POTASSIUM AMIDO TRIOXO GERMANATES(IV) - H YDROGEN BRIDGE BONDS IN K3GEO3NH2 AND K3GEO3NH2-CENTER-DOT-KNH2

Colorless crystals of K3GeO3NH2 and of K3GeO3NH2. KNH2 were obtained b y the reaction of KNH2 with GeO2 in supercritical ammonia at 450 degre es C and p(NH3) = 6 kbar in high-pressure autoclaves within 15 resp. 5 days. The crystal structures of both compounds were solved by X-ray s ingle crystal methods. K3GeO3NH2: P $($) over bar$$ 1, a = 6.390(1) An gstrom, b = 6.684(1) Angstrom, c = 7.206(1) Angstrom, alpha = 96.47(1) degrees, beta = 101.66(1)degrees, gamma = 91.66(1)degrees, Z = 2, R/R( w) = 0.020/0.022, N(I) greater than or equal to 2 sigma(I) = 3023, N(V ar.) = 82 K3GeO3NH2.KNH2: P2(1)/c, a = 10.982(6) Angstrom, b = 6.429(1 ) Angstrom, c = 12.256(8) Angstrom, beta = 106.12(1)degrees, Z = 4, R/ R(w) = 0.022/0.029, N(F) greater than or equal to 3 sigma(F) = 1745, N (Var.) = 107 In K3GeO3NH2 tetrahedral ions GeO3NH23- are connected to chains by N-H...O bridge bonds with 2.18 Angstrom less than or equal t o d(H...O) less than or equal to 2.40 Angstrom for d(N-H) = 1.0 Angstr om and by potassium ions while in K3GeO3NH2.KNH2 bridge bonds between NH2 groups of GeO3NH23- and NH2- ions as accepters occur with 2.41 Ang strom less than or equal to d((N-)H...NH2-) less than or equal to 2.61 Angstrom for d(N-H) = 1.0 Angstrom.