Structure of microporous QUI-MnGS-1 and in situ studies of its formation using time-resolved synchrotron x-ray powder diffraction

The structure of QUI-MnGS-1 has been determined from single-crystal X-ray diffraction on a similar to 0.03 x 0.03 x 0.02 mm sample using synchrotron radiation. This material [(C7H13N)Mn0.25Ge1.75S4 . H2O] crystallizes in space group I (4) over bar 2d with unit cell a = 11.581(1) and c = 18.741(3) A. The extended framework of this structure consists of corner-linked [Ge4S10](4-) clusters, the centers of which occupy nodes of a distorted diamond lattice. The B-rings defined by this lattice form channels that contain the water and organic components of this compound. In situ synchrotron X-ray diffraction studies of its synthesis indicate that an Mn-free precursor phase forms prior to transformation to QUI-MnGS-1. In situ calcination experiments demonstrate that this material is thermally stable to approximately 360 degrees C.