钒磷酸盐(NH3CH2CH2NH2)[VOPO4]的水热合成和结构表征

标题化合物是在反应物摩尔比为V2O5H3PO4H2NCH2CH2NH2H2O=0.5543.6265时,175℃水热反应5 d合成的.其结构特点是钒八面体[VO5N]共用角顶的氧形成"之"字型链,链间由[PO4]共角项连接成层;乙二胺分子的一个N直接与V配位,并伸向层间.相邻层间存在强氢键.晶体学数据单斜晶系,P21/c(No.14),a=0.92108(2)nm,b=0.72851(1)nm,c=0.98204(2)nm,β=101.269(7)°,V=0.6462(4)nm3,Z=4,Dc=2.303g·cm-3,R1=0.0417,wR2=0.0999.     

[CH3NH3][NH3(CH2)6NH3]H3[P2Mo2W16O62]·H2O的水热合成与表征

首次合成了[CH3NH3][NH3(CH2)6NH3]H3[P2Mo2W16O62]·H2O,通过元素分析、红外光谱和X射线单晶衍射对合成产物进行了表征,并用TGA-DSC研究了化合物的热稳定性.晶体属单斜晶系,P21/m空间群,a=1.2596(3)nm,b=1.8715(4)nm,c=1.9816(4)nm,α=γ=90°,β=90.16(3)°,V=4.671(2)nm3,Z=2,Mr=4358.66,Dc=3.100g·cm-3,μ=19.978mm-1,F(000)=3792,R=0.0835,Rw=0.2026.结果表明,在晶体结构内形成了0.7364nm×0.8354nm的微孔.     

链状[NH3CH2CH2NH3]AgAsS4的溶剂热合成及表征

利用溶剂热方法合成了链状[NH3CH2CH2NH3]AgAsS4,通过单晶X射线衍射技术对其进行了晶体结构分析,该化合物晶体属单斜晶系,空间群C2/c,晶胞参数a=1.35805(8)nm,b=0.65331(3)nm,c=2.27711(9)nm,β=106.42(3)°,Z=8.化合物具有有趣的梯子状双链结构,该阴离子链由AsS4与AgS3共用顶点交替连接而成,有机阳离子在阴离子链之间存在较强的N—H…S氢键.DSC和Tg分析结果表明化合物在200℃以下是稳定的.     

新型三维结构亚磷酸钒(Ⅲ)[V2(HPO3)3·(H2O)3]·H2O的水热合成与晶体结构

在具有开放骨架结构的过渡金属磷酸盐微孔材料的合成中，钒磷酸盐因在催化和磁学方面具有潜在的性质和特殊结构特征而引起人们的广泛兴趣．近年来，人们正在尝试用假四面体结构的[HPO3]^2-替代四面体结构的[PO4]^3-，因为{HPO3}结构基元同钒原子的连接方式与{PO4}结构基元和钒原子的连接方式具有明显的差别，     

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…     

无机-有机杂化钼磷酸盐化合物(NH3CH2CH2NH3)2Mo5O15(HPO4)2的合成与表征

0引言 钼磷酸盐由于具有丰富的晶体结构特点和化学特性使得这种材料在催化、离子交换剂和材料科学等领域有着更加广阔的应用前景[1～3].     

二维层状磷酸亚磷酸钒(Ⅳ)化合物[V2O2(OH)(HPO3)(HPO3)0.7(PO3OH)0.3].(C6N2H16)0.5的水热合成与结构表征

迄今, 在中温水热条件下已合成了大量具有空旷骨架结构的过渡金属磷酸盐微孔材料[1], 这类材料在非线性光学材料、磁性材料、超导材料及催化等诸多方面具有潜在的应用前景[2～5].     

新型磷酸钒孔道结构化合物(H3NCH2CH2NH3)3- [ (VO)4(PO4)2 (HPO4)4]的水热 合成及结构表征

以有机分子乙二胺作为模板剂合成了新型磷酸钒孔道化合物(H3NCH2CH2NH3)3^-[(VO)4(PO4)2(HPO4)4,并通过X射线单晶衍射实验进行了结构表征,晶体学数据为：C2/c,a=1.8505(9)nm,b=0.7089(4)nm,c=2.3304(10)nm,β=96.43(3)°,V-3.038(3)nm^3,Z=8,R=0.067,Rw^b=0.1635,该化合物具有非常独特和规整的二维孔道骨架结构,进一步的晶体化学研究表明该化合物为一新的VPO物相。     

[C6N2H18]2[Mo5O15(HPO4)2]·H2O的水热合成与结构表征

通过水热法合成了一个新化合物[C6N2H18]2[Mo5O15(HPO4)2]·H2O,并通过IR光谱、ICP、元素分析、差热与热重分析和X射线单晶衍射分析等手段进行了表征.结果表明,晶体属三方晶系,P3(2)21空间群,a=1.1231(1)nm,c=2.2802(5)nm,V=2.4911(7)nm3,Dx=2.835Mg/m3,Z=6,最后的一致性因子R=0.0227,wR=0.0675.阴离子中Mo5O15构成一环状结构,2个HPO4一个连在环的下方,一个连在环的上方,形成类似于“飞碟”状的结构,阳离子为2个质子化的四甲基乙二胺.     

新型磷酸钒孔道结构化合物(H3NCH2CH2NH3)3- [ (VO)4(PO4)2 (HPO4)4]的水热 合成及结构表征

以有机分子乙二胺作为模板剂合成了新型磷酸钒孔道化合物(H3NCH2CH2NH3)3^-[(VO)4(PO4)2(HPO4)4,并通过X射线单晶衍射实验进行了结构表征,晶体学数据为：C2/c,a=1.8505(9)nm,b=0.7089(4)nm,c=2.3304(10)nm,β=96.43(3)°,V-3.038(3)nm^3,Z=8,R=0.067,Rw^b=0.1635,该化合物具有非常独特和规整的二维孔道骨架结构,进一步的晶体化学研究表明该化合物为一新的VPO物相。     

Hydrothermal Synthesis and Characterization of (H3N(CH2)4NH3)[V6O14]

A new layered vanadium oxide [H₃N(CH₂)₄NH₃](V₆O₁₄) was synthesized hydrothermally under autogenous pressure at 180°C for 48 h from a mixture of H₂N(CH₂)₄NH₂ and V₂O₅ in aqueous solution. Its structure was determined from single-crystal X-ray diffraction at room temperature with final R=0.0774 and R_w=0.0893. It crystallizes in the monoclinic system (space group P2₁/n with a=9.74(2) Å, b=6.776(5) Å, c=12.60(2) Å, β=96.1(1)°, V=827(2) ų and Z=2). This compound contains mixed-valence V⁵⁺/V⁴⁺ vanadium oxide layers built from [V^VO₄] tetrahedra and pairs of edge-sharing [V^IVO₅] square pyramids with protonated organic amines occupying the interlayer space.     

Solvothermal Synthesis and Characterization of （ NH3 CH2 CH2 NH3） HgSnS4 with a Column Structure

IntroductionSulfide-based open-framework materials are in-triguing compounds.They possess very diverse and in-teresting structures,and exhibit potential applicationsas a newgeneration of molecular sieves with the proper-ties of semiconductor materials[1].…     

具有[344484]笼状结构单元的微孔磷酸镓Ga3P2O8(OH)3(H2O)的合成、晶体结构及表征

Open-framework metal phosphates have been the subject of intense research owing to their interesting structural chemistry and potential applications in catalysis and ion exchange. The gallium phosphate family has exhibits rich structural chemistry. A novel gallium phosphate Ga₃P₂O₈(OH)₃(H₂O)(GaPO-CJ36) has been prepared in a hydrothermal reaction system of GaO(OH)-H₃PO₄-Co(chxn)₃Cl₃-H₂O at 180 ℃ for 7 days. Single-crystal X-ray analysis shows that GaPO-CJ36 crystallizes in the P2₁/c space group with a=1.833 35(12) nm, b=0.503 94(3) nm, c=1.062 90(9) nm, V=0.982 01(12) nm³, and Z=4. The connection of GaO₂(OH)₃(H₂O) octahedra, PO₄ and GaO₄ tetrahedra through vertex oxygen atoms forms a three-dimensional open framework, which contains 8-ring channels along the [010] direction. Its structure is composed of interesting [3⁴4⁴8⁴] cages, which have not been found in known gallium phosphates. CSD: 416779.     

Hydrothermal Synthesis and Crystal Structure of the First Ammonium Indium(III) Phosphate NH4In(OH)PO4 with Spiral Chains of InO4(OH)2

An ammonium indium hydrogen phosphate, NH₄In(OH)PO₄, was synthesized under mild hydrothermal conditions, and the crystal structure was characterized by single-crystal X-ray diffraction method. The compound crystallizes with the RbIn(OH)PO₄ type with the following data: M_r=244.84, tetragonal, tP104, P4₃2₁2 (No.96), a=9.416(2) Å, c=11.159(3) Å, V=989.9(3) ų, Z=8, D_x=3.288 g cm⁻³, λ=0.71073 Å, μ=50.34 cm⁻¹, F(000)=928, T=293 K, R1=0.0606, wR2=0.1472 for 91 variables and 1813 contributing unique reflections. The structure is characterized by chiral InO₄(OH)₂ chains along the c axis formed by sharing OH corners. The chains are isolated by PO₄ tetrahedra leading to a three-dimensional framework structure with channels occupied by NH₄⁺ ions. The framework structure is similar to that of KIn(OH)PO₄ and γ-NaTiOPO₄. The hydrogen bonds formed by NH₄⁺ with the polyhedral oxygen atoms play an important role in the anisotropic changes of the lattice with respect to its alkali metal analogues. The topological construction of the title structure can be considered as an augmented 4,6-net with larger porosity.     

两种有机-无机复合杂多化合物的水热合成及结构表征

利用水热法制备了基于饱和Keggin结构阴离子构筑的有机-无机复合多金属氧酸盐(4,4′-bipy)4H4[PMo12O40](CH3COO).1.5H2O(1)和(4,4′-Hbipy)2(4,4′-bipy)2H[PW12O40].3.5H2O(2)(4,4′-bipy=4,4′-联吡啶),并借助元素分析、红外光谱、紫外光谱、热分析和X射线单晶衍射分析了两种化合物的组成和结构.结果表明,化合物1和2均属于单斜晶系,P2(1)/c空间群.化合物的晶胞参数为:a=1.869 40(13)nm,b=1.404 23(9)nm,c=2.707 76(18)nm,β=105.848 0(10)°,V=6.837 9(8)nm3,Z=4,R1=0.095 4;化合物2的晶胞参数为:a=1.884 80(12)nm,b=1.409 89(9)nm,c=2.664 92(17)nm,β=105.368 0(10)°,V=6.828 4(8)nm3,Z=2,R1=0.097 2.两种化合物结构类似,其结构单元均是由饱和Keggin阴离子与游离的4,4′-联吡啶分子通过静电作用相结合形成的.     

New Gallium Phosphate Frameworks Containing 1,4-Diaminobutane and 1,5-Diaminopentane: [NH3(CH2)xNH3][Ga4(PO4)4(HPO4)] and [NH3(CH2)xNH3][Ga(PO4)(HPO4)] (x=4 and 5)

Two new gallium phosphates, [NH₃(CH₂)₄NH₃][Ga₄(PO₄)₄ (HPO₄)] (I) and [NH₃(CH₂)₄NH₃][Ga(PO₄)(HPO₄)] (II), have been synthesized under solvothermal conditions in the presence of 1,4-diaminobutane and their structures determined using room-temperature single-crystal X-ray diffraction data. Compound (I) (M_r=844.90, triclinic, space group P-1, a=9.3619(3), b=10.1158(3) and c=12.6456(5) Å, α=98.485(1), β=107.018(2) and γ=105.424(1)°; V=1070.39 ų, Z=2, R=3.68% and R_w=4.40% for 2918 observed data [I>3(σ(I))]) consists of GaO₄ and PO₄ tetrahedra and GaO₅ trigonal bipyramids linked to generate an open three-dimensional framework containing 4-, 6-, 8-, and 12-membered rings of alternating Ga- and P-based polyhedra. 1,4-Diaminobutane dications are located in channels bounded by the 12-membered rings in the two-dimensional pore network and are held to the framework by hydrogen bonding. Compound (II) (M_r=350.84, monoclinic, space group P2₁/c, a=4.8922(1), b=18.3638(6) and c=13.7468(5) Å, β=94.581(1)°; V=1227.76 ų, Z=4, R=2.95% and R_w=3.37% for 2050 observed data [I>3(σ(I))]) contains chains of edge-sharing 4-membered rings of alternating GaO₄ and PO₄ tetrahedra constituting a backbone from which hang ‘pendant’ PO₃(OH) groups. Hydrogen bonding between the GaPO framework and the diamine dications holds the structure together. A previously reported phase, [NH₃(CH₂)₄NH₃][Ga₄(PO₄)₄(HPO₄)] (V), structurally related but distinct from its stoichiometric equivalent, (I), has been prepared as a pure phase by this method. Two further materials, [NH₃(CH₂)₅NH₃][Ga₄(PO₄)₄(HPO₄)] (III) (tricli- nic, lattice parameters from PXD: a=9.3565(4), b=5.0156(2) and c=12.7065(4) Å, α=96.612(3), β=102.747(4) and γ=105.277(3)°) and [NH₃(CH₂)₅NH₃][Ga(PO₄)(HPO₄)] (IV) (M_r=364.86, monoclinic, space group P2₁/n, a=4.9239(2), b=13.2843(4) and c=19.5339(7) Å, β=96.858(1)°; V=1268.58 ų, Z=4, R=3.74% and R_w=4.44% for 2224 observed room-temperature data [I>3(σ(I))]), were also prepared under similar conditions in the presence of 1,5-diaminopentane. (III) and (IV) are structurally related to, yet distinct from (I) and (II) respectively.