The novel 8-coordinate zirconium compound (NH4)(6)[Zr(PMo12O40)(PMo11O39)].26H(2)O (1) has been synthesized and characterized by single-crystal X-ray diffraction, elemental analysis, and vibrational and P-31 NMR spectroscopy. It is the first example of a metal complex containing both parent, [PMo12O40](3-), and monovacant lacunary, [PMo11O39](7-), anions. Furthermore, this is the first crystallographic determination of the [PMo11O39](7-) anion.
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