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A new metastable phase, featuring a lithium-stabilized mixed-valence cobalt(II,III) hydroxide phosphate framework, Co 11.0(1) Li 1.0(2) [(OH) 5 O][(PO 3 OH)(PO 4 ) 5 ], corresponding to the simplified composition Co 1.84(2) Li 0.16(3) (OH)PO 4 , is prepared by hydrothermal synthesis. Because the pH-dependent formation of other phases such as Co 3 (OH) 2 (PO 3 OH) 2 and olivine-type LiCoPO 4 competes in the process, a pH value of 5.0 is crucial for obtaining a single-phase material. The crystals with dimensions of 15 μm × 30 μm exhibit a unique elongated triangular pyramid morphology with a lamellar fine structure. Powder X-ray diffraction experiments reveal that the phase is isostructural with the natural phosphate minerals holtedahlite and satterlyite, and crystallizes in the trigonal space group P31m (a = 11.2533(4) Å, c = 4.9940(2) Å, V = 547.70(3) Å 3 , Z = 1). The three-dimensional network structure is characterized by partially Li-substituted, octahedral [M 2 O 8 (OH)] (M = Co, Li) dimer units which form double chains that run along the [001] direction and are connected by [PO 4 ] and [PO 3 (OH)] tetrahedra. Because no Li-free P31m-type Co 2 (OH)PO 4 phase could be prepared, it can be assumed that the Li ions are crucial for the stabilization of the framework. Co L-edge X-ray absorption spectroscopy demonstrates that the cobalt ions adopt the oxidation states +2 and +3 and hence provides further evidence for the incorporation of Li in the charge-balanced framework. The presence of three independent hydroxyl groups is further confirmed by infrared spectroscopy. Magnetization measurements imply a paramagnetic to antiferromagnetic transition at around T = 25 K as well as a second transition at around 9-12 K with a ferromagnetic component below this temperature. The metastable character of the phase is demonstrated by thermogravimetric analysis and differential scanning calorimetry, which above 558 °C reveal a two-step decomposition to CoO, Co 3 (PO 4 ) 2 , and olivine-type LiCoPO 4 with release of water and oxygen.

inorganic chemistry

Co11Li[(OH)5O][(PO3OH)(PO4)5], a Lithium-Stabilized, Mixed-Valent Cobalt(II,III) Hydroxide Phosphate Framework