Cation-exchanged polymer resin beads have been used as a heterogeneous controlled-release source of metal cations in phase pure and/or high yielding solvothermal syntheses of novel transition metal–organic frameworks. The introduction of the resin beads has a dramatic effect on the outcome of solvothermal reactions. We report the syntheses of a series of transition metal-containing MOFs via the resin-assisted solvothermal methods, four novel MOFs are reported that could not be synthesised by traditional methods. These MOFs have been characterized using elemental analysis, powder XRD, single crystal XRD, FESEM, EPR, B.E.T. surface analysis, and solid state magnetic measurements.
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