A chiral material, d-Co(en) 3 [H 3 Ga 2 P 4 O 16 ] (en ) 1,2-diaminoethane), with a three-dimensionally connected framework has been prepared hydrothermally, using optically pure d-Co-(en) 3 3+ as a structure directing agent, and the structure characterized by X-ray diffraction. Aluminum-containing analogues of this material have also been synthesized. The material can be thought of as a diamondlike network, consisting of tetrahedrally coordinated gallium sites linked by doubly bridging phosphates, with the metal complex sitting in the interstices.Ga 1.25 Al 0.75 P 4 O 16 ], M r ) 729.51, monoclinic, I2, a ) 9.567(1)Å, b ) 12.6923-(5)Å, c ) 9.9241(5)Å, β ) 97.601( 8) o , Z ) 2, F calc ) 2.028 g cm -3 , F obs ) 2.08 g cm -3 , Cu KR, R F ) 0.026.

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