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Synthesis, crystal structures and IR spectra of the first representatives of calcium hydrogen selenite halides are reported. Colourless prismatic crystals of calcium hydrogen selenite chloride Ca(HSeO 3 )Cl and corresponding hydrated analogue Ca(HSeO 3 )Cl(H 2 O) were produced upon evaporation of aqueous solutions. Ca(HSeO 3 )Cl is monoclinic,  P 2 1 / c ,  a  = 7.0031(11) Å,  b  = 7.7336(12) Å,  c  = 8.5024(13) Å, β = 109.889(3)°,  V  = 433.02(12) Å 3 ,  R  1  = 0.039. Ca(HSeO 3 )Cl(H 2 O) is orthorhombic,  Pbca ,  a  = 6.222(4) Å,  b  = 10.413(7) Å,  c  = 16.875(10) Å,  V  = 1093.3 (12) Å 3 ,  R  1  = 0.041. Ca(HSeO 3 )Cl and Ca(HSeO 3 )Cl(H 2 O) represent new structure types. In both structures, Ca 2+  cations adopt mixed-ligand environments formed by oxygen atoms of hydrogen selenite anions (and water molecules for Ca(HSeO 3 )Cl(H 2 O)) and chloride ions. Both structures are layered. The crystal structure of Ca(HSeO 3 )Cl(H 2 O) demonstrates a rare phenomenon of hydrogen-bonded assembly of water and chloride in the interlayer space.

Layered calcium hydrogen selenite chlorides Ca(HSeO 3 )Cl and Ca(HSeO 3 )Cl(H 2 O), the first halides obtained in СaCl 2 –H 2 SeO 3 –H 2 O system