A 3D diamondoid network, [Ni(cyclam)]2[MTB]•9H2O•4DMF (1), has been assembled from [Ni(cyclam)](ClO4)2 and methanetetrabenzoic acid (H4MTB). X-ray crystal structure of 1 shows four fold interpenetration, which generates 1D channels of effective window size 13.8 Å x 13.8 Å. The auto-redox reaction between 1 and the solutions of Ag(I), Pt(IV), and Pd(II) affords Ag (2-3 nm), Pt, and Pd (1-2 nm) nanoparticles, respectively, at room temperature without an extra reducing agent.

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