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Synthesis: 2 mmol of M(CH3COO)2·H 2O (M, Co, Ni) and 3 mL of concentrated H3PO4 (14.6 mol/L) were charged into a 50-mL Teflon reactor and heated at 220°C for 4 days. After cooling to room temperature, the solid products were isolated by washing with alcohol or cold water. CoH2P2O7 is not stable in hot water. The single crystals are purple for Co and green for Ni. The yield of the product is about 80% according to the transition metal. Other transition-metal resources such as divalent metal chlorides or nitrates are also effectual. Analyses: crystals of CoH2P2O 7 of about 0.2 x 0.2 x 0.3 mm3 were used for single-crystal data collection at 293 K on a Rigaku AFC6S diffractometer with graphite-monochromated Mo Kα radiation (λ, 0.710 73 Å) by the ω-2θ scan method. The structure was solved by using direct methods and r
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