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1.
The copper aminotropones Cu[ON(R′)C7H4R-4]2 [R = H, R′ = Me (13), Et (14), n-Pr (15), n-Bu (16), Bz (17), MenOCH2CH2 (20); R = i-Pr, R′ = Me (18), n-Pr (19), MenOCH2CH2 (21)] have been prepared from the corresponding aminotropones HN(R′)OC7H4R-4 (17) by reacting with copper(II) acetate in aqueous ethanol. 20, 21 contain the flavourant, menthol, as part of the ligand. The structures of 5 (R = H, R′ = Bz), a hydrogen-bonded dimer, 14 and 20, both incorporating square-planar, four-coordinate copper centres, have been determined by X-ray crystallography. The antibacterial activities of complexes 13, 17, 20 and 21 have been assayed against Staphylococcus waneri, an in vitro model of plaque inhibition effects, and found to be more active than a commercial toothpaste formulation, but less active than the O,O-chelated copper(II) complex of ethylmaltol.  相似文献   

2.
The diiron ynamine complex [Fe2(CO)7{μ-CR)C(NEt2)}] (1:R=Me,2:R = C3H5.3:R=SiMe3.4:R = Ph) reacts at room temperature with diphenyldiazomethane Ph2CN2, in hexane to yield complexes [Fe2(CO)6{C(R)C(NEt2)N (NCPh2)] (5a:R=Me,6a:R=C3H5.7a R=SiMe3.8a:R=Ph) resulting from the insertion of the terminal nitrogen atom into the Fe=C carbene bond. Insertion the second nitrogen atom and formation of compounds [Fe2(CO)6zμ-C(R)C(NEt2)NN(CPh2)}] (5b:R=Me,6b:R=C3H5,7b:R=SiMe3,8b:R=Ph) is observed when compounds5a-5a are treated in refluxing hexane. Transformation of compoundsa tob is also obtained at room temperature within a few days. All compounds were identified by their1H NMR spectra. Compounds6a, 7a, 8a, and8b were characterized by single crystal X-ray diffraction analyses. Crystal data: for6a: space group = P21/n,a=12.853(1) A,b=24.800(7) A,c=8.947(6) A,β=99.29(3)°,Z=4, 2227 rellectionsR=0,038; for7a: space group=Pl,a=ll.483(4) A,b=14.975(4) A,c = 17.890(8) A,α = 82.80(3)°,β=94.29(7)°,γ=85.42(2),Z = 4, 5888 reflectionR = 0.035: for8a: space group = Pcab.a = 31.023(8) A.b=20.137(1) A.c=9.686(2) A.Z=8. 1651 reflections,R=0.071; for8b: space group=P21/n,a=21.459(4),b=10,100(3) A,c=28,439(8) A,ß=103.86(4)°,Z=8. 2431 reflections.R=0.057.  相似文献   

3.
A series of organotin (IV) complexes with 6-amino-1,3,5-triazine-2,4-dithiol of the type [(RnSnCl4−n)2 (C3H2N4S2)] (n = 3: R = Me 1, n-Bu 2, PhCH23, Ph 4; n = 2: R = Me 5, n-Bu 6, PhCH27, Ph 8) have been synthesized. All the complexes 1-8 have been characterized by elemental analysis, IR, 1H and 13C NMR spectra. Among them complexes 1, 4, 5 and 8 have also been characterized by X-ray crystallography diffraction analyses, which revealed that the tin atoms of complexes 1, 4, 5 and 8 are all five-coordinated with distorted trigonal bipyramid geometries.  相似文献   

4.
A new series of di- and tri-organotin(IV) compounds with the general formula R4?n SnL n , where R?=?Me (1,2), Et (3), n-Bu (4,5), n-Oct (6), Ph (7) and L?=?(E)-3-(4-methoxyphenyl)-2-(4-chlorophenyl)-2-propenoate, were synthesized by reaction of silver salt of ligand or ligand acid with diorganotin dichloride/oxide and triorganotin chloride in 2:1 and 1:1 molar ratio, respectively. These compounds were characterized by elemental analyses, FT-IR, multinuclear (1H, 13C, 119Sn) NMR and mass spectrometry. The spectroscopic results revealed that all the diorganotin(IV) compounds possess trigonal bipyramidal structures in solution and octahedral geometry in the solid state around the tin atom. A linear polymeric trigonal bipyramidal structure in the solid state and a tetrahedral environment around the tin atom in non-coordinating solvents has been proposed for the triorganotin(IV) compounds. All synthesized compounds were tested in vitro against a number of microorganisms to assess their biocidal activity. These studies revealed that ligand acid and some of its organotin compounds show promising activity against different strains of bacteria and fungi but lowered than reference drugs.  相似文献   

5.
One new cadmium coordination polymer, [Cd(2,4-Dcp)2(4,4-Bipy)] n (I) (2,4-HDcp = 2,4-dichlorophenoxyacetic acid, 4,4′-Bipy = 4,4′-bipyridine) with 2D layer structure, has been prepared by the hydrothermal synthesis and characterized by elemental analysis, IR, TGA and single-crystal X-ray diffraction. Complex I crystallizes belong to monoclinic system and has C2/c space group. Each Cd2+ ion is six-coordinated and located at an octahedral geometry. The Cd2+ ions are linked by bidentate 2,4-Dcp groups into a linear chain in which the benzene rings of 2,4-Dcp ligands point alternately up and down. These chains are further connected into a sandwich-like layer though 4,4′-Bipy ligands. Furthermore, the photoluminescence and life-time of I in the solid state have been studied.  相似文献   

6.
The triorganotin(IV) derivatives of 2-mercapto-4-quinazolinone (HSqualone) of the type, R3SnL (R = Ph 1, CH32, PhCH23, p-F-PhCH24, o-F-PhCH25, n-Bu 6), were obtained by the reaction of the R3SnCl and HSqualone with 1:1 molar ratio in benzene. All complexes 1-6 were characterized by elemental analyses, IR, 1H and 13C NMR spectroscopy and the crystal structures of complexes 1-3 were also confirmed by X-ray crystallography. The structure analyses reveal that the tin atoms of complexes 1-3 are all distorted tetrahedral geometries. Furthermore, the dimeric structures in complexes 1-3 have also been found linked by intermolecular O-H?N or N-H?O hydrogen bonding interaction. Interestingly, the dimers of complexes 2 and 3 are further linked into one-dimensional chain through intermolecular C-H?S and C-H?O weak hydrogen bonding interactions, respectively.  相似文献   

7.
The organotin(IV) complexes R2Sn(tpu)2 · L [L = 2MeOH, R = Me (1); L = 0: R = n-Bu (2), Ph (3), PhCH2 (4)], R3Sn(Hthpu) [R = Me (5), n-Bu (6), Ph (7), PhCH2 (8)] and (R2SnCl)2 (dtpu) · L [L = H2O, R = Me (9); L = 0: R = n-Bu (10), Ph (11), PhCH2 (12)] have been synthesized, where tpu, Hthpu and dtpu are the anions of 6-thiopurine (Htpu), 2-thio-6-hydroxypurine (H2thpu) and 2,6-dithiopurine (H2dtpu), respectively. All the complexes 1-12 have been characterized by elemental, IR, 1H, 13C and 119Sn NMR spectra analyses. And complexes 1, 2, 7 and 9 have also been determined by X-ray crystallography, complexes 1 and 2 are both six-coordinated with R2Sn coordinated to the thiol/thione S and heterocyclic N atoms but the coordination modes differed. As for complex 7 and 9, the geometries of Sn atoms are distorted trigonal bipyramidal. Moreover, the packing of complexes 1, 2, 7 and 9 are stabilized by the hydrogen bonding and weak interactions.  相似文献   

8.
Homobimetallic complexes with oxygen and sulphur donor ligand have been synthesized at room temperature under stirring conditions using R2SnCl2 (R?=?Me, n-Bu) and R3SnCl (R?=?Me, n-Bu, Ph) in 1:1 molar ratio. The synthesized complexes have been characterized by elemental analysis, IR and multinuclear NMR (1H, 13C) spectroscopy. These complexes have also been screened for their biological activities. IR data show that the ligand acts in a bidentate manner and exhibits trigonal bipyramidal geometry in solid state which is also confirmed by semi-empirical study. NMR data show that reported complexes exhibit tetrahedral geometry in solution. Results of antimicrobial screening activities indicated that complexes (6) and (7) are very effective antibacterial and antifungal agents, respectively, and they might indeed be a potential source of antimicrobial agents, while the complex (3) exhibits significant free radical scavenging ability with lower IC50 value of 99.47?±?1.2???g/mL. Results of cytotoxicity/haemolytic activity showed the significant value of % haemolysis for complex (7) (18.101?±?2.3), while complex (4) was found to be least cytotoxic (5.733?±?1.0). Only a few colonies are observed in mutagenicity testing by Ames test.  相似文献   

9.
Eight new organoantimony(V) complexes with 1-phenyl-1H-tetrazole-5-thiol [L1H] and 2,5-dimercapto-4-phenyl-1,3,4-thiodiazole [L2H] of the type RnSbL5 − n (L = L1: n = 4, R = n-Bu 1, Ph 2, n = 3, R = Me 3, Ph 4; L = L2: n = 4, R = n-Bu 5, Ph 6, n = 3, R = Me 7, Ph 8) have been synthesized. All the complexes 1-8 have been characterized by elemental, FT-IR, 1H and 13C NMR analyses. Among them complexes 2, 6 and 8 have also been confirmed by X-ray crystallography. The structure analyses show that the antimony atoms in complexes 2 and 6 display a trigonal bipyramid geometry, while it displays a distorted capped trigonal prism in complex 8 with two intramolecular Sb?N weak interactions. Furthermore, the supramolecular structure of 2 has been found to consist of one-dimensional linear molecular chain built up by intermolecular C-H?N weak hydrogen bonds, while a macrocyclic dimer has been found in complex 6 linked by intermolecular C-H?S weak hydrogen bonds with head-to-tail arrangement. Interestingly, one-dimensional helical chain is recognized in complex 8, which is connected by intermolecular C-H?S weak hydrogen bonds.  相似文献   

10.
The title complexes (1, X = F;2, X = C 1; 3, X = Br and isomorphous with2; 4, X = I) have been prepared and characterized by X-ray crystallography. Crystal data, Mo radiation:1, space groupCc,Z =4,a = 12.017(3),b = 14.263(5),c = 17.210(7) Å,β = 103.06(2)°, andR F =0.053 for 2044 observed data;2, space groupCc,Z = 4,a = 12.817(3),b = 11.072(2),c = 16.781(5) Å,β =90.74(2)°,R F = 0.044 for 2249 data;3,a = 12.873(4),b = 11. 119(2),c = 16.957(2) Å,β = 89.11(2)°,R F = 0.049 for 2059 data;4, space groupP21/n,Z = 4,a = 8.858(2),b = 14.358(3),c = 15.379(3) Å,β = 93.88(1)°,R F = 0.068 for 3119 data. In all four structures each thiourea molecule interacts with adjacent thiourea molecules via N-H ... S hydrogen bonds to give a ribbon-like arrangement, and also forms a pair of ‘chelating’ N-H ... X hydrogen bonds with a halide ion, resulting in an anionic framework (in1–3) or composite ribbon (in4) as a component in the crystal packing. The measured ranges of N... X distances are: 2.819(5)-2.994(7) Å for1, 3.252(3)-3.291(3)Å for 2, 3.353(6)-3.459(6)Å for3, and 3.564(5)-3.680(5) Å for 4.  相似文献   

11.
The coordination chemistry of a rigid periodinated ligand, 2,3,5,6-tetraiodo-1,4-benzenedicarboxylic acid (H2BDC-I4), with a series of transition metal ions has been explored to afford five new coordination polymers {[M(BDC-I4)(MeOH)4](H2BDC-I4)(MeOH)2} n (M?=?ZnII for 1, CdII for 2, CoII for 3 and MnII for 4) and {[Mn(BDC-I4)(MeOH)4](DMF)} n (5). All these complexes have been characterized by elemental analysis, IR spectroscopy, thermogravimetric (TG) analysis, and X-ray crystallography. Single-crystal X-ray diffraction reveals that complexes 1?C4 are isostructural and have a one-dimensional chain structure. Upon the addition of the solvent DMF, the infinite linear chain array in 4 is converted to a 1-D wave-like chain motif in 5 with a different space group ( $ P\overline{1} $ for 4 and P21/c for 5). The difference between structures 1?C4 and 5 can be attributed to the coordination mode of carboxylate changing from trans to cis fashion. The ZnII and CdII complexes 1 and 2 display similar emissions in the solid state, which essentially are intraligand transitions.  相似文献   

12.
The reaction of Ru3(CO)12 with MeO2C(H)C=C=C(H)CO2 Me has yielded two isomeric productsanti-Ru2(CO)6[μ-η 3-η 1-MeO2C(H)CCC(H)CO2Me],1 in 70% yield andsyn-Ru2(CO)6[μ-η 3-η 1-MeO2C(H)CCC(H)CO2Me],2 in 5% yield. Both compounds were characterized by single crystal X-ray diffraction analysis. Both products are diruthenium complexes with bridging di(carboxylate)allene ligands in which the oxygen atom of the carbonyl group of one of the carboxylate groupings is coordinated to one of the metal atoms. Compound1 isomerizes partially to2 at 68°C. Crystal Data for1: space group=P21/n,a=11.131(1) Å,b=10.228(2) Å,c=15.978(2) Å,β=102.01(1)°,Z=4, 1653 reflections,R=0.025; for2: space group=P $\bar 1$ ,a=9.340(1) Å,b=14.925(4) Å,c=6.778(2) Å,α=99-02(2)°,β=104 62(2)°,γ=94.58(2)°,Z=2, 1857 reflections,R=0.027.  相似文献   

13.
A series of new organotin (IV) complexes with 3-hydroxy-2-pyridinecarboxylic acid (3-OH-2-picH) of two types: R2SnCl(3-OH-2-pic) (I) (R = Me 1, n-Bu 2, Ph 3, PhCH24) and R2 Sn(3-OH-2-pic)2 (II) (R = Me 5, n-Bu 6, Ph 7, PhCH28)have been synthesized by reactions of diorganotin (IV) dichloride with 3-hydroxy-2-pyridinecarboxylic acid in the presence of sodium ethoxide. All complexes are characterized by elemental analyses, IR spectra and NMR spectra analyses. Among them, complexes 1, 5, 6 and 7 are also characterized by X-ray crystallography diffraction analyses. Complex 1 is a 1D polymeric chain with six-coordinate tin atoms and the packing of complex 1 is stabilized by the C-H?Cl intermolecular weak interactions, thus a 2D network of 1 is formed. Complex 5 is also a 1D polymeric chain with seven-coordinate tin atoms. Complex 6 is a zigzag polymeric chain linked by Sn?O intermolecular weak interactions. Complex 7 is a monomeric complex with distorted octahedral geometry.  相似文献   

14.
A series of organotin(IV) complexes with 2,5-dimercapto-1, 3, 4-thiodiazole (HHdmt) of the type (RnSnClm)2(dmt) (m=0, n=3, R=Ph 1, PhCH22, n-Bu 3; m=1, n=2, R=Ph 4) and [R2Sn(dmt) · L]n (L=0.5C6H6, R=CH35; L=0, n=5, R=n-Bu 6) have been synthesized. All complexes 1-6 were characterized by elemental analysis, IR, 1H and 13C NMR spectra. And except for 3, complexes 1, 2, 4, 5 and 6 were also determined by X-ray crystallography. The tin atoms of complexes 1, 2, 3 and 4 are all five-coordinated. The geometries at tin atoms of 1, 2, 3 and 4 are distorted trigonal bipyramidal. The tin atoms of complexes 5 and 6 are six-coordinated and their geometries are distorted octahedral.  相似文献   

15.
Two novel homobinuclear ytterbium(III) complexes, [Yb2(2AMB)6(H2O)4] · 2C2H6O (I) and Yb2(3AMB)6(H2O)4] · 3H2O (II) (2AMB = 2-aminobenzoic acid, 3AMB = 3-aminobenzoic acid) have been synthesized and characterized by elemental analysis, infrared spectroscopy, thermogravimetric analysis and X-ray crystallography (CIF files CCDC nos. 950103 (I), 921652 (II)). Complex I crystallizes in triclinic space group \(P\bar 1\) and complex II crystallizes in monoclinic space group P21/n. X-ray analysis shows that both complexes (I, II) have the dinuclear structure. The central Yb3+ ions in both complexes are eight-coordinated adopting distorted YbO8 dodecahedral geometry. Each Yb3+ ion is coordinated to two O atoms from bridging carboxylate, four O atoms from the chelating carboxylate ligands and two O atoms of water molecules. The crystal structure of I and II are stabilized by N-H…O, O-H…O, O-H…N, and C-H…O hydrogen bonds, C-H…π interactions and weak π-π stacking interactions.  相似文献   

16.
A series of new triorganotin(IV) pyridinecarboxylates with 6-hydroxynicotinic acid (6-OH-3-nicH), 5-hydroxynicotinic acid (5-OH-3-nicH) and 2-hydroxyisonicotinic acid (2-OH-4-isonicH) of the types: [R3Sn (6-OH-3-nic)·L]n (I) (R = Ph, L = Ph·EtOH, 1; R = Bn, L = H2O·EtOH, 2; R = Me, L = 0, 3; R = n-Bu, L = 0, 4), [R3Sn (5-OH-3-nic)]n (II) (R = Ph, 5; R = Bn, 6; R = Me, 7; R = n-Bu, 8), [R3Sn (2-OH-4-isonic·L)]n (III) (R = Bn, 9, L = MeOH; R = Me, L = 0, 10; R = Ph, 11, L = 0.5EtOH) have been synthesized. All the complexes were characterized by elemental analysis, TGA, IR and NMR (1H, 13C, 119Sn) spectroscopy analyses. Among them, except for complexes 5 and 6, all complexes were also characterized by X-ray crystallography diffraction analysis. Crystal structures show that complexes 1-10 adopt 1D infinite chain structures which are generated by the bidentate O, O or N, O and the five-coordinated tin centers. Significant O-H?O, and N-H?O intermolecular hydrogen bonds stabilize these structures. Complex 11 is a 42-membered macrocycle containing six tin atoms, and forms a 2D network by intermolecular N-H?O hydrogen.  相似文献   

17.
Two cobalt(II) coordination polymers, [Co(L1)(tbi)(H2O)] n (1) and [Co(L2)(tbi)] n (2) (L1 = 1,4-bis(benzimidazole)butane, L2 = 1,4-bis(2-methylbenzimidazole)butane, H2tbi = 5-tert-butyl isophthalic acid) have been synthesized under hydrothermal conditions and characterized by physicochemical and spectroscopic methods as well as by single-crystal X-ray diffraction analysis. Both complexes exhibit similar 2D (4,4) layer structures, constructed from tbi2? and bis(benzimidazole)-based bridging ligands. The cobalt centers display different coordination environments, with an octahedral geometry in 1 and a distorted square-pyramidal configuration in 2. The thermal stabilities, fluorescence and catalytic properties of both complexes have been investigated.  相似文献   

18.
The organotin (IV) derivatives of 2-mercapto-4-methylpyrimidine (Hmpymt) R3SnL (R = Ph 1, PhCH22, n-Bu 3), R2SnClmLn (m = 1, n = 1, R = CH34, Ph 5, n-Bu 6, PhCH27; m = 0, n = 2, R = CH38, n-Bu 9, Ph 10, PhCH211) were obtained by the reaction of the organotin(IV) chlorides R3SnCl or R2SnCl2 with 2-mercapto-4-methylpyrimidine hydrochloride (HCl · Hmpymt) in 1:1 or 1:2 molar ratio. All complexes 1-11 were characterized by elemental analyses, IR, 1H, 13C and temperature-dependent 119Sn NMR spectra. Except for complexes 3 and 6, the structures of complexes 1, 2, 4, 5, 7, 8-11 were confirmed by X-ray crystallography. Including tin-nitrogen intramolecular interaction, the tin atoms of complexes 1-7 are all five-coordinated and their geometries are distorted trigonal bipyramidal. While the tin atoms of complexes 8-11 are six-coordinated and their geometries are distorted octahedral. Besides, the ligand adopts the different coordination modes to bond to tin atom between the complexes 1, 6, 7 and 2, 3, 4, 5, 8-11. Furthermore, intermolecular Sn?N or Sn?S interactions were recognized in crystal structures of complexes 4, 7 and 11, respectively.  相似文献   

19.
The self-assembly of unsymmetrical tecton 3-nitro-5-(pyridin-4-yl)benzoic acid (HL)with cobalt chloride under hydrothermal conditions affords a new 2D coordination polymer [Co(L)2] n (1, L = 3-nitro-5-(pyridin-4-yl)benzoate), which is characterized by elemental analysis, infrared spectroscopy, thermogravimetric analysis, powder X-ray diffraction analysis, and single crystal X-ray diffraction. Compound 1 is of the triclinic system, space group P-1 with a = 9.7857(12) Å, b = 10.3417(13) Å, c = 10.8463(13) Å, α = 85.155(2)°, β = 74.785(2)°, γ = 88.962(2)°, V = 1055.4(2) Å3. The crystal structural analysis of complex 1 shows that the cobalt center is six-coordinated in an octahedral geometry by four O atoms from four different L ligands and two N atoms from two different L ligands; the Co(II) cations are bridged by μ3-L into an interesting two-dimensional network structure. It should be pointed out that the thermal analysis results indicate that complex 1 is quite stable up to 420°C.  相似文献   

20.
A series of new tin(IV) complexes based on 2-hydroxy-3,6-di-tert-butyl-para-benzoquinone (LH) of the general formula L2SnR2 (R = Me (I), Et (II), Bu n (III), Ph (IV)) and LSnMe3 (V) were synthesized. The obtained compounds were characterized by IR and 1H, 13C and 119Sn NMR spectroscopy and elemental analysis. The X-ray diffraction analysis was carried out for complexes L2Sn(Bu n )2 (III) and LSnMe3 (V). The low-frequency region of the IR spectra, which has not earlier been studied in detail, was interpreted for compounds I–V and previously described complex LSnPh3 (VI). The electrochemical properties of LH and related tin complexes I–VI were studied. The nature of the hydrocarbon groups at the metal atom affects the stability of the intermediates formed in the electrochemical reactions.  相似文献   

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