Hydrothermal Synthesis and Characterization of a Novel Organic Inorganic Hybrid Compound [Co（dien）2]（dienH3）（H3O）7[P2Mo5O23]2·14H2O

A new compound,[Co（dien）2]（dienH3）（H3O）7[P2Mo5O23]2·14H2O, has been hydrothermallly synthesized by using Na2MoO4,CoCl2, H3PO4 and dien, and structurally characterized by elemental analysis, X-ray powder diffraction analysis, SEM, IR and TG analysis. The results show that the compound is composed of a polyanion [P2Mo5O23]2^12, complex [Co（dien）2]^2＋ cation, protonated [dienH3]^3＋ , and forteen crystallization water molecule.     

[Na_2(Himi)_2(H_2O)_2](Himi)_2[P_2W_(18)O_(62)]·6H_2O的合成与晶体结构

合成了离子晶体[Na2(Himi)2(H2O)2](Himi)2[P2W18O62]·6H2O(imi=C3N2H4;Himi=C3N2H5),用X-射线单晶衍射、元素分析、红外光谱和热重对晶体的结构进行了表征.该晶体属于三斜晶系,P1=空间群,a=1.41164(10)nm,b=1.48792(11)nm,c=2.26166(17)nm,α=72.1320(10)°,β=81.334 0(10)°,γ=62.580 0(10)°,V=4.013(5)nm3,Z=2,F(000)=4 144,R1=0.009 55,wR2=0.187 2.在该晶体结构中,带相反电荷的多阴离子簇、质子化的咪唑分子、Na+和水分子在分子中交替排列,通过离子键及抗衡阳离子间的弱配位键连接形成了具有一维链状结构.     

[H_2N(CH_2CH_2)_2O]_3[Cr(OH)_6Mo_6O_(18)]·6H_2O的合成及晶体结构

应用常温水溶液方法,合成了1个吗啉分子为抗衡阳离子的多酸化合物[H2N(CH2CH2)2O]3[Cr(OH)6Mo6O18]·6H2O,用X-射线单晶衍射、元素分析、红外光谱和热重对晶体结构进行了表征.该晶体属于三斜晶系,P-1空间群,a=0.793 85(6)nm,b=1.370 67(11)nm,c=1.984 58(16)nm,α=70.037 0°,β=80.392 0(10)°,γ=77.229 0(10)°,V=1.969 6(3)nm3,Z=2,R1=0.068 3,wR2=0.193 4.在该晶体结构中,Anderson结构多阴离子簇、抗衡阳离子吗啉阳离子以静电引力结合,并交错排列.     

化合物[Cu(bipy)(SiMo_(12)O_(40))_0.5](H_2bipy)_(0.5)·H_2O的合成、结构及电化学性质

采用水热法合成了一个基于Keggin型多金属氧酸盐的新型杂化物[Cu(bipy)(SiMo12O40)0.5](H2bipy)0.5·H2O(1).用元素分析、红外光谱和X-射线单晶衍射对化合物1的结构进行了表征.结构解析表明,化合物1属于三斜晶系,p-1空间群,晶胞参数a=1.084 85(6)nm,b=1.179 30(7)nm,c=1.328 96(8)nm,α=105.328(5)°,β=102.773(5)°,γ=114.872(6)°,V=1.376 21(14)nm3,Z=2,R1=0.047 9,ωR2=0.116 0.该化合物具有梯形的一维链状结构.此外还对对化合物1的电化学性质进行了研究.     

配位聚合物{[Cu(C_(10)H_2O_8)(C_3H_4N_2)_2(H_2O)_2][Cu(C_3H_4N_2)_4(H_2O)_2]·2H_2O}_n的合成与晶体结构

利用水热技术合成了配位聚合物{[Cu(C10H2O8)(C3H4N2)2(H2O)2][Cu(C3H4N2)4(H2O)2]22H2O}n(1),用X-射线单晶衍射及元素分析对晶体结构进行了表征.该晶体属于三斜晶系,P-1空间群,a=9.995(2),b=10.643(2),c=11.111(2),α=115.52(3)°,β=91.40(3)°,γ=111.69(3)°,V=967.0(3)3,Z=1,F(000)=480,S=1.015,R1=0.040 0,wR2=0.101 2[I>2σ(I)].CCDC:865259     

单核铁(Ⅲ)配合物[Fe(hmb)_2(N_3)(H_2O)]的合成及其晶体结构

利用3-甲氧基水杨醛、叠氮化钠与六水合氯化铁在室温下合成了一个新型单核铁配合物[Fe(hmb)2(N3)(H2O)],对其进行了X射线单晶衍射仪、元素分析测试。该配合物属于三斜晶系,P1空间群。晶胞参数:a=0.856 03(8)nm,b=0.958 54(9)nm,c=1.112 74(9)nm,α=78.957(7)°,β=87.317(7)°,γ=80.061(8)°。中心铁离子以六配位的模式与氧原子、氮原子连接形成八面体的构型,配合物分子首先通过C—H…N氢键连接成一维链状结构,进一步通过π…π共轭和氢键作用构成三维空间结构。     

三核镍配合物[Ni_3(Htrz)_6(H_2O)_6](SO_4)_3·8H_2O的合成与晶体结构

用常规水溶液法合成了三核配合物[Ni3(Htrz)6(H2O)6](SO4)3.8H2O(1),其中Htrz=1,2,4-1H-三氮唑.用X-射线单晶衍射、元素分析、红外光谱、热重分析对晶体结构进行了表征.该晶体属于三斜晶系,P-1空间群,a=11.802(2),b=12.120(3),c=18.663(4),α=71.28(0)°,β=86.66(0)°,γ=62.04(0)°,V=2 219.5(8)3,Z=2,F(000)=1 666,R1=0.1217,wR2=0.360 0.CCDC:831634     

[H_2N(CH_2CH_2)_2O]_2[NiMo_6O_(24)H_6(NaO_2)_2]·2H_2O的合成及晶体结构

合成了有机-无机杂化化合物[H_2N(CH_2CH_2)_2O]_2[Ni Mo6O_(24)H6(Na O_2)_2]·_2H_2O,对晶体进行了X-射线单晶衍射和红外光谱测试和解析;应用元素分析、紫外光谱和热重对晶体进行了性质表征.该晶体属于单斜晶系,Pc空间群,a=0.69799(5)nm,b=1.42_210(9)nm,c=1.563_27(10)nm,α=90°,β=98.4140(10)°,γ=90°,V=1.535(18)nm~3,Z=2,R1=0.0396,wR_2=0.091.在该晶体结构中,带相反电荷的Anderson结构多阴离子簇、抗衡阳离子Na+和吗啉阳离子以静电引力结合,并交错排列.     

Synthesis and Characterization of (PEO)_x~-(V_(0.85)Mo_ (0.15)_2O_5 Nanocomposite Films

1　IntroductionSomeinorganiclayeredcompounds ,suchasMoO3 andV2 O5,belongtoarapidlygrowingfieldofcontempo raryresearchinterest,becausetheycanbeintercalatedbyavarietyofalkaliions (Li+ ,Na+ ,etc .) ,atomsorlargermoleculestoformintercalationhost guestcompounds ,whichareexpectedtobepromisingcandidatematerialsforcathodesofsecondaryLibatteriesandelectrochromicdevices[1] .Polymer layeredoxidenanocompositesareat tractingmuchattentionduetotheirspecialstructureaswellassuperiorelectrical,electrochemical…     

Thermal Hydrolysis Synthesis and Characterization of Monoclinic Metahewettite CaV_6O_(16)·3H_2O

Monoclinic metahewettite CaV 6 O 16 ·3H 2 O has been fabricated via thermal hydrolysis of calcium vanadate(Ca 10 V 6 O 25). High purity calcium vanadate precipitate, featuring column structure with surface area of 8.61 m2/g, can be obtained by reacting sodium orthovanadate(Na 3 VO 4) with calcium oxide at 90 ℃ for 2 h. By acidifi cation of calcium vanadate in hot water at pH of 1.0-3.0, the monoclinic metahewettite crystals with uniform particle distribution, layered structure and nonporous structure can be fabricated. With the well crystallized layered structure, CaV 6 O 16 ·3H 2 O may be a potential cathode material for secondary batteries as well as super capacitor materials.     

配位聚合物[Nd_2(pyip)(ox)_(2.5)(H_2O)_5]_n的合成及晶体结构研究

在水热条件下,以5-(4-吡啶基)间苯二甲酸(H2pyip)和草酸阴离子为混合的桥连配体与Nd2O3反应得到无色块状晶体.通过单晶X射线衍射、元素分析、红外分析、热重分析和粉末衍射对该配位聚合物进行表征.通过单晶X射线衍射分析可知:该配位聚合物属于单斜晶系,P21/c空间群.在结构中存在由平行四边形的次级结构单元构筑的二维稀土草酸层,相邻的稀土草酸层进一步通过pyip2-桥连形成三维框架结构.     

吗啉修饰的硅钨酸盐化合物[H_2N(CH_2CH_2)_2O]_4[SiW_(12)O_(40)]·4H_2O的合成、晶体结构及电催化性质研究

应用一步合成方法,合成了一种吗啉为抗衡阳离子的硅钨酸盐化合物[H_2N(CH_2CH_2)_2O]_4[SiW_(12)O_(40)]·4H_2O,通过元素分析、X-射线单晶衍射、红外光谱、紫外光谱和热重对晶体进行了表征.该化合物晶体属于单斜晶系,P21/C空间群,a=1.027 3(3)nm,b=4.402 8(14)nm,c=1.230 0(4)nm,β=112.943(9)°,V=5.211(3)nm3,Z=4.电化学实验证明,该硅钨酸盐化合物在水溶液中对NO-2具有良好的电催化活性.     

新型硫/氧钼配合物(Et_4N)_2[MoO(S_4)(bdtX_2)]和(Et_4N)_2[Mo_2O_2(m_2-S)_2(bdtX_2)]的合成及晶体结构（英文）

在乙腈中,用摩尔比为1∶1的1,2-苯二硫醇(H_2bdt)或3,6-二氯-1,2-苯二硫醇(H_2bdtCl_2)与(Et_4N)_2[MoIVO(S_4)_2]进行取代反应,得到单硫烯钼(IV)氧化合物(Et_4N)_2[MoO(S_4)(bdt X_2)](X=H,1;X=Cl,2)。在热的乙腈中,用摩尔比为1∶1的1,2-芳二硫醇继续与化合物1和2反应,得到双硫桥联的双核钼(V)化合物(Et4N)2[Mo_2O_2(m_2-S)_2(bdt X_2)_2](X=H,3;X=Cl,4)。通过UV-3000紫外分光光度计对这四种配合物进行谱学表征,并采用X射线单晶衍射仪对其中配合物2,3和4的结构进一步测定,结果表明:在化合物3和4结构中,端氧的位置处于Mo_2S_2平面的同侧,为顺式构型。     

Crystal Growth of[Ca_3Al(OH)_6?12H_2O]_2·(SO_4)_3?2H_2O (Ettringite) Studied Under Microgravity Conditions

On parabolic flights,the growth of ettringite,[Ca_3Al(OH)_6·12H_2O]2·(SO_4)_3·2H_2O,a major reaction product of cement with water which forms instantaneously,was crystallized under microgravity conditions and studied.In the experiments,Ca(OH)_2/Al_2(SO_4)_3 solutions were combined and reacted for 10?s,followed by immediate filtration of the suspension and subsequent quenching with acetone.For the ettringite crystals,the size,aspect ratios,quantity and morphology were determined and the results were compared with those from identical experiments performed under terrestric gravity.Under microgravity,generally smaller crystals (l-2.9 μm) precipitated in larger amount than under normal gravity (l-3.5 μm).The aspect ratios of the crystals grown under terrestric or microgravity condition were comparable at about 5.6.It is assumed that the reason for the smaller ettringite crystals is the absence of convection leading to more initial nuclei,but slower crystal growth which is diffusion limited.Apparently,no preference relative to the ion transport to the different faces of the crystals exists.The results contribute to the understanding of the mineralization of inorganic salts under microgravity conditions for which hitherto only a handful of examples were reported.     

K(H_2O)_6Al(H_2O)_6(SO_4)_2和K(C_4H_5O_6)(C_4H_5O_6=D,L-酒石酸)的结构:钾离子和氧原子之间成键研究(英文)

利用水合硫酸铝在氢氧化钾存在的条件下在水中发生共晶作用得到无色块状的配合物K(H2O)6Al(H2O)6(SO4)2晶体,其中钾离子(K+)形成KO6八面体的配位几何构型。将D,L-酒石酸和相同当量的KOH反应生成配合物K(C4H5O6)(C4H5O6=D,L-酒石酸),其中K+以KO8多面体的形式被8个氧原子围绕形成一个扭曲的立方体形式。     

[N(CH_2CH_2CH_2CH_3)_4]_3[AsMo_(12)O_(40)]的合成、晶体结构及磁性研究

合成了有机无机杂化化合物[N(CH2CH2CH2CH3)4]3[AsMo12O40],用X-射线单晶衍射、元素分析、红外光谱和变温磁化率对晶体结构进行了表征.该晶体属于单斜晶系,Pc空间群,a=1.416 48(14)nm,b=1.753 25(17)nm,c=2.280 7(2)nm,β=101.626(2)°,V=5 547.9(9)nm3,Z=2,R1=0.076 5,wR2=0.240 9.在该晶体结构中,带相反电荷的Keggin结构多阴离子[AsMo12 O40]3-簇和四丁基胺阳离子以静电引力结合,并交错排列.     

鱼骨状一维链结构配位聚合物Cu(C_(10)H_(14)N_4)(C_7H_4O_3)_2·3H_2O的合成与晶体结构

采用常规水溶液法合成了一个结构新颖的配位聚合物Cu(C_(10)H_(14)N_4)(C_7H_4O_3)_2·3H_2O(1)(C10H14N4=1,1'-(1,4-丁基)双咪唑(bbi);C7H4O3=对羟基苯甲酸),用X-射线单晶衍射、红外光谱、元素分析和X射线粉末衍射对晶体结构进行了表征.该晶体属于单斜晶系,R-3c空间群,a=20.614(19),b=12.349(11),c=12.003(11),α=90°,β=116.840(14)°,γ=90°,V=2 726(4)3,Z=4,F(000)=1 892,S=1.054,R1=0.1044,wR2=0.206 2[I2σ(I)].     

三维孔状配位聚合物:[(H_2O)_2Co(VO_3)_2]的水热合成与晶体结构(英文)

采用水热合成法制备了一个孔状的无机混合金属钒-钴化合物[(H2O)2Co(VO3)2](1),通过单晶X-射线衍射分析对该配合物进行结构表征。化合物晶体属于六方晶系,Pnma空间群。晶胞参数:a=5.5647(1),b=10.6877(1),c=11.8514(1),V=704.848(15)3,Z=4,Mr=292.84,Dc=2.760g/cm3,μ(MoKα)=4.922mm-1,F(000)=564,S=1.072,R=0.0131,wR=0.332[I2σ(I)]。配合物1由共享角的VO4四面体链组成,它通过钴-氧共价作用结合配合物阳离子[Co(H2O)2]2+部分形成了一个三维网状结构。     

RE(Met)_4(NO_3)_3·4H_2O的熔化焓

本文在水相中合成了11种稀土硝酸盐与蛋氨酸的配合物,其通式为RE(Met)_4(NO_3)_3·4H_2O(RE=La,Ce,Pr,Nd,Sm,Eu,Gd,Tb,Dy,Er,Y:Met=D—L—Methionine),利用DSC技术测得了它们的熔化焓和熔点。     

纳米(CeO_2)_(0.86)(Sm_2O_3)_(0.14)的形貌控制与表征

以Ce(NO3)3.6H2O和(NH4)2CO3为沉淀源,搀杂稀土氧化物Sm2O3,利用柠檬酸作为络合剂和分散剂,制备出纳米(CeO2)0.86(Sm2O3)0.14.并采用TEM、XRD等方法对其热分解所得纳米(CeO2)0.86(Sm2O3)0.14的形貌及结晶性等进行了表征.结果表明:随着柠檬酸加入量的增加,焙烧生成的纳米(CeO2)0.86(Sm2O3)0.14颗粒的形貌从纳米线向类球形颗粒变化,所得(CeO2)0.86(Sm2O3)0.14为立方萤石结构,且随焙烧温度的提高,晶化程度增大.