Lian-Yi Cui

Synthesis, spectroscopic properties and crystal structure of organophosphoryl polyoxotungstate α-[Bu4N]3H[PhCH2P(O)]2SiW11O39

Reaction of the monovacant heteropolyanions α-[SiW11O39]8− with PhCH2PO(OH)2 leads to the formation of the organophosphoryl derivative α-[Bu4N]3H[PhCH2P(O)]2SiW11O39 (1). Single-crystal X-ray diffraction analysis shows that the crystal is monoclinic with space group P21 /n and the unit cell parameters: a = 14.386 (3) Å, b = 27.015 (5) Å, c = 25.480 (5) Å, α = 90°, β = 91.44 (3)°, γ = 90°, V = 9899 (3) Å3. Z = 4, D c = 2.467 g cm−1, λ (Mo-Kα) = 0.071073 nm, R 1 = 0.0638, wR 2 = 0.1364. The hybrid anion consists of an α-[SiW11O39]8− framework on which two equivalent organophosphoryl groups are grafted through P−O−W bridges; each of the two PhCH2P(O) groups are connected to two terminal oxygen atoms belonging to a triad and a diad, respectively.

Hydrothermal syntheses, crystal structures, and thermal stability of two new 3D open-framework metal(II) phosphonates

This article reports the hydrothermal synthesis and characterization of two new phosphonate compounds NaCo[O3PCH(OH)CO2] (1) and NaMn[O3PCH(OH)CO2] (2) based on 2-hydroxyphosphonoacetic acid (H3L). Their structures have been characterized by single-crystal X-ray diffraction as well as with elemental analysis, infrared spectroscopy and thermogravimetric analysis. The two isomorphous compounds crystalline in the orthorhombic, space group Pbca: Crystal data for 1: a = 10.1827(8) Å, b = 9.6673(8) Å, c = 10.7853(9) Å, V = 1061.70(15) Å3, Z = 8, R 1 = 0.0252, wR 2 = 0.0577; Crystal data for 2: a = 10.4309(18) Å, b = 9.7913(17) Å, c = 10.9012(19) Å, V = 1113.4(3) Å3, Z = 8, R 1 = 0.0194, wR 2 = 0.0536. In the two compounds, the metal atoms are octahedrally coordinated; all oxygen atoms from the H3L ligand are involved in coordination. The overall structures can be described as a 3D open framework with channels running along the a axis and the charge-compensating Na+ cations being located at the intersections of these channels.

Hydrothermal synthesis, crystal structure and thermal stability of a new 2D layered metal(II) phosphonate: [NH3CH2CH2NH3][Fe2(O3PCH(OH)CO2)2(H2O)2]·2H2O

In the presence of ethylenediamine template agents, a metal(II) phosphonate, [NH3CH2CH2NH3][Fe2(O3PCH(OH)CO2)2(H2O)2] · 2H2O (1) has been synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction as well as infrared spectroscopy, elemental analysis and thermogravimetric analysis. The compound crystallines in the monoclinic space group P21/n: Crystal data for 1: a = 8.4523(8) Å, b = 9.8196(9) Å, c = 10.9217(10) Å, β = 105.9500(10)°, V = 871.58(14) Å, Z = 2, D c = 2.103 g cm−3, R 1 = 0.0290, wR 2 = 0.0811. The Fe (II) cation is octahedrally coordinated by six oxygen atoms from the three ligands and one coordinated water molecule to form a 2D layered structure with a one-dimensional channel system in the a-axis direction.

Synthesis and spectroscopic characterization of organophosphoryl polyoxotungstates α-[PhP(Y)]2X n +W11

Organophosphoryl polyoxotungstate derivatives α-[PhP(Y)]2X n +W11 (X n + = Ge4+, B3+; Y = O, S) have been obtained by the reaction of the monovacant α-[X n +W11O39](12− n )− (X n + = Ge4+, B3+) anions with PhP(O)Cl2 or PhP(S)Cl2 in acetonitrile. These new organic–inorganic hybrid anions have been characterized by elemental analysis, IR, 31P and 183W NMR spectroscopy. According to the elemental analysis and spectroscopic data, the hybrid anions consist of an α-[XW11O39] framework on which are grafted two equivalent PhP(O) or PhP(S) groups through P–O–W bridges. The six-line 183W NMR spectrum indicates that the hybrid anions possess C s symmetry in acetonitrile.