同多化合物[C6H5CH2NH(CH3)2]4[Mo8O26]·4H2O的合成与晶体结构

以MoO3和C6H5CH2N(CH3)2为原料,制得[C6H5CH2NH(CH3)2]4[Mo8O26]·4H2O,并通过扩散法得到无色透明晶体.X射线单晶衍射表明,晶体属三斜晶系,空间群为P墿,晶胞参数a=1.0685(2)nm,b=1.4050(3)nm,c=1.0643(2)nm,α=93.12(3)°,β=110.26(3)°,γ=71.41(3)°,V=1.4179(5)nm3,R=0.0383.     

八钼酸根阴离子有机胺化合物的合成与结构

由MoO3和(CH3)3N或(C2H5)3N反应合成了两种分子组成分别为[(CH3)3NH]4Mo8O26·2H2O(1)和[(C2H5)3NH]4Mo8O26·2H2O(2)的化合物.单晶X衍射结构分析表明,化合物(1)属三斜晶系,空间群为P1,晶胞参数a=1.0500(2)nm,b=1.0533(2)nm,c=1.0765(2)nm,α=100.21(3)°,β=101.93(3)°,γ=118.47(3)°,V=0.9698(3)nm3,R1=0.0524.化合物(2)属单斜晶系,空间群为P21,晶胞参数a=1.1512(2)nm,b=1.3097(3)nm,c=1.7610(4)nm,β=101.40(3)°,V=2.6028(9)nm3,R=0.0428.结构分析表明,两种化合物中Mo8O264-阴离子均发生畸变,有机阳离子增大,Mo-O键键长缩短,阴离子畸变增大.     

Dawson结构 [(HOCH_2CH_2)_2NH_2]_6·P_2W_(18)O_(62)·6H_2O的合成、表征、晶体结构

由二乙醇胺与H6P2W18O62·nH2O合成了[(HOCH2CH2)2NH2]6·P2W18O62·6H2O(I).单晶结构解析结果表明晶体属三方晶系,空间群为R-3,晶胞参数:a=b=c=1.36298(16)nm,α=β=γ=106.490(17)°,Z=1,V=2.1374(4)nm3,R=0.0837,Rw=0.2219.化合物分子由一个P2W18O626 阴离子、六个质子化的二乙醇胺、六个结晶水组成.标题化合物具有可逆光色性.热分析表明,化合物阴离子在463℃左右分解.     

Dawson结构α-H_6P_2W_(18)O_(62)·3(CH_3)_2NH·H_2O的合成、表征和晶体结构(英文)

由二甲胺与H6P2W18O62·nH2O合成了电荷转移化合物α H6P2W18O62·3(CH3)2NH·H2O.单晶结构解析结果表明晶体属单斜晶系,空间群为P21／c,晶胞参数:a=1.2964(3)nm,b=1.3621(3)nm,c=4.1559(8)nm,β=90.02(3)°,V=7.338(3)nm3,Z=4.标题化合物具有可逆光色性.热分析表明,化合物阴离子在430.5℃左右分解.     

含有十二元环交叉孔道的新颖亚磷酸铟[In4(HPO3)7(H2O)3](NH3CH2CH2NH3)·(H2O)的水热合成与表征

在含有HF的体系中, 用乙二胺作模板剂, 通过水热方法合成了一个新的三维亚磷酸铟[In4(HPO3)7(H2O)3](NH3CH2CH2NH3)·(H2O), 并对其进行了红外光谱、热重、ICP和CHN元素分析等表征. 单晶X射线衍射分析结果表明, 该化合物属于三方晶系, P3空间群, 晶胞参数a=1.37883(7) nm, c=0.93450(9) nm, V=1.53862(2) nm3, Z=2, Dc=2.489 Mg/m3, 最终一致性因子R1[I >2σ(I)]=0.0526, wR2[I>2σ(I)]=0.1328, GOF=1.082. 其结构中的InO6八面体、InO5(H2O)八面体和HPO3假四面体通过O原子共顶点连接, 分别沿a, b轴方向形成含有十二元环的交叉孔道, 客体水分子和双质子化的乙二胺分子存在于孔道中.     

[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.     

六亚甲基四胺锑(Ⅲ)、铋(Ⅲ)配合物的固相合成与表征

通过固相反应,合成了新的配合物六亚甲基四胺锑(Ⅲ)、铋(Ⅲ):SbCl3(C6H12N4)2·H2O(1)、BiCl3(C6H12N4)2·H2O(2).经元素分析、X 射线粉末衍射、远红外光谱和差热 热重分析进行表征,确定了配合物的组成和结构.对XRD谱指标化,确定其晶系和晶胞参数.SbCl3(C6H12N4)2·H2O(1):a=1.2490nm,b=1.4583nm,c=1.6870nm,β=91.78°,V=3.0706nm3;BiCl3(C6H12N4)2·H2O(2):a=1.3250nm,b=1.3889nm,c=1.7449nm,β=98.94°,V=3.1725nm3.     

新型层状磷酸铝[Al6P8O32][(C2H5)2NHCH2CH2NH3]2·[C2H5NH2CH2CH2NH2C2H5] 的合成、表征及其共模板作用

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.     

Dawson结构α-H6P2W18O62·3(CH3)2NH·H2O的合成、表征和晶体结构

由二甲胺与H6P2W18O62·nH2O合成了电荷转移化合物α-H6P2W18O62·3(CH3)2NH·H2O.单晶结构解析结果表明晶体属单斜晶系,空间群为P21/c,晶胞参数a=1.2964(3)nm,b=1.3621(3)nm,c=4.155 9(8)nm,β=90.02(3)°,V=7.338(3)nm3,Z=4.标题化合物具有可逆光色性.热分析表明,化合物阴离子在430.5℃左右分解.     

新型超分子化合物(H3NCH2CH2NH3)2[(HPO4)2Mo5O15]的晶体结构

首次通过水热方法合成了新型超分子化合物(H3NCH2CH2NH3)2[(HPO4)2Mo5O15]的晶体结构,并通过X衍射进行了结构表征,晶体学数据为:单斜晶系,C2/c空间群,a=1.766 6(4)nm,b=1.003 4(2)nm,c=1.376 7(3)nm,α=90°,β=96.90(3)°,γ=90°,ν=2.422 7(8)nm3,Z=4,R=0.043 1,wR2=0.128 7.     

On the icosahedral quasicrystal structure

The icosahedral quasicrystal structure is derived with local symmetry operations. Calculated Fourier transforms are compared with electron diffraction patterns. It is proposed that the structure building operations are models for the crystal growing process.     

Synthesis and Structure of a Zinc(Ⅱ)Complex:[Zn(Pybta)·Cl2]n

The title compound, [Zn(Pybta)Cl2]n (Pybta = 1-(2-pyridylmethyl)benzontriazole), has a zigzag chain structure. It crystallizes in the monoclinic system, space group P21/c with a = 9.0103(11), b = 17.0276(18), c = 9.2288(11) A, β = 101.309(6)°, Mr= 346.51, V= 1388.4(3) (A)3, Z= 4, Dc= 1.658 g/cm3, F(000) = 696, μ = 2.143 mm-1, the final R = 0.0492 and wR = 0.1236 for 2545 observed reflections with Ⅰ 2σ(Ⅰ). The Zn atom is four-coordinated by two N and two Cl atoms, forming a slightly distorted tetrahedral geometry. Each zigzag chain links its adjacent symmetry-related equivalents via multiple π-π interactions, which are not frequently observed in the previously reported architectures.     

铕与PMBP配合物晶体结构和电子结构的研究

本文测定了 Eu(PMBP) 3 · 2 H2 O的晶体结构 ,该晶体属于单斜晶系 ,空间群 P2 1 / n,a=14 .982 1(1) ,b=14 .75 18(8) ,c=2 4 .4 979(9) ,β=10 1.5 2°,Z=4 ,V=5 30 2 .2 3 ,M=10 0 1.9,Dc=1.2 5 4 g/ cm3 ,μ=12 .315 cm-1 。 Eu与 PMBP及水中的 8个氧原子形成四方反棱柱配位多面体 ,根据选用的模型计算其电子结构 ,分子能量 ,净电荷分布和 Mulliken键级 ,进而讨论了配合物的结构和化学键的特征。实　验　部　分按 Eu(Cl O4) 3 · 2 H2 O中 Eu( )与 HPMBP摩尔比 1∶ 3反应 ,得到配合物固体。置于水与无水乙醇中 ,数周后…     

Syntheses and Crystal Structures of(H_3O)(C_3H_5N_2)[Mn(OH)_6Mo_6O_(18)]·3.5H_2O and (H_3O)_3[Co(OH)_6Mo_6O_(18)]·7H_2O

1 INTRODUCTION Polyoxometalates, a rich and remarkable classof inorganic cluster system[1], exhibit diverse appli-cation possibilities due to their topological and elec-tronic properties, ranging from their well-known roleas reagents in analytical, b…     

三维网状结构聚金属氧酸盐K4SiW12O40·16H2O的合成及其X射线晶体结构分析

以钨酸钠(Na2WO4·2H2O),硅酸钠(Na2SiO3·9H2O)和氯化钾(KCl)为原料在水溶液中反应制得了标题化合物,单晶X射线结构分析表明,属单斜晶系,空间群Cc,晶胞参数a=2.0180(4),b=2.0178(4),c=1.2498(3)nm,β=90.08(3)°,V=5.0892(18)nm3,Z=4,Dc=4.290g/cm3.对5850个独立的衍射点[I>2σ(I)]进行全矩阵最小二乘法修正后,可靠性因子R1=0.0598.     

Ba14Zn5−xAl22+x: a new polar intermetallic compound with a novel 2D network

A new ternary, intermetallic compound, Ba₁₄Zn_5−xAl_22+x, was synthesized by heating the pure elements at 900°C. This compound crystallizes in the monoclinic space group I2/m, Z=2, with a=10.474(2) Å, b=6.0834(14) Å, c=34.697(8) Å and β=90.814(4)°. The crystal structure of Ba₁₄Zn_5−xAl_22+x consists of [Zn_5−xAl_22+x] slabs that are built with a novel, two-dimensional (2D) network of Zn and Al atoms involving eight-membered rings sandwiched between two layers of trigonal bipyramids interconnected by three-center bonding. Tight-binding, linear muffin-tin orbital (TB-LMTO-ASA) calculations have been performed to understand the relationship between composition and orbital interactions in the electronegative element framework. This new structure is closely related to the high-pressure, cubic Laves-type structure of BaAl₂ as well as the ambient pressure binary compound, Ba₇Al₁₃. The degree of valence electron charge transfer from the electropositive Ba atoms is related to the Al:Ba molar ratio in the Ba-Zn-Al system.     

一个新拓扑结构的镧配合物

设计并合成了1,2,5-噻二唑-3,4-二酸(tdzdc),并以其为配体与镧元素通过水热法合成了1种配合物,对其进行了元素分析及单晶衍射结构解析.单晶结构解析表明:标题配合物{[La2(tdzdc)3(H2O)]·4H2O}n为二维层状结构,属于P21空间群,三斜晶系.在该晶体结构中,只有1种配位模式的tdzdc2-配体和2种La3+离子.对于每个tdzdc2-配体,其配位结合位点被3个La3+离子占据,配体分子两侧采用羧酸和环上N原子的螯合配位模式,而配体分子下方采用2个羧酸的螯合配位模式.在空间上,由于晶体的这种连接方式,而形成了三维网络连接,当把由配体连接的3个La3+简化为三角形节点时,得到一个尚未被报道过的三维拓扑结构.在这个三维的空间网格a方向上,存在着一维的孔道,孔道中由水分子占据,当去除掉水分子后经PLATON程序计算其孔隙率为23.5%.     

A Study on Molybdenite Electronic Structure

ＡＳｔｕｄｙｏｎＭｏｌｙｂｄｅｎｉｔｅＥｌｅｃｔｒｏｎｉｃＳｔｒｕｃｔｕｒｅＬＯＮＧＸｉａｎｇ－ｙｕｎａｎｄＷＡＮＧＦｅｎｇ－ｚｈｅｎ（Ｄｅｐｔ．ｏｆＣｈｅｍ．，ＣｅｎｔｒａｌＳｏｕｔｈＵｎｉｖｅｒｓｉｔｙｏｆＴｅｃｈｎｏｌｏｇｙ，Ｃｈａｎｇｓｈａｈ...     

新磺酰脲类化合物的合成、结构及构效关系研究(Ⅵ)1—N-〔2-(4-甲基)嘧啶基〕-2-甲酸甲酯-苄基磺酰脲的晶体及分子结构

合成了标题化合物 C6H4 (CO2 CH3 ) CH2 SO2 NHCONHC4 N2 H2 CH3 (C15H16N4 O5S,Mr=36 4 .38) ,用 X-射线晶体衍射法测定了其晶体结构。它属单斜晶系 ,空间群为P2 1/ c,a=10 .2 2 0 (1) ,b=9.938(1) ,c=17.2 4 6 (2 ) ,β=10 6 .2 6 (2 )°,V=16 81.6(3) 3 ,Z=4 ,Dc=1.4 39Mg/ m3 ,μ=0 .2 2 7mm-1,F (0 0 0 ) =76 0。结构由直接法解出 ,全矩阵最小二乘法修正 ,最终偏离因子 R=0 .0 4 98,w R=0 .132 7(I>2 σ(I) ) ,独立可观测点数为 3448。分子中的嘧啶磺酰脲、苯环及酯基分别形成 3个独立的平面共轭体系。     

Syntheses and Crystal Structures of (H3O)(C3H5N2)[Mn(OH)6 Mo6O18]·3.5H2O and (H3O)3[Co(OH)6Mo6O18]·7H2O

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.