首页 | 本学科首页   官方微博 | 高级检索  
相似文献
 共查询到20条相似文献,搜索用时 218 毫秒
1.
Reaction of the potassium salts of podand-containing bis(dithiophosphonate)s [PhO(4-C6H4)P(S)(SH)OCH2CH2]2O (H 2 L) with Co(II), Ni(II) and Cd(II) in aqueous EtOH leads to complexes of formulae M2(L-S,S′)2. The structural formulae of the compounds were deduced by physico-chemical and spectroscopic methods. It was established that complex Ni 2 L 2 recognizes CH2Cl2.  相似文献   

2.
Reaction of O,O’-diisopropylthiophosphoric acid isothiocyanate (iPrO)2P(S)NCS with diethyl 4-aminobenzylphosphonate (EtO)2P(O)CH2C6H4-4-NH2 leads to the new N-thiophosphorylated thiourea (EtO)2P(O)CH2C6H4-4-[NHC(S)NHP(S)(OiPr)2] (HL). Reaction of the potassium salt of HL with Zn(II), Cd(II) and Co(II) in aqueous EtOH leads to complexes of formula M(L-S,S’)2 (ML2). Heteroligand copper(I) complex of HL and triphenylphosphine was prepared by the reaction of the potassium salt KL and Cu(PPh3)3I. Copper in complex Cu(PPh3)L is bound by one PPh3 and one SCNPS fragment of the chelating ligand. Compounds obtained were investigated by IR, UV–Vis, 1H and 31P{1H} NMR spectroscopy, and microanalysis. The structures of HL and Cu(PPh3)L were investigated by single crystal X-ray diffraction analysis.  相似文献   

3.
The reaction of the potassium salt of the N-(thio)phosphorylated thioureas AdNHC(S)NHP(O)(OiPr)2 (HLI , Ad = Adamantyl) and MeNHC(S)NHP(S)(OiPr)2 (HLII ) with Co(II) and Zn(II) in aqueous EtOH leads to [MLI,II 2] chelate complexes. They were investigated by UV-vis, 1H and 31P NMR spectroscopy, and microanalysis. The molecular structures of [MLI 2] were elucidated by single crystal X-ray diffraction analysis. The metal centers in both complexes are found to be in a distorted-tetrahedral O2S2 environment formed by the C=S sulfur atoms and the P=O oxygen atoms of two deprotonated LI ligands. The photoluminescence properties of [ZnLII 2] are also reported.  相似文献   

4.
The reaction of O,O′-diisopropylphosphoric acid isothiocyanate (iPrO)2P(O)NCS with 2-methylaniline 2-MeC6H4NH2, 2,6-dimethylaniline 2,6-Me2C6H3NH2, or 2,4,6-trimethylaniline 2,4,6-Me3C6H2NH2 leads to the N-phosphorylated thioureas RNHC(S)NHP(O)(OiPr)2 (R = 2-MeC6H4?, HLI ; 2,6-Me2C6H3?, HLII ; 2,4,6-Me3C6H2?, HLIII ). Reaction of the potassium salts of HLI III with Ni(II) in aqueous EtOH leads to [Ni(LI–III-N,S)2] ([NiLI–III 2 ]) chelate complexes. The compounds obtained were investigated by 1H, 31P{1H} NMR spectroscopy and microanalysis. The molecular structure of the thiourea HLIII was elucidated by single crystal X-ray diffraction analysis. Single crystal X-ray diffraction studies showed that HLIII forms both intra- and intermolecular hydrogen bonds, which in turn leads to the formation of polymeric chains. One of the intermolecular hydrogen bonds is of the type N?H…S. Moreover, the formation of intermolecular C?H…η6-phenyl interactions was established.

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   

5.
Reaction of the potassium salt of N-(diisopropoxyphosphoryl)-p-bromothiobenzamide p-BrC6H4C(S)NHP(O)(OiPr)2 (HL) with Cd(II) cations in freshly dried and distilled EtOH leads exclusively to the complex [Cd(p-BrC6H4C(S)NH2-S)(L-O,S)2] ([Cd(LI)L2]), while the same reaction in H2O leads to the complex [Cd(HL-O)2(L-O,S)2] ([Cd(HL)2L2]). The corresponding reactions with Zn(II) always lead to the complex [Zn(L-O,S)2] ([ZnL2]) regardless of the solvent. The crystal structure of [Cd(HL)2L2].2/3H2O reveals to be a polymorph to the previously reported anhydrous [Cd(HL)2L2].  相似文献   

6.
New Co(II), Ni(II), and Cu(II) complexes with 4-(3-hydroxyphenyl)-1,2,4-triazole (L) with the compositions [Co3L6(H2O)5(C2H5OH)](NO3)6 · 2H2O · C2H5OH (I), [Ni3L6(H2O)6](NO3)6 · 2H2O (II), and [M3L6(H2O)6](ClO4)6 · nH2O (M = Co2+, n = 2 (III); Ni2+, n = 2 (IV); Cu2+, n = 0 (V)) are synthesized. The complexes are studied by X-ray structure analysis, X-ray diffraction analysis, UV and IR spectroscopy, and the statistical magnetic susceptibility method. All compounds have the linear trinuclear structure. Ligand L is coordinated to the metal ions by the N(1) and N(2) atoms of the heterocycle according to the bidentate bridging mode. In all compounds the coordination polyhedron of the metal atom is a distorted octahedron. The molecular and crystal structures of compound I, [Co3L6(H2O)6](ClO4)6 · 8C2H5OH (IIIa), and [Ni3L6(H2O)6](ClO4)6 · 8C2H5OH (IVa) are determined.  相似文献   

7.
The redox reaction of bis(2-benzamidophenyl) disulfide (H2L-LH2) with [Pd(PPh3)4] in a 1:1 ratio gave mononuclear and dinuclear palladium(II) complexes with 2-benzamidobenzenethiolate (H2L), [Pd(H2L-S)2(PPh3)2] (1) and [Pd2(H2L-S)2 (μ-H2L-S)2(PPh3)2] (2). A similar reaction with [Pt(PPh3)4] produced only the corresponding mononuclear platinum(II) complex, [Pt(H2L-S)2(PPh3)2] (3). Treatment of these complexes with KOH led to the formation of cyclometallated palladium(II) and platinum(II) complexes, [Pd(L-C,N,S)(PPh3)] ([4]) and [Pt(L-C,N,S) (PPh3)] ([5]). The molecular structures of 2, 3 and [4] were determined by X-ray crystallography.  相似文献   

8.
The oxalato-bridged dinickel(II) complex with the title ligand, [Ni2(L a H)2(μ-ox)](ClO4)2·2H2O (1), was prepared and its structure was determined by X-ray crystallography, as well as that of the monomeric nickel(II) complex, [Ni(L a H)ox]ClO4·3H2O (2). In Complexes 1 and 2, the ligand, L a , is folded along the N(4)–Ni(1)–N(11) axis. The antiferromagnetic coupling between the two nickel(II) centers in 1 was revealed and the coupling constant, J?=??17.4?cm?1, and g?=?2.11 were estimated. It was found that the oxalato-bridged dimer 1 was readily converted to the mononuclear cis-nickel(II) complex [NiL a (OH2)](ClO4)2 (3a), in basic aqueous solution. In [NiL a (CH3CN)]I2 (3b), which was derived from 3a, the aminomethyl pendant arm is coordinated to the Ni(II) ion and L a is folded along the N(1)–Ni(1)–N(8) axis.  相似文献   

9.
Five coordination compounds of bismuth, lanthanum and praseodymium nitrate with the oxygen‐coordinating chelate ligand (iPrO)2(O)PCH2P(O)(OiPr)2 (L) are reported: [Bi(NO3)3(L)2] ( 1 ), [La(NO3)3(L)2] ( 2 ), [Pr(NO3)3(L)2] ( 3 ), [La(NO3)3(L)(H2O)] ( 4 ) and [Pr(NO3)3(L)(H2O)] ( 5 ). The compounds were characterized by means of single crystal X‐ray crystallography, 1H and 31P NMR spectroscopy in solution, solid‐state 31P NMR spectroscopy, IR spectroscopy, DTA‐TG measurements ( 1 , 2 and 4 ), conductometry and electrospray ionization mass spectrometry (ESI‐MS). In addition, DFT calculations for model compounds of 1 and 2 support our experimental work. In the solid state mononuclear coordination compounds were observed for 1 — 3 , whereas compounds 4 and 5 gave one‐dimensional hydrogen‐bonded polymers via water‐nitrate coordination. Despite of the similar ionic radii of bismuth(III), lanthanum(III) and praseodymium(III) for a given coordination number the bismuth and lanthanide compounds 1 — 3 are not isostructural. The bismuth compound 1 shows a 9‐coordinate bismuth atom whereas lanthanum(III) and praseodymium(III) atoms are 10‐coordinate in the lanthanide complexes 2 — 5 . The general LnO10 coordination motif in compounds 2 — 5 is best described as a distorted bi‐capped square antiprism. The BiO9 polyhedron might be deduced from the LnO10 polyhedron by replacing one oxygen ligand with a stereochemically active lone pair. The one‐to‐one complexes 4 and 5 dissociate in solution to give the corresponding one‐to‐two complexes 2 and 3 , respectively, and solvated Ln(NO3)3. In contrast to the lanthanides, the one‐to‐two bismuth complex 1 is less stable in CH3CN solution and partially dissociates to give solvated Bi(NO3)3 and (iPrO)2(O)PCH2P(O)(OiPr)2.  相似文献   

10.
The S2O2-donor macrocycle, L(5,8-dioxa-2,11-dithia-[12]-o-cyclophane or 3,4-benzo-1,6-dithia-9,12-dioxocyclo-tetradecane-3-ene) was synthesized by ring closure reaction of 2,2'-(ethylenedioxy)diethanethiol with ,'-dibromo-o-xyleneunder high dilution and crystallized from methanol. The X-ray structure of L has a C2 axis and is shown to have two S atoms oriented exodentate and two O atoms positionedendodentate to the ring cavity. Reaction of AgNO3 with L affords monomeric [Ag(L)(NO3)], (1)in which the Ag atom is in a distorted trigonal plane coordinated by two S atoms in a ring and to one O atom from the NO3 - ion. The behavior of complex 1 in solution was also characterized by NMR titration. Reaction between K2PtCl4 and L affords [Pt(L)Cl2], (2) in which the Pt atom has a distorted square-planar environment, coordinated to two S atoms of Land to two Cl- ions in a cis arrangement.  相似文献   

11.
12.
Copper Complexes of the New Chelate Ligand 1‐Methyl‐2‐(2‐thiophenolato)‐1H‐benzimidazole (mtpb) and of its Oxidation Products Anodic electrolysis of copper in acetonitrile in the presence of Hmtpb leads to formation of yellow [Cu4(mtbp)4] which was crystallized as a dichloromethane solvate with two crystallographically independent cluster molecules in the unit cell. The copper(I) atoms exhibit slightly pyramidal S2N coordination with bridging thiolate sulfur atoms. The two clusters contain the four copper atoms arranged in a more (Cu1‐Cu4) or less (Cu5‐Cu8) distorted bisphenoidal arrangement. Reaction of mtpb with Cu(ClO4)2 under anoxic conditions also produces [Cu4(mtpb)4]. However, the admittance of O2 in the reaction of mtpb with copper(II) acetate in methanol causes oxidation of the sulfur atoms; a square‐pyramidal configurated copper(II) complex [Cu(CH3CO2‐κ2O)(L1‐κN)(L2‐κN, O)] has been isolated and crystallographically characterized in which L1 is the neutral sulfinic methyl ester and L2 is the sulfonate derived from mtpb.  相似文献   

13.
(S)-N-二茂铁甲基苯丙氨酸钠为配体,与Zn(Ac)2反应合成了一个新型手性单核配合物(S)-[Zn(FcCH2NHCH(CH2Ph)COO)2·H2O](H2O)。X-射线单晶结构分析表明,中心离子Zn(Ⅱ)与2个FcCH2NHCH(CH2Ph)COO-和1个水分子配位,形成树状的骨架构型。该配合物晶体属正交晶系,P212121空间群。晶胞参数为:a=0.893 4(2) nm;b=1.669 8(4) nm;c=2.588 4(6) nm。电化学测试表明该配合物的氧化和还原峰电位同配体相比向高电位方向移动。室温下,标题化合物呈现出较强的固体双重荧光性能,量子化学计算给出了初步的解释。  相似文献   

14.
Heteronuclear complexes containing oxorhenium(V), with Fe(III), Co(II), Ni(II), Cu(II), Cd(II) and UO2(VI) ions were prepared by the reaction of the complex ligands [ReO(HL1)(PPh3)(OH2)Cl]Cl (a) and/or [ReO(H2L2)(PPh3)(OH2)Cl]Cl (b), where H2L1?=?1-(2-hydroxyphenyl)butane-1,3-dione-3-(5,6-diphenyl-1,2,4-triazine-3-ylhydrazone) and H3L2?=?1-(2-hydroxyphenyl)butane-1,3-dione-3-(1H-benzimidazol-2-ylhydrazone), with transition and actinide salts. Heterodinuclear complexes of ReO(V) with Fe(III), Co(II), Ni(II), Cu(II) and Cd(II) were obtained using a 1?:?1 mole ratio of the complex ligand and the metal salt. Heterotrinuclear complexes were obtained containing ReO(V) with UO2(VI) and Cu(II) using 2?:?1 mole ratios of the complex ligand and the metal salts. The complex ligands a and b coordinate with the heterometal ion via a nitrogen of the heterocyclic ring and the nitrogen atom of the C=N7 group. All transition metal cations in the heteronuclear complexes have octahedral configurations, while UO2(VI)?complexes have distorted dodecahedral geometry. The structures of the complexes were elucidated by IR, ESR, electronic and 1H NMR spectra, magnetic moments, conductance and TG-DSC measurements. The antifungal activities of the complex ligands and their heteronuclear complexes towards Alternaria alternata and Aspergillus niger showed comparable behavior with some well-known antibiotics.  相似文献   

15.
Three mercury(II) complexes containing double-betaine and halide ligands, [(HgCl2)2(L1)] n (1), [(HgBr2)2(L1)(H2O)2] n (2), and [2HgCl2(HL1)·Hg2Cl6] n (3) [L1=O2CCH2N+(CH2CH2)3-N+H2CO2 ], have been prepared and shown to have polymeric structures by single-crystal X-ray analysis. Complex (1) exhibits an infinite zigzag chain in which each mercury(II) atom is coordinated by pairs of carboxylate oxygen atoms and chloride ligands in a distorted tetrahedral geometry. In complex (2), the mercury(II) atom is in an unusual square-planar coordination geometry, and weak mercury-ligand and hydrogen bonding extend the structural skeletons into a three-dimensional network. Complex (3) consists primarily of an assembly of HgCl2(HL1) moieties and [Hg2Cl6] anions, and the mercury(II) atoms are in planar T-shaped and distorted tetrahedral coordination environments, respectively. The resulting three-dimensional network is based on the cross-linkage of nearly planar, wide ribbons running in thea direction.  相似文献   

16.
2‐Aminopyrimidine (L1) and 2‐amino‐4,6‐dimethylpyrimidine (L2) have been used to create the two novel title complexes, [Ag2(NCS)2(C4H5N3)]n, (I), and [Ag(NCS)(C6H9N3)]n, (II). The structures of complexes (I) and (II) are mainly directed by the steric properties of the ligands. In (I), the L1 ligand is bisected by a twofold rotation axis running through the amine N atom and opposite C atoms of the pyrimidine ring. The thiocyanate anion adopts the rare μ3‐κ3S coordination mode to link three tetrahedrally coordinated AgI ions into a two‐dimensional honeycomb‐like 63 net. The L1 ligands further extend the two‐dimensional sheet to form a three‐dimensional framework by bridging AgI ions in adjacent layers. In (II), with three formula units in the asymmetric unit, the L2 ligand bonds to a single AgI ion in a monodentate fashion, while the thiocyanate anions adopt a μ3‐κ1N2S coordination mode to link the AgL2 subunits to form two‐dimensional sheets. These layers are linked by N—H...N hydrogen bonds between the noncoordinated amino H atoms and both thiocyanate and pyrimidine N atoms.  相似文献   

17.
Two triangular molybdenum‐tellurium clusters, Mo3Te7‐[S2CN (CH2CH2OH2]3I (1) and Mo3Te4Y3[S2P(iPrO)2]3I (Y3 = 1. 43Te+ 1.57S) (2), were obtained from the reaction of K · HOdtc [HOdtc = S2CN(CH2CH2OH)2] or K·iPr2dtp (iPr2dtp = S2P[OCH(CH3)2]2) with a mixed product of elements Mo, Te(S) and I2 at high temperature. The structures of the two compounds were determined by X‐ray crystallography study. Crystal data are, (1): monoclinic, P21/n, a = 1.6256(3), b = 1.3264(2), c = 1.8808(4) nm, β=96.923°, V = 4.025.9 (14) nm3, Dcal = 3.050g·cm‐3, Z = 4, and (2): monoclinic, P21/n, a = 1.4564(2), b = 2.3917(4), c = 1.5094(3) nm, β = 114.35(2)°, V = 4.0259(14) nm3, Dcal = 2.449 g·cm?3 and Z = 4. Single crystal analyses show that 1 consists of discrete Mo3Te7[S2CN(CH2CH2OH)2]3I connected into three‐dimensional framework via hydrogen bonds, while 2 forms a linear chain via Te(S)—I interaction.  相似文献   

18.
Four new nickel(II), zinc(II), and cobalt(II) complexes, [Zn(L1)2]?·?H2O (1), [Ni(L1)2]?·?H2O (2), [Ni(L2)2] (3), and [Co(L3)2]?·?H2O (4), derived from hydroxy-rich Schiff bases 2-{[1-(5-chloro-2-hydroxyphenyl)methylidene]amino}-2-methylpropane-1,3-diol (HL1), 2-{[1-(2-hydroxy-3-methoxyphenyl)methylidene]amino}-2-ethylpropane-1,3-diol (HL2), and 2-{[1-(5-bromo-2-hydroxyphenyl)methylidene]amino}-2-methylpropane-1,3-diol (HL3) have been synthesized and characterized by elemental analyses, infrared spectroscopy, and single-crystal X-ray determination. Each metal in the complexes is six-coordinate in a distorted octahedral coordination. The Schiff bases coordinate to the metal atoms through the imino N, phenolate O, and one hydroxyl O. In the crystal structures of HL1 and the complexes, molecules are linked through intermolecular O–H···O hydrogen bonds, forming 1-D chains. The urease inhibitory activities of the compounds were evaluated and molecular docking study of the compounds with the Helicobacter pylori urease was performed.  相似文献   

19.
In N,N′‐di‐tert‐butyl‐N′′,N′′‐dimethylphosphoric triamide, C10H26N3OP, (I), and N,N′,N′′,N′′′‐tetra‐tert‐butoxybis(phosphonic diamide), C16H40N4O3P2, (II), the extended structures are mediated by P(O)...(H—N)2 interactions. The asymmetric unit of (I) consists of six independent molecules which aggregate through P(O)...(H—N)2 hydrogen bonds, giving R21(6) loops and forming two independent chains parallel to the a axis. Of the 12 independent tert‐butyl groups, five are disordered over two different positions with occupancies ranging from to . In the structure of (II), the asymmetric unit contains one molecule. P(O)...(H—N)2 hydrogen bonds give S(6) and R22(8) rings, and the molecules form extended chains parallel to the c axis. The structures of (I) and (II), along with similar structures having (N)P(O)(NH)2 and (NH)2P(O)(O)P(O)(NH)2 skeletons extracted from the Cambridge Structural Database, are used to compare hydrogen‐bond patterns in these families of phosphoramidates. The strengths of P(O)[...H—N]x (x = 1, 2 or 3) hydrogen bonds are also analysed, using these compounds and previously reported structures with (N)2P(O)(NH) and P(O)(NH)3 fragments.  相似文献   

20.
Summary Nickel(II), palladium(II), cobalt(II) and copper(II) complexes of the ligandN,N-1,2-propane-bis(methyl 2-amino-cyclopent-1-ene-dithiocarboxylate) (H2L1),N,N-1,3-propane-bis(methyl 2-aminocyclopent-1-ene-dithiocarboxylate) (H2L2) andN,N-[bis(methyl 2-aminocyclopent-1-ene-dithiocarboxylate)] diethylenetriamine (H2L3) have been synthesised. Both H2L1 and H2L2 form complexes of the type ML, and all but the copper(II) complexes, are square planar. In the copper(II) complexes tetrahedral distortion is significantly more with CuL2. From H2L3 square planar complexes of the type [M(HL3)X] (M=Ni, X=Cl, Br, I or SCN; M=Pd, X=Cl or Br) have been obtained in which the donor unit involved is N2SX. The composition of the cobalt(II) and copper(II) complexes is [M(H2L3)X2] (X=Cl or Br) which contain the chromophore [MN3X2].  相似文献   

设为首页 | 免责声明 | 关于勤云 | 加入收藏

Copyright©北京勤云科技发展有限公司  京ICP备09084417号