Synthesis and characterization of ZP-4 (KZnPO4•0.8H2O), a new zincophosphate microporous material:: Structure solution from a 2.5 x 2.5 x 8 μm single crystal using a third generation synchrotron X-ray source

New techniques for handling crystals and collecting data allow structure solution from micrometer-sized crystals. Our experience using these techniques for determining the crystal structure of ZP-4 (KZnPO4. 0.8H(2)O), a new potassium zincophosphate microporous material, is described. Crystals were mounted using a micromanipulator attached to a Nikon optical microscope. Data on a 2.5 x 2.5 x 8 mu m single crystal were collected at Beamline Insertion Device 13 at the European Synchrotron Radiation Facility (ESRF). Lattice constants of the orthorhombic cell in space group Ccc2 are a = 13.812(3), b = 13.836(3), and c = 13.134(3) Angstrom, The structure refined to a final RI = 0.0680 using all 1876 reflections. The structure of ZP-4 is similar to the naturally occurring zeolite edingtonite (structure type EDI). It consists of a four-connected three-dimensional framework of alternating Zn and P tetrahedra producing a three-dimensional eight-ring channel system. The channels are nearly circular along the a- and b-axis directions, but are elliptical along c. The structure is disordered and was modeled by adding a second component to the single-crystal refinement.. Electron diffraction spots reveal streaking along the [100] direction and weak systematic absence Violations consistent with a disordered model involving EDI/THO intergrowths.