The hydroxy yttrium hexaborate,Y[B2O3(OH)]3,has been synthesized under mild hydrothermal conditions at 458 K.The crystal structure was solved and refined from single-crystal X-ray diffraction.It adopts a trigonal space group R3c(No.161) with a = 8.3942(4),c = 20.6484(12) ,V = 1260.03(12) 3,YB6H3O12,Mr = 348.79,Z = 6,Dc = 2.758 g/cm3,F(000) = 1008,μ = 7.015 mm-1,R = 0.0321 and wR = 0.0772.Its crystal structure is made up of six-membered rings,alternating three-connected [BO3(OH)] tetrahedra and planar [BO3] trigonal groups,which are interconnected with each other by sharing their common oxygen corners to form a three-dimensional framework structure with six-membered ring channels that are occupied by the yttrium atoms and run along the c axis.FT-IR,Raman,and TG-DTA results are also presented.
A vanadyl phosphate containing a new member of tancoite-like single chain,(DAPH2)[VIVO(HPO4)2]·xH2O(x≈0.2,DAP=1,3-diaminopropane,C3H10N2),has been synthesized under hydro(solvo)thermal conditions.It crystallizes in orthorhombic space group P21212(No.18)with a=7.1730(14),b=19.252(4),c=8.6557(17),Z=4,V=1195.3(4)3,C3H14.38N2P2VO9.19,Mr=338.47,Dc=1.881 g/cm3,μ(MoKα)=1.138 mm–1and F(000)=692.The final full-matrix least-squares refinement converged to R=0.0408,wR=0.1046 for 2498 observed reflections with I>2(I)and R=0.0456 and wR=0.1080 for all data(2750)and S=1.001.Its one-dimensional structure consists of tancoite-like1{VIVO(HPO4)2}2–single chains surrounded by DAPH22+ions and water molecules.The single chain is built from trans-corner-sharing octahedral{VIV=O···VIV}backbone loop-branched by HPO4groups like staple forming a new member of tancoite single chain.Due to the special coordination of VIVO6,the1{VO(HPO4)2–}chain adopts a larger M–O–M angle(V–O–V=135o)than those of tancoite chains reported before.The corner-sharing linear{VIV=O···VIV}chain structure also leads to a one-dimensional weak antiferromagnetic interaction at low temperature.The magnetic measurements confirm the 4+valence state of vanadium.IR and TG results of the title compound are also discussed.
A novel inorganic-organic hybrid compound,{[Co(dien)]4[(PO4)MoV8(WVI0.56MoVI0.44)4-O33(OH)3]}·nH2O(1,n≈1,dien=diethylenetriamine),has been synthesized hydrothermally and characterized by single-crystal X-ray diffraction.Compound 1 crystallizes in the triclinic system with a=11.927(2),b=13.328(3),c=19.306(4),α=93.76(3),β=94.14(3),γ=109.99(3)o,V=2863.2(12)3,space group P1 and Z=2 at 173 K.The final full-matrix least-squares refinement converged to R=0.049 for 9621 observed reflections with I>2σ(I)and wR=0.139 for all data(9871)and S=1.073.Crystal structure analysis shows that 1 contains a kind of the first reported mixed-valence and molybdenum-tungsten mixed-distributedε-Keggin structural polyanion capped by four Co(dien)fragments with the main group element P occupying the center site.These results were further confirmed by energy-dispersive X-ray spectroscopy(EDS),X-ray powder diffraction(XRD),Fourier transform infrared spectroscopy(FTIR),Raman spectroscopy,Thermogravimetry(TG)and X-ray photoelectron spectroscopy(XPS)analyses.
Polyoxometalates(POMs) with Cd-coordination complexes acting as supporting units are rarely reported. The linkage of the supporting units with inorganic building block(polyanion) is generally established on terminal O-atoms, but scarcely via bridging O-atoms. By introducing liquid small organic molecule(pyridine, C5NH5) as assistant "structure-directing agent", we obtained a novel organic-inorganic hybrid polytungstate,(Hpy)4[Cd(phen)2(P2W18O62)]·nH2O(1, n ≈ 3, py = pyridine, phen = 1,10-phenanthroline), under hydrothermal conditions. The single-crystal X-ray diffraction analysis shows that 1 is the first compound containing an asymmetric heteropolyanion, [Cd(phen)2(P2W18O62)]4–, a Wells-Dawson-type polyanion monosupported by Cd-coordination complex via di-bridging O-atoms.
