The Crystal Structure of Bis(N,N-diethyl-N′ -benzoylselenoureato)nickel(II) Ni(C12H15N2OSe)2 crystallizes in the monoclinic space group P21/c. The cell parameters are a = 11.399(3), b = 16.016(4), c = 14.910(6) Å, β = 104.64(3)° and Z = 4. The structure was solved with Patterson and direct methods and was refined to a final R-value of 5.43%. Nickel is coordinated to two N,N-diethyl-N′ -benzoylselenourea molecules to form a bidentally coordinated chelate complex with cis arrangement of the donor atoms. Coordinaton around the nickel atom is planar while the chelate rings diverge from planarity. The ethyl groups of one diethylamino group are disordered. The Ni? Se bond lengths are 2.244(1) and 2.264(1) Å, the Ni? O bond lengths are 1.871(4) and 1.883(4) Å, respectively. 相似文献
Three copper(II) complexes, [Cu2(OAc)4L2] · 2CH3OH ( 1 ), [CuBr2L′2(CH3OH)] · CH3OH ( 2a ), and [CuBr2L′2(DMSO)] · 0.5CH3OH ( 2b ) {L = N‐(9‐anthracenyl)‐N′‐(3‐pyridyl)urea and L′ = N‐[10‐(10‐methoxy‐anthronyl)]‐N′‐(3‐pyridyl)urea} have been synthesized by the reaction of L with the corresponding copper(II) salts. Complex 1 shows a dinuclear structure with a conventional “paddlewheel” motif, in which four acetate units bridge the two CuII ions. In complexes 2a and 2b , the anthracenyl ligand L has been converted to an anthronyl derivative L′, and the central metal ion exhibits a distorted square pyramidal arrangement, with two pyridyl nitrogen atoms and two bromide ions defining the basal plane and the apical position is occupied by a solvent molecule (CH3OH in 2a and DMSO in 2b ). 相似文献
The single crystal X‐ray analysis data of the new hepta‐coordinate cadmium(II) complex of N,N‐dimethyl‐N‐(4‐pyridyl)amine (DMPA), [Cd(DMPA)3(NO2)2]·0.5H2O, shows that the coordination environment around the CdII is pentagonal bipyramidal. Furthermore, self‐assembly of this complex as molecular squares that interlink via π–π stacking interactions is observed. This network contains voids that are filled by water molecules. 相似文献
A series of Zn (II), Pd (II) and Cd (II) complexes, [(L) n MX 2 ] m (L = L‐a–L‐c; M = Zn, Pd; X = Cl; M = Cd; X = Br; n, m = 1 or 2), containing 4‐methoxy‐N‐(pyridin‐2‐ylmethylene) aniline ( L‐a ), 4‐methoxy‐N‐(pyridin‐2‐ylmethyl) aniline ( L‐b ) and 4‐methoxy‐N‐methyl‐N‐(pyridin‐2‐ylmethyl) aniline ( L‐c ) have been synthesized and characterized. The X‐ray crystal structures of Pd (II) complexes [L 1 PdCl 2 ] (L = L‐b and L‐c) revealed distorted square planar geometries obtained via coordinative interaction of the nitrogen atoms of pyridine and amine moieties and two chloro ligands. The geometry around Zn (II) center in [(L‐a)ZnCl 2 ] and [(L‐c)ZnCl 2 ] can be best described as distorted tetrahedral, whereas [(L‐b) 2 ZnCl 2 ] and [(L‐b) 2 CdBr 2 ] achieved 6‐coordinated octahedral geometries around Zn and Cd centers through 2‐equivalent ligands, respectively. In addition, a dimeric [(L‐c)Cd(μ ‐ Br)Br] 2 complex exhibited typical 5‐coordinated trigonal bipyramidal geometry around Cd center. The polymerization of methyl methacrylate in the presence of modified methylaluminoxane was evaluated by all the synthesized complexes at 60°C. Among these complexes, [(L‐b)PdCl 2 ] showed the highest catalytic activity [3.80 × 104 g poly (methyl methacrylate) (PMMA)/mol Pd hr?1], yielding high molecular weight (9.12 × 105 g mol?1) PMMA. Syndio‐enriched PMMA (characterized using 1H‐NMR spectroscopy) of about 0.68 was obtained with Tg in the range 120–128°C. Unlike imine and amine moieties, the introduction of N‐methyl moiety has an adverse effect on the catalytic activity, but the syndiotacticity remained unaffected. 相似文献
Copolymers of 2‐(N,N‐dimethylamino)ethyl acrylate (DMAEA) and 2‐(tert‐Boc‐amino)ethyl acrylate (t BocAEA) are synthesized by reversible addition–fragmentation chain transfer polymerization in a controlled manner with defined molar masses and narrow molar masses distributions (Ð ≤ 1.17). Molar compositions of the P(DMAEA‐co‐t BocAEA) copolymers are assessed by means of 1H NMR. A complete screening in molar composition is studied from 0% of DMAEA to 100% of DMAEA. Reactivity ratios of both comonomers are determined by the extended Kelen–Tüdos method (r DMAEA = 0.81 and rtBocAEA = 0.99).
In this article, we have developed a novel and simple one‐pot reductive acetylation of aromatic nitro compounds with sodium borohydride (NaBH4) in ethyl acetate (EtOAc) under reflux conditions in the presence of the bis(dimethylglyoximato)copper(II) complex [Cu(Hdmg)2] as an efficient and cost‐effective copper‐containing catalyst. Notably, using the above‐mentioned one‐pot reaction, the corresponding acetamide derivatives were obtained in high to excellent yields. 相似文献
Cuprous chloride was coordinated by diazabutadiene (DAB‐R) ligands to form Cu(I)‐(DAB‐R) complexes, most of which have a 1:1 ratio of Cu to DAB‐R as reported. In the case of a special DAB‐iPP, N,N′‐bis(2,6‐diisopropylphenyl)‐1,4‐diaza‐1,3‐butadiene, an unexpected composition of complex was found with the formula Cu(I)Cl(DAB)2. When employed as catalyst for triarylamine synthesis from the coupling of aryl halides with primary and secondary arylamines, the new Cu(I)‐(DAB‐iPP) complex displayed high efficiency. 相似文献
The reaction of N,N′‐di(2‐pyridyl)formamidine (HDpyF) with MnCl2‐4H2O afforded the complex MnCl2(HDpyF), which was characterized by X‐ray crystallography. The HDpyF ligand chelates to the Mn(II) center through the first and the third nitrogen atoms to form a six‐membered ring, leaving the second and the fourth nitrogen atoms uncoordinated. The HDpyF ligand is crystallographically disordered such that two different molecules can be solved. The neutral HDpyF ligand adopts the new s‐cis‐syn‐s‐trans conformation. 相似文献
Reactions of the thiocarbamoyl‐molybdenum complex [Mo(CO)2(η2‐SCNMe2)(PPh3)2Cl] 1 , and ammonium diethyldithiophosphate, NH4S2P(OEt)2, and potassium tris(pyrazoyl‐1‐yl)borate, KTp, in dichloromethane at room temperature yielded the seven coordinated diethyldithiophosphate thiocarbamoyl‐molybdenum complexe [Mo(CO)2{η2‐S2P(OEt)2}(η2‐SCNMe2)(PPh3)] β‐3 , and tris(pyrazoyl‐1‐yl)borate thiocabamoyl‐molybdenum complex [Mo(CO)2(η3‐Tp)(η2‐SCNMe2)(PPh3)] 4 , respectively. The geometry around the metal atom of compounds β‐3 and 4 are capped octahedrons. The α‐ and β‐isomers are defined to the dithio‐ligand and one of the carbonyl ligands in the trans position in former and two carbonyl ligands in the trans position in later. The thiocabamoyl and diethyldithiophosphate or tris(pyrazoyl‐1‐yl)borate ligands coordinate to the molybdenum metal center through the carbon and sulfur and two sulfur atoms, or three nitrogen atoms, respectively. Complexes β‐3 and 4 are characterized by X‐ray diffraction analyses. 相似文献
The binuclear praseodymium(III) complex with N‐(1‐carboxyethylidene)‐salicylhydrazide (C10H10N2O4, H2L) was prepared in H2O‐C2H5OH mixed solution, and the crystal structure of [Pr2L2(HL)2(H2O)4]·3H2O·C6H6 was determined by X‐ray single crystal diffraction. The crystal complex crystallizes in the triclinic system with space group P‐1, and in the structure each Pr atom is 9‐coordinated by carboxyl O and acyl O and azomethine N atoms of two tridentate ligands to form two stable five‐membered rings sharing one side in keto‐mode and two water molecules. The coordination polyhedron around Pr3+ was described as a monocapped square antiprism geometry. In an individual molecule, four tridentate ligands were coordinated by two negative univalent (HL) and two bivalent forms (L) respectively. Two negative univalent ligands were coordinated via μ2‐bridging mode. 相似文献
A simple and eco‐friendly method for the preparation of 1,5‐diaryl‐3‐(arylamino)‐1H‐pyrrol‐2(5H)‐ones via the cyclo‐condensation reaction of aldehydes, amines and ethyl pyruvate in the presence of silica supported ferric chloride (SiO2‐FeCl3) as reusable heterogeneous catalyst is described. The present methodology offers several advantages such as excellent yields, simple procedure and short reaction times. 相似文献
Two new copper(II) complexes of saccharinate (sac) with bis(2‐pyridylmethyl)amine (bpma) and N,N′‐bis[1‐(pyridin‐2‐yl)ethylidene]ethane‐1,2‐diamine (bapen), [Cu(bpma)(sac)2] · H2O ( 1 ) and [Cu(bapen)(sac)2] ( 2 ), were synthesized and characterized by elemental analysis, TG‐DTA, X‐ray diffraction, and UV/Vis and IR spectroscopy, respectively. In 1 , the copper(II) ion is coordinated by two N‐bonded sac ligands, and three nitrogen atoms of bpma, in a distorted square‐pyramidal coordination arrangement, whereas the arrangement around the copper ion in 2 is a distorted octahedron with two N‐coordinated sac ligands and a tetradentate bapen ligand. In addition to hydrogen bonding involving the water molecule in 1 , the mononuclear species of 1 and 2 are further connected by weak intermolecular C–H ··· π and C–H ··· O interactions to form a three‐dimensional network. Both complexes are luminescent at room temperature and their emissions seem to be due to ligand‐based π–π* transitions. 相似文献
The reaction of Pb(CH3COO)2·3H2O with N‐benzesulfonyl‐L‐glutamic acid in the presence of 2, 2′‐bipyridine (bipy) or 1,10‐phenanthroline (phen) produced two novel complexes [Pb2(Bs‐glu)2(bipy)2] ( 1 ) and [Pb2(Bs‐glu)2(phen)2] ( 2 ) (Bs‐glu = N‐benzesulfonyl‐L‐glutamic acid dianion). In 1 chains bearing alternative 16‐membered rings and Pb2O3 nodes are constructed from the interactions of PbII ions with the carboxylates of Bs‐glu ligands. To the best of our knowledge, this is the first lead(II) complex of carboxylates with the formation of chains of Pb2O3. In 2 the 16‐membered ring units are connected by centrosymmetric Pb2O2 nodes to form chains. Complexes 1 and 2 construct the 3‐D supramolecular architectures through versatile hydrogen bonds and π‐π stacking interactions. 相似文献
Ruthenium(II) Complexes of Orthometallated O'Donnell Schiff Bases (Diphenylmethylene Glycine Esters) [1] The reaction of diphenyl methylene glycine esters with [Ru(PPh3)3Cl2] gives the orthometallated complexes [Ru(PPh3)2(Cl){(C6H4)(C6H5)C=NCH2CO2R}] (R = H, Et, CMe3) in which the ester group is coordinated to the ruthenium atom and which were characterized by IR, NMR, MS data and by cyclovoltammetry. 相似文献
Crystal structures are reported for four (2,2′‐bipyridyl)(ferrocenyl)boronium derivatives, namely (2,2′‐bipyridyl)(ethenyl)(ferrocenyl)boronium hexafluoridophosphate, [Fe(C5H5)(C17H15BN2)]PF6, (Ib), (2,2′‐bipyridyl)(tert‐butylamino)(ferrocenyl)boronium bromide, [Fe(C5H5)(C19H22BN3)]Br, (IIa), (2,2′‐bipyridyl)(ferrocenyl)(4‐methoxyphenylamino)boronium hexafluoridophosphate acetonitrile hemisolvate, [Fe(C5H5)(C22H20BN3O)]PF6·0.5CH3CN, (IIIb), and 1,1′‐bis[(2,2′‐bipyridyl)(cyanomethyl)boronium]ferrocene bis(hexafluoridophosphate), [Fe(C17H14BN3)2](PF6)2, (IVb). The asymmetric unit of (IIIb) contains two independent cations with very similar conformations. The B atom has a distorted tetrahedral coordination in all four structures. The cyclopentadienyl rings of (Ib), (IIa) and (IIIb) are approximately eclipsed, while a bisecting conformation is found for (IVb). The N—H groups of (IIa) and (IIIb) are shielded by the ferrocenyl and tert‐butyl or phenyl groups and are therefore not involved in hydrogen bonding. The B—N(amine) bond lengths are shortened by delocalization of π‐electrons. In the cations with an amine substituent at boron, the B—N(bipyridyl) bonds are 0.035 (3) Å longer than in the cations with a methylene C atom bonded to boron. A similar lengthening of the B—N(bipyridyl) bonds is found in a survey of related cations with an oxy group attached to the B atom. 相似文献