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Visual observations through a microscope and in situ Raman scattering measurements of a synthesized nitrogen hydrate have been performed at pressures up to 6 GPa and 296 K. High-pressure transformations have been found at 0.85 and 1.45 GPa. The cubic structure II (sII) nitrogen hydrate initially transforms to the hexagonal structure (sH) at 0.85 GPa and finally forms the orthorhombic dihydrate (sO) above 1.45 GPa. The sO phase of nitrogen hydrate exists up to at least 6 GPa. A variety of Raman spectra composed of three peaks have been sometimes observed in sII phase below 0.50 GPa, which implies that the guest nitrogen molecules doubly occupy the large hexakaidecahedron cages. Two Raman bands of the guest nitrogen vibrations with nearly equal intensities appearing in sH phase suggest that five nitrogen molecules are filling in extra large icosahedron cages.

Direct observations through a microscope and in-situ Raman scattering measurements of synthesized single-crystalline Kr hydrate have been performed at pressures up to 5.2 GPa and 296 K. We have observed that the initial cubic structure II (sII) of Kr hydrate successively transforms to a cubic structure I (sI), a hexagonal structure, and an orthorhombic structure (sO) called "filled ice" at 0.45, 0.75, and 1.8 GPa, respectively. The sO phase exists at least up to 5.2 GPa. In addition to these transformations, we have also found the new phase behavior at 1.0 GPa, which is most likely caused by the change of cage occupancy of host water cages by guest Kr atoms without structural change. Raman scattering measurements for observed phases have shown that the lattice vibrational peak at around 130 cm(-1) disappears in the pressure region of sI, which enables us to distinguish the sI phase from sII and sH phases.

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