Hydrothermal synthesis and structures of two novel chain-like heteropolymolybdate formed by Keggin cluster units

Two novel heteropolymolybdate, [H2bpy]2 [Hbpy] [PCuMo11O39]·H2O 1 and [H2bpy]2 [Hbpy] [PZnMo11O39]·2.75H2O 2, have been prepared under mild hydrothermal conditions and structurally characterized by single-crystal X-ray diffraction. The two compounds are isostructural and crystallize in the monoclinic space group P2(1)/n (No. 14) with a=13.440(3) A, b=26.660(5) A, c=15.240(3) A, β=99.55(3) deg., and Z=4 for the compound 1, and a=13.610(3) A, b=26.781(5) A, c=15.205(3) A, β=100.40(3) deg., and Z=4 for the compound 2. Compound 1 and 2 exhibit a zigzag chain structure in which Keggin anions are connected through a common oxygen atom. They are the first characterized compounds containing 1D chains of transition-metal substituted Keggin heteropolymolybdate. Other characterizations by elemental analysis, IR, EPR, TG, and XRPD are also described