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.
 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.  相似文献   

3.
The reaction of α-[SiMo12O40]4? with trivalent cations Ln3+ and N-methyl-2-pyrrolidone leads to a series of complexes of formula [Ln(NMP)4(H2O) n ]H[SiMo12O40]?·?2NMP?·?mH2O [where Ln?=?La (1), Pr (2), Nd (3), Sm (4), Gd (5), n?=?4, Ln?=?Dy (6), Er (7), n?=?3. NMP?=?N-methyl-2-pyrrolidone]. The syntheses, X-ray crystal structures, IR, and ESR spectra and thermal properties of the complexes 1, 2, 4, 6, 7 have been reported previously. Here, we report X-ray crystal structures, IR, UV, ESR spectra and thermal properties of the complexes [Nd(NMP)4(H2O)4]H[SiMo12O40]?·?2NMP?·?1.5H2O (3), and [Gd(NMP)4(H2O)4]H[SiMo12O40]?·?2NMP?·?H2O (5). In addition, the electrochemical behaviour of this series of complexes in aqueous solution and aqueous-organic solution has been investigated and systematic comparisons have been made. All these complexes exhibit successive reduction process of the Mo atoms.  相似文献   

4.
New cobalt trans-dioximate complexes with isoniconinamide have been synthesized: [CoII(DmgH)2(Inia)2] (I), [CoIII(DmgH)2(Inia)2][PF6] · 1.5H2O (II), [CoIII(NioxH)2 (Inia)2][PF6] · H2O · CH3OH (III), and [CoIIICl(DmgH)2(Inia)] · H2O (IV), where DmgH and NioxH are the dimeth-ylglyoxime and 1,2-cyclohexanedionedioxime monoanions, respectively; Inia is the isonicotinamide molecule. The structures of compounds I–IV have been determined by X-ray crystallography. In I–IV, Co(II) or Co(III) has an octahedral environment with the pseudomacrocyclic (DioxH)2 moiety (DioxH is the dioximate monoanion) in the equatorial plane. The latter is stabilized by O-H…O hydrogen bonds. The isonicotinamide molecules in all four complexes are monodentately bound to the metal ion through the heterocyclic nitrogen atom.  相似文献   

5.
Four metal complexes of N,N′-bis(salicyl)-2,6-pyridine-dicarbohydrazide ligand (H6L), [CoII(H4L)(H2O)2]·2DMF (1), [ZnII(H4L)(H2O)2]·2DMF (2), [CdII(H4L)(Py)2]·DMF·Py (3), and [CoIICo2III(H4L)4(H2O)4]·DMF·H2O (4), were synthesized and characterized by elemental analysis, IR, and single-crystal X-ray diffraction analysis. Structural studies revealed that complexes 13 present discrete mononuclear structures and complex 4 displays a centrosymmetric mixed-valence trinuclear structure. All four complexes are further extended into interesting two- or three-dimensional supramolecular frameworks. The luminescent properties of 2 and 3 were studied, which show emissions with maxima at 485 nm upon excitation at 396 nm for 2 and 476 nm upon excitation at 397 nm for 3, respectively.  相似文献   

6.
Magnetic susceptibility investigations have been carried out on a family of the tetra-transition-metal sandwiched Weakley-type germanotungstates Na11H[Co4(H2O)2(α-GeW9O34)2]·31H2O (1), (C6N2H18)4[Co(H2O)6]H2[Co4(H2O)2(α-GeW9O34)2]·5.5H2O (2) and Na(H2O)2(C6N2H18)4.75H1.5[Ni4(H2O)2(α-GeW9O34)2]·1.5H2O (3) with the intention of studying the magnetic exchange properties of the rhomb-like four transition-metal ions in the central belt. The Co–Co and Ni–Ni ferromagnetic exchange interactions are dominant in the rhomb-like M4O16 units in 13. Furthermore, magnetic susceptibility measurements also reveal that the magnetic coupling constant J is a sensitive parameter that is closely realted to the M–O–M angles and M···M separations in the rhomb-like magnetic core. Variable-temperature ac susceptibilities exhibit that magnetic properties of 2 and 3 are related to the spin glassy behaviors.  相似文献   

7.
Ten new complexes, [Cu2(L1)(NO3)2]·2H2O (1), [Cu4(L1)2]·4ClO4·H2O (2), [Cu2(L1)(H2O)2]·(adipate) (3), [Cu6(L1)2(m-bdc)4]·2DMF·5H2O (4), [Cu2(L1)(Hbtc)]·5H2O (5), [Cu2(L1)(H2O)2]·(ntc)·3H2O (6), [Co2(L2)]·[Co(MeOH)4(H2O)2] (7), [Co3(L2)(EtOH)(H2O)] (8), [Ni6(L2)2(H2O)4]·H2O (9) and [Zn4(L2)(OAc)2]·0.5H2O (10), have been synthesized. 1 displays a [Cu2(L1)(NO3)2] monomolecular structure. 2 shows a supramolecular chain including [Cu2L1]2+. In 3, two Cu(II) ions are connected by L1 to form a [Cu2(L1)(H2O)2]2+ cation. In 4, the m-bdc anions bridge Cu(II) ions and L1 anions to form a layer. Both 5 and 6 display 3-D supramolecular structures. 7 consists of both [Co2L2]2? and [Co(MeOH)4(H2O)2]2+ units. 8 and 9 show infinite chain structures. In 10, Zn(II) dimers are linked by L2 to generate a 3-D framework. The magnetic properties for 4 and 8 and the luminescent property for 10 have been studied.  相似文献   

8.
以2,2'-联吡啶-3,3',6,6'-四羧酸(H4bptc)为配体,通过水热合成的方法与过渡金属盐合成了3个配合物,其分子式分别为[Co2(H2bptc)2(H2O)4]·bpe·9H2O(1),[Ni2(H2bptc)2(H2O)4]·bpe·9H2O(2),[Ni2(H2bptc)2(H2O)4]·0.5bpp·7H2O(3)(bpe=1,2-二(4-吡啶基)乙烯,bpp=1,2-二(4-吡啶基)乙烷)。用红外光谱,X-射线单晶衍射对化合物的晶体结构进行了表征,并对这3个配合物的热稳定性进行了测试。化合物1~3为单核结构的配合物,它们均通过分子间氢键形成三维超分子结构。  相似文献   

9.
New bi- and trihomonuclear Mn(II), Co(II), Ni(II), and Zn(II) complexes with sulfa-guanidine Schiff bases have been synthesized for potential chemotherapeutic use. The complexes are characterized using elemental and thermal (TGA) analyses, mass spectra (MS), molar conductance, IR, 1H-NMR, UV-Vis, and electron spin resonance (ESR) spectra as well as magnetic moment measurements. The low molar conductance values denote non-electrolytes. The thermal behavior of these chelates shows that the hydrated complexes lose water of hydration in the first step followed by loss of coordinated water followed immediately by decomposition of the anions and ligands in subsequent steps. IR and 1H-NMR data reveal that ligands are coordinated to the metal ions by two or three bidentate centers via the enol form of the carbonyl C=O group, enolic sulfonamide S(O)OH, and the nitrogen of azomethine. The UV-Vis and ESR spectra as well as magnetic moment data reveal that formation of octahedral [Mn2L1(AcO)2(H2O)6] (1), [Co2(L1)2(H2O)8] (2), [Ni2L1(AcO)2(H2O)6] (3), [Mn3L2(AcO)3(H2O)9] (5), [Co3L2(AcO)3(H2O)9] · 4H2O (6), [Ni3L2(AcO)3(H2O)9] · 7H2O (7), [Mn3L3(AcO)3(H2O)6] (9), [Co2(HL3)2(H2O)8] · 4H2O (10), [Ni3L3(AcO)3(H2O)9] (11), [Mn3L4(AcO)3(H2O)9] · H2O (13), [Co2(HL4)2(H2O)8] · 5H2O (14), and [Ni3L4(AcO)3(H2O)9] (15) while [Zn2L1(AcO)2(H2O)2] (4), [Zn3L2(AcO)3(H2O)3] · 2H2O (8), [Zn3L3(AcO)3(H2O)3] · 3H2O (12), and [Zn3L4(AcO)3(H2O)3] · 2H2O (16) are tetrahedral. The electron spray ionization (ESI) MS of the complexes showed isotope ion peaks of [M]+ and fragments supporting the formulation.  相似文献   

10.
The coordination compounds of group 12 halides with 2,2′-bipyridine (bpy) and 1,10-phenanthroline (phen), 2[CdF2(bpy)2]·7H2O (1), [ZnI(bpy)2]+·I3? (2), [CdI2(bpy)2] (3), [Cd(SiF6)H2O(phen)2]·[Cd(H2O)2(phen)2]2+·F·0.5(SiF6)2–·9H2O (4), [Hg(phen)3]2+·(SiF6)2–·5H2O (5), [ZnBr2(phen)2] (6), 6[Zn(phen)3]2+·12Br·26H2O (7) and [ZnI(phen)2]+·I (8), have been synthesized and characterized by X-ray crystallography, IR spectroscopy, elemental and thermal analysis. Structural investigations revealed that metal?:?ligand stoichiometry in the inner coordination sphere is 1?:?2 or 1?:?3. A diversity of intra- and intermolecular interactions exists in structures of 18, including the rare halogen?halogen and halogen?π interactions. The thermal and spectroscopic properties were correlated with the molecular structures of 18. Structural review of all currently known coordination compounds of group 12 halides with bpy and phen is presented.  相似文献   

11.
邴颖颖  吴振廷  胡明 《无机化学学报》2015,31(10):2059-2064
以2,2'-联吡啶-3,3',6,6'-四羧酸(H4bptc)为配体,通过水热合成的方法与过渡金属盐合成了3个配合物,其分子式分别为[Co2(H2bptc)2(H2O)4]·bpe·9H2O(1),[Ni2(H2bptc)2(H2O)4]·bpe·9H2O(2),[Ni2(H2bptc)2(H2O)4]·0.5bpp·7H2O(3)(bpe=1,2-二(4-吡啶基)乙烯,bpp=1,2-二(4-吡啶基)乙烷)。用红外光谱,X-射线单晶衍射对化合物的晶体结构进行了表征,并对这3个配合物的热稳定性进行了测试。化合物1~3为单核结构的配合物,它们均通过分子间氢键形成三维超分子结构。  相似文献   

12.
以1,2,4,5-苯四甲酸(H_4BETA)与1,2,3,4-丁烷四羧酸(H_4BTCA)为有机配体,采用溶剂热法,成功合成了3个金属有机框架(Metal-Organic Frameworks,MOFs):{[Co_5(BETA)_2(OH)_2(H_2O)_2]·10H_2O}_n(1)、{[Zn_5(BETA)_2(OH)_2(H_2O)_2]·10H_2O}_n(2)和{[Mn_2(BTCA)(H_2O)_3]·H_2O}_n(3),并利用X射线单晶衍射、红外光谱(IR)、荧光光谱(PL)和热重分析(TG/DTG)等测试手段对其进行了表征。单晶结构研究表明3个MOFs均属于单斜晶系,P21/n空间群;框架1和2都是由1,2,4,5-苯四甲酸与五核的金属簇连接形成三维框架结构,沿a轴方向具有一维孔道结构,孔径大小为0.990 nm×1.307 nm;框架3是由1,2,3,4-丁烷四羧酸与Mn~(2+)连接形成4,8-c网络的三维框架结构。  相似文献   

13.
The reaction of Nb2O5 and Ta2O5 with an aqueous solution of hydrofluoric acid, HF in the presence of biphenyl-20-crown-6 (BP20C6, L1) or [1.5]dibenzo-18-crown-6 ([1.5]DB18C6, L2) results in the complexes [L1·(H3O)][NbF6] (1), [L1 (H3O)][TaF6] (2), [2L2·(H7O3)][NbF6] (3) and [2L2·(H7O3)][TaF6] (4). Complexes 1–4 were identified by the elemental and X-ray structural analysis and IR spectroscopy. Complexes 1 and 2 are isostructural, with the H3O+ oxonium ion embedded in one crown molecule via OH···O hydrogen bonds. Complexes 3 and 4 represent the supramolecular isomers distinctive by the crown conformations and crystal packing, with the (H7O3)+ cation enclosed in the cage of two crown molecules. Being poor H-bond acceptors, NbF6 and TaF6 anions do not compete with the crown oxygen atoms for the oxonium hydrogen atoms, but are involved in the numerous C–H···F short contacts responsible for the extended supramolecular architectures in all cases. A change of crown ethers’ conformation in complexes 1–4 and a correlation between the degree of proton hydration and an accessibility of the crown ether oxygen atoms is observed. Electronic Supplementary Material Supplementary material is available for this article at and is accessible for authorized users.  相似文献   

14.
Negative ion mass spectra of series of bis-(N, N-dithiocarbamato)nickel(II) complexes of formula [NiS2C·NR1R2]2 (where·NR1R2 ? ·NEt2 ·NPr2, ·NBu2, pyrrolidinyl, piperidyl, morpholinyl, and ·NEtPh) have been obtained by secondary electron capture. Intense molecular anions are given for all compounds, with most fragments originating from these ions. Metastable data indicate that CS2 is eliminated from all molecular anions.  相似文献   

15.
The reactions of the oxalate complexes [M3Q7(C2O4)3]2− (M = Mo or W; Q = S or Se) with MnII, CoII, NiII, and CuII aqua and ethylenediamine complexes in aqueous and aqueous ethanolic solutions were studied. The previously unknown heterometallic complexes [Mo3Se7(C2O4)3Ni(H2O)5]·3.5H2O (1) and K3{[Cu(en)2H2O]([Mo3S7(ox)3]2Br)}·5.5H2O (2) were synthesized. In these complexes, the oxalate clusters serve as monodentate ligands. The K(H2en)2[W3S7(C2O4)3]2Br·4H2O salt (3) was isolated from solutions containing CoII, NiII, or CuII aqua complexes and ethylenediamine. The reaction of [Mo3Se7(C2O4)3]2− with HBr produced the bromide complex [Mo3Se7Br6]2−, which was isolated as (Bu4N)2[Mo3Se7Br6] (4). Complexes 1–3 were characterized by X-ray diffraction, IR spectra, and elemental analysis. The formation of 4 was detected by electrospray mass spectrometry. Dedicated to Academician G. A. Abakumov on the occasion of his 70th birthday. Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 9, pp. 1645–1649, September, 2007.  相似文献   

16.
From the reaction between Zn(II), Cd(II) and Hg(II) with 5-methyl-1-(2′-pyridyl)pyrazole-3-carboxamide (MP y P z CA) in ethanol, the complexes [Zn(MP y P z CA)2(NO3)]+ [(NO3)0.60(ClO4)0.40]?·H2O, Cd(MP y P z CA)2Cl2 and Hg(MP y P z CA)(SCN)2 were obtained. These compounds have been characterized by IR and CHN analyses. The structure of [Zn(MP y P z CA)2NO3]+[(NO3)0.60(ClO4)0.40]?·H2O has been solved by X-ray crystallography. The coordination environment around the Zn(II) may be described as a trigonal bipyramid in which the ligands are both bidentate, but coordinated differently. The coordination sphere is completed with the oxygen atom of a nitrate anion as a unidentate ligand.  相似文献   

17.
The desolvation process in lanthanide pyridine-3,5-dicarboxylates of the formulae [Tb2pdc3(dmf)2]·dmf (1), [Ho2pdc3(dmf)2]·dmf (2), [Erdc3(dmf)2]·dmf (3), and [Yb2pdc3(dmf)2]·dmf (4) where pdc-C5H3N(COO)22−, dmf-N,N′-dimethylformamide) has been investigated by means of the TG–DSC, TG–FTIR, IR and XRD methods. Heating of the complexes in the range 30–260 °C lead to evolution of weakly bonded dmf molecules included in the channels as well those directly bonded with lanthanide atoms. The kinetic analysis revealed a multistep desolvation pattern.  相似文献   

18.
Four new 3d–4f heterometallic coordination polymers [Cu3Eu2(2,5-pydc)6(H2O)12]·4(H2O) (1), [Zn2Eu2(2,5-pydc)5(H2O)2]·3(H2O) (2), and [Co3Ln2(2,6-pydc)6(H2O)6]·4(H2O) (Ln = Eu, 3; Dy, 4) (H2pydc = pyridinedicarboxylic acid) have been synthesized and characterized. All of these compounds have extended 3D coordination frameworks containing supramolecular 1D channels, in which lattice water molecules are located. Hydrogen bonds stabilize the 3D frameworks. Additionally, a study of their fluorescence properties has indicated that compounds 1 and 2 show the characteristic transitions of Eu3+. Weak antiferromagnetic interactions are observed in compound 3.  相似文献   

19.
Five cobalt(II) complexes based on 1H-indazole-3-carboxylic acid (H2L), [Co(phen)(HL)2]·2H2O (1), [Co(5,5′-dimethyl-2,2′-bipy)(HL)2] (2), [Co(2,2′-bipy)2(HL)2]·5H2O (3), [Co2(2,9-dimethyl-1,10-phen)2(L)2] (4) and [Co2(6,6′-dimethyl-2,2′-bipy)2(L)2]·H2O (5) (2,2'-bipy = 2,2′-bipyridine, phen = 1,10-phenanthroline), have been synthesized and structurally characterized by elemental analyses, IR and UV-vis spectroscopies and single-crystal X-ray crystallography. The results indicate that 1–3 possess mononuclear Co(II) structures, while 4 and 5 exhibit binuclear structure. 1D water tape which is linked by the multiple hydrogen bonds was embedded in the 3D motif of complex 3. Complexes 4 and 5 show two orthogonal planes of motif that was constituted by phen/2,2′-bipy and indazole acid, respectively. The intermolecular interactions including hydrogen bonding and π-π stacking interactions are stabilizing these complexes. The interactions of the synthesized complexes with calf-thymus DNA (CT-DNA) have been investigated by UV-vis absorption titration, ethidium bromide displacement assay and viscosity measurements. The results reveal that the complexes could interact with CT-DNA via a groove binding mode. Their behavior rationalization was further theoretically studied by molecular docking.  相似文献   

20.
Three octamolybdate compounds, namely [Cu(H2biim)2]2[β-Mo8O26{Cu(H2biim)2}2][β-Mo8O26] (1), [{Fe(H2biim)2(Hbiim)}2(γ-Mo8O26)]·5H2O (2), and [{Co(H2biim)2(Hbiim)}2(γ-H2Mo8O26)]·5 H2O (3) (H2biim = 2,2′-biimidazole) have been hydrothermally synthesized from the reaction of mixtures of hexamolybdochromate ({CrMo6}), transition metal, and H2biim in acetate buffer solution, and characterized by physico-chemical and spectroscopic methods. They represent the first examples of the conversion of hexamolybdochromate to octamolybdate. Single-crystal X-ray diffraction analysis reveals that compound 1 is composed of a β-[Mo8O26]4− polyoxoanion bi-supported by two [Cu(H2biim)2]2+ complex cations, an isolated β-[Mo8O26]4− anion, and two [Cu(H2biim)2]2+ complex cations. The copper complex cations are situated at two different sites and associate with β-[Mo8O26]4− anions to give 2D layers, which are further packed into a 3D framework via strong hydrogen bonding interactions. Compounds 2 and 3 are isostructural, and contain a γ-[Mo8O26N2] unit and two symmetrical {M(H2biim)2(Hbiim)} (M=Fe or Co) fragments grafted onto the polyoxoanion through Mo–N bonds. The two compounds also exhibit 3D supramolecular frameworks involving hydrogen bonding interactions.  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