Transfer approximately 20 to 30 milligrams of the crystalline solid MOF product to a silicon PXRD sample holder and place it in the diffractometer. Close the door of the instrument and collect the PXRD pattern from 4 to 40 2-theta. Compare the data to the simulated powder pattern of silicon palladium low-valent MOF.
The PXRD pattern of the pristine tin-palladium low-valent MOF is shown in this figure. Here, blue is the experimental PXRD pattern, and black is the simulated PXRD pattern of the silicon palladium low-valent MOF obtained from its crystalled structure. The PXRD pattern obtained for an amorphous sample of the tin-palladium low-valent MOF is shown here.
The sample was prepared without any triphenylphosphine modulator, resulting in an amorphous or poorly crystalline material.