Na6In4[P7O24(OH)5]·4H2O的水热合成与表征

具有开放骨架结构的金属酸盐在作为微孔材料、非线性光学材料、催化剂载体和离子交换剂等方面具有应用前景 [1] .自从报道第一个具有微孔结构的磷酸铝 [2 ]以来 ,许多其它具有开放骨架结构的金属磷酸盐被合成出来 ,它们的性质和潜在的应用研究也备受关注 [3～ 8] .本文采用温和条件下的水热法 ,合成得到了具有螺旋链状结构的磷酸铟钠盐 [Na6 In4 [P7O2 4 ( OH) 5]· 4H2 O,并采用 X射线单晶衍射方法进行结构测定 ,其结构中包含了共顶角的多面体连接成的螺旋链 ,链间的连接形成多面体四元环和八元环 ,3个四元环围成了一个三配位氧为中心…     

具有新结构类型的化合物CsIn[PO3(OH)]2的合成与结构(英)

水热法合成了新结构类型化合物CsIn[PO₃(OH)]₂，并通过单晶X-射线衍射表征结构。标题化合物空间群为P1 2₁/c 1 (No.14)，晶体学参数为：M_r=439.69，mP56，a=0.532 86(6) nm，b=0.916 53(7) nm，c=1.478 39(14) nm，β=93.849(9)°，V=0.720 4(1) nm³，Z=4，D_x=4.054 g·cm^-3，μ=8.713mm^-1，F(000)=800，R₁= 0.032 5，wR₂=0.087 4。在该化合物中，2个InO₆八面体和4个PO₄四面体形成交连的六元环柱，并沿a轴方向形成近六方密堆积并连接成Cs⁺离子占据的十二元环结构隧道，六元环和十二元环连接构筑了三维网络结构。与类似化学计量比化合物Na₂In₂[PO₃(OH)]₄·H₂O比较，标题化合物中十二元环的形成明显取决于隧道阳离子的大小，其拓扑构造可看作扩展的6，3-网格连接，化合物 RbIn[PO₃(OH)]₂与之同构。     

具有新结构类型的化合物Csln[PO3(OH)]2的合成与结构

水热法合成了新结构类型化合物CsIn[P03(0H)]2,并通过单晶X-射线衍射表征结构.标题化合物空间群为P121/c1(No.14),晶体学参数为:M=439.69,mP56,a=0.532 86(6)nm,b=0.91653(7)nm,c=1.478 39(14)nm,β=93.849(9).,V=0.7204(1)nm3,Z=4,Dx=4.054 g·cm-3,μ=8.713 mm-1,F(000)=800,R1= 0.0325,wR2=0.0874.在该化合物中,2个In06八面体和4个PO4四面体形成交连的六元环柱,并沿a轴方向形成近六方密堆积并连接成Cs+离子占据的十二元环结构隧道,六元环和十二元环连接构筑了三维网络结构.与类似化学计量比化合物Na2In2[PO3(0H)]4·H2O比较,标题化合物中十二元环的形成明显取决于隧道阳离子的大小,其拓扑构造可看作扩展的6,3-网格连接,化合物RbIn[PO3(0H)]2与之同构.     

A New Modification of Tellurite Phosphate: β-Te_3O_3(PO_4)_2

A new modification of tellurite phosphate, β-Te_3O_3(PO_4)_2, has been synthesized under hydrothermal conditions and its crystal structure was determined by single-crystal X-ray diffraction. It crystallizes in the monoclinic space group P2_1/n(No. 14), with a = 11.115(5), b = 4.7033(19), c = 17.287(7) ?, β = 106.086(5)°, V = 868.3(6) ?~3, Z = 4, P_2 Te_3 O_(11), M_r = 620.74, D_c = 4.748 g/cm~3, μ(Mo Kα) = 10.438 mm~(–1) and F(000) = 1096. The final full-matrix least-squares refinement converged to R = 0.0227, wR = 0.0534 for 1984 observed reflections with I 2σ(I), and R = 0.0240, w R = 0.0540 for all data(2070) and S = 1.117. β-Te_3O_3(PO_4)_2 is polymorphic with the known α-Te_3O_3(PO_4)_2(Weil H. M. et al. Z. Anorg. Allg. Chem. 2003, 629, 1068-1072). The crystal structure of β-Te_3O_3(PO_4)_2 features a three-dimensional(3D) network composed of Te_6 O_(22)~(20)-hexanuclear clusters interconnected by PO_4 groups. Te_6 O_(22) hexanuclear cluster is built from three Te_2 O_8 dimers(edge-sharing TeO_5 square pyramids) linked to each via sharing O-corners. The structure difference between α-and β-forms of Te_3O_3(PO_4)_2 lies in the polymerization of tellurite oxides Te_nO_m. 1D infinite ~1_∞{[Te_3 O_(11)]~(10-)} single chains are presented in α-Te_3O_3(PO_4)_2, while 0D discrete Te_6 O_(22) hexanuclear clusters are observed for β-Te_3O_3(PO_4)_2. Moreover, thermal analyses, infrared spectra and UV-Vis-NIR diffuse reflectance are also presented.     

Two Alkali Metal Germanophosphates Na3[Ge(OH)(PO4)2]·2H2O and Li2Na[GeO(HPO4)(PO4)]:Crystal Structures and Thermal Stability

Two new alkali metal germanophosphates,namely,Na₃[Ge(OH)(PO₄)₂]·2 H2 O and Li₂Na[GeO(HPO₄)(PO₄)],have been prepared by solvothermal method,and their crystal structures were determined by single-crystal X-ray diffraction.The title two compounds crystalize in the same orthorhombic space group Pbcm(No.57)and feature similar chain-like structure which is built from zig-zag GeO₆ octahedral thread loop branched by PO₄ tetrahedra.For Na₃[Ge(OH)(PO₄)₂]·2 H₂O,a=10.1650(9),b=13.1975(12),c=6.9751(7)?,V=935.73(15)?³,Z=4,R=0.0356 and wR=0.1109;and for Li₂Na[GeO(HPO₄)(PO₄)],a=6.9855(5),b=14.5809(18),c=6.6620(5)?,V=678.56(11)?³,Z=4,R=0.0286,and w R=0.0762.The partial substitution of Na ions by Li ions not only significantly influences the total structural features and the water molecule contents,but also impacts on their thermal stabilities.Li₂Na[GeO(HPO₄)(PO₄)]is thermally stable up to 400℃,whereas only 150℃ for Na₃[Ge(OH)(PO₄)₂]·2 H2 O.     

具有新结构类型的化合物CsIn[PO_3(OH)]_2的合成与结构(英文)

水热法合成了新结构类型化合物CsIn[PO3(OH)]2,并通过单晶X--射线衍射表征结构。标题化合物空间群为P121/c1(No.14),晶体学参数为:Mr=439.69,mP56,a=0.53286(6)nm,b=0.91653(7)nm,c=1.47839(14)nm,β=93.849(9)°,V=0.7204(1)nm3,Z=4,Dx=4.054g·cm-3,μ=8.713mm-1,F(000)=800,R1=0.0325,wR2=0.0874。在该化合物中,2个InO6八面体和4个PO4四面体形成交连的六元环柱,并沿a轴方向形成近六方密堆积并连接成Cs 离子占据的十二元环结构隧道,六元环和十二元环连接构筑了三维网络结构。与类似化学计量比化合物Na2In2[PO3(OH)]4·H2O比较,标题化合物中十二元环的形成明显取决于隧道阳离子的大小,其拓扑构造可看作扩展的6,3-网格连接,化合物RbIn[PO3(OH)]2与之同构。