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1.
以哌嗪为模板剂, 在水热条件下合成了一个新的具有二维拓展骨架结构的稀土硫酸盐[C4N2H12]3[Ce2(SO4)6(H2O)2]·H2O, 并对其进行了结构表征和热分析. 单晶结构解析结果表明, 该化合物晶体属于单斜晶系, P21/c空间群, 晶体学参数a=0.66335(10) nm, b=2.8088(4) nm, c=1.02212(15) nm, β=96.160(2)°, V=1.8935(5) nm3, R1=0.0466, wR2=0.1226. 该化合物由[—Ce—S3—Ce—S1—Ce— S3—Ce—S1—]八元环连接形成二维层状结构, 无机层间通过氢键连接成三维无限结构.  相似文献   

2.
三维亚磷酸铁(H3O)2·[FeⅡ5(HPO3)6]的水热合成与结构表征   总被引:3,自引:1,他引:2  
于中温水热条件下合成出一种三维亚磷酸铁(H3O)2·[FeⅡ5(HPO3)6], 并对其进行了单晶解析、 热重及磁性等系列表征. 晶体属三方(Trigonal)晶系, P3c1空间群, a=1.026 9(5) nm,  b=1026 9(5) nm,  c=0.929 5(6) nm,  Z=2. 化合物中心铁原子采取略变形八面体构型, 与亚磷酸根假四面体连接形成三维骨架结构, 沿c轴方向有一六元环孔道.  相似文献   

3.
通过三缺位Keggin结构杂多阴离子[α-A-PW9O34]9-和二氯甲基苯基硅烷在乙腈溶液中反应,合成了一例结构新颖的甲基苯基硅衍生物[(C4H9)4N]3[α-A-PW9O34(C6H5SiCH3)3](1),并对其进行元素分析,红外光谱,紫外光谱,热分析和X-射线单晶衍射等表征。该配合物属于三方晶系,空间群为R3m,晶胞参数:a=2.261 3(2)nm,b=2.261 3(2)nm,c=1.797 6(4)nm,V=7.960 2(18)nm3,Z=3。在配合物中,阴离子[α-A-PW9O34(C6H5SiCH3)3]3-呈C3v对称,3个甲基苯基硅基团连接在三缺位的阴离子[α-A-PW9O34]9-表面,整个阴离子显示"开放结构"。  相似文献   

4.
利用CuCl2·2H2O,1,2,4-三氮唑(TA),L-丝氨酸与Na3[α-PW12O40]·6H2O在乙醇的水溶液中合成了一种有机-无机复合Keggin结构磷钨酸盐[HTA]3[α-PW12O40]·6H2O;利用红外光谱和X射线单晶衍射表征了合成产物的结构,利用元素分析测定了其组成.结果表明,标题化合物属于菱方晶系R-3空间群,晶胞参数为:a=1.793 73(12)nm,b=1.793 73(12)nm,c=2.440 7(3)nm,α=β=90°,γ=120°,Z=6,V=6.800 7(11)nm3,Dc=4.682g·cm-3,GOOF=1.079,R1=0.051 6,wR2=0.137 4.就分子结构而言,标题化合物分子由一个饱和Keggin结构多阴离子[α-PW12O40]3-,三个游离的质子化[HTA]+阳离子和六个结晶水分子组成.  相似文献   

5.
[CH3NH3][NH3(CH2)6NH3]H3[P2Mo2W16O62]·H2O的水热合成与表征   总被引:4,自引:0,他引:4  
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.  相似文献   

6.
在溶剂热体系中,以N,N-二乙基乙二胺为结构导向剂,合成了Al/P为3/4的层状磷酸铝[Al6P8O32][(C2H5)2NHCH2CH2NH3]2·[C2H5NH2CH2CH2NH2C2H5]单晶,并通过X射线单晶衍射结构分析.XRD,ICP,元素分析,差热-热重分析等手段进行了表征.该化合物属单斜晶系,P2(1)/c空间群,晶胞参数:a=0.90945(2)nm,b=1.46424(4)nm,c=1.87572(5)nm,β=102.672(2)°,Z=4.其阴离子层由AlO4四面体和PO3(=O)四面体单元交替连接构成,形成四、六、八元环拓扑结构,无机层以ABAB方式堆积,两种质子化的有机胺分子N,N-二乙基乙二胺及其重排产物N,N′-二乙基乙二胺填充在层间.用分子动力学模拟方法,考察了标题化合物中有机胺与无机层间的相互作用,讨论了这两种有机胺的共模板作用.  相似文献   

7.
合成了双核银配合物[Ag2(μ-(4-MeC6H4O)2PS2)2(Phen)2](phen为1,10-邻菲咯啉),用元素分析、红外光谱、紫外-可见光谱和热重分析进行了表征,并用X-射线衍射法测定了晶体结构。该晶体属于正交晶系,Pbca空间群,晶胞参数为:a=1.2035(2)nm,b=1.638 3(3)nm,c=2.517 1(5)nm,V=4.963 1(17)nm 3,Dc=1.599 g.m-3,Z=4,F(000)=2 416,μ(Mo Kα)=1.072 mm-1,S=1.066,(Δ/σ)max=0.001,R1=0.037 6,wR2=0.088 8(I>2σ(I))。晶体结构研究表明每个Ag原子与不同配体(4-MeC6H4O)2PS2-的2个S原子和1个phen配体的2个N原子配位形成了具有椅式构型的八元环Ag2S4P2,Ag原子为畸变四面体AgS2N2构型,配合物通过phen的π-π堆积形成了一维结构,分子间的弱氢键C-H…O和C-H…π作用使分子进一步形成了三维网络结构。  相似文献   

8.
利用水热技术合成了一种新型[Co(bim)x]配合物修饰的磷钼多金属氧酸盐超分子化合物[Co(bim)3] [Co(Hbim)2( H2 O) P2 Mo5 O23]·5H2O.通过元素分析、红外光谱、热重分析和X射线单晶衍射对化合物进行了表征.化合物属于单斜晶系,P2(1)空间群;晶胞参数:a=11.505 (2) nm,b=19.123 (3) nm,c=13.852(2) nm,α=90.00°,β=100.073(2)°,γ=90.00°,V=3 000.6(8)nm3,F(000)=1 756.0,Z=2.并测试了合成化合物的电化学性质.  相似文献   

9.
H2L[N,N’-二(3-吡啶基)-2,6-吡啶羧酸二酰胺]与CuSO4.5H2O反应合成了新型大环双核铜配合物——[Cu2(H2L)2(SO4)2(H2O)6]·CH3OH·6H2O(1),其结构经IR,XRD和元素分析表征。1属单斜晶系,空间群P21/C,晶胞参数a=26.870(5),b=7.563 7(15),c=28.316(6),α=90°,β=114.91(3)°,γ=90°。1在催化2,6-二甲基苯酚氧化偶联反应时表现出较好的选择性及催化活性。  相似文献   

10.
采用常温晶化法合成了1个新的金属配合物与氟化锆的复合物[Co(en)3]2(Zr2F12)(ZrF6H2O)·H2O(1), 并对其单晶结构进行了解析. 该化合物属单斜晶系, C2/c 空间群, a=3.06110(17) nm, b=0.877680(5) nm, c=1.50811(9) nm, β=118.897(4)°, V =3.547(4) nm3, Z=8. 该化合物由双核氟化锆阴离子簇 [Zr2F12]4-和单核氟化锆阴离子簇 [ZrF6H2O]2-与钴胺配合物阳离子 [Co(en)3]3+ 及水分子组成, 氟化锆与钴胺配合物之间存在大量的氢键. 该化合物的表面光电压谱在339 nm处出现了光电信号. 这种特殊的光电现象有可能归因于该化合物的钴胺配合物阳离子与氟化锆阴离子簇之间存在的协同作用.  相似文献   

11.
1 INTRODUCTION A new class of materials of metal oxide clusters based on anionic molybdenum phosphate frameworks has received much attention as a consequence of their potential applications in catalysis and materials science [1]. As a result, some molybdenum phosphates have been studied [2,3]. Recently we have studied the structure of NaPMO material[4] and the spectrum of multicomponent compound with Keggin struc- ture [5]. Here we report the synthesis and crystal structure of a new…  相似文献   

12.
Guo M  Yu J  Li J  Li Y  Xu R 《Inorganic chemistry》2006,45(8):3281-3286
The first two low-dimensional beryllium phosphates, [C5H14N2]2[Be3(HPO4)5].H2O (BePO-CJ29) and [C6H18N2]0.5[Be2(PO4)(HPO4)OH].0.5 H2O (BePO-CJ30), have been successfully synthesized under mild hydrothermal/solvothermal conditions. BePO-CJ29 is built up from strict alternation of BeO4 and HPO4 tetrahedra forming a unique one-dimensional double chains with 12-ring apertures. There are pseudo-10-ring apertures enclosed by two double chains through H-bonds. BePO-CJ29 can also be viewed as a pseudo 2-D layered structure stabilized by strong H-bonds. The diprotonated 2-methylpiperazium cations are located at three positions (i.e., inside the 12-ring aperture, inside the pseudo-10-ring aperture, and in the interlayer of the inorganic pseudo-layers. BePO-CJ30 is constructed by the alternation of Be-centered tetrahedra (including BeO4 and HBeO4) and P-centered tetrahedra (including PO4 and HPO4) resulting in a two-dimensional layered structure parallel to the (0 1 1) direction. The complex layer is composed of coupled 4.8 net sheets. The diprotonated 1,6-hexandiamine cations and water molecules reside in the interlayer regions and interact with the inorganic layers through H-bonds. Crystal data are as follows: [C5H14N2]2[Be3(HPO4)5].H2O (BePO-CJ29), triclinic, P1 (No. 2), a = 8.1000(9) A, b = 8.4841(14) A, c = 19.665(2) A, alpha = 89.683(10) degrees, beta = 78.182(8) degrees, gamma = 87.932(9) degrees, V = 1321.9(3) A3, Z = 2, R1 = 0.0523 (I > 2sigma(I)), and wR2 = 0.1643 (all data); [C6H18N2]0.5[Be2(PO4)(HPO4)OH].0.5 H2O (BePO-CJ30), orthorhombic, Pccn (No. 56), a = 26.01(4) A, b = 8.431(12) A, c = 9.598(13) A, V = 2105(5) A3, Z = 8, R1 = 0.0833 (I > 2sigma(I)), and wR2 = 0.2278 (all data).  相似文献   

13.
采用低温技术,用X射线单晶衍射法测定了标题化合物的结构。晶体属P4/mnc空间群,=12.515(3),c=17.636(7)A,Z=2.用788个独立可观测反射精修所有结构参数得R=0.061.钼钒磷杂多酸阴离子中,PO4四面体是无序的,P-O键长1.54A.M(Mo,V)是6配位,M-O键长1.62-2.48A,K是7配位,K-O键长2.84-3.10A。  相似文献   

14.
The crystals of the title compounds (H3O)(C3H5N2)[Mn(OH)6Mo6O18]·3.5H2O 1 and (H3O)3[Co(OH)6Mo6O18]·7H2O 2 have been prepared and structurally determined by X-ray single-crystal diffraction. Compound 1 crystallizes in monoclinic, space group C2/c with a = 21.5018(9), b = 10.9331(5), c = 11.8667(5)A,β = 95.3570(10)o, V = 2777.5(2)A3, Z = 4, Dc = 2.802 g/cm3, Mr = 1171.80,μ(MoKα) = 3.173 mm-1, F(000) = 223, the final R = 0.0458 and wR = 0.1041 for 2093 observed reflections (I>2σ(I)); Compound 2 crystallizes in monoclinic, space group P21/c with a = 11.4042(12), b = 10.9481(11), c = 11.6722(12)A, β= 99.948(2)o, V = 1435.4(3)A3, Z = 2, Dc = 2.794 g/cm3, Mr = 1207.80,μ(MoKα) = 3.223 mm-1, F(000) = 1160, the final R = 0.0544 and wR = 0.1066 for 1906 observed reflections (I > 2σ(I)). Both compounds 1 and 2 adopt the Anderson structure, in which the anion is of centrosymmetry and formed by six octahedral edge-sharing MoO6 units surrounding the central MO6 (M = Mn or Co) octahedron.  相似文献   

15.
The title compound Na5H37P6Mo18O90 1 (Mr=1658) was synthesized under hydrothermal condition and its crystal structure was determined by X-ray diffraction. It crystallized in the monoclinic system, space group P21 with a =14.957(1), b =16.535(1), c = 16.159(1)?,β=108.586(2)°, V=3787.85?3, Dc =3.040g/cm3, Z=2,μ(MoKα)=3.17mm-1, F(000)=3242. The final R and wR are 0.0500 and 0.1535 for 6643 observable reflections with I≥2σ(I), respectively. The result of structure analysis indicates that [Na(HPO4)2(PO4)4-Mo18 O49]5-anions 2 in 1 has the symmetry of C2V, in which each MoVIO6 octahedron is connected to adjacent PO4 tetrahedra through corner-sharing and to adjacent octahedra through edge-sharing or corner-sharing.  相似文献   

16.
研究了一种可循环并且环境友好的催化体系:[π-C5H5N(CH2)15CH3]3[PMoW3O24]/过氧化氢/乙酸乙酯/烯烃.此体系不仅可以催化烯烃的环氧化反应,而且避免了对含氯溶剂的使用.反应在过氧化氢/乙酸乙酯的两相体系中进行,可以将多种烯烃转化为相应的环氧化物,且产率较高.此催化剂具有反应控制相转移的特征,反应结束后可以回收再利用.采用Raman,IR,^31P MAS NMR和^31P NMR等手段对新鲜及重复使用过的催化剂进行表征.结果表明:新鲜催化剂[π-C5H5N(CH2)15CH3]3[PMoW3O24]是一种混合物,含有多种过氧磷钼钨酸盐,如{PO4[MoO(O2)2]4}^3-,[(PO4){Mo3WO20}]^3-,[(PO4){Mo2W2O20}]^3-,[(PO4){MoW3O20}]^3-和{PO4[WO(O2)2]4}^3-.当过氧化氢被完全消耗后,这些小的活性物种就会聚合成具有混合多原子的Keggin型杂多阴离子,形成M-Ob—M(M=W或Mo)和M-Oc-M键.  相似文献   

17.
(H_2en)_2[Se_2Mo_5O_(21)]2H_2O的水热合成、晶体结构与光谱研究   总被引:4,自引:0,他引:4  
在水热条件下, 以SeO2、V2O5、MoO3、K2CO3、en(乙二胺)作为起始原料, 得到了标题化合物(H2en)2[Se2Mo5O21]2H2O, 利用IR、UV、荧光光谱、单晶-X射线衍射等方法对其进行了表征。结构测定表明, 该化合物属于正交晶系, 空间群: P212121, 化学式: C4H24- Mo5N4O23Se2, 晶胞参数: a = 12.1386(7), b = 17.7118(8), c =11.7092(5) ? V = 2517.4(2) ?, Z = 4, Dc = 2.987 g/cm3, Mr = 1133.89, m = 5.419 mm-1, F(000) = 2144, 最终结构偏离因子R = 0.0285, wR = 0.0400, S = 0.904。该化合物由2个双质子化的en、2个H2O分子以及杂多阴离子[Se2Mo5O21]4-组成。其中,杂多阴离子由5个畸变的MoO6八面体以共边或共顶点形式连接构成一个平面骨架; 2个畸变的SeO3四面体和MoO6八面体以共顶点形式连接, 且位于平面的两侧;质子化的en位于4个[Se2Mo5O21]4-离子围成的四面体空位中, 与杂多阴离子和水分子通过氢键连接成无限三维结构。最后我们用B3LYP方法研究了阴离子簇的电子结构。  相似文献   

18.
Shivaiah V  Das SK 《Inorganic chemistry》2005,44(24):8846-8854
Two Anderson-type heteropolyanion-supported copper phenanthroline complexes, [Al(OH)6Mo6O18[Cu(phen)(H2O)2]2]1+ (1c) and [Al(OH)6Mo6O18[Cu(phen)(H2O)Cl]2]1- (1a) complement their charges in one of the title compounds [Al(OH)6Mo6O18[Cu(phen)(H2O)2]2][Al(OH)6Mo6O18[Cu(phen)(H2O)Cl]2].5H2O [1c][1a].5 H2O 1. Similar charge complementarity exists in the chromium analogue, [Cr(OH)6Mo6O18[Cu(phen)(H2O)2]2][Cr(OH)6Mo6O18[Cu(phen)(H2O)Cl]2].5 H2O [2c][2a].5 H2O 2. The chloride coordination to copper centers of 1a and 2a makes the charge difference. In both compounds, the geometries around copper centers are distorted square pyramidal and those around aluminum/chromium centers are distorted octahedral. Three lattice waters, from the formation of intermolecular O-H.....O hydrogen bonds, have been shown to self-assemble into an "acyclic water trimer" in the crystals of both 1 and 2. The title compounds have been synthesized in a simple one pot aqueous wet-synthesis consisting of aluminum/chromium chloride, sodium molybdate, copper nitrate, phenanthroline, and hydrochloric acid, and characterized by elemental analyses, EDAX, IR, diffuse reflectance, EPR, TGA, and single-crystal X-ray diffraction. Both compounds crystallize in the triclinic space group P. Crystal data for 1: a = 10.7618(6), b = 15.0238(8), c = 15.6648(8) angstroms, alpha = 65.4570(10), beta = 83.4420(10), gamma = 71.3230(10), V = 2182.1(2) angstroms3. Crystal data for 2: a = 10.8867(5), b = 15.2504(7), c = 15.7022(7) angstroms, alpha = 64.9850(10), beta = 83.0430(10), gamma = 71.1570(10), V = 2235.47(18) angstroms3. In the electronic reflectance spectra, compounds 1 and 2 exhibit a broad d-d band at approximately 700 nm, which is a considerable shift with respect to the value of 650-660 nm for a square-pyramidal [Cu(phen)2L] complex, indicating the coordination of [M(OH)6Mo6O18]3- POM anions (as a ligand) to the monophenanthroline copper complexes to form POM-supported copper complexes 1c, 1a, 2c, and 2a. The ESR spectrum of compound 1 shows a typical axial signal for a Cu2+ (d9) system, and that of compound 2, containing both chromium(III) and copper(II) ions, may reveal a zero-field-splitting of the central Cr3+ ion of the Anderson anion, [Cr(OH)6Mo6O18]3-, with an intense peak for the Cu2+ ion.  相似文献   

19.
A novel compound [H2Mo5.5V10.5O40(PO4)][Cu(en)2]4*7H2O(1) was synthesized from V2O5, MoO3, CuCl2*2H2O, en, H3PO4 and H2O in an aqueous solution via the hydrothermal method and characterized by means of single-crystal X-ray diffraction, elemental analyses, IR, EPR spectra and thermal analyses. C16H80Cu4Mo5.5N16O51PV10.5 crystallized in a triclinic system, the space group is P1 with M=2660.63, a=1.283590(10) nm, b=1.289910(10) nm, c=1.387870(10) nm, V=1.80942(2) nm3, Z=2, Dx=4.883 g/cm3, F(000)=2599, μ=6.956 mm-1, (Δ/σ)=0.000, S=1.089. The crystal structure was solved by the direct methods with the final R=0.0752 and wR=0.1988 for 6311 observed reflections with I≥2σ(I). The X-ray crystallography reveals that compound 1 is a novel two-dimensional framework material constructed from the mixed Mo/V polyoxometalate and coordination groups.  相似文献   

20.
The reaction of MoO2(acac)2 with 2-amino-6-methyl-pyridine (amp) in the mixed solvent of DMF (N,N-dimethylformamide) and water affords the title complex [H-amp]4- [Mo8O26(DMF)2]·2H2O which was characterized by elemental analysis, IR spectroscopy and single-crystal X-ray diffraction analysis with the following crystallographic data: C30H54Mo8N10O30, Mr = 1802.35, monoclinic, P21/n, a = 8.631(1), b = 24.260(3), c = 13.351(2)A,β= 104.688(3)°, V = 2704.2(7) A3, Z = 2, Dc = 2.213 g/cm3, μ =1.890 mm-1 and F(000) = 1760. The final R = 0.0281 and Wr = 0.0620 for 4935 observed reflections with I > 2σ(I). X-ray structure analysis has confirmed the existence of γ-[Mo8O26]4- anion in the molecule. Eight MoO6 distorted octahedra share edges with short terminal Mo-O bonds from 1.691(3) to 1.749(2)A, medium bonds from 1.868(2) to 1.965(2) A And long bonds from 2.059(2) to 2.450(2) A. In the terminal site there exist two DMF ligands bound to the Mo atom through O atoms with the Mo-ODMF bond length of 2.166(3) A, affording a bond strength of 0.433. A three-dimensional network structure was formed through hydrogen bonds.  相似文献   

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