SU-77: An Open-Framework Germanate Containing 12 × 10 × 10-Ring Channels Solved by Combining Rotation Electron Diffraction and Powder X-ray Diffraction
2014 (English)In: Crystal Growth & Design, ISSN 1528-7483, E-ISSN 1528-7505, Vol. 14, no 10, 5072-5078 p.Article in journal (Refereed) Published
A novel open-framework germanate, denoted as SU-77, was prepared by hydrothermal synthesis using ethylenediamine as the structure directing agent. The as-synthesized SU-77 is monoclinic with space group P21/a and a = 13.52427(5) Å, b = 12.64862(5) Å, c = 9.60578(3) Å, β = 92.8599(4)°. The structure of SU-77 is built from a novel Ge6O17(C2H8N2)F (Ge6) cluster building unit. The Ge6 clusters are connected to form chains along the c-axis. These chains are further connected in the  and [1–10] directions to form a three-dimensional framework with 12 × 10 × 10-ring channels. The as-synthesized monoclinic SU-77 became orthorhombic while being observed in a transmission electron microscope (TEM) or when heated to 200 °C in air. The orthorhombic structure of SU-77 was solved from micrometer-sized crystals by rotation electron diffraction (RED). The monoclinic structure was built from the orthorhombic structure and subsequently refined against synchrotron powder X-ray diffraction data. SU-77 is the first example of an open-framework germanate with mixed coordination polyhedra solved by electron diffraction.
Place, publisher, year, edition, pages
2014. Vol. 14, no 10, 5072-5078 p.
IdentifiersURN: urn:nbn:se:su:diva-102757DOI: 10.1021/cg500681kISI: 000342609300027OAI: oai:DiVA.org:su-102757DiVA: diva2:713237