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Figure 1
(a) X-ray diffraction images of the high-pressure cryocooled crystallization solution at different temperatures. The peak positions of amorphous ices at 80 K and 150 K are clearly distinguishable, indicating the density difference between HDA ice and LDA ice. The diffraction peaks of cubic ice and hexagonal ice are shown at 180 and 230 K, respectively. Note that the peak position at 150 K, which is at around 3.65 Å, matches the positions of the main sharp peaks at 180 and 230 K. The diffraction at 230 K includes diffraction from a small quantity of type I hydrate, presumably formed from the tartrate. (b) X-ray diffraction images of the high-pressure cryocooled thaumatin crystal at different temperatures. Crystal diffraction spots are seen superimposed on diffuse rings. These diffuse rings are due to oil (innermost ring) around the crystal and ice (second ring) inside the crystal. The broad ice peak is located at the Q value of 2.03 Å−1 (d = 3.10 Å) at 80 K, confirming that HDA ice formed inside the crystal by high-pressure cryocooling. The HDA ice transformed into LDA ice, cubic ice and hexagonal ice upon crystal warming. Note that the innermost diffraction ring from the oil changes little as the temperature is raised.

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APPLIED
CRYSTALLOGRAPHY
ISSN: 1600-5767
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