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Two novel hexa-nickel(II)-substituted Keggin-type {NiPW}-based tungstophosphates [Ni( μ-Tris)(en)( Pr)(damp)(HO)(B- α-PWO)]·10HO ( 1) and [Ni( μ-Tris)(en)(damp)(HO)(B- α-PWO)]·7HO ( 2) (en = ethylenediamine, Pr = CHCHCOO, damp = 2-aminoisobutyrate, Tris = pentaerythritol) were hydrothermally synthesized and characterized by IR spectra, elemental analyses, powder X-ray diffraction, thermogravimetric analyses, and single-crystal X-ray diffraction. Crystal data for 1: orthorhombic, Pca2, a = 21.6962(7) Å, b = 20.6398(5) Å, c = 14.7825(4) Å, β = 90º, V = 6619.7(3) Å, Z = 4; for 2: orthorhombic, Pca2, a = 21.6978(9) Å, b = 20.6658(7) Å, c = 14.7767(4) Å, β = 90º, V = 6625.9(4) Å, Z = 4. 1 consists of a {Ni( μ-Tris)(en)( Pr)(damp)(HO)} core and a [B- α-PWO] (PW) unit and is covalently functionalized by one Pr and one damp, as well as en and Tris ligands. The structure of 2 is the same to 1 except that the Pr anion in 1 is substituted by the other damp ligand. Most interestingly, 1 contains four kinds of organic ligands, while 2 includes three kinds of organic ligands, which are first observed in polyoxometalate chemistry. [ABSTRACT FROM AUTHOR]

Four new hexa-nickel(II)-substituted Keggin-type tungstophosphates [Ni(μ-OH)(oeen)(HO)(B-α-PWO)]·6HO ( 1, oeen = N-(2-hydroxyethyl)enediamine), [Ni(μ-OH)(oeen)(HO)(B-α-PWO)]·13HO ( 2), [Ni(μ-OH)(oeen)(tran)(HO)(B-α-PWO)]·3HO ( 3, tran = 1,4,7-triazonane) and [Ni(μ-OH)(oeen)(tran)(HO)(B-α-PWO)]·6HO ( 4) have hydrothermally made by controlling their reaction temperatures. 1- 4 have been characterized by elemental analyses, IR spectra, powder X-ray diffraction, thermogravimetric analyses and single-crystal X-ray diffraction, respectively. Structural analyses reveal that they consist of {Ni(μ-OH)(HO)} cores and B-α-PWO (PW) units, and further are stabilized by organic neutral oeen/tran molecules. 1- 3 are isolated clusters while 4 is the 1D chain structure. It should be noted that the tran molecules in 3 and 4 are derived from the oeen molecules in the starting materials. [ABSTRACT FROM AUTHOR]