,analogue of the mineral wadeite, crystallizing in the orthorhombic system, a = 7.076 Å, b = 12.123 Å, c = 10.451Å, V = 904.5 Å3.