Synthese und Kristallstruktur von LiHSO4

Synthesis and Crystal Structure of LiHSO₄ Single crystals of the new compound LiHSO₄ are synthezised from the system Lithiumsulfate/Sulfuric acid. The up to day not determined structure of the title compound is monoclinic, space group P2₁/c with the lattice constants a = 5.234(2), b = 7.322(1) and c = 8.363(1) Å, b? = 90.02(2)°. The volume of the unit cell has been determined to V = 320.5 ų, the number of formula units to Z = 4 and the density to D_x = 2.156 g cm^?3. There are crystallographically identical SO₃(OH)- and LiO₄-tetrahedra in the structure. Every tetraheda is linked to four different tetrahedra of the other sort. Two neighboured LiO4 terahedra form a common edge. In that way layers are formed running parallel the yz-plane. These layers are connected over hydrogen bonds.     

Synthesis and structures of zirconium(IV) hydrogensulfato and carboxylato complexes with Kläui’s oxygen tripodal ligand

Interaction of [L_OEtZrF₃] ( = [Co(η⁵-C₅H₅){P(O)(OEt)₂}₃]⁻) (1) with 3 equivalents of bis(trimethylsilyl) sulfate afforded the Zr^IV hydrogensulfato complex [(L_OEt)₂Zr₂(SO₄)₂(HSO₄)₂] (2) that reacted with Et₃N to give [Et₃NH][L_OEtZr(H₂O)(SO₄)₂] (3). Treatment of complex 1 with 3 equivalents of trimethylsilyl acetate afforded [L_OEtZr(OCOCH₃)₃] (4), whereas that with 1 and 2 equivalents of trimethylsilyl trimethylsiloxyacetate yielded [L_OEtZrF(OCOCH₂O)]₂ (5) and [L_OEtZr(OCOCH₂OH)(OCOCH₂O)]₂ (6), respectively. The crystal structures of complexes 2 and 6 have been determined.     

Kaliumhydrogensulfat-Dihydrogensulfat,K(HSO4)(H2SO4) – Synthese und Kristallstruktur

Potassium Hydrogensulfate Dihydrogensulfate, K(HSO₄)(H₂SO₄) – Synthesis and Crystal Structure Single crystals with the composition KH₃(SO₄)₂ have been synthesized from the system Potassium sulfate/sulfuric acid. The hitherto crystallographically not investigated compound crystallizes in the monoclinic space group P2₁/c (14) with the unit cell parameters a = 7.654(3), b = 11.473(5) and c = 8.643(3) Å, β = 112.43(3)°, V = 701.6 ų, Z = 4 and D_x = 2.22 g · cm^?3. The structure contains two types of tetrahedra, SO₃(OH) and SO₂(OH)₂. These tetrahedra form tetramers via hydrogen bonds consisting of both, two SO₃(OH) and two SO₂(OH)₂ tetrahedra. The tetramers are linked to each other via hydrogen bonds. Potassium is coordinated by 9 oxygen atoms which belong to both kinds of tetrahedra. These potassium oxygen polyhedra are connected by common faces forming chains running parallel z.