Two new dodecahydrate trisodium triphosphates Na3MP3O10·12H2O (M = Co (1), Ni (2)) were synthesized using a wet chemistry route and characterized by X-ray diffraction and FT-IR spectroscopy. They are isotypic, monoclinic (P21/ , ), with pseudoorthorhombic unit cell parameters (？,°): ( (4), (2), (4), (2), for (1) and (3), (2), (3), (16) for (2)). Values of / are 0.0267/0.0738 and 0.0284/0.0907, respectively, for (1) and (2). Both compounds were found to be systematically twinned by 180° rotation around . Their frameworks are made by slabs parallel to plane, resulting from the cohesion of two kinds of metallic chains. IR spectrum confirms the presence of characteristic bands from P3O10 phosphate group. 1. Introduction Phosphates containing polyanions ( and 2) have been intensively investigated during the last few decades because of their applications in different fields: solid electrolytes for energy stockage, Li-ion batteries, ceramics, luminescence, and magnetism [1]. Kanonerovite, Na3MnP3O10·12H2O, is a natural triphosphate mineral [2]; few other synthetic triphosphates have been reported in the literature: Na3CuP3O10·12H2O [3], LiZn2P3O10·8H2O [4], NaZn2P3O10·9H2O [5], and Na3CdP3O10·12H2O [6]. Anhydrous triphosphates have been also studied: LiFe2P3O10 [7], LiM2P3O10, M = Co and Ni [8, 9], RbBe2P3O10 [10], Cs2MP3O10 (M = Ga, Al, Cr) [11]. These latter ternary phosphates, with the frameworks consisting in associated [PO4] and [MO6], are efficiently used for waste storage hosts [12]. We deal in the present work with the synthesis and structural study of two new hydrated phases: Na3MP3O10·12H2O, M = Co (1) and Ni (2). 2. Experimental 2.1. Synthesis The title compounds Na3M(P3O10)·12H2O (M = Co (1), Ni (2)) were obtained by mixing two solutions made of following reactants, each dissolved in 10？mL distilled water: Na5P3O10 (0.3219？g) and, respectively, CoCl2·6H2O (0.2378？g) (1) and NiCl2·6H2O (0.2375？g) (2). The mixtures were stirred for 1？h and then allowed to stand at room temperature. After 2 weeks pink crystals of compound (1) and light green crystals of compound (2) were collected by filtration. The crystals were washed with a water-ethanol (80？:？20？v/v) mixture. 2.2. Single Crystal Study The X-ray diffraction data for (1) and (2) were collected in a four-circles diffractometer Gemini of Oxford Diffraction (now Agilent Technologies), using graphite monochromatized CuKα radiation ( ？？) collimated by mirrors, detector Atlas. The intensity data were corrected for Lorentz and polarization effects. A numerical absorption correction based on the crystal
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