Synthesis and Characterization of a Chiral 3D-Framework Material: d-Co(en)₃[H₃Ga₂P₄O₁₆]

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. Co(C 2 N 2 H 8 ) 3 [H 3 Ga 2 P 4 O 16 ], M r = 761.56, monoclinic, I 2, a = 9.580(2)Å, b = 12.6789(5)Å, c = 9.9631(6)Å, β = 97.85(2)°, Z = 2, ρ calc = 2.109 g cm - 3, ρ obs = 2.11 g cm - 3, Cu Kα, R F = 0.032. Co(C 2 N 2 H 8 ) 3 [H 3 Ga 1.25 Al 0.75 P 4 O 16 ], M r = 729.51, monoclinic, I 2, a = 9.567(1)Å, b = 12.6923(5)Å, c = 9.9241(5)Å, β = 97.601(8) o, Z = 2, ρ calc = 2.028 g cm - 3, ρ obs = 2.08 g cm - 3, Cu Kα, R F = 0.026.