Single crystals of an organically templated holmium hydrogen phosphate sulfate, [enH2]0.5[Ho(HPO4)(SO4)(H2O)] (en; ethyl-enediamine) were prepared by hydrothermal reaction and its crystal structure was determined by single crystal X-ray diffrac-tion data. This compound crystallized in the monoclinic system, space group P21/a (No. 14) and the unit cell parameters are a = 12.938(5), b = 6.834(3), c = 9.100(2) Å, and β = 88.12(2)°. The crystal structure is similar to that of [enH2]0.5[Ce(HPO4)(SO4)(H2O)] which had a layered structure built up by Ce centered polyhedra and HPO4 and SO4 tetrahedra, and the diprotonated ethylene-diamine cations were located in the interlayer. For other rare earth elements two types of compounds were obtained under hydrothermal conditions. The compounds of R = La, Pr, Nd, Sm and Eu are isostructural with [enH2]0.5[Ce(HPO4)(SO4)(H2O)] and those of Gd, Tb, Dy, Er and Yb with [enH2]0.5[Ho(HPO4)(SO4)(H2O)]. The unit cell volumes of these compounds decrease by lanthanide contraction. The compounds of R except La, Sm and Eu exhibited the Curie-Weiss paramagnetic behavior.
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