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By Vinay D.S., Kwon B.S.

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Less perfect crystals may be grown at a slightly higher infusion speed. All other crystdgrowth techniques that have been tried yielded only small crystals less than 2 *Fifty-milliliter polypropylene syringes were obtained from Becton, Dickinson & Co. , Dun Laoghaire, Dublin, Ireland. Single-Crystal Growth by a Double-Infusion Technique 17 mm in edge length. Characteristically, the yellow A & H J I O ~crystals always adopt the shape of rhombohedra. The ammonium salt (NH,), H3106is prepared similarly.

A n efficienr fume hood should be used for reuctions involving chlorine or bromine. The chlorination apparatus, Fig. 1, consists of a 24-mm od quartz tube with a ground joint socket joined by way of a quartz-Pyrex seal to a collection flask. For metal quantities of about 20 g a 250-mL flask should be used and for 5-g quantities a 100-mL flask is convenient. Inlet for H,, N,, and CI, 824 quartz socket 24 mm od quartz tube t 2ol +=yB Electric furnace Outlet to bubblers and fume Thermocouple Quartz wool Trap cooled in Fig.

A. Levy,J. ,1912, 1081. H . Terrey, J. ,1928, 202. J. S. Miller, Science, 194, 189 (1976). T. R. Koch, 3. A. Abys, and J. Williams, Inorg. , 19,9 (1979). Galbraith Laboratories, Knoxville, TN. Midwest Microlabs, Indianapolis, IN. This laboratory does not perform Rb or Pt analyses. lodine-tluosulfate titrations were performed by Ms. E. Streets of Argonne National Laboratory. It is difficult to assess the true oxidation state of the platinum atom because the structure likely contains (small amounts of) additional species such as H30+ or HSO;.

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4-1BB by Vinay D.S., Kwon B.S.

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