首页 | 本学科首页   官方微博 | 高级检索  
相似文献
 共查询到20条相似文献,搜索用时 15 毫秒
1.
Summary.  Oxo peroxo glycolato complexes of vanadium(V) (M 2[V2O2(O2)2(C2H2O3)2nH2O (n=0, 1; M=NBu4 + (1), K+ (2), NH4 + (3), Cs+ (4), NPr4 + (5)) as well as (NBu4)2[V2O4(C2H2O3)2]ċ H2O (6) have been prepared and characterized by spectroscopic methods. X-Ray structure analysis of 1 revealed the presence of dinuclear [V2O2(O2)2(C2H2O3)2]2− anions with a (chemical structure) bridging core and six coordinated vanadium(V) atoms in a distorted pentagonal pyramidal array. Received July 12, 1999. Accepted (revised) October 28, 1999  相似文献   

2.
Abstract

Reactions of Mo(CO)6 with Na2WO4 · 2H2O in refluxing carboxylic anhydride produce the triangular bioxo-capped mixed-metal carboxylate clusters Na[MoW2O2(O2CR)9] (R = Me, 1; Et, 2), the propionate being hydrolyzed in 2M HCl containing ZnCl2 to form [MoW2O2(O2CEt)6(H2O)3]ZnCl4·2H2O (3). Cluster 2 is converted to the incomplete cuboidal tetraanion [MoW2O4(O2CEt)8]4- upon reacting with Cr(CO)6 in propionic anhydride at 120°, the latter species being trapped by Cr and Na± ions in the reaction mixture to afford the octanuclear heterometallic chain-like cluster Na2Cr2 [MoW2O4(O2CEt)8]2 (4). Clusters 1, 3 and 4 have been characterized by X-ray crystallography with the following crystal data, for 1: monoclinic, space group P21/c, a = 16.666(8), b = 11.096(3), c = 16.541(7) Å, β = 94.60(4)°, V = 3048.9 Å3, Z = 4, R, Rw = 0.070, 0.079; for 3, monoclinic, space group Cm, a = 10.259(3), b = 15.756(3), c = 10.870(3) Å, β = 96.18(3)°, V = 1746.8 Å3, Z = 2, R, Rw = 0.028, 0.034; for 4, triclinic, space group P-1, a = 13.013(5), b = 14.005(4), c = 12.357(4) Å, α = 109.71(2), β = 117.77(3), γ = 90.41(3)°, V = 1838.9 Å3, Z = 1, R, Rw = 0.037, 0.042.  相似文献   

3.
[Pb2(TNR)2(CHZ)2(H2O)2]4H2O的结构及热分解机理   总被引:1,自引:0,他引:1  
The coordination compound of [Pb 2(TNR) 2(CHZ) 2(H 2O) 2]•4H 2O was prepared by using the aqueous solution of carbohydrazide, lead nitrate and sodium styphnate. The molecular structure of [Pb 2(TNR) 2(CHZ) 2(H 2O) 2]•4H 2O(C 7H 13 N 7O 12 Pb, Mr=594.43) was determined by using a single crystal diffraction analysis .The thermal decomposition mechanism of the title compound was studied by TGDTG, DSC and IR techniques. The crystal belongs to monoclinic with space group P2 1/n.The unit cell parameters are as follows: a=0.64700(10)nm, b=1.6074(3)nm, c=1.4883(3)nm,β=97.42(2)°,V=1.5349(5)nm3, Z=2, DC=2.572g•cm -3 ,μ(Mo, Kα)=11.080cm -1 , F(000)=1128. R=0.0422, Rw=0.0735. The binuclear lead coordination compound is bridged by two carbohydrazide molecules. The molecule has a symmetrical center. TNR 2- ,CHZ and H 2O coordinate with the central ions simultaneously.  相似文献   

4.
[Mn2(TNR)2(CHZ)2(H2O)4]·2H2O的合成和晶体结构   总被引:3,自引:0,他引:3  
将MnCO3与2,4,6-三硝基间苯二酚(斯蒂芬酸、TNR)分散于蒸馏水中,加热搅拌制备出斯蒂酚酸锰溶液,再与碳酰肼(CHZ)水溶液反应制备〖Mn2(TNR)2(CHZ)2(H2O)4〗·2H2O(C14H26Mn2N14O24,Mr=884.36),并对其进行了元素分析和红外表征,利用单晶分析测定了晶体结构。该化合物为双核配合物,属三斜晶系,空间群为^-P1,晶体学数据如下:a=7.280(1)  相似文献   

5.
用碳酰肼 (CHZ ,NH2 NHCONHNH2 )、硝酸铅和三硝基间苯二酚 (TNR ,斯蒂酚酸 )的水溶液制备 [Pb2 (TNR) 2 (CHZ) 2 (H2 O) 2 ]·4H2 O .采用单晶分析的方法测定它的分子结构 ,并用TG DTG、DSC和 IR相结合的技术研究它的热分解机理 .所得晶体属单斜晶系 ,P2 1/n空间群 .晶体学参数为 :a=0 .6470 0 ( 10 )nm ,b =1.60 74 ( 3)nm ,c=1.4 883( 3)nm ,β =97.4 2 ( 2 )° ,V =1.534 9( 5)n ,Z =2 ,DC=2 .572 g·cm- 3,μ(Mo ,Kα) =11.0 80cm- 1,F( 0 0 0 ) =112 8.最终偏离因子R =0 .0 4 2 2 ,Rw=0 .0 735.该配合物分子呈中心对称 ,两个羰基O原子形成两个氧桥 ,TNR2 - ,CHZ和H2 O同时参与了与中心离子的配位  相似文献   

6.
7.
Calcium titanate (CaTiO3) was conveniently synthesized by thermal decomposition of a single-source precursor [Ca(H2O)3]2[Ti2(O2)2O(NC6H6O6)2]·2H2O at low temperature. This single-source precursor was characterized by elemental analysis, IR spectrum, thermal gravimetric analysis and X-ray single crystal diffraction. The calcined products at different temperature were further characterized by powder X-ray diffractions and IR spectra. The morphology, microstructure, and crystallinity of the resulting CaTiO3 materials have been characterized by SEM and TEM. The BET measurement revealed that the CaTiO3 powders had a surface area of 14.0 m2/g. In addition, the microwave dielectric properties of the resulting CaTiO3 material have been measured.  相似文献   

8.
A novel germanotungstate derivative based on the dysprosium cation and monovacant Keggin anion, [Cu(en)2]2[Cu(en)2(H2O)]2H3{[Cu(en)2]2[Na2(H2O)1.75][K(H2O)3][Dy2(H2O)2(GeW11O39)3]} · 6H2O(en = ethylenediamine) 1, has been synthesized by hydrothermal method and characterized by elemental analysis, IR-UV spectroscopy, thermal analysis and single-crystal X-ray diffraction. In the compound, one kind of clusters with the Dy3+/[GeW11O39]8? ratio of 2:3 was observed. Especially, the 2:3 type displays the novel cluster based on the rare earth and monolacunary Keggin polyoxometalate.  相似文献   

9.
Compounds p-HOOCC6F4COOH · H2O (H2L · H2O), [Tb2(H2O)4(L)3 · 2H2O] n (I), and Tb2(Phen)2(L)3 · 2H2O (II) are synthesized. According to the X-ray structure analysis data, the crystal structure of H2L · H2O is built of centrosymmetric molecules H2L and molecules of water of crystallization. The crystal structure of compound I is built of layers of coordination 2D polymer [Tb2(H2O)4(L)3] n and molecules of water of crystallization. The ligands are the L2? anions performing both the tetradentate bridging and pentadentate bridging-chelating functions. The coordination polyhedron TbO9 is a distorted three-capped trigonal prism. Acid H2L manifests photoluminescence in the UV region (??max = 368 nm). Compounds I and II have the green luminescence characteristic of the Tb3+ ions, and the band with ??max = 545 nm (transition 5 D 4?? 7 F 5) is maximum in intensity. The photoluminescence intensity of compound II is higher than that for compound I.  相似文献   

10.
The reaction of [Sb(2)W(22)O(74)(OH)(2)](12-) and [Fe(4)(H(2)O)(10)(β-TeW(9)O(33))(2)](4-) with (NH(4))(2)[RuCl(6)] in aqueous solution resulted in the novel ruthenium(IV)-containing polyanions [{Ru(IV)(4)O(6)(H(2)O)(9)}(2)Sb(2)W(20)O(68)(OH)(2)](4-) and [{Ru(IV)(4)O(6)(H(2)O)(9)}(2){Fe(H(2)O)(2)}(2){β-TeW(9)O(33)}(2)H](-), exhibiting two cationic, adamantane-like, tetraruthenium(IV) units {Ru(4)O(6)(H(2)O)(9)}(4+) bound to the respective polyanion in an external, highly accessible fashion.  相似文献   

11.

Reaction of a freshly prepared Ni(OH)2?2 x (CO3) x ·yH2O with maleic acid in H2O at room temperature afforded [Ni(H2O)6][Ni(H2O)2(C4H2O4)]·4H2O, which consists of [Ni(H2O)6]2+ cations, [Ni(H2O)2(C4H2O4)]2? anions and lattice H2O molecules. Ni atoms in cations are octahedrally coordinated and Ni atoms in anions are each octahedrally coordinated by bidentate chelating maleato ligands and two water molecules at trans positions. Cations and anions are interlinked by hydrogen bonds to form 1D chains, which are hexagonally arranged and connected by the lattice water molecules. When heated in a flowing argon stream, the compound decomposes, with complete dehydration being followed by dissociation of nickel maleate into NiO and maleic anhydride.  相似文献   

12.
Two new malonato-bridged copper(II) complexes of the composition [Cu2(mal)2(datz)2(H2O)]·5H2O (1) and [Cu2(mal)2(atz)2(H2O)]·3H2O (2) (mal = malonate, atz = 4-amino-1,2,4-triazole, datz = 3,5-diamino-1,2,4-triazole) are prepared and characterized by X-ray crystal structure determination and magnetic studies. The environment of each copper atom in 1 and 2 has distorted square pyramidal and octahedral geometries. The intrachain copper-copper separation is 6.305 Å and 3.640 Å across the carboxylates and trizolates bridges respectively for complexes 1 and 2. The magnetic properties of 1 and 2 are investigated in the temperature range 2–300 K. The overall antiferromagnetic behavior is observed in both cases.  相似文献   

13.
Two Cu(II) hydroxo succinates [Cu3(H2O)2(OH)2(C4H4O4)2]?·?4H2O (1) and [Cu4(H2O)2(OH)4(C4H4O4)2]?·?5H2O (2) and one Cu(II) hydroxo glutarate [Cu5(OH)6(C5H6O4)2]?·?4H2O (3) have been prepared and structurally characterized by single crystal X-ray diffraction methods. They feature 1D and 2D copper oxygen connectivity of elongated {CuO6} octahedra in “4?+?1?+?1” and “4?+?2” coordination geometries. Within 1, linear trimers of three edge-sharing {CuO6} octahedra are connected into copper oxygen chains, which are bridged by the anti conformational succinate anions to generate 2D layers with mono terminally coordinating gauche succinate anions on both sides. The layers are assembled into a 3D framework by interlayer hydrogen bonds with lattice H2O molecules distributed in channels. Different from 1, the principal building units in 2 are linear tetramers of four edge-sharing {CuO6} octahedra. The tetramers are condensed into copper oxygen chains and the succinate anions interlink them into a 3D framework with triangular channels filled by lattice H2O molecules. The {CuO6} octahedra in 3 are edge-shared to form unprecedented 2D inorganic layers with mono terminally coordinating glutarate anions on both sides. Interlayer hydrogen bonding interactions are responsible for supramolecular assembly of the layers into a 3D framework with lattice H2O molecules in the channels. The inorganic layers in 3 can be described as hexagonal close packing of oxygen atoms with the Cu atoms in the octahedral cavities. The title compounds were further characterized by elemental analyses, IR spectra and thermal analyses.  相似文献   

14.
The compound Na2[(UO2)2(SeO4)3(H2O)2] · 6.5H2O (I) is studied using X-ray diffraction. The compound crystallizes in the monoclinic crystal system with the unit cell parameters a = 19.7366(8) Å, b = 10.8206(4) Å, c = 21.3577(8) Å, β = 103.4311(1)°, Z = 4, and the space group P21/c, R 1 = 0.0379. Compound I is found to be a representative of the crystal-chemical group A2T 2 3 B2M 2 1 (A = UO 2 2+ ) of uranyl complexes and contains the cage group [(UO2)2(SeO4)3(H2O)2]2?.  相似文献   

15.
Abstract

In an attempt to form new multi-dimensional structures of cyano complexes including cadmium(II) and copper(I), four new complexes were obtained successively from an aqueous solution at intervals of from a few days to a few months. The complex 1 obtained first was unstable in the atmosphere. The crystal structures of the other complexes (2–4) obtained from second to fourth were determined by single crystal X-ray structure determinations. Their crystal data are as follows: 2 Cd(H2O)2 Cu(CN)3·2H2O, monoclinic, C2/m, a = 14.038(1), b = 9.944(1), c = 7.738(1) Å, β = 116.019(7)°, Z = 4; 3 K[Cd(H2O)2Cu2(CN)5]·2H2O, triclinic, PI, a = 17.429(9), b = 16.519(7), c = 10.085(5) Å, α = 128.60(3), β = 137.44(2), γ = 45.82(2)°, Z = 4; 4 K2[Cd(H2O)Cu4(CN)8]·1.5H2O, monoclinic, C2/c, a = 19.387(2), b = 16.056(3), c = 12.663(2)Å, β = 110.419(9)°, Z = 4. The main structural feature found in the complexes is that the whole framework consists of two networks, a Cd-Cu(I)-CN complex network that has an infinite network formed with bridging cyano groups between the metal atoms and a network formed with hydrogen bonding among water molecules. The second network is connected to Cd in the Cd-Cu(I)-CN complex network via a water ligand coordinated to Cd. In 2 a planar network of [CdCu(CN)3] complexes are stacked along the c axis and the second network links the stacked complexes. 3 has a stacked structure of [Cd(H2O)2Cu(CN)5]2? in a bi-layered structure. The second network of 3, which includes K+ ions with an electrostatic interaction, spreads over the crystal, penetrating vacant spaces of the metal complex network. 4 has a double lattice structure with a pair of enantiomeric three-dimensional [Cd(H2O)Cu4(CN)8]2? complexes inter-penetrating each other. There are three structural factors for forming these framwork structures: (1) a non-planar coordination structure for Cd(II) that extends the planar structure of the Cu(I)-CN complex to a three-dimensional structure for the Cd-Cu(I)-CN complex; (2) a trigonal planar coordination structure for Cu(I) that generates vacant space in the metal complex network and makes possible hydrogen bonds to form the second network; (3) structural distortions of bridging cyano groups and a coordination structure of Cu(I) that cause variations of the metal complex network structure.  相似文献   

16.
将MnCO3 与2,4,6-三硝基间苯二酚(斯蒂芬酸、TNR)分散于蒸馏水中, 加热搅拌制备出斯蒂酚酸锰溶液,再与碳酰肼(CHZ)水溶液反应制备〔Mn2 (TNR)2(CHZ)2(H2O)4〕·2H2O(C14H26Mn2N14O24, Mr= 884.36),并对其进行了元素分析和红外表征,利用单晶分析测定了晶体结构。该化合物为双核配合物,属三斜晶系,空间群为P1,晶体学数据如下:a= 7.280(1),b= 10.318(1),c= 11.106(1),α= 94.56(1),β= 91.86(1),γ= 106.88(1)°,V= 794.4(2)3,Z= 1,Dc= 1.849g.cm - 3, μ=9.15cm - 1, F(000)= 450, I> 2σ(I)的独立可观测点个数为2783,最终偏离因子R=0.0272, Rw = 0.0639。分子为中心对称,配位多面体为略有畸变的五角双锥体构型。  相似文献   

17.
合成了以 5 -氨基四唑为配体的镉配合物 [Cd(ATZ) 4(H2 O) 2 ](PA) 2 ·2H2 O ,并对其进行了晶体结构测定 .测定结果表明 ,该配合物分子具有中心对称性 ,每个Cd2 +分别与 2个水分子中的氧原子和 4个 5 -氨基四唑 (ATZ)分子中的 4-位氮原子配位 ,形成六配位畸变八面体结构 ;在配合物分子间存在大量氢键 ,增加了整个晶体结构的稳定性 .通过DSC和TG -DTG分析 ,提出了标题化合物的热分解机理  相似文献   

18.
该文报道了N,N′-(2-苯并咪唑基甲基)亚氨基甲基膦酸{bbimpH_2,[(C7H5N2)CH2]2NCH2PO3H2}的2个镍化合物Ni2(bbimp)2(4,4′-bipy)(H2O)2·2H2O(1)和[Ni2(bbimp)2(H2O)2][Ni(bbimp)(H2O)2]2·4H2O(2)。化合物1是4,4′-联吡啶作为桥连配体的中性双核结构。化合物2含有1个中性的[Ni2(bbimp)2(H2O)2]双核分子与2个中性的[Ni(bbimp)(H2O)2]单核分子。双核分子单元中的2个Ni!离子被2个膦酸氧桥连。在化合物2中,膦酸氧桥连的2个Ni!离子之间存在铁磁性相互作用。  相似文献   

19.
在二甲亚砜(DMSO)中,以MnCl_2·2H_2O和K_3[Cr(OX)_3]·3H_2O为原料,合成了离子型配合物[Mn(phen)_2(H_2O)_2]_2[Cr(OX)_3][HOCH_2CH_2O]·4H_2O.晶体结构测定表明,该晶体属单斜晶系,P2/c空间群.晶体学参数:a=1.0602(3),b=1.3515(3),c=2.1508(3)nm,β=102.57(2)°,V=3.008(1)nm~3,Z=2,Dc=1.49g/cm~3,F(000)=1392.最后的偏差因子R=0.067.测定了化合物的UV-Vis-NIR,IR,XPS,ESR光谱和变温磁化率,讨论了相应的性质.  相似文献   

20.
N 酰化氨基酸含有肽键,结构与肽链羧基末端结构相似[1,2],并能直接参与生物过程,显示重要的生物作用。N 磺酰化氨基酸是N 酰化氨基酸中的一类,具有良好的生物活性。二十世纪七十年代到九十年代初,是国外一批学者研究过渡金属与N 磺酰化氨基酸配合物的热点时期[3 9],但到目前为止,稀土与N 磺酰化氨基酸配合物的研究报道尚未多见。随着稀土微肥、稀土饲料添加剂的使用,稀土已通过各种途径进入环境,所以研究稀土与N 酰化氨基酸、肽生物配体的配位作用对认识稀土离子在体内的存在形式和作用机理以及与蛋白质的构效关系有重要意义。本文合…  相似文献   

设为首页 | 免责声明 | 关于勤云 | 加入收藏

Copyright©北京勤云科技发展有限公司  京ICP备09084417号