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1.
Shobhana Sharma Asha Jain Sanjiv Saxena 《Phosphorus, sulfur, and silicon and the related elements》2013,188(7):1676-1688
Titanium(IV) complexes of the general formula TiL(OPr i )2 [where LH2 = R CH3 where R = ─C6H5, ─C6H4Cl(p)] were prepared by the interaction of titanium isopropoxide with sterically hindered Schiff bases derived from heterocyclic β -diketones in 1:1 molar ratio in dry benzene. The complexes TiL(OPr i )2 were used as versatile precursors for the synthesis of other titanium(IV) complexes. Titanium(IV) complexes of the type TiLL'(OPr i ) (where L'H═R1R2C═NOH, R1 = R2 = ─CH3; R1 = ─CH3,R2 = ─C6H5; R1 = ─COC6H5, R2 = ─C6H5) were synthesized by the reaction of TiL(OPr i )2 with ketooximes (L'H) in equimolar ratio in dry benzene. Another type of titanium(IV) complexes having the general formula TiLGH(OPr i ) (where GH2═HO─G─OH, G = ─CH2─CH2─) have been prepared by the reaction of TiL(OPr i )2 with glycol in 1:1 molar ratio in dry benzene. Plausible structures of these new titanium(IV) complexes have been proposed on the basis of analytical data, molecular weight measurements, and spectral studies. 相似文献
2.
Reactions of bis(acetylacetonato)aluminum(III)‐di‐μ‐isopropoxo‐di‐isopropoxo aluminum(III), [(CH3COCHCOCH3)2Al(μ‐OPri)2Al(OPri)2] with aminoalcohols, (HO R NR1R2) in 1:1 and 1:2 molar ratios in refluxing anhydrous benzene yielded binuclear complexes of the types [(CH3COCHCOCH3)2Al(μ‐OPri)2Al(O R NR1R2)(OPri)] and [(CH3COCHCOCH3)2Al(μ‐OPri)2Al(O R NR1R2)2] (R (CH2)3 , R1 = R2 = H; R = CH2C(CH3)2 , R1 = R2 = H; R = (CH2)2 , R1 = H, R2 = CH3; and R (CH2)2 , R1 = R2 = CH3), respectively. All these compounds are soluble in common organic solvents and exhibit sharp melting points. Molecular weight determinations reveal their binuclear nature in refluxing benzene. Plausible structures have been proposed on the basis of elemental analysis, molecular weight measurements, IR, NMR (1H, 13C, and 27Al), and FAB mass spectral studies. 27Al NMR spectra show the presence of both five‐ and six‐coordinated aluminum sites. © 2003 Wiley Periodicals, Inc. Heteroatom Chem 14:518–522, 2003; Published online in Wiley InterScience (www.interscience.wiley.com). DOI 10.1002/hc.10184 相似文献
3.
Hexaisopropoxoniobates/tantalates of lathanides of the type [Ln{(μ‐OPri)2M(OPri)4}3] (M = Nb, Ln = Y( 1 ), La( 2 ), Nd( 3 ), Er( 4 ), Lu( 5 ); M = Ta, Ln = Y( 6 ), Gd( 7 )) have been prepared by the reactions of LnCl3.3PriOH with three equivalents of KM(OPri)6 in benzene. Reactions in 1:2 molar ratio of LnCl3.3PriOH with KTa(OPri)6 yielded derivatives of the type [{(PriO)3Ta(μ‐OPri)3}Ln{(μ‐OPri)2Ta(OPri)4}(Cl)] (Ln = Y( 8 ), Gd( 9 )), which on interactions with one equivalent of KOPri afforded [{(PriO)3Ta(μ‐OPri)3}Ln {(μ‐OPri)2Ta(OPri)4}(OPri)] (Ln = Y( 10 ), Gd( 11 )). All these derivatives have been characterized by elemental analyses and molecular weight measurements as well as by their spectroscopic [IR, 1H and 13C NMR (Y, La, Lu), electronic (Nd, Er)] studies. 89Y NMR studies have also been carried out on derivatives ( 6 ), ( 8 ), and ( 10 ). 相似文献
4.
Shobhana Sharma Asha Jain Sanjiv Saxena 《Phosphorus, sulfur, and silicon and the related elements》2013,188(7):1689-1701
Zirconium(IV) Schiff base chelates having the general formula ZrL(OPr i )2 [where LH 2 = R CH 3 , R = –C 6 H 5 , –C 6 H 4 Cl(p)] were synthesized by the reaction of Zr(OPr i )4.Pr i OH with sterically constrained sulfur-containing Schiff bases of heterocyclic β -diketones in a 1:1 molar ratio in dry refluxing benzene. The complexes ZrL(OPr i ) 2 were used as important precursors for the synthesis of the complexes of the type Zr(L) 2 . The complexes, Zr(L) 2 , were prepared by the interaction of precursor ZrL(OPr i ) 2 with sterically constrained sulfur-containing Schiff bases of heterocyclic β -diketones in a 1:1 molar ratio in dry benzene. The structures of these zirconium(IV) chelates have been discerned with the help of elemental analyses, physicochemical studies, and spectral [IR and NMR ( 1 H and 13 C)] data. A distorted trigonal bipyramidal and a distorted octahedral geometry may be assigned to zirconium(IV) chelates of the types ZrL(OPr i ) 2 and Zr(L) 2 , respectively. 相似文献
5.
Mohammad Nasir Uddin Md. Shaharier Amin Md. Saifur Rahman Sonia Khandaker Wahhida Shumi Md. Atiar Rahman Sheikh Mahbubur Rahman 《应用有机金属化学》2021,35(1)
Symmetrical bis‐Schiff bases (LH 2) have been synthesized by the condensation of 1,6‐hexanediamine (hn) and carbonyl or dicarbonyl. One of the synthesized Schiff bases has been subjected to the molecular docking for the prediction of their potentiality against coronavirus (SARS‐CoV‐2). Molecular docking revealed that tested Schiff base possessed high binding affinity with the receptor protein of SARS CoV‐2 compared with hydroxychloroquine (HCQ). The ADMET analysis showed that ligand is non‐carcinogenic and less toxic than standard HCQ. Schiff bases acting as dibasic tetra‐dentate ligands formed titanium (IV) complexes of the type [TiL(H2O)2Cl2] or [TiL(H2O)2]Cl2 being coordinated through ONNO donor atoms. Ligands and complexes were characterized by the elemental analysis and physicochemical and spectroscopic data including FTIR, 1H NMR, mass spectra, UV‐Visible spectra, molar conductance, and magnetic measurement. Optimized structures obtained from quantum chemical calculations supported the formation of complexes. Antibacterial, antifungal, and anti‐oxidant activity assessments have been studied for synthesized ligands and complexes. 相似文献
6.
Yolanda Pérez Mariano Fajardo Antonio Otero 《Journal of organometallic chemistry》2003,679(2):220-228
A family of titanium(IV) alkoxide compounds [{Ti(OPri)3(OR)}2], [{Ti(OPri)2(OR)2}2], and Ti(OR)4 (1-12) have been prepared using two different routes: by metathesis reaction of TiCl(OPri)3 and TiCl2(OPri)2 with ROH in the presence of Et3N and alternatively by alcohol exchange of Ti(OPri)4 and the corresponding higher boiling alcohol (ROH=adamantanol, 1,2:3,4-di-O-isopropylidene-α-d-galactopyranose, 1,2:5,6-di-O-isopropylidene-α-d-glucofuranose, 1R,2S,5R-(−)-menthol). These tetra alkoxide titanium(IV) compounds have been characterized by spectroscopic techniques. In addition, some of these chiral Lewis acid titanium compounds, derived from diacetone galactose and diacetone glucose, have been studied in the asymmetric epoxidation of cinnamyl alcohol in order to evaluate their catalytic activity and stereoselectivity. 相似文献
7.
A series of some new mixed ligand complexes have been synthesized with an objective for evaluation as antimicrobials. Reactions of diorganotin(IV) dichloride with dibenzoyl methane and O‐alkyl trithiophosphates in a 1:1:1 molar ratio in refluxing benzene yield products of the type [PhCOCHCOPh]R2Sn‐[SSH(S)POR'] [where R = Me, Bu, Ph; R' = Me, Et, Pri, Bui, Ph]. The newly synthesized complexes are light yellow colored crystalline solids, non‐volatile, soluble in common organic solvents, monomeric in nature and highly sensitive towards atmospheric moisture. These complexes are characterized by elemental analysis, IR and multinuclear NMR (1H, 31P and 119Sn) spectral studies. Spectral studies of these complexes indicate that dibenzoyl methane and O‐alkyl trithiophosphate moieties are bidentate and the central tin atom is hexacoordinated in nature. A few of these compounds were tested for their antibacterial activity using standard drugs. 相似文献
8.
Heterobimetallic alkoxides of Cu(II) of the types [Cu{η4-Ti2(OEt)9}Cl] (1) and [Cu{η3-Ti2(OR)9}2] [R = Pri
(2), R = Et(3)] have been prepared for the first time by the reactions of CuCl2 · xROH with KTi2(OR)9 in 1:1 and 1:2 molar ratios, respectively, in benzene medium. The chloro(nonaalkoxo dititanato)copper(II) complexes undergo
chloride replacement reactions by a variety of monodentate alkoxo (−OPri, −OEt) and chelating [Al(OPri)
4
−
, Al(OEt)
4
−
, Nb(OPri)
6
−
, Zr2(OPri)
9
−
, Sn2(OPri)
9
−
, and Sn2(OEt)
9
−
] ligands to form interesting hetero(bi-and tri-)metallic complexes. Alcoholysis (with methyl alcohol and tert-butyl alcohol) and hydrolytic [with Ba(OH)2 · 8H2O powder] reactions of a few typical compounds have also been investigated. All of these have been characterized by elemental
analyses, molecular weight determinations, spectral (i.r. and visible) and magnetic studies. On attempted volatilization under
reduced pressure these complexes liberated titanium alkoxides as a volatile component leaving nonvolatile residues. 相似文献
9.
Reena Agrawal Jyoti Sharma Yashpal Singh Durgesh Nandani Amla Batra 《Phosphorus, sulfur, and silicon and the related elements》2013,188(3):516-525
Chloro bis(alkylenedithiophosphato)antimony(III) complexes of the type [OGOP(S)S]2SbCl (1–5) [where G = —C(Me)2—CH2—CH(Me)—1 —C(Me)2—C(Me)2—2, —CH2—C(Me)2—CH2—3, —CH(Me)—CH(Me)—4 and –CH(Me)—CH2—CH2—5] have been synthesized by the reaction of SbCl3 with sodium salts of alkylenedithiophosphoric acids in a 1:2 molar ratio in refluxing benzene. Reactions of chloro bis(alkylenedithiophosphato) antimony(III) compounds, [OGOP(S)S]2SbCl with sodium tetraisopropoxoborate, NaB(OPri)4, in a 1:1 molar ratio in refluxing benzene yielded some new heterobinuclear derivatives of antimony(III) and boron(III) of the type[OGOP(S)S]2Sb(μ—OPri)2B(OPri)2. These newly synthesized complexes have been characterized by elemental analysis and molecular weight measurement, and their plausible structures have been proposed on the basis of IR, NMR (1H, 13C,31P,11B), and FAB-mass spectral studies. On the basis of the spectroscopic evidence, a pseudo octahedral geometry around antimony and tetrahedral geometry around boron atom has been proposed. Cyclic O,O′-alkylenedithiophosphate ligands and their corresponding chloro bis(alkylenedithiophosphato)antimony(III) compounds have been screened for microbial activities. These compounds showed significant antifungal activity against Fusarium and Trichoderma and antibacterial activity against E. Coli and Pseudomonas. 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
10.
Novel termetallic isopropoxides are reported which may be represented by the general formulae: [(PriO)3M(μ-OPri)2Be(μ-OPri)2Al(OPri)2], [(PriO)2M(μ-OPri)2Be(μ-OPri)2Al(OPri)2]2 [where M = Ti(IV), Zr(IV) and Hf(IV)] and [(PriO)4M(μ-OPri)2Be(μ-OPri)2Al(OPri)2] [where M = Nb(V) and Ta(V)]. Attempts to synthesize derivatives with the general formula, [(PriO)7M2(μ-OPri)2Be(μ-OPri)2Al(OPri)2] [where M = Ti(IV), Zr(IV) or Hf(IV)], were unsuccessful and in all such cases a mixture of M(OPri)4 and [(PriO)3M(μ-OPri)2Be(μ-OPri)2Al(OPri)2] was obtained. All these derivatives are soluble in common organic solvents and with the exception of titanium(IV) derivatives, they can be volatilised without noticeable disproportionation. These products have been characterized by elemental analyses, molecular weights, IR, 1H NMR and (in representative cases) mass spectral studies also. 相似文献
11.
Cristiano Egevardt Siddhartha O. K. Giese Alan D. da C. Santos Andersson Barison Eduardo L. de Sá Arion Zandoná Filho Thiago A. da Silva Sônia F. Zawadzki Jaísa F. Soares Giovana G. Nunes 《Journal of polymer science. Part A, Polymer chemistry》2014,52(17):2509-2517
The ionic [Ti3(µ3‐OPri)2(µ‐OPri)3(OPri)6][FeCl4] halo‐alkoxide ( A ) was investigated for its activity towards the bulk polymerization of rac‐lactide (rac‐LA) and ?‐caprolactone (?‐CL) in various temperatures, monomer/ A molar proportions, and reaction times. The reactivity of A in the ring‐opening polymerization (ROP) of both monomers is mainly due to the cationic [Ti3(OPri)11]+ unity and proceeds through the coordination–insertion mechanism. Molecular weights ranging from 6,379 to 13,950 g mol?1 and PDI values varying from 1.22 to 1.52 were obtained. Results of ROP kinetic studies for both ?‐CL and rac‐LA confirm that the reaction rates are first‐order with respect to monomers. The production of poly(?‐caprolactone) shows a higher sensitivity of the reaction rate to temperature, while the polymerization of rac‐LA is slower and more dependent on the thermal stability of the active species during the propagation step. © 2014 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2014 , 52, 2509–2517 相似文献
12.
Reactions of [ZnAl2(OPri)8] [A] with acetoxime in different molar ratios in refluxing anhydrous benzene, yield complexes of the type [ZnAl2(OPri)8?n{(CH3)2CNO}n] {where, n = 1–4}. All the complexes are transparent viscous/foamy solids. They were characterized by elemental analyses, FT-IR and NMR (1H, 13C {1H}) spectral studies. 27Al NMR spectrum of [ZnAl2(OPri)4{(CH3)2CNO}4] [4] in CDCl3 suggests presence of four coordination around both the aluminum atoms. IR spectra suggest that the oximato ligands bind the aluminum atoms in a side on manner in all the complexes. The ESI-mass spectrum of the representative derivative [4] suggests its monomeric nature while the thermo-gravimetric curve shows its low thermal stability. Sol–gel transformations of the precursors (A), (1), and (4) yielded nano-sized ZnAl2O4 samples (a), (b) and (c) at ~500 °C, respectively. The XRD patterns of (a), (b) and (c) indicate formation of cubic phase nano-sized zinc aluminate in all the samples. Surface morphologies of these samples were investigated by SEM images. IR spectra as well as EDX analyses indicate formation of pure zinc aluminate in all the cases. TEM image of sample (c) shows spherical (~5–8 nm) morphology. 相似文献
13.
ZrCl4 reacts with the potassium salt of the bifunctional tridentate Schiff base HOC6H4C(H)=NCH2CH(Me)OH (LH2) in a 1:1 molar ratio in benzene to give a new complex Zr(L)Cl2 which, on reaction with different potassium isopropoxymetallates [e.g., KAl(OPr
i
)4, KTi(OPr
i
)5, and KNb(OPr
i
)6], yield novel heterobimetallic derivatives. These new homo and heteronuclear coordination compounds have been characterized by elemental (N, Cl, Al, Ti, and Nb) analyses, molecular weight (ebullioscopic) measurements and spectral [i.r., n.m.r. (1H, 13C and 27Al)] studies and probable structures for them have been suggested. 相似文献
14.
Ln(R)3, Ln(R)2(OPri), and Ln(R)(OPri)2 (where Ln = La, Pr, Nd, and Sm; R = deprotonated furfuryl alcohol, RH) were prepared from lanthanide isopropoxide and furfuryl alcohol in 1:3, 1:2 and 1:1 stoichiometric ratios respectively in anhydrous benzene under reflux. Ln(R)2-(OPri) and Ln(R)(OPri)2 were also obtained at room temperature. The isopropoxy group(s) of these derivatives were replaced by tertiary butoxy group(s) during the alcohol exchange reactions with tertiary butanol. All these derivatives are soluble in benzene except the tertiary butoxy derivatives which are only sparingly soluble. However, they become insoluble on standing. These furfuroxides did not distil at ~300°C/102 torr but decomposed. Isopropoxy/butoxy furfuroxides were characterized by the elemental analysis and also by estimating the liberated isopropanol. The i.r. spectra of Ln(R)3 clearly supports the presence of furfuroxide groups in these derivatives. 相似文献
15.
Z. Z. Baroš B. K. Adnađević 《Russian Journal of Physical Chemistry A, Focus on Chemistry》2011,85(13):2295-2298
The influence of the molar ratio h = [H2O]/[Ti(OR)4] (R = Pr
i
) on the kinetics of the titanium-oxo-alkoxy clusters (TOAC) nucleation was studied. Clusters were formed by the titanium
tetraisopropoxide Ti(OPr
i
)4 chemical reaction with H2O in n-propanol solution, with the fixed concentration of Ti(OPr
i
)4 (c = 0.04 M), molar ratio h ∈ {11, 14, 17, 20} and temperature T ∈ {298, 308, 318} K. It was determined that the isothermal rate of clusters nucleation is a power law function of the molar
ratio h. The kinetic parameter β value changes complexly as h and T change. The value of apparent activation energy of the nucleation process (E
a) decreases with the increase of value h. It was found that nucleation is a reaction with complex kinetics whose elementary stages are hydrolysis Ti(OR)4 to Ti(OR)3OH and formation of titanium-oxo-alkoxy clusters [Ti
n + βOβ](OR)4n + 2β through the alcoxolation reaction. 相似文献
16.
U. N. Tripathi A. Siddiqui Mohd. Safi Nitya Sharma Neetu Srivastava 《Phosphorus, sulfur, and silicon and the related elements》2013,188(9):1993-2001
Dichlorotitanium(IV) trithiophosphates of the type TiCl2[(RO)P(S)S2] (where R = Me, Et, Prn, Pri, Bun, Bus, Bui, Ami, Ph and cyclohexyl) have been synthesized for the first time by the reaction of titanium tetrachloride with potassium trithiophosphates in a 1:1 molar ratio in anhydrous benzene. Sol-gel chemistry of these titanium(IV) compounds has been studied in dry benzene by treatment with hydrogen sulfide gas. These newly synthesized derivatives have been characterized by elemental analysis (C, H, S, Cl, and Ti), molecular weight measurement, and spectral [IR and multinuclear NMR (1H, 13C, and 31P)] studies. The bonding mode of trithiophosphate ligands and tentative structure around titanium(IV) are discussed. 相似文献
17.
Sharma Kanupriya Sharma Malti Singh Anirudh Mehrotra Ram C. 《Transition Metal Chemistry》2002,27(3):326-328
Ti(OPr
i
)4 or Zr(OPr
i
)4 · Pr
i
OH react with hydrocarbon-insoluble complexes M{(OCH2CH2)NH(CH2CH2OH)}2 (M = Mg, Ca, Sr, Ba) in a 2:1 molar ratio to yield hydrocarbon-soluble heterobimetallic diethanolaminate isopropoxide complexes [M{(OCH2CH2)2NH}2{M(OPr
i
)3}2] (M = Mg, Ca, Sr, Ba; M = Ti, Zr), which have been characterized by elemental analyses, molecular weight measurements and spectroscopic [i.r., n.m.r. (1H and 13C)] studies. 相似文献
18.
Spectroscopic,DFT and antimicrobial activity of Zn(II), Zr(IV), Ce(IV) and U(VI) complexes of N,N‐ chelated 4,6‐bis (4‐chlorophenyl)‐2‐amino‐1,2‐dihydropyridine‐3‐carbinitrile
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Four novel metal complexes of 4,6‐bis (4‐chlorophenyl)‐2‐amino‐1,2‐dihydropyridine‐3‐carbinitrile (H2L) with Zn(II), Zr(IV), Ce(IV) and U(VI) were synthesized. The structure was elucidated using elemental analysis, melting point, molar conductivity; spectroscopic techniques (IR, 1H NMR, UV–Vis., mass spectra) as well as thermo gravimetric analysis. The spectroscopic data proved that H2L chelated with the metal ions as a bidentate ligand through Namino and Ncarbinitrile atoms. The molecular structure of the complexes was determined using density functional theory (DFT). The central metal ion in each complex is six‐coordinate and the angles around it vary from 62.74° to 166.46°; these values agree with distorted octahedral geometry. The calculated total energy of the complexes found in the region – 406.342 to ?459.717 au and the dipole moment change from 4.675 to 13.171D. The antibacterial and antifungal activities of the ligand, metal salts and complexes were estimated on some microorganisms. The complexes showed significant antibacterial profile in comparison to the free ligand. 相似文献
19.
《Journal of Coordination Chemistry》2012,65(4):381-392
Reactions of bis ( g -diketonato) aluminium(III)-di- w -isopropoxo-di-isopropoxo-aluminium (III), [CH3COCHCOR)2Al( w -OPri)2Al(OPri) 2], with triphenylsilanol, Ph3SiOH, in 1:1 and 1:2 molar ratios and with diphenylsilanediol, Ph2Si(OH)2, in a 1:1 molar ratio, have resulted in the synthesis of [(CH3COCHCOR)2Al( w -OPri)2Al(OSiPh3)(OPri)], [(CH3COCHCOR)2Al( w -OPri)2Al(OSiPh3)2] and [(CH3COCHCOR)2Al( w -OPri)2Al(OSiPh2O], respectively. These are soluble in a variety of organic solvents ( e.g. , benzene, chloroform and dimethylsulfoxide) and show dinuclear behaviour in chloroform. These derivatives have been characterized by elemental analyses, molecular weight measurements, IR and NMR (1H, 13C and 27Al) studies. 相似文献
20.
Totally sixteen new titanium and zirconium non-Cp complexes supported by Schiff-base, or thiophene diamide ligands have been synthesized. The complexes are obtained by the reaction of M(OPr-i)4(M=Ti,Zr) with the corresponding Schiff-base ligand in 1:1 molar ratio in good yield. The thiophene diamide titanium complex has been prepared from trimethylsilyl amine [N,S,N] ligand and TiCl4 in toluene at 120℃. All complexes are well charac-terized by ^1H NMR, IR, MS and elemental analysis. When activated by excess methylaluminoxane (MAO), complexes show moderate catalytic activity for ethylene polymerization, and complex If (R^1=CH3,R^2=Br) exhibits the highest activity for ethylene and styrene polymerization. When the complexes were preactivated by triethylaluminum (TEA), both polymerization activities and syndiotacticity of the polymers were greatly improved. 相似文献