THIOUREA-HALIDE LATTICES .1. CRYSTAL-STRUCTURES OF (NORMAL-C4H9)4N+F-.3(NH2)2CS, (NORMAL-C4H9)3(CH3)N+X-.2(NH2)2CS (X=CL,BR), AND (NORMAL-C3H7)4N+I-.(NH2)2CS

The title complexes (1, X = F;2, X = C 1; 3, X = Br and isomorphous with 2; 4, X = I) have been prepared and characterized by X-ray crystallography. Crystal data, Mo Kα radiation:1, space group Cc, Z =4, a = 12.017(3), b = 14.263(5), c = 17.210(7) Å, β = 103.06(2)°, and RF=0.053 for 2044 observed data;2, space group Cc, Z = 4, a = 12.817(3), b = 11.072(2), c = 16.781(5) Å, β =90.74(2)°, RF = 0.044 for 2249 data;3, a = 12.873(4), b = 11. 119(2), c = 16.957(2) Å, β = 89.11(2)°, RF = 0.049 for 2059 data;4, space group P21/n, Z = 4, a = 8.858(2), b = 14.358(3), c = 15.379(3) Å, β = 93.88(1)°, RF = 0.068 for 3119 data. In all four structures each thiourea molecule interacts with adjacent thiourea molecules via N-H ... S hydrogen bonds to give a ribbon-like arrangement, and also forms a pair of 'chelating' N-H ... X hydrogen bonds with a halide ion, resulting in an anionic framework (in 1-3) or composite ribbon (in 4) as a component in the crystal packing. The measured ranges of N... X distances are: 2.819(5)-2.994(7) Å for 1, 3.252(3)-3.291(3)Å for 2, 3.353(6)-3.459(6)Å for 3, and 3.564(5)-3.680(5) Å for 4. © 1990 Kluwer Academic Publishers.