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1.
New Ba acylpyrazolonate derivatives of formula [Ba(Q)2(tetraglyme)] (HQ = HQtbu = 1-Ph-3-Me-4-C(O)CH2But-5-pyrazolone; tetraglyme = 2,5,8,11,14-pentaoxapentadecane), [Ba(Q)2(tmeda)2] (HQ = HQtbu or HQpiv, where HQpiv = 1-Ph-3-Me-4-C(O)But-5-pyrazolone; tmeda = N,N,N′,N′-tetramethylethylenediamine), [Ba(Q)2(pmdien)(H2O)] (HQ = HQtbu or HQpiv; pmdien = N,N,N′,N″,N″-pentamethyldiethylenetriamine) and [Ba(Q)2(pmdien)(Meim)] (HQ = HQtbu or HQpiv; Meim = 1-methylimidazole) have been synthesized and analytically and spectroscopically characterized. They are mononuclear air and solution stable compounds containing an eight-coordinated barium atom. The X-ray crystal structures of the hydrates [Ba(Qtbu)2(pmdien)(H2O)] and [Ba(Qpiv)2(pmdien)(H2O)] show the water molecule directly bonded to Ba and involved in intermolecular H-bonding network. In the X-ray crystal structure of [Ba(Qpiv)2(pmdien)(Meim)], the Meim ligand substitutes the water of previous derivatives and decreases the strength of intermolecular interactions, lowering the melting point. The derivative [Ba(Qtbu)2(pmdien)(NEt3)] has been prepared from interaction of [Ba(Qtbu)2(pmdien)(H2O)] with excess triethylamine in acetonitrile.  相似文献   

2.
The synthesis and characterization of new lanthanide complexes of formulae [M(Q)3(H2O)(EtOH)], NBu4[M(Q)4] and [M(Q)3(L)] (M = Eu or Tb; HQ = 1-phenyl-3-methyl-4-R-pyrazol-5-one: R = cyclopentylcarbonyl, HQ = HQCP; R = cyclopentylpropionyl, HQ = HQEtCP; L = 1,10-phenanthroline (phen) or 4,7-diphenyl-1,10-phenanthroline (bathophen)) are reported. The crystal structure of the tetrakis (β-diketonate) complex [NBu4][Eu(QETCP)4] containing an eight-coordinated Eu atom in a distorted square antiprismatic environment has been determined. Luminescence studies have been performed on selected derivatives: the data suggested a strong influence of the nature of the acyl moiety in Q ligands and of Ph groups in bathophen (with respect to phen) on the luminescence properties.  相似文献   

3.
New silver(I) acylpyrazolonate derivatives [Ag(Q)], [Ag(Q)(PR3)]2 and [Ag(Q)(PR3)2] (HQ = 1-R1-3-methyl-4-R2(CO)pyrazol-5-one, HQBn = R1 = C6H5, R2 = CH2C6H5; HQCHPh2 = R1 = C6H5, R2 = CH(C6H5)2; HQnPe = R1 = C6H5, R2 = CH2C(CH3)3; HQtBu = R1 = C6H5, R2 = C(CH3)3; HQfMe = R1 = C6H4-p-CF3, R2 = CF3; HQfEt = R1 = C6H5, R2 = CF2CF3; R = Ph or iBu) have been synthesized and characterized in the solid state and solution. The crystal structure of 1-(4-trifluoromethylphenyl)-3-methyl-5-pyrazolone, the precursor of proligand HQfMe and of derivatives [Ag(QnPe)(PPh3)2] and [Ag(QnPe)(PiBu3)]2 have been investigated. [Ag(QnPe)(PPh3)2] is a mononuclear compound with a silver atom in a tetrahedrally distorted AgO2P2 environment, whereas [Ag(QnPe)(PiBu3)]2 is a dinuclear compound with two O2N-exotridentate bridging acylpyrazolonate ligands connecting both silver atoms, their coordination environment being completed by a phosphine ligand.  相似文献   

4.
Four new bis(phosphino)amine ligands (Ph2P)2N-C6H3-R, where R = 3,5-OMe (1), 2,5-OMe (2), 2,4-OMe (3) or 3,4-OMe (4), were prepared via aminolysis of the corresponding dimethoxyanilines with 2 equiv. of diphenylphosphine chloride in the presence of triethyl amine. Oxidation of these ligands with aqueous H2O2, elemental S8 or Se powder afforded the corresponding chalcogen oxides 1a-4a, sulfides 1b-4b and selenides 1c-4c in good yields. Reaction of 1-4 with [MCl2(cod)] (M = Pt, Pd; cod = cycloocta-1,5-diene) in equimolar ratios afforded cis-[MCl2{(Ph2P)2N-C6H3-R}] (M = Pt; R = 3,5-OMe 1d, R = 2,5-OMe 2d, R = 2,4-OMe 3d, and R = 3,4-OMe 4d. M = Pd; R = 3,5-OMe 1e, R = 2,5-OMe 2e, R = 2,4-OMe 3e, and R = 3,4-OMe 4e). Similarly, reaction of [Cu(CH3CN)4]PF6 with the 1-4 in 1:2 ratio gave [Cu{(Ph2P)2N-C6H3-R}2]PF6 (R = 3,5-OMe 1f, 2,5-OMe 2f, 2,4-OMe 3f and 3,4-OMe 4f). All new compounds were fully characterized by spectroscopy and elemental analysis and the molecular structures of seven representative compounds were determined by single-crystal X-ray crystallography. In addition, the palladium complexes were investigated as pre-catalysts in C-C coupling reactions.  相似文献   

5.
New (Q)2SnR2 derivatives (HQ in general; in detail: HQCHPh2 = 4-diphenylacetyl-3-methyl-1-phenyl-5-pyrazolone; HQBn = 3-methyl-1-phenyl-4-phenylacetyl-5-pyrazolone; HQnaph = 3-methyl-4-naphthoyl-1-phenyl-5-pyrazolone; R = CH3, C2H5, C6H11, n- and t-C4H9, C6H5,) have been synthesised and characterised by analytical and spectral techniques. Variable temperature NMR studies of (QCHPh2)2SnR2 derivatives (R = CH3 and C2H5) in chlorohydrocarbon solvents indicate a fluxional behaviour, with rapid interconversion between six- and five-coordinate species, the latter containing a bidentate acylpyrazolonate and a monodentate one. The X-ray crystal structures of the diorganotin(IV) derivatives (QCHPh2)2SnMe2, (QCHPh2)2SnEt2, (QBn)2SnMe2 and , inclusive of a representative of each Qx family, show the metal centres in a skewed trans octahedral configuration. The 4-acyl moiety of the β-diketonate donor exerts a steric effect which is correlated to structural behaviour in the solid and solution state. A solid state 119Sn CPMAS NMR study of the (QBn)2SnR2 (R = CH3, C2H5, t-C4H9 and C6H5) complexes shows a marked deshielding effect and upfield movement of the 119Sn isotropic chemical shift (δiso) through this series. The 119Sn chemical shift spans (Ω) are the largest reported for directly oxo-coordinated Sn(IV) systems, although the markedly reduced Ω value for the (QBn)2SnPh2 complex may be indicative of a cis octahedral coordination, in contrast to the trans octahedral coordination characterising the other complexes of this suite.  相似文献   

6.
Neutral tris(trimethylsilylmethyl) complexes [Ln(CH2SiMe3)3(L)] (Ln = Sc (1), Lu (2)) and cationic bis(trimethylsilylmethyl) complexes [Ln(CH2SiMe3)2(L)(THF)]+[BPh4], (Ln = Sc (3), Lu (4)) that contain bis(2-methoxyethyl)(trimethylsilyl)amine (L = Me3SiN(CH2CH2OMe)2) as a neutral, tridentate ligand were synthesized and characterized by NMR spectroscopy. X-ray structural analysis was performed for the scandium complex 1 and exhibited a distorted octahedral coordination geometry with a facially arranged ligand at the neutral scandium center. NMR spectroscopy corroborated the coordination of the tertiary amine function of the ligand to the metal. Complexes 3 and 4 expand the still limited range of cationic rare-earth metal alkyl complexes with known neutral, multidentate ligands.  相似文献   

7.
Four new diorganotin(IV), (R = Me, Bu), and triorganotin(IV), (R = Me, Ph), derivatives of the phosphomycin disodium salt antibiotic[(1R,2S)-1,2-epoxypropylphosphonate]Na2 have been synthesized and their solid state configuration studied by X-ray crystallography, FT-IR, Mössbauer, UV-Vis spectroscopies. The X-ray diffraction investigation, performed on the bis[trimethyltin(IV)]phosphomycin, showed that the coordination geometry at all the Sn atoms is trigonal bipyramidal. The structure of the complex forms an unusual polymeric zig-zag planar network. The FT-IR and the 119Sn Mössbauer studies supported the formation of trigonal bipyramidal (Tbp) molecular structures, both in the diorganotin(IV) and triorganotin(IV) derivatives, even if, in the case of diorganotin(IV) derivatives, the tetrahedral structure cannot be a priori excluded. The group of phosphomycin coordinates the organotin(IV) centers originating a monodimensional polymeric network, as inferred by variable temperature 119Sn Mössbauer spectroscopy, used to investigate lattice dynamics of the bis-[trimethyltin(IV)]phosphomycin complex.  相似文献   

8.
The silver(I) salts [AgOR] (3a, R = C9H6N; 3b, R = C6H4-2-CHO, 3c, R = C6H4-2-Cl; 3d, R = C6H4-2-CN; 3e, R = C6H4-2-NO2) are accessible by the stoichiometric reaction of [AgNO3] (1) with HOR (2a, R = C9H6N; 2b, R = C6H4-2-CHO; 2c, R = C6H4-2-Cl; 2d, R = C6H4-2-CN; 2e, R = C6H4-2-NO2) in presence of NEt3. Treatment of 3a-3e with PnBu3 (4), P(OMe)3 (5a) or P(OCH2CF3)3 (5b) in the ratios of 1:1 and 1:2, respectively, produced complexes [LmAgOR] (L = PnBu3, = 1: 6a, R = C9H6N; 6b, R = C6H4-2-CHO; 6c, R = C6H4-2-Cl; 6d, R = C6H4-2-CN; 6e, R = C6H4-2-NO2. = 2: 7a, R = C9H4; 7b, R = C6H4-2-CHO; 7c, R = C6H4-2-Cl; 7d, R = C6H4-2-CN; 7e, R = C6H4-2-NO2. L = P(OMe)3, = 1: 8a, R = C6H4-2-CHO; 8b, R = C6H4-2-NO2. = 2: 9, R = C6H4-2-NO2. L = P(OCH2CF3)3, = 1: 10, R = C6H4-2-NO2). Based on TGA, temperature-programmed and in situ molecular beam mass spectrometry metal-organic 7e was applied as CVD precursor in the deposition of silver onto glass substrates. The resulting silver films were characterized by XRD. The SEM image of a film grown from 7e at 350 °C showed a homogeneous surface with grain sizes of 40 nm. The molecular structures of 8b and 10 in the solid state were determined. They are isostructural and are cubane-like structured. Low-temperature 31P{1H} NMR studies showed that the title complexes are dynamic in solution and exchange at room temperature their ligands.  相似文献   

9.
Complexes have been synthesised with bis(2-pyridine carboxaldehyde) ethylenediimine (1) and bis(2-pyridine carboxaldehyde)propylene-1,3-diimine (2) with all of the available lanthanide trinitrates. Crystal structures were obtained for all but one complex with 1 and for all but one complex with 2. Four distinct structural types were established for 1 but only two for 2, although in all cases the structures contained one ligand bound to the metal in a tetradentate fashion. With 1, the four different structures of the lanthanide(III) nitrate complexes included 11-coordinate [Ln(1)(NO3)3(H2O)] for Ln = La; 10 coordinate [Ln(1)(NO3)3(H2O)] with one monodentate and two bidentate nitrates for Ln = Ce, then 10-coordinate [Ln(1)(NO3)3] for Ln = Pr-Yb with three bidentate nitrates; and 9-coordinate [Ln(1)(NO3)3] with one monodentate and two bidentate nitrates for Ln = Lu. On the other hand for 2 only two distinct types of structure are obtained, the first type with Ln = La-Pr and the second type for Ln = Sm-Lu, although all are 10-coordinate with stoichiometry [Ln(2)(NO3)3]. The difference between the two types is in the disposition of the ligand relative to the nitrates. With the larger lanthanides La-Pr the ligand is found on one side of the coordination sphere with the three nitrate anions on the other. In these structures, the ligand is folded such that the angle between the two pyridine rings approaches 90°, while with the smaller lanthanides Sm-Lu, two nitrates are found on one side of the ligand and one nitrate on the other and the ligand is in an extended conformation such that the two pyridine rings are close to being coplanar. In both series of structures, the Ln-N and Ln-O bond lengths were consistent with the lanthanide contraction though there are significant variations between ostensibly equivalent bonds which are indicative of intramolecular hydrogen bonding and steric crowding in the complexes.  相似文献   

10.
Reactions of H2L [H2L = N,N′-bis(3-methoxysalicylidene)propane-1,2-diamine] and Ln(NO3)3 · 6H2O give rise to two different mononuclear 4f complexes, namely, {[(H2L)La(NO3)3(MeOH)] · H2O}n (1) and [(H2L)Nd(NO3)3] (2). Further additions of Cu(Ac)2 · H2O to the mononuclear 4f complexes yield expected heterodinuclear Cu-4f complexes [LCu(Me2CO)Ln(NO3)3] (3, Ln = Nd; 4, Ln = Eu; 5, Ln = Dy). Complex 1 is a unique 1D polymeric chain structure, and 2 is one of the few structurally characterized discrete hexadentate salen-type mononuclear 4f complexes. Complexes 3-5 are similar to their analogues. However, they are prepared by a reversed synthetic route in contrast to their isomorphic complexes. Electrochemical behavior of heterodinuclear Cu-4f complexes 3-5 has been examined by cyclic voltammetry in acetonitrile. The redox potential of heterodinuclear Cu-4f complexes 3-5 shows significant anodic shift comparing to that of mononuclear copper complex (LCu). A tendency of anodic shift was observed in a sequence of 3 < 4 < 5. This results from the modulating effect of coordination geometry around Cu(II) ion on redox potential.  相似文献   

11.
Novel triorganotin(IV) derivatives of β-diketonate Q ligands (HQ in general, in detail HQfur = 1-phenyl-3-methyl-4-(2-furancarbonyl)-pyrazol-5-one, HQthi = 1-phenyl-3-methyl-4-(2-thienylcarbonyl)-pyrazol-5-one) of general formula (Q)SnR3·xH2O (R = Ph, x = 0; R = Bun or Me, x = 1) have been synthesized and spectroscopically and thermally characterized. Triphenyltin(IV) complexes have been isolated as anhydrous compounds while trialkyltin(IV) are always monohydrated. The structures of (Qfur)SnPh3 and (Qthi)SnMe3(OH2) are recorded. The tin atoms are five-coordinate in both. In the first, the pyrazolonate ligand behaves as an O,O′-bidentate; there are two similar but independent molecules in the structure. In the quasi-trigonal-bipyramidal environments, Sn-O(acyl) are 2.478(3), 2.364(3), Sn-O(pyrazolonate) 2.050(2), 2.079(2), Sn-C 2.123(4)-2.162(3) Å with the longer O(acyl) and a phenyl group quasi-trans (O-Sn-C 162.5(1), 160.8(1)°). In (Qthi)SnMe3(OH2), the three methyl groups are equatorial (Sn-C 2.1259(9)-2.1380(8) Å); Sn-O(Qthi,OH2) are 2.2143(5), 2.3350(6) Å, O-Sn-O 175.36(2)°. Trimethyltin(IV) derivatives decompose on heating with release of H2O and SnMe4 and formation of (Q)2SnMe2. Decomposition occurs also within two days after dissolution of (Q)SnMe3(OH2) in chloroform.  相似文献   

12.
A series of pyrazolyl palladium(II), platinum(II) and gold(III) complexes, [PdCl2(3,5-R2bpza)] {R = H (1), R = Me (2), bpza = bis-pyrazolyl acetic acid}, [PtCl2(3,5-R2bpza)] {R = H (3a), R = Me (4)}, [AuCl2(3,5-R2bpza)]Cl {R = H (5a), R = Me (6a)} and [PdCl2(3,5-R2bpzate)] {R = Me (7)} have been synthesised and structurally characterised. Single crystal X-ray crystallography showed that the pyrazolyl ligands exhibit N^N-coordination with the metals. Anticancer activities of six complexes 1-6a were investigated against CHO cells and were found to have low activities. Substitution reactions of selected complexes 1, 2, 3a and 5a with l-cysteine show that the low anticancer activities compounds and that the rate of substitution with sulfur-containing compounds is not the cause of the low anticancer activities.  相似文献   

13.
Consecutive synthesis methodologies for the preparation of a series of copper(I) formates [LmCuO2CH] (L = nBu3P: 4a, m = 1; 4b, m = 2; 5, L = [Ti](CCSiMe3)2, m = 1, [Ti] = (η5-C5H4SiMe3)2Ti) and [LmCuO2CH·HO2CR] (L = nBu3P: 7a, m = 1, R = H; 7b, m = 2, R = H; 7c, m = 2, R = Me; 7d, m = 2, R = CF3; 7e, m = 2, R = Ph. L = (cC6H11)3P, R = H: 8a, m = 2; 8b, m = 3. L = (CF3CH2O)3P, R = H: 9a, m = 2; 9b, m = 3. L = (CH3CH2O)3P, R = H: 10a, m = 2; 10b, m = 3. L = [Ti](CCSiMe3)2; m = 1: 11a, R = H; 11b, R = Ph) is reported using [CuO2CH] (1) and L (2a, L = nBu3P; 2b, L (cC6H11)3P; 2c, L = (CF3CH2O)3P; 2d, L = (CH3CH2O)3P; 3, L = [Ti](CCSiMe3)2) as key starting materials. Addition of formic acid (6a) or carboxylic acid HO2CR (6b, R = Me; 6c, R = CF3; 6d, R = Ph) to the afore itemized copper(I) formates 4 and 5 gave metal-organic or organometallic 7-11. The molecular structures of 8a and 11a in the solid state are reported showing a threefold coordinated copper(I) ion, setup by either two coordinatively-bonded phosphorus atoms and one formate oxygen atom (8a) or two π-bonded alkyne ligands and one oxygen atom (11a). A formic acid molecule is additionally hydrogen-bonded to the CuO2CH moiety. The use of 7b as suitable precursor for the deposition of copper onto TiN-coated oxidized silicon wafers by the spin-coating process below 300 °C is described. Complex 7b offers an appropriate transformation behavior into metal phase by an elimination-decarboxylation mechanism. The morphology of the copper films strongly depends on the annealing conditions. A closed grain network densified by a post-treatment is obtained (8 °C min−1, N2/H2 carrier gas). Hydrogen post-anneal to 420 °C after film deposition gave a copper film showing resistivities from 2.5 to 3.7 μΩ cm. This precursor was also used for gap-filling processes.  相似文献   

14.
The reaction of halflanthanidocene aryloxides CpR′Ln(OArtBu,R)2 (Ln = Y, La, Lu; CpR′ = C5Me5, C4Me4H; R = H, Me) and halflanthanidocene alkoxides [(C5Me5)Ln(OCH2CMe3)2]2 (Ln = Y, Lu) with trimethylaluminum (TMA) was investigated. Monomeric CpR′Ln(OArtBu,R)2, derived from the ortho-tBu-substituted OC6H2tBu2-2,6-R-4 (R = H, Me) ligands, form mono(tetramethylaluminate) complexes CpR′Ln(OArtBu,R)(AlMe4) for the smaller lanthanide metal centers yttrium and lutetium. Such an [aryloxide] → [aluminate] ligand exchange was not observed at the larger lanthanum metal center. The mobility of the tetramethylaluminate ligands of complexes CpR′Ln(OArtBu,R)(AlMe4) (Ln = Y, Lu) was examined by variable-temperature (VT) 1H NMR spectroscopy, revealing two signals for bridging and terminal methyl groups at lower temperatures. The treatment of complexes CpR′Ln(OArtBu,R)(AlMe4) with donor solvent d8-THF gave CpR′Ln(OArtBu,R)(Me)(d8-THF)2 (Ln = Y, Lu) with terminal methyl groups, according to a donor-induced aluminate cleavage reaction. Dimeric [(C5Me5)Ln(OCH2CMe3)2]2 (Ln = Y, Lu) was synthesized from (C5Me5)Ln(NiPr2)2(THF) and reacted with two equivalents of TMA per Ln center to yield monomeric bis(TMA) adduct complexes (C5Me5)Ln(OCH2CMe3)2(AlMe3)2(Ln = Y, Lu). VT NMR spectroscopic studies confirmed a high mobility of the Ln(μ-OCH2CMe3)(μ-Me)AlMe2 moieties at an ambient temperature. Both bis(TMA) adduct complexes were characterized by X-ray structure analysis.  相似文献   

15.
A series of organotin(IV) complexes with Schiff base ligand pyruvic acid 3-hydroxy-2-naphthoyl hydrazone [R2SnLY]2, L = 3-HO-C10H6-2-CONHNC(CH3)COOH, R = n-C4H9, Y = CH3OH (1), R = n-C4H9, Y = N (2), R = PhCH2 (3), R = Ph, Y = CH3OH (4), R = Me, (5) and [R3SnLY], L = 3-HO-C10H6-2-CONHNC(CH3)COOH, R = n-C4H9, Y = H2O, (6), R = Ph (7), R = Me (8) have been synthesized. These complexes have been characterized by elemental analysis, IR, 1H and 119Sn NMR spectra. The crystal and molecular structure of complexes 1, 2 and 6 have been determined by X-ray single crystal diffraction. Results showed that complex 1 has a dimeric structure and the central tin atom is rendered seven-coordinate in a distorted pentagonal-bipyramid configuration. The complex 2 has a monoclinic structure and the central tin atom is rendered six-coordinate in octahedrally configuration with a planar of SnO3N unit and two apical aryl C atoms. And the whole structure consists of molecular units connected by weak intermolecular Sn?N and O-H?N interactions. In the complex 6, the central tin atom is five-coordinate in distorted trigonal-bipyramidal geometry.  相似文献   

16.
Nine triorganotin(IV) complexes of the type R3SnL (L = L1 R = Me 1, Ph 2, PhCH23; L = L2 R = Me 4, Ph 5, PhCH26; L = L2 R = Me 7, Ph 8, PhCH29) have been obtained by reaction of new Schiff base HL1, HL2 or HL3 with triorganotin(IV) chloride in the presence of sodium ethoxide. All the complexes 1-9 were characterized by elemental, IR and NMR spectra analyses. Except for complexes 3, 4, 6, 9, the others were also characterized by X-ray crystallography diffraction analyses, which revealed that complexes 1, 2, 5, 7, 8 were four coordinated and displayed a capped tetrahedron.  相似文献   

17.
The new aryl phosphinites PPh2OR (R = 2,4,6-Me3C6H2, 1; R = 2,6-Ph2C6H3, 2) have been prepared from chlorodiphenylphosphine and the corresponding phenols. In these ligands, the ortho-positions of the aromatic phosphite function are blocked by methyl and phenyl substituents, which allows coordination to metal centres without ortho-metallation. Thus, reaction with [PdCl2(cod)] leads to the complexes trans-[PdCl2(PPh2OR)2] (R = 2,4,6-Me3C6H2, 3; R = 2,6-Ph2C6H3, 4), while the reaction with [Rh2(CO)4Cl2] gives trans-[Rh(CO)Cl(PPh2OR)2] (R = 2,4,6-Me3C6H2, 5; R = 2,6-Ph2C6H3, 6). The single-crystal X-ray structure analyses of 3 and 5 confirm the trans-coordination of the new ligands in these square-planar complexes.  相似文献   

18.
Four organotin(IV) complexes with general formula [RSnCln−1(TCB)] [R = Ph2, n = 2 (2); R = Me, n = 3 (3); R = Bu, n = 3 (4); R = Ph, n = 3 (5)] have been synthesized by direct reaction of thiophene-2-carboxaldehyde benzhydrazone ligand [HTCB, (1)], base and organotin(IV) chloride in absolute methanol under N2 atmosphere. All organotin(IV) complexes were characterized by elemental analyses, molar conductivity, UV-Vis, FT-IR, 1H and 13C NMR spectral studies. Among them, diphenyltin(IV) complex (2) has also been characterized by X-ray crystallography diffraction analyses. The cytotoxicity of the hydrazone ligand as well as its organotin(IV) complexes (2-5) were determined with Artemia salina. While no-choice bioassay was employed on Coptotermes sp. to evaluate the termiticidal effect of all the complexes. Besides, the ligand (1) and its organotin(IV) complexes (2-4) were also tested against five types of bacteria namely Bacillus subtilis, Staphylococcus aureus, Escherichia coli, Pseudomonas aeruginosa and Salmonella typhi.  相似文献   

19.
Two new inorganic-organic hybrid polymers [ClBzQl]2[Cd(SCN)3.5Br0.5]·0.25H2O (1) and [ClBzMePy][Cd(SCN)3] (2) (ClBzQl = 1-(4′-Cl-benzyl)quinolinium cation and ClBzMePy = 1-(4′-Cl-benzyl)-2-methylpyridinium cation) have been synthesized and characterized by IR, UV, elemental analysis and X-ray crystallography. Crystal structure analyses show that two polymers belong to the monoclinic space group P2/n (1) and P21/c (2) with a = 18.548(2) Å, b = 9.526(1) Å, c = 20.689(2) Å, β = 94.008(1)°, V = 3646.6(5) Å3 for 1, and a = 11.195(2) Å, b = 16.415(3) Å, c = 10.751(2) Å, β = 102.930(3)°, V = 1925.7(7) Å3 for 2. The Cd atom exhibits a distorted octahedral coordination geometry for 1 and 2. For 1, a pair of 1,1-μ-SCN anions and a pair of 1,3-μ-SCN anions are alternately bridge adjacent Cd centers to form infinite polymeric chains. For 2, adjacent Cd atoms are linked by three 1,3-μ-SCN anions to form infinite [Cd(SCN)3] polymeric chains. The luminescent properties of the two polymers in the solid state at room temperature were investigated.  相似文献   

20.
The reaction of imidoyl chlorides [V(NR)Cl3] (R = Ph 1, Tol 2, tBu 3) and calix[4]arene methyl ether H3Mecalix unexpectedly leads to the formation of the structurally characterized vanadium (IV) complex [VCl(Mecalix)] (4). Calix[4]arene methyl ether stabilized imido complexes of the type [V(NR)(Mecalix)] (R = Ph 7, Tol 8, tBu 9) were afforded from the reaction of [V(NR)Cl3] (R = Ph 1, Tol 2, tBu 3) and the tris(lithium) or tris(sodium) salt of the calix[4]arene ether. The lithium salt [{Li3(Mecalix)}2] (5) is a dimer in the solid state, in which two monomeric trianions are bridged by lithium cations. Imido complexes [M(NR)(Mecalix)] (M = Nb: R = tBu, 12, R = Tol 13, R = Mes 14, R = Dipp 15; M = Ta: R = tBu 16, R = Tol 17) (Tol = 4-C6H4Me, Mes = 2,6-C6H3Me2; Dipp = 2,6-C6H3iPr2) have been prepared from structurally characterized [NbCl2(Mecalix)] (10) and previously known [TaCl2(Mecalix)] (11) via reaction with two equivalents of the appropriately metallated (Li, K) primary amine. The molecular structures of 13 and 15 confirm the mononuclear nature of these complexes.  相似文献   

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