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Oxysulfide chlorides, M 4 OS 4 Cl 2 , of the lanthanides (M = La - Nd) are obtained upon the oxidation of the metals with sulfur in the presence of MOCl (or M 2 O 3 ) and MCl 3  in appropriate molar ratios. Additional NaCl or an excess of MCl 3  serving as a flux provide even single crystalline material after reactions at 850 °C for seven days in sealed tantalum capsules. The crystal structure of M 4 OS 4 Cl 2  (hexagonal, P6 3 mc, no. 186, Z = 2; M = La: a = 933.19(3), c = 701.22(4) pm, c/a = 0.7514, R = RH = 0.020; M = Ce: a = 925.49(3), c = 694.13(3) pm, c/a = 0.7500; M = Pr: a = 919.72(4), c = 688.53(4) pm, c/a = 0.7486; M = Nd: a = 914.25(4), c = 683.12(4) pm, c/a = 0.7472, R = 0.022, R w  = 0.019) contains isolated O 2- -centered (M 3+ ) 4  tetrahedra which are surrounded by twelve S 2-  and six Cl - , capping vertices, edges, and faces of each tetrahedron and linking to other [OM 4 ] units. Basically, the structure is identical to that of Ba 4 OCl 6  if Ba 2+  is substituted by M 3+  and 2/3 of the CL -  anions are replaced by S 2-  to secure charge neutrality in M 4 OS 4 Cl 2 . Different models for the Cl - /S 2-  replacement are presented on the basis of comparisons of the Madelung part of the lattice energy (MAPLE) with the MAPLE sum of the binaries (M 2 O 3 , M 2 S 3 , and MCl 3 ).

Oxidsulfidchloride der Lanthanide vom Typ M 4 OS 4 Cl 2 (M = La-Nd) / M 4 OS 4 Cl 2 -Type Oxysulfide Chlorides of the Lanthanides (M = La -Nd)