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Investigation of the GeO₂-1,6-Diaminohexane-Water-Pyridine-HF Phase Diagram Leading to the Discovery of Two Novel Layered Germanates with Extra-Large Rings

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Bing Guo†‡^#, Andrew K. Inge‡^#, Charlotte Bonneau‡, Junliang Sun‡, Kirsten E. Christensen§, Zhong-Yong Yuan†, and Xiaodong Zou*‡

^† Institute of New Catalytic Materials Science, College of Chemistry, Nankai University, Tianjin 300071, People’s Republic of China

^‡ Inorganic and Structural Chemistry and Berzelii Center EXSELENT on Porous Materials, Department of Materials and Environmental Chemistry, Stockholm University, SE-106 91 Stockholm, Sweden

^§ Diamond Light Source Ltd., Diamond House, Chilton, Didcot, Oxfordshire, OX11 0DE, United Kingdom

Inorg. Chem., 2011, 50 (1), pp 201–207

DOI: 10.1021/ic1017505

Publication Date (Web): November 30, 2010

*To whom correspondence should be addressed. E-mail: xzou@mmk.su.se .,

Current address: ERATO Kitagawa Integrated Pores Project, Science and Technology Agency (JST), Kyoto Research Park Bldg #3, Shimogyo-ku, Kyoto, 600-8815, Japan, and Institute for Integrated Cell-Material Science (iCeMS), Kyoto University, Yoshida, Sakyo-ku, Kyoto 606-8501, Japan

Section:

Inorganic Chemicals and Reactions

Abstract

The systematic exploration of the phase diagram of the GeO₂-1,6-diaminohexane-water-pyridine-HF system has allowed the identification of specific roles of the HF, H₂O contents, and HF/H₂O ratio in the formation of Ge₇X₁₉ (Ge₇), Ge₉X₂₅₋₂₆ (Ge₉), and Ge₁₀X₂₈ (Ge₁₀) clusters (X = O, OH, F). This work has led to the discovery of two novel structures with extra-large 18-membered rings accommodating 1,6-diaminohexane (DAH): SU-63, |1.5H₂DAH|[Ge₇O₁₄X₃]·2H₂O, a layered germanate constructed from Ge₇ clusters with the Kagomé topology, and SU-64, |11H₂DAH|[Ge₉O₁₈X₄][Ge₇O₁₄X₃]₆·16H₂O, a germanate built of two-dimensional slabs containing both Ge₇ and Ge₉ clusters (X = OH or F). We also put SU-64 in context with previously reported cluster germanate compounds with related topologies by means of a simple crystal deconstruction study.