By crystallization from strongly acidic aqueous solutions, nickel and zinc tetrahydrogen-decaoxodiperiodate hexahydrate, NiH4I2O10·6H2O and ZnH4I2O10·6H2O, have been obtained and found to be isotypic to CuH4I2O10·6H2O (P21/c, no. 14) with the lattice parameters a = 1070.3, b = 544.0, c = 1187.2 pm, β = 112.6° for the Ni compound and a = 1073.3, b = 545.3, c = 1189.5 pm and β = 112.5° for the Zn compound. The crystal structure of MgH4I2O10·6H2O has been reinvestigated and contrary to former

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... ts found to be isotypic to the Cu compound as well. IR and Raman spectra are given and analyzed with respect to the internal vibrations of the H4I2O102− ion and the hydrogen bonding system. According to high-temperature Raman spectra and DTA and TG measurements, the compounds decompose in the temperature range up to 300 °C via unknown salts with the anions H4IO62− and IO4− to the corresponding iodates. In the case of the Ni compound the exothermic decomposition to the iodate occurs in two steps.