Zn(Ⅱ),Cd(Ⅱ)与混合配体构筑三维贯穿金属有机配位聚合物的合成、结构与荧光性能

在中温混合溶剂热条件下, 分别用锌离子和镉离子与二羧酸和二吡啶基配体反应合成出2个新颖的金属有机配位聚合物[Zn(BPDC)(BPE)·(DMF)₂](JUC-91)和[Cd(BPDC)(BPE)·(DMF)₂](JUC-92)[BP-DC:4,4'-联苯二羧酸,BPE:反式1,2-二(4-吡啶基)乙烯,DMF:N,N'-二甲基甲酰胺], 并通过X射线单晶衍射、 元素分析、 热重分析、 粉末X射线衍射、 拓扑结构分析和荧光光谱对化合物的结构、 组成和性质进行了表征. X射线单晶衍射结果表明, 化合物JUC-91和JUC-92均具有三维开放骨架结构, 其中, JUC-91具有五重贯穿的金刚石拓扑结构, JUC-92具有双重贯穿的简单立方格子结构.     

基于3,4′，5-联苯三羧酸构筑的钕配合物的合成、结构、荧光、光催化及磁性质（英文）

采用NdCl_3·6H_2O和3,4′,5-联苯三羧酸(H3bpt)为原料在DMF/H_2O混合溶剂热条件下合成得到一个三维钕配合物{[Nd(bpt)(DMF)(H_2O)]·2H_2O}_n (1),并通过红外光谱、元素分析、单晶及粉末X射线衍射表征了配合物1的结构。单晶衍射结果表明,配合物1具有(5,5)-连接的三维结构,拓扑符号为(44·63·83)(4862)。此外,对配合物1的热稳定性、荧光性质、光催化降解染料及磁性质进行了详细研究。     

含烟碱配体的一维链状Cd(Ⅱ)配聚物的合成、晶体结构及其荧光性质

以氯化镉、烟碱(Nicotine)为原料在N,N-二甲基甲酰胺(DMF)溶液中反应,合成了1个新的一维链状Cd髤配聚物[Cd3(μ-Cl)6(Nicotine)2(DMF)2(H2O)2]n,用红外光谱、粉末X衍射、X-射线单晶衍射和热重分析对配合物进行了表征。X-射线单晶衍射表明,配合物属单斜晶系,空间群P21,晶胞参数:a=0.998 02(19)nm,b=1.836 89(15)nm,c=1.082 6(2)nm,β=95.809(3)°,V=1.974 5(5)nm3,Z=2,μ(Mo Kα)=2.045 mm-1,F(000)=1 044.0,R1=0.049 9,wR2=0.118 8[Ⅰ>2σ(Ⅰ)]。配合物中镉离子位于扭曲的配位八面体中心,相邻镉离子通过2个氯离子桥连形成了一维链结构,Nicotine、DMF、H2O占据配位八面体的剩余配位点,配聚物一维链平行于a轴。室温固态荧光测试显示,配聚物在448.5、573 nm处具有强的荧光发射。     

三角柔性多羧酸金属有机骨架化合物的合成、结构及荧光性质（英文）

以柔性1,3,5-三(4-羧酸苯氧基)苯(H3TCPB)为配体,以4,4′-联吡啶(4,4′-BPY)为辅助配体,在溶剂热条件下合成了2个新颖的分别具有三核锌簇和三核钴簇的金属有机骨架化合物:{[Zn3(TCPB)2(4,4′-BPY)]·DMF·3H2O}n(1)和{[Co1.5(TCPB)(DMF)(H2O)]·DMF}n(2),通过单晶X射线衍射,红外光谱,元素分析,热重分析和粉末X射线衍射对其结构进行了表征。单晶X射线衍射分析表明化合物1属于三斜晶系,P1空间群,表现出三维(3,8)连接的网状结构,拓扑符号为:{43}2·{46·618·84}·{6};化合物2也属于三斜晶系,P1空间群,为二维(3,6)连接的网络层状结构,拓扑符号为:{43}4·{46·618·84}。此外,荧光性质研究表明固态化合物1在室温条件下发射出源于TCPB3-和4,4′-BPY配体的淡蓝色荧光,而化合物2在相似的条件下没有荧光发射。     

两个基于双(4-吡啶-4-苯基)胺的钴(Ⅱ)、锌(Ⅱ)配合物的合成和晶体结构

以双(4-吡啶-4-苯基)胺(BPPA)和4,4-(六氟)双(苯甲酸)(H2hfipbb)或对苯二甲酸(p-H2bdc)为配体,采用溶剂热法与M(NO3)2·6H2O(M=Co、Zn)组装合成了2个新的配合物{[Co2(BPPA)(hfipbb)2·(H2O)3]·6H2O}n(1)、{[Zn2(BPPA)2(p-bdc)2]·H2O·DMF}n(2),利用元素分析、X射线粉末衍射(PXRD)、红外光谱等手段分别对它们进行了表征,并用X射线单晶衍射仪测定了配合物的单晶结构。X射线单晶衍射测定结果表明:配合物1和2均为二维结构。配合物1具有新的拓扑结构。配合物2的二维结构又可以组成三维框架结构。配合物1为正交晶系,Pnna空间群,a=2.640 9(2)nm,b=1.715 78(13)nm,c=1.504 11(11)nm,V=6.8154(9)nm3,Z=4,μ=0.571 mm-1,F(000)=2 592,Dc=1.245 g·cm-3,Mr=1 383.76,R1=0.066 6,w R2=0.208 9(I>2σ(I));配合物2为单斜晶系,C2/c空间群,a=2.796 70(9)nm,b=1.814 82(6)nm,c=2.303 13(7)nm,β=102.136 0(10)°,V=11.428 3(6)nm3,Z=8,μ=0.906 mm-1,F(000)=4 944,Dc=1.391 g·cm-3,Mr=1 196.85,R1=0.039 8,w R2=0.106 4(I>2σ(I))。此外,热重分析表明配合物1和2均具有良好的热稳定性。     

两个基于双(4-吡啶-4-苯基)胺的钴(Ⅱ)、锌(Ⅱ)配合物的合成和晶体结构（英文）

以双(4-吡啶-4-苯基)胺(BPPA)和4,4-(六氟)双(苯甲酸)(H2hfipbb)或对苯二甲酸(p-H2bdc)为配体,采用溶剂热法与M(NO3)2·6H2O(M=Co、Zn)组装合成了2个新的配合物{[Co2(BPPA)(hfipbb)2·(H2O)3]·6H2O}n(1)、{[Zn2(BPPA)2(p-bdc)2]·H2O·DMF}n(2),利用元素分析、X射线粉末衍射(PXRD)、红外光谱等手段分别对它们进行了表征,并用X射线单晶衍射仪测定了配合物的单晶结构。X射线单晶衍射测定结果表明:配合物1和2均为二维结构。配合物1具有新的拓扑结构。配合物2的二维结构又可以组成三维框架结构。配合物1为正交晶系,Pnna空间群,a=2.640 9(2)nm,b=1.715 78(13)nm,c=1.504 11(11)nm,V=6.8154(9)nm3,Z=4,μ=0.571 mm-1,F(000)=2 592,Dc=1.245 g·cm-3,Mr=1 383.76,R1=0.066 6,w R2=0.208 9(I2σ(I));配合物2为单斜晶系,C2/c空间群,a=2.796 70(9)nm,b=1.814 82(6)nm,c=2.303 13(7)nm,β=102.136 0(10)°,V=11.428 3(6)nm3,Z=8,μ=0.906 mm-1,F(000)=4 944,Dc=1.391 g·cm-3,Mr=1 196.85,R1=0.039 8,w R2=0.106 4(I2σ(I))。此外,热重分析表明配合物1和2均具有良好的热稳定性。     

一维Z形链状吡啶三唑-Zn(Ⅱ)化合物的合成、晶体结构及荧光性能

通过水热法成功合成了一例一维"Z"形链状结构的化合物[(4,3′-Hbpt)_2Zn(adp)]_n(1)(4,3′-Hbpt=3-(4-吡啶基)-5-(3-吡啶基)-1-H-1,2,4-三唑;adp=己二酸离子)),并通过X射线单晶衍射、元素分析、X射线粉末衍射和荧光光谱等方法对该化合物进行了结构表征和性质研究.X射线单晶衍射分析表明,化合物1属于单斜晶系,C2/c空间群,晶胞参数为a=1.938 8 nm,b=0.877 6 nm,c=1.844 1 nm,α=90°,β=109.1°,γ=90°,V=2.965 0 nm~3,D_c=1.470 g/cm~3,Z=4,F(000)=1 352,GOOF=0.957.在化合物1中,Zn~(2+)离子通过己二酸桥接形成一维"Z"形链状结构.此外,通过荧光光谱对化合物1的荧光性质进行了研究.     

配合物Zn(C3H4N2)2(C8H6O2Br)2的水热合成、晶体结构及性质

在140℃下,以3-溴-4-甲基苯甲酸和咪唑为配体,通过水热法在甲醇/水混合溶剂中反应24 h合成了锌(Ⅱ)配合物Zn(C3H4N2)2(C8H6O2Br)2。通过元素分析、红外光谱、热重分析和X射线粉末衍射对配合物进行了结构表征,同时用X射线单晶衍射分析确定了其晶体结构。结果表明,其晶体属单斜晶系,空间群为C2/c,晶胞参数:a=13.257(3),b=9.765(2),c=20.494(4),β=107.79(3)°,V=2526.3(9)3,Dc=1.655g·cm-3,μ=4.170mm-1,F(000)=1248,Z=4,最终残差因子R1=0.0552,wR2=0.1378。配合物为单核结构,中心锌(Ⅱ)离子与来自2个3-溴-4-甲基苯甲酸根的2个O原子及2个咪唑分子的2个N原子配位,形成了畸变的四方锥几何体。晶体内,分子间则通过N—H…O氢键作用在ab面形成了层状结构。研究了配合物的发光性质。     

以5-甲基-3-吡唑甲酸为配体构建的具有六方孔道的钴(Ⅱ)、镍(Ⅱ)超分子化合物：合成、晶体结构和性质

利用5-甲基-3-吡唑甲酸,分别与CoCl2·6H2O和Ni(NO3)2·6H2O反应,得到了配合物[M(MPA)2(H2O)2](1:M=Co;2:M=Ni)(HMPA=5-甲基-3-吡唑甲酸)。用元素分析、红外光谱、X-单晶衍射结构分析对其进行了表征。配合物1和2的晶体结构参数如下:配合物1和2的晶体都属于六方晶系,空间群为R3c。配合物1的晶胞参数为a=1.483 94(4)nm,b=1.483 94(4)nm,c=3.207 66(6)nm,V=6.117 2(3)nm3,Z=18;配合物2的晶胞参数为a=1.466 53(14)nm,b=1.466 53(14)nm,c=3.243 0(6)nm,V=6.04 03(14)nm3,Z=18。金属离子与来自2个5-甲基-3-吡唑甲酸配体中的2个氮原子及2个氧原子,2个水分子中的2个氧原子配位,形成八面体配位构型。配合物中的独立结构单元[M(MPA)2(H2O)2]通过分子间氢键形成具有六方孔道的三维结构。热重分析表明配合物1和2具有较高的热稳定性。此外,考察了配合物1和2的荧光和电化学性质。CCDC:900677,1;900678,2。     

以[α-P2W18O62]6-阴离子为构筑块的一维链状稀土配位聚合物[Nd(DMF)6(H2O)2][Nd(DMF)6(H2O)]P2W18O62的合成﹑结构及性质研究

以Nd2O3,DMF和α-H6P2W18O62·nH2O等为原料合成了Dawson结构杂多阴离子有机-无机配位聚合物[Nd(DMF)6(H2O)2][Nd(DMF)6(H2O)]P2W18O62,并对其进行了IR,UV光谱表征及电化学性质研究.X-射线衍射单晶结构分析结果表明,晶体属单斜晶系,Cc空间群,晶胞参数a1.8991(3)nm,b=2.2047(3)nm,c=2.6448(4)nm,β=102.272(3)°,并有Z=4,R1=0.043 8,wR2=0.1107.聚合物中存在2种构型的Nd配离子,Nd(1)以九配位的三加冠三棱柱结构通过端氧与[P2W18O62]6-阴离子赤道位的W相连,Nd(2)以九配位畸变的单加冠四方反棱柱结构通过端氧与[P2W18O62]6-阴离子极位的W相连,从而构成分子结构单元[{Nd(DMF)6(H2O)2}{Nd(DMF)6(H2O)}(P2W18O62)],毗邻的结构单元又通过W-O-Nd(1)-O-W桥联形成一维锯齿无限链状结构.     

Molecular precursors for ferroelectric materials: synthesis and characterization of Bi2M2(mu-O)(sal)4(Hsal)4(OEt)2 and BiM4(mu-O)4(sal)4(Hsal)3(O(i)Pr)4 (sal = O2CC6H4O,Hsal = O2CC6H4OH) (M = Nb,Ta)

Reactions between triphenyl bismuth, salicylic acid, and niobium or tantalum ethoxide have been explored. Four new coordination complexes incorporating bismuth and the group 5 metals niobium or tantalum have been synthesized and characterized spectroscopically, by elemental analysis, and by single crystal X-ray diffraction. The new complexes are Bi(2)M(2)(mu-O)(sal)(4)(Hsal)(4)(OEt)(2) (1a, M = Nb; 1b, M = Ta) and BiM(4)(mu-O)(4)(sal)(4)(Hsal)(3)(O(i)Pr)(4) (sal = O(2)CC(6)H(4)-2-O, Hsal = O(2)CC(6)H(4)-2-OH) (2a, M = Nb; 2b, M = Ta). Complexes 1a and 1b are isomorphous, as are 2a and 2b. The thermal and hydrolytic decomposition of 1a has been explored by DT/TGA and powder X-ray diffraction, while scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX) were used to characterize the morphology and composition of the oxides. The heterobimetallic molecules are completely converted to the amorphous bimetallic oxide by heating to 500 degrees C in air. Decomposition of 1a or 1b at 650 degrees C produces the metastable high temperature form of BiNbO(4) as the major crystalline oxide phase. Heating samples of 1a to 850 degrees C favors conversion of the materials to the low temperature phase as well as disproportionation into Bi(5)Nb(3)O(15) and Nb(2)O(5). Thermal decomposition of 1a and 1b produces porous oxides, while hydrolytic decomposition of the complexes has been shown to produce nanometer scale bimetallic oxide particles. The potential of the complexes to act as single-source precursors for ferroelectric materials is considered.     

三维无机-有机杂化骨架微孔材料──[Co3(BTC)(HBTC)(H2BTC)(C2H4O2)3]·3(DMF)·6(H3O)的合成与结构

沸石和分子筛微孔晶体材料是指以硅酸盐、硅铝酸盐、磷铝酸盐和无机金属磷酸盐为骨架的晶体材料[1,2 ] .最近 ,Yaghi,Williams,Zaworotko,Kitagawa和游效曾等 [3～ 11] 利用刚性和热稳定性较好的有机分子 (如芳香多酸和多碱 )和金属离子作为结构单元 ,制备出了新型无机 -有机杂     

Distinct Hydrogen-bonded MII(H2O)8 Clusters as Second Building Units for 1-D, 2-D and 3-D Supramolecular Architectures (M = Cobalt and Nickel)

Two mononuclear metal-organic complexes, [Co(Hmpdc)2(H2O)4]·4H2O 1 and [Ni(Hfmpdc)2(H2O)4]·6H2O 2, were prepared from 2,6-dimethylpyridine-3,5-dicarboxylic acid (H2mpdc) and 4-furyl-2,6-dimethylpyridine-3,5-dicarboxylic acid (H2fmpdc) with M(NO3)2 salts, respectively, and characterized by single-crystal X-ray diffraction, elemental analyses, IR spectroscopy, and photoluminescent measurement. Complex 1 crystallizes in triclinic, space group P with a = 7.634(5), b = 8.695(5), c = 10.757(6)(A), α = 69.647(7), β = 69.957(8), γ = 83.733(7)°, V = 628.9(7)(A)3, Dc = 1. 561 g/cm3, μ(MoKα) = 0.763 mm-1, F(000) = 309, Z = 1, the final R = 0.0553 and wR = 0.1469 for 1909 observed reflections (I > 2σ(I)). Complex 2 crystallizes in monoclinic, space group P21/n with a = 9.5934(16), b = 12.422(2), c = 14.826(3)(A), β = 105.201(2)°, V = 1705.0(5)(A)3, Dc = 1. 479 g/cm3, μ(MoKα) = 0.655 mm-1, F(000) = 796, Z = 2, the final R = 0.0351 and wR = 0.0889 for 2387 observed reflections (I > 2σ(I)). In the crystal structures of 1 and 2, diverse supramolecular motifs from 1-D chains/ladders to 3-D networks are constructed from corresponding distinct [MⅡ(H2O)8] ion clusters as the second building units, respectively. The solid state compounds of 1 and 2 show similar photoluminescent spectra with emission maximum at ca. 466 nm at room temperature.     

一种新的三维超分子化合物[Ni(H2O)6(fum)]·2(hmt)·4H2O的合成和晶体结构(fum=反丁烯二酸根；hmt=六次甲基四胺)

The synthesis of nickel supramolecular compound with hexamethylenetetramine and fumarate ligands is reported. The compound [Ni(H₂O)₆(fum)]·2(hmt)·4H₂O (1) (fum=fumarate; hmt=hexamethylenetetramine) were characterized by elemental analysis, crystal structure, IR. Compound 1 crystallizes in the triclinic system, space group P1, and with Z=1. Cell parameters: a=0. 934 6(1), b=0.933 8(1), c=0.938 8(2) nm, α=79.46(1)°, β=77.84(1)°, γ=61.29 6(7)°. Every metal ion has a octahedral coordination geometry formed by six oxygen atoms from six water molecules, and the relative independent components [Ni(H₂O)₆]²⁺, fumarate anions, hmt and H₂O molecules are linked together by two kinds of hydrogen bonds (O-H…O, and O-H…N) to form a three-dimensional structure. CCDC: 256355.     

Cd3(H2O)3((O3PCH2)2NH-CH2C6H4-COOH)2].11H2O: a layered cadmium phosphonate with reversible dehydration/hydration properties

In a recent systematic study on the influence of the reaction temperature on the structure formation in the system CdCl2/H(HO3PCH2)2NH-CH2C6H4-COOH (H5L) /NaOH, [Cd3(H2O)3((O3PCH2)2NH-CH2C6H4-COOH)2].11H2O was obtained as a microcrystalline compound. We have now been able to elucidate the structure from single-crystal data: triclinic, P; a=5.4503(9), b=12.880(2), and c=16.417(3) A; alpha=67.841(6) degrees, beta=80.633(6) degrees, gamma=87.688(8) degrees, V=1052.9(3) A3; Z=1; R1=0.1143, R2=0.2108 (all data); 0.0705, 0.1823 ((I>2sigmaI)). The structure of [Cd3(H2O)3((O3PCH2)2NH-CH2C6H4-COOH)2].11H2O is built up of cadmium phosphonate layers connected by water-mediated hydrogen bonds between aryl-carboxylic acid groups and water molecules coordinated to Cd2+ ions of adjacent layers (C-OH...H2O...H2O-Cd2+). The title compound was characterized by IR spectroscopy and energy dispersive X-ray, elemental, and thermogravimetric analyses. Furthermore, temperature-dependent X-ray diffraction data are presented. [Cd3(H2O)3((O3PCH2)2NH-CH2C6H4-COOH)2].11H2O can be reversibly dehydrated, and mechanical stress and grinding in the presence of water leads to the intercalation of additional water molecules.     

Polyoxometalate-supported transition metal complexes and their charge complementarity: synthesis and characterization of [M(OH)6Mo6O18[Cu(Phen)(H2O)2]2][M(OH)6Mo6O18[Cu(Phen)(H2O)Cl]2].5H2O (M = Al(+, Cr3+)

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.     

Synthesis, characterization and magnetic properties of four new organically templated metal sulfates [C5H14N2][M(II)(H2O)6](SO4)2, (M(II) = Mn, Fe, Co, Ni)

A series of novel organically templated metal sulfates, [C(5)H(14)N(2)][M(II)(H(2)O)(6)](SO(4))(2) with (M(II) = Mn (1), Fe (2), Co (3) and Ni (4)), have been successfully synthesized by slow evaporation and characterized by single-crystal X-ray diffraction as well as with infrared spectroscopy, thermogravimetric analysis and magnetic measurements. All compounds were prepared using a racemic source of the 2-methylpiperazine and they crystallized in the monoclinic systems, P2(1)/n for (1, 3) and P2(1)/c for (2,4). Crystal data are as follows: [C(5)H(14)N(2)][Mn(H(2)O)(6)](SO(4))(2), a = 6.6385(10) ?, b = 11.0448(2) ?, c = 12.6418(2) ?, β = 101.903(10)°, V = 906.98(3) ?(3), Z = 2; [C(5)H(14)N(2)][Fe(H(2)O)(6)](SO(4))(2), a = 10.9273(2) ?, b = 7.8620(10) ?, c = 11.7845(3) ?, β = 116.733(10)°, V = 904.20(3) ?(3), Z = 2; [C(5)H(14)N(2)][Co(H(2)O)(6)](SO(4))(2), a = 6.5710(2) ?, b = 10.9078(3) ?, c = 12.5518(3) ?, β = 101.547(2)°, V = 881.44(4) ?(3), Z = 2; [C(5)H(14)N(2)][Ni(H(2)O)(6)](SO(4))(2), a = 10.8328(2) ?, b = 7.8443(10) ?, c = 11.6790(2) ?, β = 116.826(10)°, V = 885.63(2) ?(3), Z = 2. The three-dimensional structure networks for these compounds consist of isolated [M(II)(H(2)O)(6)](2+) and [C(5)H(14)N(2)](2+) cations and (SO(4))(2-) anions linked by hydrogen-bonds only. The use of racemic 2-methylpiperazine results in crystallographic disorder of the amines and creation of inversion centers. The magnetic measurements indicate that the Mn complex (1) is paramagnetic, while compounds 2, 3 and 4, (M(II) = Fe, Co, Ni respectively) exhibit single ion anisotropy.     

Cluster-type basic lanthanide iodides [M6(mu6-O)(mu3-OH)8(H2O)24]I8(H2O)8 (M = Nd, Eu, Tb, Dy)

Ln6(mu6-O)(mu3-OH)8(H2O)24]I8(H2O)(8) (Ln = Nd, Eu, Tb, Dy) compounds are obtained as the final hydrolysis products of lanthanide triiodides in an aqueous solution. Their X-ray crystal structure features a body-centered arrangement of oxygen-centered {Ln6X8}8+ cluster cores: [Nd6(mu6-O)(mu3-OH)8(H2O)24]I8(H2O)8 [Pearson code oP156, orthorhombic, Pnnm (No. 58), Z = 2, a = 1310.4(3) pm, b = 1502.1(3) pm, c = 1514.9(3) pm, 3384 reflections with I0 > 2sigma(I0), R1 = 0.0340, wR2 = 0.0764, GOF = 1.022, T = 298(2) K], [Eu6(mu6-O)(mu3-OH)8(H2O)24]I8(H2O)8 [Pearson code oP156, orthorhombic, Pnnm (No. 58), Z = 2, a = 1306.6(2) pm, b = 1498.15(19) pm, c = 1499.41(18) pm, 4262 reflections with I0 > 2sigma(I0), R1 = 0.0540, wR2 = 0.0860, GOF = 0.910, T = 298(2) K], [Tb6(mu6-O)(mu3-OH)8(H2O)24]I8(H2O)8 [Pearson code oP156, orthorhombic, Pnnm (No. 58), Z = 2, a = 1296.34(5) pm, b = 1486.13(7) pm, c = 1491.88(6) pm, 4182 reflections with I0 > 2sigma(I0), R1 = 0.0395, wR2 = 0.0924, GOF = 1.000, T = 298(2) K], and [Dy6(mu6-O)(mu3-OH)8(H2O)24]I8(H2O)8 [Pearson code oP156, orthorhombic, Pnnm (No. 58), Z = 2, a = 1296.34(5) pm, b = 1486.13(7) pm, c = 1491.88(6) pm, 3329 reflections with I0 > 2sigma(I0), R1 = 0.0389, wR2 = 0.0801, GOF = 0.992, T = 298(2) K.     

Synthesis and Crystal Structure of a Cyano-bridged Bimetallic Complex:[NdFe(CN)_6(DMF)_4(H_2O)_3]H_2O

1 INTRODUCTION In recent years, cyano-bridged heterometallic coordination compounds have inspired remarkable attention due to their rich and interesting structures and magnetic behaviors. However, these studies were mainly focused on the transition metals. Although several unusual cyanide bridging lanthanide-transition metal complexes have been re- ported[1～6], this field continuously possesses tre- mendous researching potentialities. As regardsPrussian Blue lanthanide complex, divers…     

Synthesis, structure, and characterization of novel two- and three-dimensional vanadates: Ba2.5(VO2)3(SeO3)4.H2O and La(VO2)3(TeO6).3H2O

Two new vanadates, Ba(2.5)(VO2)3(SeO3)4.H2O and La(VO2)3(TeO6).3H2O, have been synthesized by hydrothermal methods using BaCO3, Ba(OH)2.H2O, La(NO3)3.6H2O, V2O5, TeO2, and H2SeO3 as reagents. The structures were determined by single-crystal X-ray diffraction. Ba(2.5)(VO2)3(SeO3)4.H2O exhibits a two-dimensional layered structure consisting of VO(5) square pyramids and SeO3 polyhedra, whereas La(VO2)3(TeO6).3H2O has a three-dimensional framework structure composed of VO(4) tetrahedra and TeO6 octahedra. Infrared and Raman spectroscopy, UV-vis diffuse reflectance spectroscopy, and thermogravimetric analysis are also presented. Crystal data: Ba(2.5)(VO2)3(SeO3)4.H2O, trigonal, space group P (No. 147) with a = b = 12.8279(15) A, c = 7.2631(9) A, V = 1035.1(2) A(3), and Z = 2; La(VO2)3(TeO6).3H2O, trigonal, space group R3c (No. 161) with a = b = 9.4577(16) A, c = 23.455(7) A, V = 1816.9(7) A3, and Z = 6.