The tetraazido dinuclear Cu(II) complexes 1 and 2 of the polyaza-polyoxa macrocyclic ligands 4, [24]ane-N2Oe, and 5, [24]ane-N602, respectively, have been prepared, and their crystal structures have been determined. In both cases the two copper ions are contained inside the molecular cavity and are bound to the ONO and NNN chelating subunits situated at the two poles of the macrocycles 4 and 5, respectively. 1 crystallizes in the monoclinic system, space group P2\/n (a = Dihedral Angles N(l)-C(2)-C(3)-0(4) 59.6 C(2)-C(3)-0(4)-C(5) -165.6 C(3)-0(4)-C(5)-C(6) 178.9 0(4)-C(5)-C(6)-0(7) 65.3 C(5)-C(6)-0(7)-C(8) -167.1 C(6)-0(7)-C(8)-C(9) 158.9 O(7)-C(8)-C(9)-O(10) -69.4 C(8)-C(9)-O(10)-C(U) 179.9 C(9)-O(10)-C(ll)-C(12) -179.3 O(10)-C(ll)-C(12)-N(13) -59.8 C(ll)-C(12)-N(13)-C(14) -166.6 C(12)-N(13)-C(14)-C(15) 175.1 N(13)-C(14)-C(15)-0(16) 61.4 C(14)-C(15)-0(16)-C(17) -176.2 C(15)-0(16)-C(17)-C(18) 169.1 0(16)-C( 17)-C( 18)-0(19)64.8 C(17)-C(18)-O(19)-C(20) -174.0 C(18)-O(19)-C(20)-C(21) 170.2

of mass collision energy (421 eV) for these C60"+ collisions with argon.Capture of simple molecular gases undergoing high-energy collisions with fullerene ions could not be documented previously.6For example, collisions of C60*+ with D2 gave rise to no Dor D2-containing products.6 We were able, however, to detect both CeoD-1" and C60D2,+ (see Figure 4). The inability to detect lower mass product ions containing D or D2 in the experiments reported here and elsewhere6 may be due to rupture of the D-D bond with subsequent loss of the deuteriums.The results given here will be elaborated in a comprehensive report of the products and energetics of high-energy collisions of C60,+, C70*+, and other fullerene radical cations with a number of target gases.10 Other issues addressed include the kinetic energy of product ions that contain the target gas, the variation of the spectra of product ions as a function of both energy and number of collisions, and the end points in the capture processes. Comparison of the predicted kinetic energies of product ions with the observed values convinces us that the majority of the fullerene product ions produced from high-energy collisions with small target gases result from fragmentation of the intermediate fullerene endohedral complex.10 Acknowledgment. This work was supported by the National Science Foundation (Grant No. CHE 9017250). We acknowledge Robert Bateman of VG Analytical (Fisons Instruments), who designed the four-sector tandem mass spectrometer and provided advice on experimental aspects of this work.

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The tritopic hexa-aza-macrocycle (1) binds three Cull ions in solution and leads in particular to the assembly of a trinuclear bis-p3-hydroxo bridged complex whose crystal structure has been determined; it may be considered as a cryptate of a cationic cluster [ C U ~( O H ) ~] ~+ held inside the macrocyclic cavity of the ligand.