Synthesis and crystal structure of (dmaaH)(2)(dmaH)(2)[P12S12N12(NH)(2)]center dot 4 dmaa, dmaa = N,N-dimethylacetamide, dma = dimethylamine, an anhydrous example of the P12N14 cage

摘要

The title compound (dmaaH)(2)(dmaH)(2)[P12S12N12(NH)(2)] . 4 dmaa (1) was obtained by crystallization from a saturated solution of anhydrous P12S12N8(NH)(6) in N,N-dimethylacetamide (dmaa) as large single crystals. According to the X-ray structure determination (P2(1), a=1421.8(1), b=1556.5(2), c=1645.8(1) pm, beta =112.207(6)degrees, Z=2, 6388 observed reflections, R1=0.046, wR2=0.111) the anionic cage is built up from twelve P3N3 rings in boat conformation. N,N-dimethylammonium ions (dmaH(+)) are directly connected to the cage, and pairs of N,N-dimethylacetamidonium ions (dmaaH(+)) and N,N-dimethylacetamide molecules (dmaa) are interconnected by hydrogen-bonds. [References: 12]