Single crystals of layer compounds with compositions ZrSxSe2–x, where x varies within the range 0 to 2, have been grown by the iodine vapour transport technique to widths of at least 5 mm. The mixed crystals are found to be isomorphous over the whole range of composition. Growth conditions and X‐ray crystal lattice parameters have been determined for the series, and are compared with previously published values.
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