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1.
Two trans‐bis(saccharinato) (sac) complexes of cadmium(II ) with 2‐aminomethylpyridine (ampy) and 2‐aminoethylpyridine (aepy) were synthesized and characterized by means of elemental analysis, FT‐IR spectroscopy and thermal analysis. In addition, their solid‐state structures were determined by single crystal X‐ray diffraction studies. The [Cd(sac)2(ampy)2] ( 1 ) and [Cd(sac)2(aepy)] ( 2 ) complexes consist of neutral monomeric units and crystallize in the orthorhombic (Pbca) and monoclinic (P21/c) crystal systems, respectively. The cadmium(II ) ions in 1 and 2 sit on inversion centres andexhibit distorted octahedral coordination by two sac anions and two aminopyridine ligands. The sac ligands in both complexes are N‐coordinated and located in trans positions, while the ampy and aepy ligands act as a bidentate ligand forming two symmetrically chelate rings around cadmium(II ). IR spectra and thermal decompositions of the complexes are also discussed.  相似文献   

2.
The title saccharinate complexes, aqua[1,2‐benzisothiazol‐3(2H)‐onato 1,1‐dioxide‐N]bis(1,10‐phenanthroline‐N,N′)man­ganese(II) 1,2‐benz­isothia­zol‐3(2H)‐onate 1,1‐dioxide,[Mn(C7H4NO3S)(C12H8N2)2(H2O)](C7H4NO3S), and aqua[1,2‐benz­iso­thiazol‐3(2H)‐onato 1,1‐dioxide‐N]­bis­(2,2′‐bi­pyri­dine‐N,N′)­cobalt(II) 1,2‐benz­iso­thia­zol‐3(2H)‐onate 1,1‐di­oxide, [Co­(C7H4NO3S)­(C10H8N2)2­(H2O)]­(C7H4NO3S), have been prepared and their crystal structures determined at 150 K. The structure of the manganese complex consists of repeated alternating [Mn(phen)2(sac)(H2O)]+ cations and non‐coordinated saccharinate anions. The water molecule, bound to manganese as part of a slightly distorted octahedral arrangement, is hydrogen bonded to an O atom of the SO2 group in the saccharinate counter‐ion. In contrast, the cobalt complex has one pseudo‐octahedral [Co(bipy)2(sac)(H2O)]+ cation, with the cobalt‐bound water molecule hydrogen bonded to the N atom of the accompanying free saccharinate anion.  相似文献   

3.
New mixed-anion cadmium(II) complexes of 2,2′-bipyridine (bpy) and 1,10-phenanthroline (phen) ligands, [Cd(phen)2(NO2)1.65(NO3)0.35] and Cd(bpy)(ClO4)(CH3COO) have been synthesized and characterized by elemental analysis, IR-, 1H NMR-, 13C- NMR and 113Cd NMR spectroscopy. The single crystal X-ray data of [Cd(phen)2(NO2)1.65(NO3)0.35] show the complex to be a monomer and that the Cd atom has an unsymmetrical eight-coordinate geometry, being coordinated by four nitrogen atoms of ‘phen’ ligands and four oxygen atoms of the nitrite and nitrate anions. There is a short ππ stacking interaction between parallel aromatic rings.  相似文献   

4.

The first 2-pyridylethanol (pyet) complexes of manganese(II), iron(II), cobalt(II), nickel(II), copper(II) and zinc(II) saccharinates, were synthesized and characterized by elemental analyses, magnetic measurements, UV-Vis, and IR spectroscopic techniques. Crystal and molecular structures of the iron(II) and copper(II) complexes were determined by single crystal X-ray diffractometry. The experimental data showed that all the complexes are mononuclear with a general formula [M(H2O)2(pyet)2](sac)2, where sac is the saccharinate anion. All the metal ions are octahedrally coordinated by two aqua and two pyet ligands. The pyet ligand acts as a bidentate ligand through its amine nitrogen and hydroxyl oxygen atoms forming a six-membered chelate ring, while the sac ions remain outside the coordination sphere. All the complexes are isomorphous with a monoclinic space group P21/n and Z = 2.  相似文献   

5.
A complex with eight‐coordinate lead(II ) atom and saccharinate (sac) and 2‐aminomethylpyridine ligands was characterized by IR, elemental analysis and X‐ray crystallography. The lead(II ) complex crystallizes in the monoclinic crystal system with space group P21/c. The single crystal X‐ray analysis shows that the complex is a coordination polymer, [Pb(ampy)(μ‐sac)2]n, in which the lead(II ) ions have a highly distorted bicapped trigonal antiprism coordination. Lead(II ) ions are bridged by carboxyl groups of sac forming one‐dimensional linear chains, running parallel to the a axis. The intrachain Pb···Pb distances are 4.4490(3) and 4.4679(3)Å. The individual chains are connected by N—H···Osulfonyl and Campy—H···Osulfonyl type hydrogen bonds, resulting in a three‐dimensional network. The sac ligand acts as bidentate and bridging ligand, while ampy behaves as an N, N′ donor. The IR spectra of the lead(II ) complex are discussed in detail.  相似文献   

6.
Cadmium acetate reacts with sulfamethoxazole (5‐methyl‐3‐isoxazolyl sulfanilamide) and with DMF / DMSO / pyridine to give the crystalline polymers [Cd(sulfamethoxazolato)2(L2)]n {L = DMF ( 1 ), DMSO ( 2 )} and [Cd(sulfamethoxazolato)2(Py)2]n·n(Py) ( 3 ). Complexes 1 , 2 and 3 confirm the tectonic character of the [Cd(sulfamethoxazolato)2(L)2] moieties and the remarkable ability of the {Cd(sulfamethoxazolato)4} fragments to be non selectively stabilized by monodentate ligands. In the polymeric assemblies of the title complexes the cadmium(II) atoms are linked through sulfamethoxazolato anions which alternate in their coordination with the isoxazolic N‐atoms and the aromatic amino groups. The chains of vicinal rings build tunnels along the crystallographic c axis.  相似文献   

7.
Treatment of [M(AMP)Cl2] (M = PtII, PdII; AMP = 2-aminomethylpyridine) with 1 mole of AgX (X = ClO4, BF4, PF6) in dmso yields [M(AMP)(dmso)Cl]X. Single crystal X-ray structure determinations of the PdII and PtII complexes indicate that dmso is S-bondedtrans to the pyridyl ring in both complexes. (2-Aminomethylpyridine)chloro(dimethylsulphoxide-S) palladium(II) tetrafluoroborate.  相似文献   

8.
The preparation and characterization of three metal(II) chlorido complexes with 1,2‐di(1H‐tetrazol‐1‐yl)ethane (dte) ( 1 ) as ligand is presented. The complexes have the following formula: [CoCl2(μ‐dte)(dte)2]n ( 2 ), [CuCl2(μ‐dte)2]n ( 3 ), and [Cd(μ‐Cl)2(μ‐dte)]n ( 4 ). Single crystal X‐ray diffraction of all three metal complexes was performed and the structures are discussed. All three central metal atoms are connected to polynuclear structures by the μ‐bridging ligand. Cobalt and copper are connected to one‐dimensional chains. The central cadmium(II) atoms are additionally connected by the chloride anions to a two‐dimensional network. Further, the cobalt(II) complex represents a special case with two terminal dte ligands.  相似文献   

9.
The structure of the title complex consists of isolated [Cd(C7H4NO3S)2(C4H11NO2)2] units. The Cd2+ cation lies on an inversion centre and is octahedrally coordinated by two N,O‐bidentate diethanol­amine (dea) and two N‐bonded saccharinate (sac) ligands [saccharin is 1,2‐benziso­thia­zol‐3(2H)‐one 1,1‐dioxide]. The dea ligands constitute the equatorial plane of the octahedron, forming two five‐membered chelate rings around the CdII ion, while the sac ligands are localized at the axial positions. The Cd—Nsac, Cd—Ndea and Cd—Odea bond distances are 2.3879 (12), 2.3544 (14) and 2.3702 (13) Å, respectively. The H atoms of the free and coordinated hydroxyl groups of the dea ligands are involved in hydrogen bonding with the carbonyl and sulfonyl O atoms of the neighbouring sac ions, while the amine H atom forms a hydrogen bond with the free hydroxyl O atom. The individual mol­ecules are held together by strong hydrogen bonds, forming an infinite three‐dimensional network.  相似文献   

10.
A novel ZnII complex of the saccharinate ligand (sac) with tris‐hydroxymethylaminomethane (tham) was synthesized and characterized by elemental analysis, FT‐IR spectroscopy, simultaneous TG and DTA techniques, and X‐ray diffraction. The complex, [Zn(sac)(tham)2](sac), crystallizes in monoclinic system with space group P21/c [a = 7.55954(3) Å, b = 13.0532(6) Å, c = 27.7777(10) Å, β = 100.539(3)°, Z = 4]. The ZnII ion has a distorted octahedral coordination. The tham ligand has chemically different functions in the structure, acting as both bidentate and tridentate ligands. There are also sac moieties to act as N‐bonded ligand and as a counter anion. The molecular packing of the complex is provided by moderate hydrogen bonds as well as π···π interactions between the sac moieties. The IR spectra and the thermal decomposition of the complex are also discussed.  相似文献   

11.
The complex [Pb(H2O)(μ‐OAc)(μ‐sac)]n with acetate (OAc) and saccharinate (sac) ligands was characterized by IR, elemental analysis and X‐ray crystallography. The mixed‐anion lead(II) complex crystallizes in the triclinic crystal system with the space group of P1¯. The single crystal X‐ray analysis shows that the complex is a coordination polymer in which the lead(II) ions have a highly distorted pentagonal bipyramidal coordination geometry. Lead(II) ions are bridged by carboxylate groups in a zigzag arrangement forming one‐dimensional infinite chains, which are also linked by sac bridges and aromatic π‐π contacts between the adjacent phenyl rings of sac ligands, resulting in a three‐dimensional network. One water molecule coordinates the lead(II) ion and also forms weak hydrogen bonds with the sulfonyl oxygen atoms of the neighboring sac ligands. The sac ligand acts as a bridging ligand through the nitrogen and carbonyl oxygen atoms, while the carboxylate moiety of the acetate ligand shows an unusual (bidentate, and bridging) coordination behaviour, which was observed for the first time in the structure.  相似文献   

12.
Cadmium(II) complexes, catena-poly[bis(thiocyanato-κN)bis(N-methylthiourea)cadmium(II)], [Cd(Metu)2(NCS)2]n (1) and dicyanidobis(N-methylthiourea)cadmium(II), [Cd(Metu)2(CN)2] (2) were prepared and their structures were determined by single crystal X-ray analysis. In 1, the cadmium(II) ion is bound to four sulfur atoms of bridging Metu ligands and two nitrogen atoms of thiocyanate adopting a distorted octahedral environment. In 2, the geometry around cadmium is distorted tetrahedral attained by two cyanide ions and two methylthiourea molecules bound through the sulfur atoms. The crystal structures of both complexes show intra and intermolecular hydrogen bonding interactions. The complexes were also characterized by IR and NMR spectroscopy and the spectroscopic data were discussed in terms of the nature of bonding.  相似文献   

13.
Coordination Polymeric 1, 2‐Dithiooxalato and 1, 2‐Dithiosquarato Complexes. Syntheses and Structures of [BaCr2(bipy)2(1, 2‐dtox)4(H2O)2], [Ni(cyclam)(1, 2‐dtsq)]·2DMF, [Ni(cyclam)Mn(1, 2‐dtsq)2(H2O)2]·2H22, and [H3O][H5O2][Cu(cyclam)]3[Cu2(1, 2‐dtsq)3]2 1, 2‐Dithioxalate and 1, 2‐dithiosquarate ions have a pair of soft and hard donor centers and thus are suited for the formation of coordination polymeric complexes containing soft and hard metal ions. The structures of four compounds with building blocks containing these ligands are reported: In [BaCr2(bipy)2(1, 2‐dtox)4(H2O)2] Barium ions and pairs of Cr(bipy)(1, 2‐dtox)2 complexes form linear chains by the bisbidentate coordination of the dithiooxalate ligands towards Ba2+ and Cr3+. In [Ni(cyclam)(1, 2‐dtsq)]·2DMF short NÖH···O hydrogen bonds link the NiS2N4‐octahedra with C2v‐symmetry to an infinite chain. In [Ni(cyclam)Mn(1, 2‐dtsq)2(H2O)2]·2H2O the 1, 2‐dithiosquarato ligand shows a rare example of S‐coordination towards manganese(II). The sulfur atoms of cis‐MnO2S4‐polyedra are weakly coordinated towards the axial sites of square‐planar NiN4‐centers, thus forming a zig‐zag‐chain of Mn···Ni···Mn···Ni polyhedra. [H3O][H5O2][Cu (cyclam)]3[Cu2(1, 2‐dtsq)3]2 contains square planar [CuII(cyclam)]2+ ions and dinuclear [CuI2(1, 2‐dtsq)3]4— ions. Here each copper atom is trigonally planar coordinated by S‐donor atoms of the ligands. The Cu…Cu distance is 2.861(4)Å.  相似文献   

14.
The synthesis and structural characterization of trans‐[IrCl(NO)(PtBu2H)2]BF4 ( 1 ) is reported. The title compound was prepared in good yield in the reaction of in situ‐prepared trans‐[IrCl(coe)(PtBu2H)2] (coe = cis‐cyclooctene) with an appropriate amount of nitrosonium tetrafluoridoborate in dichloromethane at room temperature. Single crystals of 1 were grown from dichloromethane/diethyl ether and were analyzed by X‐ray crystallography.  相似文献   

15.
The synthesis of Ce(IV) complexes [Ce(sac)(2)(SO(4))(H(2)O)(4)] (1) and [Ce(sac)(2) (SO(4))(PyOH)(2)] (2) (sac=saccharinate, PyOH=2-hydroxypyridine) starting with sodium saccharinate is described. Their vibrational and nuclear magnetic resonance ((1)H, (13)C) spectra as well as their thermal mode of degradation were investigated. The data indicate that sac in complex 1 behaves as a monodentate ligand through the nitrogen atoms. Saccharinato ligand in complex 2 shows different mode of coordination, where it behaves as tridentate and binds Ce(IV) through its carbonylic oxygen, nitrogen and sulphonylic oxygen atoms. The most probable structure in complex 2 is that, units of [Ce(sac)(2)(SO(4))(PyOH)(2)] are linked by bridges of the O- of sac sulphonyl leading to polymeric chains.  相似文献   

16.
The octahedral complexes trans‐[Fe(CN)2(tOcNC)4] and trans‐[Mn(CN)(CO)(tOcNC)4] are produced by the reaction of 2‐isocyano‐2,4,4‐trimethyl‐pentane (tert. octyl‐isocyanide) with the corresponding transition metal carbonyls Fe2(CO)9 and Mn2(CO)10. In contrast to isostructural compounds with less bulky tert.‐butylisocyanide ligands the cyanide groups in trans‐[Fe(CN)2(tOcNC)4] and trans‐[Mn(CN)(CO)(tOcNC)4] do not act as hydrogen bond acceptors towards solvent molecules in the crystal structures. In addition, the corresponding cis‐isomers are configurationally unstable. The reaction of trans‐[Fe(CN)2(tOcNC)4] and trans‐[Ru(CN)2(tOcNC)4] with MnCl2, NiCl2 and Co(NO3)2 ends up in the formation of cyanide bridged coordination polymers. X‐ray structure determinations of the cobalt compounds reveal different molecular structures. Whereas the former produces highly distorted infinite polymeric chains with the nitrate anions still coordinated to the cobalt centers, the latter forms polymers with the cobalt atoms being coordinated by four ethanol molecules to which the anions are bound via hydrogen bond interactions. The coordination geometries around ruthenium and cobalt in this coordination polymer are therefore nearly perfectly octahedral and tetrahedral, respectively. Measurements of the magnetic susceptibility of the coordination polymers at different temperatures are indicative of weak antiferromagnetic coupling of the paramagnetic centers along the polymeric chains.  相似文献   

17.
New lead(II)‐saccharin complexes, [Pb(sac)2(pym)] (1) and [Pb(sac)2(pydm)] (2) (sac = saccharinate anion; pym = 2‐pyridylmethanol; pydm = pyridine‐2, 6‐dimethanol) were synthesized and characterized by IR spectroscopy and single crystal X‐ray diffractometry. Complex 1 crystallizes in the monoclinic P21/c space group with Z = 4, while the crystals of complex 2 are extremely X‐ray sensitive and decompose by the X‐ray beam within one day. Pym and pydm act as bi‐ and tridentate ligands, respectively. Most important feature of the complexes is non‐equivalent coordination of the sac ligands to the lead(II) atom. In the complex 1 , the sac ligands coordinate to the lead(II) ion in two distinct manners. One sac ligand behaves as a bridge between the lead(II) atoms through its N and carbonyl O atoms, whereas the other sac ligand acts as a bidentate chelating ligand through its N and carbonyl O atoms which is bicoordinating and also bridges the metal atoms to achieve the seven‐coordination. The structure is built up of three‐dimensional chains formed by the bridging of the PbN3O2 units and also held intermolecular hydrogen bonds. The IR spectra of the complexes were discussed in detail.  相似文献   

18.
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   

19.
The saccharinato complexes [Zn(phen)2(sac)(H2O)]sac (1) and [Zn(sac)(dmp)(H2O)](sac) (2), where phen = 1,10-phenanthroline, dmp = 2,9-dimethyl-1,10-phenanthroline, and sac =saccharinato ion/ligand, were synthesized by the reaction of [Zn(sac)2(H2O)4] · 2H2O with ligands and have been characterized by elemental analysis, IR, and 1H NMR spectroscopies. Conductivity of complexes was measured in DMSO. Compound 1 is characterized by single crystal X-ray diffraction and compared with some isomorphous zinc-saccharinate complexes reported previously. Complex 1 crystallizes in the triclinic system, space group P 1 , with Z = 2, and consists of alternating slightly distorted octahedral [Zn(phen)2(sac)(H2O)]+ and noncoordinated saccharinate. The zinc bound aqua is hydrogen bonded to an oxygen of carbonyl in the saccharinate ligand and the SO2 group in the saccharinate counter-ion from an adjacent molecule. Intermolecular and intramolecular hydrogen bonds and C–H ··· O and C–H ··· N short contacts lead to a 3-D network.  相似文献   

20.
Two novel coordination polymers, [Cd(BIM)Cl2]n ( 1 ) and [Pb(BIM)Cl2]n ( 2 ) [wherein BIM = bis(imidazol‐1‐yl)methane], were synthesized by the reactions of the BIM ligand with CdCl2 and PbCl2, respectively. They were characterized by elemental analyses, IR, TGA and X‐ray single‐crystal diffraction techniques. Single‐crystal X‐ray structure analyses showed there is a pseudooctahedral arrangement around the cadmium atom in the complex 1 . It has a three‐dimensional network which contains one‐dimensional inorganic‐organic hybrid chains and μ2‐bridging chloride ligands. A rare pentacoordinate square‐pyramidal arrangement was adopted for the lead(II) atom in the complex 2 , which has an unusual two‐dimensional layer structure of macrometallacycles crosslinked with the bridging Pb2Cl2 units. The metal atoms in both complexes were coordinated with two BIM ligands in cis arrangement and bridged by μ2‐bridging chloride ligands.  相似文献   

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