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1.
本文合成了含水杨醛缩对硝基苯甲酰腙(简写为H2L)的钒酰配合物VOL(CH3OH)(CH3O)(1,C16H16N3O7V,Mr=413.26)和钴配合物[CoL(C5H5N)3]NO3C5H5N(2,C34H29N8O7Co,Mr=720.58)。配合物1属单斜晶系,空间群为P21/c,a=7.3253(3),b=18.8237(9),c=12.9014(5)?b=91.672(1),V=1778.2(1)3,Z=4,F(000)=848,m(MoKa)=0.603mm1,R=0.0470,wR=0.1312。配合物2属单斜晶系,空间群为P21/c,a=11.4196(8),b=17.157(1),c=17.081(1)?b=96.8233(9),V=3323.0(4)3,Z=4,F(000)=1488,m(MoKa)=0.578mm1,R=0.0455,wR=0.1311。在配合物1中,钒(V)原子由周围的酰氧基原子、配体L2的3个配位原子,去质子化甲醇的甲氧基原子和配位甲醇的氧原子配位,形成畸变的VO(ONO)(O)(O)八面体配位构型。晶体内每2个分子间通过氢键作用缔合成中心对称的分子对,OH…N氢键键长为2.861(4)?键角163.20。晶体中存在着弱p-p共轭作用。在配合物2中,钴(Ⅲ)原子由1个L2的3个配位原子和3个配位吡啶分子的3个氮原子配位,呈N4O2八面体配位构型。 相似文献
2.
Ghosh Tapas Bandyopadhyay Chandrakanta Bhattacharya Sharmila Mukherjee Gurunath 《Transition Metal Chemistry》2004,29(4):444-450
Mixed-ligand oxovanadium(IV) and oxovanadium(V) complexes with a tridentate dinegative ONO donor Schiff base ligand [viz., 4-(1-hydroxybenzylidenehydrazono)-2-penten-2-ol (H2L)] and bidentate NN [viz., 2,2-bipyridine (bipy) and 1,10-phenanthroline (phen): complexes (1) and (2), respectively] or OO–[viz., ethylene glycol (H2gol), salicylaldehyde (Hsal) and vanillin (Hvan): complexes (3)–(5), respectively] donor ligands have been prepared and characterized by elemental analyses and by i.r., e.p.r., n.m.r., and u.v.–vis. spectroscopies. The complexes with NN donor ligands are one electron paramagnetic, displaying axial e.p.r. spectra and exhibiting two ligand-field transitions in the visible region, whereas the complexes with OO– donor ligands are diamagnetic and display only LMCT bands. 1H n.m.r. spectral data indicate that the pentavalent complexes (4) and (5) exist in two isomeric forms [(4A), (4B) and (5A), (5B) in 1:1 and 4:1 ratios, respectively]. The vanadyl(IV) complexes display an irreversible oxidation peak near +0.67 V while among the vanadyl(V) complexes, (3), displays an irreversible reduction peak near –0.20 V and (4) and (5) display a quasi-reversible one electron reduction peak near +0.25 V versus s.c.e. The trend in redox potential values and the selective stabilization of VO2+ and VO3+ motifs have been explained on the basis of the basicity of the bidentate auxiliary ligands. 相似文献
3.
An entirely new class of heterobimetallic homoleptic glycolate complexes of the type Nb(OGO)3{Ta(OGO)2} [where G=CMe2CH2CH2CMe2 (G1) (3); CMe2CH2 CHMe(G2) (4); CHMeCHMe (G3) (5); CH2CMe2CH2 (G4) (6); CMe2CMe2(G5) (7); CH2CHMeCH2 (G6) (8); CH2CEt2CH2 (G7) (9); CH2CMe(Prn)CH2 (G8) (10)] have been prepared by the reactions of Nb(OGO)2(OGOH) [G=G1 (1a); G2 (1b); G3 (1c); G4 (1d); G5 (1e); G6 (1f); G7 (1g); G8 (1h)] with Ta(OGO)2 (OPri) (G=G1 (2a); G2 (2b); G3 (2c); G4 (2d); G5 (2e) G6 (2f); G7 (2g); G8 (2h). In addition to the novel derivatives (2)–(10), our earlier investigations on heterobimetallic glycolate-alkoxide derivatives have been extended to derivatives of the type
Nb(OGO)
[where M=A1 n=3, G=G3 (11);G4 (12); G6 (13) G7 (14); Gs (15); G9=CH2CH2CH2 (16) and M=Ti (n=4, G=G4) (17), Zr(n=4,G=G4) (18)], which are conveniently prepared by the reactions of metalloligands Nb(OGO)2(OGOH) [G=G3 (1c); G4 (1d); G6 (1f); G7 (1g); G8 (1h); G9 (1i)] with different metal alkoxides. All of these new complexes have been characterized by elemental analyses, molecular weight
determinations, and spectroscopic (I.r. and 1H, 27Al-n.m.r.) studies. Structural features of the new derivatives have been elucidated on the basis of molecular weight and spectroscopic
data. 相似文献
4.
The oxovanadium(IV) complexes VOC2O4 · 2DMF, VOC2O4 · 2 formamide, VOC2O4 · 2 ethylene urea, VOC2O4 · 2 urea and VOC2O4 · en have been prepared and characterized. The oxalato group functions as a bidentate ligand in all these complexes. Except ethylene diamine the remaining ligands – DMF. formamide, ethylene urea and urea – act as monodentate ligand coordinating through their carbonyl oxygen. Ethylene diamine is bound to the metal through nitrogen. In all the complexes vanadium is five coordinated in distorted tetragonal-pyramidal structures. 相似文献
5.
VOCl3 and Spiro(adamantan‐2, 2′‐homoadamantan‐3‐one) form a stable 1 : 1 complex, which has been isolated and characterised. A X‐ray structure analysis reveals a close V=O···H‐C contact supporting the presence of an analogous interaction leading to C‐H activation in the corresponding CrO2Cl2 complex. For both systems such geometrical arrangements are predicted by means of DFT calculations. The reaction of Spiro(adamantan‐2, 2′‐homoadamantan‐3‐one‐4‐olate), L2 , with VOCl3 leads to a complex [ L2 2VOCl], which can be converted to the corresponding triflate [ L2 2VO(O3SCF3)] via treatment with AgO3SCF3. The latter is a mononuclear oxovanadium(V) complex with a bulky ligand sphere where one coordination site is accessible (as the triflate ligand is quite loosely bound), and as it is furthermore soluble in organic solvents, it seems an interesting complex to start from in future experiments. 相似文献
6.
The oxovanadium(IV) complexes of the Schiff bases derived from 1,3-diamino-propane-2-ol and salicylaldehyde, 3-aldehydosalicylic acid, 5-chloro-salicylaldehyde, acetyl acetone, and also of the Schiff base derived from 1.3-diaminopropane and salicylaldehyde have been isolated in the pure state and characterized. The structure of these complexes is discussed on the basis of elemental analyses, electronic spectra and magnetic moment values. These complexes are characterized as five co-ordinate compounds having the general formula [VO](L), where, LH2 = a molecule of dibasic, tetradentate Schiff base. Electronic spectra of the complexes are found to be solvent independent. The compounds are paramagnetic (μeff. = 1.76–1.79 B. M.), and are very stable in air. 相似文献
7.
Rekha Garg Mahesh Kumar Saini Nighat Fahmi R. V. Singh 《Transition Metal Chemistry》2006,31(3):362-367
The synthesis of some new manganese(II), oxovanadium(V) and dioxomolybdenum(VI) complexes with 5-chloro-1,3-dihydro-3-[2-(phenyl)-ethylidene]-2H-indol-2-one-hydrazinecarbothioamide
(L1H) and 5-chloro-1,3-dihydro-3-[2-(phenyl)-ethylidene]-2H-indol-2-one-hydrazinecarboxamide (L2H) were carried out in unimolar and bimolar ratios. All the new derivatives have been characterized by elemental analyses,
molecular weight determinations, molar conductance, magnetic measurements, i.r., 1H-n.m.r. and e.s.r. studies. The i.r. and n.m.r. spectral data suggest the involvement of sulphur/oxygen and azomethine nitrogen
in coordination to the central metal ion. The magnetic moment values of the manganese(II) complexes are in the 5.85–6.13 B.M.
range, suggesting a high spin state in these complexes. Based on these spectral studies tetrahedral geometry for the manganese(II)
complexes and octahedral geometry for the molybdenum complexes has been proposed. In the case of the oxovanadium complexes
vanadium is in the penta and hexa coordinated environments. Compounds have been synthesized in an open vessel under microwave
irradiation (MWI) using a domestic microwave oven. The reaction time decreases from hours to minutes with improved yield as
compared to conventional heating. The free ligands and their metal complexes have been tested in vitro against a number of microorganisms in order to assess their antimicrobial properties. The results indicate that the ligands
and their respective metal derivatives possess antimicrobial properties. 相似文献
8.
Russian Journal of Coordination Chemistry - Two oxovanadium(V) complexes, [VO(L)(L1)] (I) and [VOLL2] (II), where L = acetohydroxamate, H2L1 = 2-bromo-N'-(2-hydroxybenzylidene)benzohydrazide,... 相似文献
9.
《Journal of Coordination Chemistry》2012,65(6):539-544
Silver(I) complexes of selenones, [LAgNO3] and [AgL2]NO3 (where L is imidazolidine-2-selenone or diazinane-2-selenone and their derivatives) have been prepared and characterized by elemental analysis, IR and NMR (1H, 13C and 107Ag) spectroscopy. An upfield shift in the C=Se resonance of selenones in 13C NMR and a downfield shift in N-H resonance in 1H NMR are consistent with selenium coordination to silver(I). In 107Ag NMR, the AgNO3signal is deshielded by 450-650 ppm on coordination to selenones. Greater upfield shifts in 13C NMR were observed for [LAgNO3] compared to [AgL2]NO3complexes, whereas the opposite trend was observed for 1H and107Ag NMR chemical shifts. 相似文献
10.
Shalini Rangarajan Owen A. Beaumont Maravanji S. Balakrishna Glen B. Deacon Victoria L. Blair 《Molecules (Basel, Switzerland)》2022,27(22)
Reaction of [YbCp2(dme)] (Cp = cyclopentadienyl, dme = 1,2 dimethoxyethane) with bis(diphenylphosphano)methane dioxide (H2dppmO2) leads to deprotonation of the ligand H2dppmO2 and oxidation of ytterbium, forming an extremely air-sensitive product, [YbIII(HdppmO2)3] (1), a six-coordinate complex with three chelating (OPCHPO) HdppmO2 ligands. Complex 1 was also obtained by a redox transmetallation/protolysis synthesis from metallic ytterbium, Hg(C6F5)2, and H2dppmO2. In a further preparation, the reaction of [Yb(C6F5)2] with H2dppmO2, not only yielded compound 1, but also gave a remarkable tetranuclear cage, [Yb4(µ-HdppmO2)6(µ-F)6] (2) containing two [Yb(µ-F)]2 rhombic units linked by two fluoride ligands and the tetranuclear unit is encapsulated by six bridging HdppmO2 donors. The fluoride ligands of the cage result from C-F activation of pentafluorobenzene and concomitant formation of p-H2C6F4 and m-H2C6F4, the last being an unexpected product. 相似文献
11.
Subhashree P. DashSagarika Pasayat SaswatiHirak R. Dash Surajit DasRay J. Butcher Rupam Dinda 《Polyhedron》2012,31(1):524-529
Some new oxovanadium(V) complexes, [VOL1-3(OEt)(EtOH)] (1-3), have been reported, which were obtained from the reaction of the Schiff bases H2L1-3 (where H2L1 = the salicylhydrazone of diacetyl monoxime; H2L2 = the 4-methoxy salicylhydrazone of diacetyl monoxime and H2L3 = the 4-hydroxy salicylhydrazone of diacetyl monoxime) with VO(acac)2 in a 1:1 molar ratio. Three 4-R-aroylhydrazoneoximes (V) have been used as ligands in the present study, differing in the inductive effect of the substituent R (R = H, OCH3 and OH), in order to observe their influence, if any, on the redox potentials and biological activity of the complexes. All the synthesized ligands and metal complexes were successfully characterized by elemental analysis, IR, UV-Vis and NMR spectroscopy. An X-ray diffraction study of [VOL1(OEt)(EtOH)] (1) reveals that the metal center has a distorted octahedral O5N coordination sphere, where the O,N,O donor ligand and the ethoxo group constitute a satisfactory O3N basal plane. Cyclic voltammetry of the complexes show a quasi-reversible cyclic voltammetric response in the potential range 0.29-0.36 V involving a single electron V(V)-V(IV) reduction. The complexes have also been screened for their antibacterial activity against Escherichia coli, Bacillus, Proteus and Klebsiella. Minimum inhibitory concentrations of these complexes and the antibacterial activities indicate compound 1 as the potential lead molecule for drug design. 相似文献
12.
Photolysis of a series of octahedral monoazido complexes of the type [LM(III)(didentate ligand)(N(3))](n)(+)X(n) of vanadium(III), chromium(III), and manganese(III) in the solid state or in solution yields quantitatively the corresponding six-coordinate nitrido complexes [LM(V)(didentate ligand)(N)](n)(+)X(n) and 1 equiv of dinitrogen. L represents the macrocycle 1,4,7-triazacyclononane or its N-methylated derivative (L'), the didentate ligands are pentane-2,4-dionate (acac), 2,2,6,6-tetramethylheptane-3,5-dionate (tacac), picolinate (pic), phenanthroline (phen), and oxalate (ox), and X(-) represents perchlorate or hexafluorophosphate. The following nitrido complexes were prepared: [LV(V)(N)(acac)](ClO(4)) (6), [LCr(V)(N)(acac)](ClO(4)) (13), [LCr(V)(N)(tacac)](ClO(4)) (14), [LCr(V)(N)(pic)](ClO(4)) (15), [LCr(V)(N)(phen)](ClO(4))(2) (16), [LCr(V)(N)(ox)] (19), [L'Mn(V)(N)(acac)]PF(6) (21). Photolysis of [LCr(III)(N(3))(ox)] (17) in the solid state produces the &mgr;-nitrido-bridged mixed-valent species [L(2)Cr(2)(ox)(2)(&mgr;-N)](N(3)) (18). The structures of the precursor complex [L'Mn(acac)(N(3))]BPh(4) (20), of 13, and of [L'Mn(V)(N)(acac)]BPh(4) (21) have been determined by X-ray crystallography. Complex 13 crystallizes in the orthorhombic space group Pnma, with cell constants a = 27.187(5) ?, b = 9.228(2) ?, c = 7.070(1) ?, V = 1773.7(6) ?(3), and Z = 4; complex 20 crystallizes in the triclinic space group P&onemacr; with a = 14.769(5) ?, b = 16.83(1) ?, c = 16.96(1) ?, alpha = 108.19(5) degrees, beta = 105.06(4) degrees, gamma = 99.78(4) degrees, V = 3719(2) ?(3), and Z = 4; and complex 21 crystallizes in the monoclinic space group P2(1)/n with a = 10.443(3) ?, b = 16.035(4) ?, c = 21.463(5) ?, beta = 95.76(1) degrees, V = 3575.9(14) ?(3), and Z = 4. The Cr(V)&tbd1;N and Mn(V)&tbd1;N distances are short at 1.575(9) and 1.518(4) ?, respectively, and indicate a metal-to-nitrogen triple bond. 相似文献
13.
Y. Sindhu C. J. Athira M. S. Sujamol K. Mohanan 《Phosphorus, sulfur, and silicon and the related elements》2013,188(9):1955-1963
Oxovanadium(IV) complexes of Schiff bases, derived from 2-amino-4-phenyl thiazole/substituted 2-amino-4-phenyl thiazoles and thiophene-2-aldehyde have been synthesized and characterized on the basis of elemental analysis, molar conductance measurements, magnetic susceptibility data, and UV-visible, and IR spectral studies. All the complexes are monomeric possessing a 1:2 (metal:ligand) stoichiometry. On the basis of these data, a square pyramidal geometry has been assigned for the complexes. A few complexes have been subjected to thermal decomposition studies. The ligands and their metal complexes have been screened for their antibacterial activities. Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file. 相似文献
14.
15.
Russian Journal of Coordination Chemistry - Two structurally similar new oxovanadium complexes, [VO(L)(L1)] (I) and [VO(L)(L2)] (II), where L is the dianionic form of... 相似文献
16.
A new oxovanadium(V) complex with the mixed ligand of 2-oxopropionic acid benzoylhydrazone (C10H10N2O3) and benzoylhydrazine (C7H8N2O), VO(C7H7N2O)(C10H9N2O3), has been synthesized. Its structure was determined by single crystal X-ray diffraction analysis. The crystal belongs to monoclinic system with space group P21/n and cell parameters: a=1.1136(4) nm, b=0.6217(2) nm, c=2.6038(9) nm, β=97.182(6)°, V= 1.7887(11) nm^3, Z=4, F(000)=836, Mr=407.28, Dc= 1.512 g/cm^3,μ (Mo Kα) =0.592 mm^-1, R1 =0.0445, wR2= 0.1203. Vanadium atom is 6-coordinated by carboxyl and carbonyl O atoms and N atom of one tridentate C10H10N2O3 to form two stable five-membered rings with the same edge, and the other coordinated atoms of N and O come from one bidentate benzoylhydrazine C7H8N2O. The title complex has a six-coordinated V center [VO(N2O3)] with a distorted octahedral arrangement. In the crystal lattice, there are hydrogen bonding interactions between two molecules. 相似文献
17.
18.
Stefan Lis Sławomir But 《Journal of inclusion phenomena and macrocyclic chemistry》1999,35(1-2):225-231
The heteropolytungstates [(Na)P5W30O110]4– (I), [(Na)Sb9W21O86]18– (II) and [(Na)As4W40O140]27– (III) and the monovacant Keggin structure of the general formula [XW11–xMoxO39]n– (X-Si, P; n = 7 for P and 8 for Si) (IV) as well as their europium(III) complexes were studied. The structures of I–IV as well as the europium(III) encrypted [(Eu)P5W30O110]12– (VI), [(Eu)Sb9W21O86]16– (VII), [(Eu)As4W40O140]25– (VIII) and sandwiched [Eu(XW11–xMoxO39)2]n– (n =11 for P and n = 13 for Si) (V) complexes were synthesized and spectroscopically characterized. The complexes were studied using UV-Vis absorption and luminescence, as well as the laser-induced europium ion luminescence spectroscopy. Absorption spectra of Nd(III) were used to characterize the complexes formed. Excitation and emission spectra of Eu(III) were obtained for solid complexes and their solutions. The relative luminescence intensities of the Eu(III) ion, expressed as the ratio of the two strongest lines at 594 nm and 615 nm, = I615/I594, which is sensitive to the environment of the primary coordination sphere about the Eu(III) ion, was calculated. In the case of the sandwiched [Eu(XW11–xMoxO39)2]n– complexes a linear dependence of the luminescence quantum yield of Eu(III) ion, , (calculated using [Ru(bpy)3]Cl2 as a standard) on the content of Mo (number of atoms, x) in the [Eu(XW11–xMoxO39)2]n– structure was observed. 相似文献
19.
Reactions of Cp2ZrCl2 with homometallic complexes of aluminium containing one residual hydroxy group Al(OGO)(OGOH) and Al(L)(OGOH) [where G=G1=CMe2CMe2 (1a); G=G2=CMe2CH2CHMe (1b); G= G3=CMe2CH2CH2CMe2 (1c) and L=L1=OC6H4CH=NCH2CH2O, G=G1 (2a); L=L1, G=G2 (2b); L=L1, G=G3 (2c); L=L2=OC10H6CH=NCH2CH2O, G=G1 (2d); L=L2, G=G2 (2e); L=L2, G=G3 (2f)] in THF using Et3N as HCl acceptor affords novel heterobimetallic compounds of the types Al(OGO)2Zr(Cl)Cp2 and Al(L)(OGO)Zr(Cl)Cp2, respectively. All of these derivatives have been characterised by elemental analyses, molecular weight measurements, and
spectroscopic [IR, NMR (1H and 27Al)] studies. 相似文献
20.
A. Syamal 《无机化学与普通化学杂志》1970,373(2):204-208
Synthesis of few oxovanadium (IV) complexes of C2v symmetry with low symmetry β-diketones is described. Magnetic, infrared and electronic spectral studies of the complexes are reported. Splitting of the xy → xz, yz transition is observed at 77°K and is believed to be of vibrational origin. 相似文献