共查询到20条相似文献,搜索用时 15 毫秒
1.
M.N. Sokolov N.E. Fyodorova R. Paetow A.G. Ravelo V.E. Fedorov 《Inorganica chimica acta》2007,360(6):2192-2196
The reactions of [ReCl3(CH3CN)(PPh3)2] with benzil PhC(O)C(O)Ph, and with a natural 1,2-naphthoquinone derivative, β-lapachone (Lap), result in oxidative addition with the formation of Re(V) complexes with stilbenediolate, [ReCl3(PhC(O)C(O)Ph)(PPh3)] (1) and with a reduced semiquinonic form of lapachone, [ReIVCl3(Lap−)(PPh3)] (2). The structures of both compounds were established by X-ray crystallography. 相似文献
2.
The reaction of 2-(2-aminophenyl)benzothiazole (Habt) with [Re(CO)5Br] led to the isolation of the rhenium(I) complex fac-[Re(Habt)(CO)3Br] (1). With trans-[ReOCl3(PPh3)2], the ligand Habt decomposed to form the oxofree rhenium(V) complex [Re(itp)2Cl(PPh3)] (2) (itp = 2-amidophenylthiolate). From the reaction of trans-[ReOBr3(PPh3)2] with 2-(2-hydroxyphenyl)benzothiazole (Hhpd) the complex [ReVOBr2(hpd)(PPh3)] (3) was obtained. Complexes 1-3 are stable and lipophilic. 1H NMR and infrared assignments, as well as the X-ray crystal structures, of the complexes are reported. 相似文献
3.
Reactions of labile [MCl3(PPh3)2(NCMe)] (M = Tc, Re) precursors with 1H-benzoimidazole-2-thiol (H2L1), 5-methyl-1H-benzoimidazole-2-thiol (H2L2) and 1H-imidazole-2-thiol (H2L3), in the presence of PPh3 and [AsPh4]Cl gave a new series of trigonal bipyramidal M(III) complexes [AsPh4]{[M(PPh3)Cl(H2L1-3)3]Cl3} (M = Re, 1-3; M = Tc, 4-6). The molecular structures of 1 and 3 were determined by X-ray diffraction. When the reactions were carried out with benzothiazole-2-thiol (HL4) and benzoxazole-2-thiol (HL5), neutral paramagnetic monosubstituted M(III) complexes [M(PPh3)2Cl2(L4,5)] (M = Re, 8, 9; M = Tc, 10, 11) were obtained. In these compounds, the central metal ions adopt an octahedral coordination geometry as authenticated by single crystal X-ray diffraction analysis of 8 and 11. Rhenium and technetium complexes 1, 4 and rhenium chelate compounds 8, 9 have been also synthesized by reduction of [MO4]− with PPh3 and HCl in the presence of the appropriate ligand. All the complexes were characterized by elemental analyses, FTIR and NMR spectroscopy. 相似文献
4.
Valerio BertolasiAndrea Marchi Lorenza MarvelliRoberto Rossi Claudio Bianchini Isaac de los RiosMaurizio Peruzzini 《Inorganica chimica acta》2002,327(1):140-146
The reaction of the rhenium(V) nitrido complex [Re(N)Cl2(PPh3)2] with the tripodal ligand N(CH2CH2PPh2)3 (NP3) in THF gave [Re(N)Cl2(η2-P,P-NP3)] (1) in which NP3 acts as a tridentate ligand using the nitrogen and two phosphorus donors for coordination. Refluxing 1 in a polar solvent such as ethanol produced [(η4-NP3)Re(N)Cl]Cl (2) in which NP3 acts as a tetradentate ligand. Treatment of complex [Re(O)Cl3(AsPh3)2] containing the [ReO]3+ core with NP3 in THF yielded [ReCl3{η3-N,P,P-(N{CH2CH2Ph2}2{CH2CH2P(O)Ph2})}] (3). Complexes 1 and 3 have been characterized by single-crystal X-ray analyses. 相似文献
5.
Gabriele Albertin Stefano Antoniutti Giovanni Roveda 《Inorganica chimica acta》2005,358(11):3093-3105
Dithioformato [Re{η2-SC(H)S}(NO)P3]BPh4 (1), thioformamido [Re{η2-RNC(H)S}(NO)P3]BPh4 (2) (R = Et, p-tolyl), formamido [Re{η2-PhNC(H)O}(NO)P3]BPh4 (3) and formamidinato [Re{η2-p-tolylNC(H)Np-tolyl}(NO)P3]BPh4 (4) (P = PPh2OEt) complexes were prepared by allowing the hydride ReH2(NO)P3 to react first with triflic acid and then with the appropriate heteroallene CS2, RNCS, PhNCO and p-tolylNCNp-tolyl. Treatment of the ReH2(NO)L(PPh3)2 [L = P(OEt)3, PPh(OEt)2] and ReH2(NO)(PPh3)3 hydrides first with triflic acid and then with isothiocyanate RNCS (R = Et, p-tolyl) gave the [Re{η2-RNC(H)S}(NO){P(OEt)3}(PPh3)2]BPh4 (5, 6) and [Re(η2-RNC(H)S)(NO)(PPh3)3]BPh4 (7) derivatives. Depending on the nature of the phosphite, instead, the reaction of ReH2(NO)L(PPh3)2 and ReH2(NO)(PPh3)3 hydrides first with CF3SO3H and then with isocyanate R1NCO (R1 = Ph, p-tolyl) gave the chelate [Re{η2-R1NC(H)O}(NO){P(OEt)3}(PPh3)2]BPh4 (8) and [Re{η2-R1NC(H)O}(NO)(PPh3)3]BPh4(10) complexes with P(OEt)3 or PPh3, while the η1-coordinate [Re{η1-RNC(H)S}(NO){PPh(OEt)2}2(PPh3)2]BPh4 (9) derivative was obtained with the PPh(OEt)2 phosphite ligand. η1-Coordinate dithioformato [Re{η1-SC(H)S}(NO){PPh(OEt)2}2(PPh3)2]BPh4 (11) and formato [Re{η1-OC(H)O}(NO){PPh(OEt)2}2(PPh3)2]BPh4 (12) complexes, as well as the formamidinato [Re{η2-p-tolylNC(H)Np-tolyl}(NO){P(OEt)3}(PPh3)2]BPh4 (13) derivative were also prepared. 相似文献
6.
Xiao-Yi Yi 《Inorganica chimica acta》2006,359(11):3581-3588
Treatment of [Ti(OPri)2Cl2] with K(tpip) (tpip− = [N(PPh2O)2]−) followed by chlorination with HCl afforded cis-[Ti(tpip)2Cl]2 (1). Reduction of 1 with Na/Hg in THF gave [Ti(tpip)3] (2), which could also be prepared from [TiCl3(THF)3] and K(tpip). Recrystallization of [V(O)(tpip)2] (3) from CH2Cl2-Et2O in air afforded trinuclear [{V(O)}3(μ-tpip)3(μ-O)3] (4). Treatment of [Cr(NBut)2Cl2] and [Cr(NBut)Cl3(dme)] (dme = 1,2-dimethoxyethane) with [Ag(tpip)]4 led to isolation of [Cr(tpip)3] (6) and [Cr(NBut)(tpip)2Cl] (7), respectively. The Ti- and V-tpip complexes are capable of catalyzing oxidation of sulfides with tert-butyl hydroperoxide and H2O2. The crystal structures of 1, 2, and 4 have been determined. 相似文献
7.
The [ReOX3(AsPh3)(OAsPh3)] (X = Cl or Br) complexes react with two equivalents of 3,5-dimetylopyrazole (3,5-Me2pzH) in acetone at room temperature to give [{Re(O)X2(3,5- Me2pzH)2}2(μ-O)] (1 and 2). In the case of [ReOBr3(AsPh3)(OAsPh3)], a small quantity of the dinuclear rhenium complex [{Re(O)Br(3,5-Me2pzH)}2(μ-O)(μ-3,5-Me2pz)2] (3) has been isolated next to the main product 2. Treatment of [ReOX3(PPh3)2] compounds with two equivalents of 3,5-Me2pzH in acetone at room temperature leads to the isolation of symmetrically substituted dinuclear rhenium complexes [{Re(O)X(PPh3)}2(μ-O)(μ-3,5-Me2pz)2] (4 and 5). Refluxing of [ReO(OEt)X2(PPh3)2] complexes with 3,5-Me2pzH in ethanol affords unsymmetrically substituted dinuclear rhenium [{Re(O)X(PPh3)}(μ-O)(μ-3,5-Me2pz)2{Re(O)X(3,5- Me2pzH)}] complexes (6 and 7). The complexes obtained in these reactions have been characterised by IR, UV-Vis, 1H and 31P NMR. The crystal and molecular structures have been determined for 1, 2, 3, 4, 6 and 7 complexes. 相似文献
8.
A series of osmium(VI) nitrido complexes containing pyridine-carboxylato ligands OsVI(N)(L)2X (L = pyridine-2carboxylate (1), 2-quinaldinate (2) and X = Cl (a), Br (1b and 2c) or CH3O (2b)) and [OsVI(N)(L)X3]− (L = pyridine-2,6-dicarboxylate (3) and X = Cl (a) or Br (b)) have been synthesised. Complexes 1 and 2 are electrophilic and react readily with various nucleophiles such as phosphine, sulfide and azide. Reaction of OsVI(N)(L)2X (1 and 2) with triphenylphosphine produces the osmium(IV) phosphiniminato complexes OsVI(NPPh3)(L)2X (4 and 5). The kinetics of nitrogen atom transfer from the complexes OsVI(N)(L)2Br (2c) (L = 2-quinaldinate) with triphenylphosphine have been studied in CH3CN at 25.0 °C by stopped-flow spectrophotometric method. The following rate law is obtained: −d[Os(VI)]/dt = k2[Os(VI)][PPh3]. OsVI(N)(L)2Cl (L = 2-quinaldinate) (2a) reacts also with [PPN](N3) to give an osmium(III) dichloro complex, trans-[PPN][OsIII(L)2Cl2] (6). Reaction of OsVI(N)(L)2Cl (L = 2-quinaldinate) (2a) with lithium sulfide produces an osmium(II) thionitrosyl complex OsII(NS)(L)2Cl (7). These complexes have been structurally characterised by X-ray crystallography. 相似文献
9.
The reactions of [ReCl2{η2-NNC(O)Ph}(PPh3)2] (1) with t-BuOOH, in C6H6 or chlorinated solvents, at room temperature or with MeOH upon reflux in air lead to the trichloro-η1-benzoyldiazenido [ReCl3{η1-NNC(O)Ph}(PPh3)2] (2) or the methoxy-oxo [ReOCl2(OMe)(PPh3)2] (3) compound, respectively, which have been characterized by spectroscopic and FAB+-MS methods, elemental and single crystal X-ray diffraction analyses. They show distorted octahedral coordinaiton geometries with trans triphenylphosphine ligands, an essentially linear η1-diazenido moiety in 2 and the methoxy group in 3 in trans position to the oxo ligand. 相似文献
10.
Rojalin Sahu 《Inorganica chimica acta》2010,363(7):1448-63
In air, hydrated ethanolic (95%) solution of 2-(aminomethyl) substituted pyridine and quinoline, on stirring with half equivalent of Cu(OAc)2·H2O, respectively afforded [Cu(bpca)(OAc)(H2O)]·H2O (1) and [Cu(bqca)(OAc)(H2O)] (2) {bpca = bis(2-pyridylcarbonyl)diimide ion and bqca = bis(2-quinolylcarbonyl)diimide ion} in good yields. These reactions involve oxidation of the methylene group and formation of the bond between nitrogen and carbon in N-C(O) through coupling. The complex [Cu(pqca)(OAc)(H2O)]3[Cu2(OAc)4(EtOH)2]1.5 (3) {pqca = (2-pyridylcarbonyl)(2-quinolylcarbonyl)diimide ion} was synthesized by stirring an ethanolic solution of the Schiff base [(2-pyridyl)-N-((2-quinolyl)methylene)methanamine] (L1) and with one equivalent of Cu(OAc)2·H2O. A plausible mechanism for the conversion has been proposed. The free ligands were isolated as crystalline solids from compounds 1-3, by extrusion of Cu2+ ion using EDTA2−. The molecular structures of 1-3 and bqcaH were established by X-ray crystallography and compounds having quinolyl group have π-stacking interactions. 相似文献
11.
Hybrid scorpionate/cyclopentadienyl titanium and zirconium complexes with alkoxide and imido ligands
Antonio Otero Juan Fernández-Baeza Antonio Antiñolo Agustín Lara-Sánchez Margarita Sánchez-Molina Manuel Urbano-Cuadrado 《Inorganica chimica acta》2009,362(8):2909-2789
The reactivity of hybrid scorpionate/cyclopentadienyl ligand-containing trichloride zirconium complexes [ZrCl3(bpzcp)] (1) [bpzcp = 2,2-bis(3,5-dimethylpyrazol-1-yl)-1,1-diphenylethylcyclopentadienyl] and [ZrCl3(bpztcp)] (2) [bpztcp = 2,2-bis(3,5-dimethylpyrazol-1-yl)-1-tert-butylethylcyclopentadienyl] toward several lithium alkoxides has been carried out. Thus, alkoxide-containing complexes [ZrCl2(OR)(bpzcp)] (R = Me, 3; Et, 4; iPr, 5; (R)-2-Bu, 6), [ZrCl2(OR)(bpztcp)] (R = Me, 7; Et, 8; iPr, 9; (R)-2-Bu, 10) and [Zr(OR)3(bpztcp)] (R = Et, 11; iPr, 12) were prepared by deprotonation of the appropriate alcohol group with BunLi followed by reaction with 1 or 2. In addition, the imido-complex [Ti(NtBu)Cl(bpztcp)(py)] (13) were also prepared. The structures of these complexes have been proposed on basis of spectroscopic and DFT methods. 相似文献
12.
Prashant Kumar Mahendra Yadav Sanjay Kumar Singh Daya Shankar Pandey 《Inorganica chimica acta》2011,368(1):124-131
Synthesis and characterization of the ruthenium complexes [RuH(CO)Cl(κ1-P-PPh2Py)2(PPh3)] (1) and [Ru(CO)Cl2(κ1-P-PPh2Py)(κ2-P-N-PPh2Py)] (2) containing diphenyl-2-pyridylphosphine (PPh2Py) are described. Spectral and structural data suggested linkage of the PPh2Py in κ1-P bonding mode in 1 and both the κ1-P and κ2-P-N bonding modes in 2. The complex 1 reacted with N,N-donor bases viz., ethylenediamine (en), N,N′-dimethyl-(ethylenediamine) (dimen), 1,3-diaminopropane (diap), 2,2′-bipyridine (bipy), 1,10-phenanthroline (phen) and di-2-pyridylaminomethylbenzene (dpa) to afford cationic complexes of formulation [RuH(CO)(κ1-P-PPh2Py)2(N-N)]+ (3-8) [N-N = en, 3; dimen, 4; diap, 5; bipy, 6; phen, 7; and dpa, 8], which have been isolated as their tetrafluoroborate salts. The complexes under investigation have been characterized by elemental analyses, spectroscopic and electrochemical studies. Molecular structures of 2, 3, 6, and 8 have been determined by single crystal X-ray diffraction analyses. Further, the complexes 1-8 act as effective precursor catalyst in transfer hydrogenation of acetophenone/ketones in basic 2-propanol. 相似文献
13.
Lukasz Ponikiewski 《Inorganica chimica acta》2008,361(1):43-48
The synthesis and structural characterization of the copper salts [Cu2(2-Boc-benzoate)4(dme)2] (1), [Cu(2-Boc-benzoate)2(tmeda)] (2), [Cu2(2-Boc-benzoate)2(dppm)] (3), [Cu(2-Boc-nicotinate)(PPh3)2] (4), [Cu2{2-Boc-5,6-anhydride-naphthylcarboxylate}2(dppm)2] (5) [dme = 1,2-dimethoxyethane, dppm = bis(diphenylphosphino)methane, tmeda = N,N′-tetramethylethylenediamine, Boc = tert-butoxycarbonyl] prove that cyclic organic anhydrides and dianhydrides readily insert into the Cu-O bond of [CuOtBu] forming carboxylate ligands with ester functionalities in the ligand periphery. [Sb(CO2Ph-o-CO2Me)2(OMe)(tmeda)] (6) was synthesised by insertion reaction of Sb(OMe)3 with phthalic anhydride. 相似文献
14.
Bellam Sreenivasulu 《Inorganica chimica acta》2009,362(8):2735-281
Complexes [Cu(HSas)(H2O)] · 2H2O (H3Sas = N-(2-hydroxybenzyl)-l-aspartic acid) (1), [Cu(HMeSglu)(H2O)] · 2H2O (H3MeSglu = (N-(2-hydroxy-5-methylbenzyl)-l-glutamic acid) (2), [Cu2(Smet)2] (H2Smet = (N-(2-hydroxybenzyl)-l-methionine) (3), [Ni(HSas)(H2O)] (4), [Ni2(Smet)2(H2O)2] (5), and [Ni(HSapg)2] (H2Sapg = (N-(2-hydroxybenzyl)-l-aspargine) (6) have been synthesized and characterized by chemical and spectroscopic methods. Structural determination by single crystal X-ray diffraction studies revealed 1D coordination polymeric structures in 2 and 4, and hydrogen-bonded network structure in 5 and 6. In contrast to previously reported coordination compounds with similar ligands, the phenol remains protonated and bonded to the metal ions in 2 and 4, and also probably in 1. However, the phenolic group is non-bonded in 6. 相似文献
15.
Isolda C. Mendes Adaliene V.M. Ferreira Heloisa Beraldo 《Inorganica chimica acta》2009,362(2):414-420
Reaction of VOCl2 with 2-pyridineformamide thiosemicarbazone (H2Am4DH) and its N(4)-methyl (H2Am4Me), N(4)-ethyl (H2Am4Et) and N(4)-phenyl (H2Am4Ph) derivatives in ethanol gave as products [VO(H2Am4DH)Cl2] (1), [VO(H2Am4Me)Cl2] · 1/2HCl (2), [VO(H2Am4Et)Cl2] · HCl (3) and [VO(2Am4Ph)Cl] (4). Upon the dissolution of 1-4 in water, oxidation immediately occurs with the formation of [VO2(2Am4DH)] (5), [VO2(2Am4Me)] (6), [VO2(2Am4Et)] (7) and [VO2(2Am4Ph)] (8). The crystal and molecular structures of 5 and 6 were determined. Complexes 5-8 inhibited glycerol release in a similar way to that observed with insulin but showed a low enhancing effect on glucose uptake by rat adipocytes. 相似文献
16.
Lei Shen Qiao-Yun Li Xiao-Yan Tang Feng Zhou Zhu-Feng Miao Jian-Ning Jin Wei Shen 《Inorganica chimica acta》2011,370(1):150-155
Three novel metal-organic frameworks, [Zn(btze)]n (1), [Zn(btze)(H2O)]n (2) and [Mn(btze)(H2O)4]n·(H2O)2 (3) [btze = 1,2-bis(tetrazol-5-yl) ethane anion], were synthesized and characterized by elemental analysis, IR spectroscopy, X-ray crystallography and thermogravimetric analysis. The crystal structures study reveal that 1 displays a 3D framework, 2 displays a 2D layer structure and 3 displays a 1D polymeric chain. The luminescence properties of 1-3 were investigated at room temperature in solid state. 相似文献
17.
Four structurally diverse complexes, [Cd(dppz)(bdoa)]n (1), [Zn(dppz)(bdoa)(H2O)]n (2), [Fe(dppz)2(bdoa)]n·2nH2O (3), and [Co2(dppz)2(bdoa)2(H2O)]n·3nH2O (4), where H2bdoa = benzene-1,4-dioxyacetic acid and dppz = dipyrido[3,2-a:2′,3′-c]phenazine, have been hydrothermally synthesized. Compounds 1-4 feature chain structures. There exist π-π interactions in the structures of 1, 2 and 4. Two neighboring chains of 1 are linked through the π-π interactions into a double chain supramolecular structure. The chains of 2 and 4 are further extended by the π-π interactions to form 3D and 2D supramolecular structures, respectively. The structural differences among such complexes show that the transition metals have important influences on their structures. The photoluminescent property of complex 2 and the magnetic property of complex 4 have also been investigated. 相似文献
18.
Nadera Haque 《Inorganica chimica acta》2010,363(4):723-728
The reactions of trans-[(PPh3)2M(CO)Cl] (M = Rh and Ir) with benzildiimine (H2BDI = 2) derived from benzil-bis(trimethylsilyl)diimine (Si2BDI) (1) in a 1:2 and 1:1 molar ratio afforded the cationic bis-benzildiiminato complexes [Rh(PPh3)2(HBDI)2]Cl (3) and the mono-benzildiimine complex [Ir(PPh3)2(CO)(H2BDI)]Cl (4), respectively. Both complexes are fully characterized using IR, FAB-MS, NMR spectroscopy and elemental analysis. The single crystal X-ray structure analysis reveals a distorted octahedral coordination geometry for the Rh(III) in 3 and a highly distorted square pyramidal geometry for Ir(I) in 4. In addition, the solid-state structure of Si2BDI is reported here for the first time showing the substituents highly twisted because of steric reasons. 相似文献
19.
The dinuclear and trinuclear copper(II) complexes [Cu2(L)(OH)(ClO4)(phen)(H2O)]ClO4 · [Cu2(L)(OH)(ClO4)2(phen)(CH3OH)] (1) and [Cu3(L)2(OH)2(H2O)2](NO3)2 (2) (HL=2-[2-(α-pyridyl)ethyl]imino-3-butanone oxime and phen=1,10-phenanthroline) were prepared and their crystal structures have been determined by X-ray crystallography. Complex 1 is composed of [Cu2(L)(OH)(ClO4)(phen)(H2O)]ClO4 (1a) and [Cu2(L)(OH)(ClO4)2(phen)(CH3OH)] (1b). In 1a and 1b, one oximato of L and one hydroxo group bridge two copper(II) ions. The linear trinuclear cation [Cu3(L)2(OH)2(H2O)2]2+ in 2 is centrosymmetric, and one oximato and one hydroxo group bridge the central and terminal copper(II) ions. The strong antiferromagnetic interactions within the dinuclear and trinuclear complexes 1 and 2 have been observed (2J=∼−900 cm−1 for 1 and 2, respectively, H=−2JS1·S2). 相似文献
20.
Fabiola Estudiante-Negrete Simón Hernández-Ortega David Morales-Morales 《Inorganica chimica acta》2007,360(5):1651-1660
The organometallic tin(IV) complexes [SnPh2(SRF)2] SRF = −SC6F4-4-H (1), −SC6F5 (2), were synthesized and their reactivity with [MCl2(PPh3)2] M = Ni, Pd and Pt explored. Thus, transmetallation products were obtained affording polymeric [Ni(SRF)(μ-SRF)]n, monomeric cis-[Pt(PPh3)2(SC6F4-4-H)2] (3) and cis-[Pt(PPh3)2(SC6F5)2] (4) and dimeric species [Pd(PPh3)(SC6F4-4-H)(μ-SC6F4-4-H)]2 (5) and [Pd(PPh3)(SC6F5)(μ-SC6F5)]2 (6) for Ni, Pt and Pd, respectively. The crystal structures of complexes 1, 2, 3, 4 and 6 were determined. 相似文献