METHYL-1,4-BISAZONIACYCLOHEX-1-YL)METHYL]GERMANATE HYDRATE - SYNTHESIS AND CRYSTAL-STRUCTURE OF A ZWITTERIONIC LAMBDA-GE-6-GERMANATE WITH AGEF5C FRAMEWORK

The zwitterionic (molecular) lambda(6) Ge-germanate methyl-1,4-bisazon iacyclohex-1-yl)methyl]germanate (5) was synthesized by reaction of 1- methyl-4-[(trimethoxy-germyl)methyl]piperazine (8) with HF (molar rati o 1:5) in a mixture of water and ethanol at 0 degrees C and isolated a s the hydrate 5 . H2O. The zwitterion 5 is characterized by the presen ce of a hexacoordinate (formally twofold negatively charged) germanium atom and two tetracoordinate (formally positively charged) nitrogen a toms. Compound 5 . H2O was structurally characterized by single-crysta l X-ray diffraction. Crystal data are as follows: C6H17F5GeN2O, tricli nic space group P (1) over bar (no. 2); a = 7.5228(11) Angstrom, b = 1 2.174(2) Angstrom, c = 12.3041(14) Angstrom, alpha = 73.74(2)degrees, beta = 82.44(2)degrees, gamma = 74.762(10)degrees, V = 1041.7(2) Angst rom, T = 173(2) K, Z = 4, R1 = 0.0227. There are one pair each of crys tallographically independent zwitterions 5 and water molecules in the asymmetric unit, the structures of the zwitterions being very similar. Their coordination polyhedra around the germanium atoms are slightly distorted octahedra.