New azametallatranes of the type Me(2)NM(RNCH(2)CH(2))(3)N, where R = i-Pr, M = Ti (16), Zr (17), and Hf (18); R= SiMe(3), M = Ti (19), Zr (20), and Hf (21); and R = SiMe(2)(t-Bu), M = Zr (23) and Hf (24), were prepared by metathesis reactions in moderate to high yield. During the course of the preparation of 19, Me(3)SiOTi(Me(3)-SiNCH2CH2)(3)N, 25, was formed in trace amounts. The latter compound was also synthesized by a metathesis reaction in a quantitive yield. Compounds 21 and 25 were structurally characterized and both were shown to exhibit a distorted trigonal bipyramidal metal center. Crystal data : 21, orthorhombic, space group P2(1),2(1),2(1), a = 11.837(2) Angstrom, b = 14.284(3) Angstrom, c = 15.750(4) Angstrom, V = 2662.9(9) Angstrom(3), Z = 4, R = 0.0352; 25 orthorhombic, space group Pna2(1), a = 21.772(2) Angstrom, b = 11.481(4) Angstrom, c = 11.566(1) Angstrom, V = 2891(1) Angstrom(3), Z = 4, R = 0.0341.