In this review, we report isolation of unstable tri-sulfur, S
3, in a porous coordination network which is used as a crystalline molecular flask. The ozone-like structure of S
3 in a pore was determined by
ab initio X-ray powder diffraction analysis. The S
3 in the pore was interacted with iodine which faces to the pore of the network. The S
3 in the network was quite stable unlike unstable gaseous S
3 molecule because of the S-I interaction in the pore. Furthermore, the S
3 in the network could be transformed to S
6 by mechanical grinding or heating in the presence of NH
4Cl. We will introduce new chemistry of small sulfur based on crystal structure.
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