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The chemical preparation of (NH4)2[RhCl5(H2O)] is described; lattice parameters and an indexed X-ray powder pattern are given. Diammonium aquapentachlororhodate is orthorhombic with a = 13.738 (1); b = 9.762 (1); c = 7.0419 (4) Å. The space group is Pnma.
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