Preparation, Crystal Structure and Vibrational Spectra of Ca₂P₂O₆·2H₂O and [Ca(H₂O)₃(H₂P₂O₆)]·0.5(C₁₂H₂₄O₆)·H₂O

Abstract

The calcium salts Ca2P2O6·2H2O (1) and [Ca(H2O)3(H2P2O6)]·0.5(C12H24O6)·H2O (2) were prepared and structurally characterized by single‐crystal X‐ray diffraction. Compound 1 crystallizes in the orthorhombic space group Pbca and compound 2 in the monoclinic space group P21/n. The crystal structure of compound 1 consists of chains of edge‐sharing [CaO7] polyhedra linked by hypodiphosphate(IV) anions to form a three‐dimensional network. The crystal structure of compound 2 consists of alternated layers of crown ether and water molecules and respective ionic units. Within the layers of ionic units the Ca2+ cations are octahedrally coordinated by three monodentate dihydrogenhypodiphosphate(IV) anions and three water molecules. The IR/Raman spectra of the title compounds were recorded and interpreted, especially with respect to the [P2O6]4– and [H2P2O6]2– groups. The phase purity of 2 was verified by powder diffraction measurements.

Three Crystal Structures, One Chemical Formula – Barium Dihydrogen‐hypodiphosphate(IV)‐dihydrate, BaH2P2O6·2H2O

“…Letztere betragen für A 107,6 bis 117,1 °, für B 106,7 bis 118,4 ° und für C 105,9 bis 116,4 °. Die Bindungslängen und ‐winkel sind vergleichbar mit denen anderer Dihydrogenhypodiphosphate(IV) , , , …”

“…Ca 2 P 2 O 6 · 2H 2 O und BaH 2 P 2 O 6 · 2H 2 O wurden erstmals rund 80 Jahre später von Palmer synthetisiert, wurden jedoch röntgenographisch nicht untersucht. Bei vorherigen Arbeiten wurden [Mg(H 2 P 2 O 6 )(H 2 O) 4 ] und Ca 2 P 2 O 6 · 2H 2 O dargestellt und strukturell aufgeklärt , . In diesem Artikel berichten wir über die drei neuen Modifikationen des Bariumsalzes, BaH 2 P 2 O 6 · 2H 2 O.…”

New Dihydrogenhypodiphosphates of Alkaline‐Earth Metals: Preparation, Crystal Structure, Vibrational Spectrum and Thermal Behavior of AE[H2P2O6] ⋅ n H2O (AE=Ca, Sr and n=1.5, 2)

“…Ca 2 [P 2 O 6 ] ⋅ 2 H 2 O and Ba[H 2 P 2 O 6 ] ⋅ 2 H 2 O were first synthesized by Palmer in 1961 [11] . Recently, the magnesium, calcium and barium salts could be characterized by X‐ray diffraction [12–15] . The present work is a continuation of the structural studies of alkaline‐earth metal hypodiphosphates.…”

“…[11] Recently, the magnesium, calcium and barium salts could be characterized by X-ray diffraction. [12][13][14][15] The present work is a continuation of the structural studies of alkaline-earth metal hypodiphosphates.…”

Crystal engineering and structural diversity of 2-aminopyridinium hypodiphosphates obtained by crystallization and dehydration

“…Moreover, the tendency of hypodiphosphates to form networks stabilized by strong O–H⋯O hydrogen bonds, composed exclusively of hypodiphosphate anions and/or acid molecules, has been clearly indicated. 20–24 Hypodiphosphate substructures are stabilized by the formation of one, two or three hydrogen bond bridges between anions or acid molecules. In most of the known crystals of organic hypodiphosphates, two hydrogen bonds link adjacent anions giving rise to motifs as shown in Fig.…”