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 ∼0.03 × 0.03 × 0.02 mm sample using synchrotron radiation. This material [(C 7 H 13 N)Mn 0.25 Ge 1.75 S 4 ·H 2 O] crystallizes in space group I 4̄2 d with unit cell a = 11.581(1) and c = 18.741(3) Å. The extended framework of this structure consists of corner-linked [Ge 4 S 10 ] 4 - clusters, the centers of which occupy nodes of a distorted diamond lattice. The 6-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 °C.