Syntheses and Crystal Structures of the First Zinc Complex with 1,3,5-Triaza-7-phosphaadamantane (PTA), [ZnCl2(PTA)(2)], and of the Hybrid Organic-Inorganic Salts of N-Methyl-1,3,5-triaza-7-phosphaadamantane with Tetrahalozinc [PTA-Me](2)[ZnI2X2] (X

摘要

The Zn-II compounds [ZnCl2(PTA)(2)] (1) (PTA = 1,3,5-triaza-7-phosphaadamantane) and [PTA-Me](2)[ZnI2X2] [X = Cl (2a), X = I (2b); PTA-Me = N-methyl-1,3,5-triaza-7-phosphaadamantane] have been prepared by treating ZnCl2 with PTA and [PTA-Me]I, respectively, in methanol at room temperature, They are soluble in polar solvents such as water and methanol, stable in air, and have been characterized by IR, H-1 NMR, P-31(H-1) NMR, and C-13(H-1) NMR spectroscopy, ESI-MS, elemental and single-crystal X-ray diffraction structural analyses (for 1 and 2a). Compound 1 exhibits a nearly regular tetrahedral Zn coordination, with the PTA ligands displaying the uncommon N-coordination with a low P-31 NMR coordination shift. The molecular structure of 2a bears one discrete tetrahedral [ZnI2Cl2](2) anion and two cage-like [PTA-Me](+) cations, one of them being located in a void. Compound I represents the first example of a Zn complex bearing PTA or any derived ligand with a cage-like PTA core. ((C) Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2009)