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1.
Co(II), Ni(II) and Cu(II) nitrate complexes with btmpp, namely ([Co(btmpp)(H2O)2(NO3)]NO3 (1), [Ni(btmpp)(H2O)(NO3)]NO3 (2) and [Cu(btmpp)(MeOH)(NO3)]NO3 (3), where btmpp = 2,6-bis(3,4,5-trimethyl-N-pyrazolyl)pyridine), have been synthesized and characterized by physicochemical and spectroscopic methods. The crystal structure of complex 1 has been determined by single crystal diffraction at 100K. In all the complexes, btmpp is coordinated in a tridentate mode through its nitrogen atoms. One of the nitrates in complex 1 is terminally bonded to the metal center through the oxygen atom, whereas the other one is out of the coordination sphere. The Co(II) atom in complex 1 is hexa-coordinated with a CoN3O3 distorted octahedral environment. Decomposition of three complexes was analyzed thermogravimetrically. All three complexes decompose similar to explosive material.  相似文献   

2.
The reaction of Cu(ClO4)2·6H2O and Cd(ClO4)2 with di-(2-picolyl)sulfur (dps) leads to the formation of mononuclear complexes [Cu(dps)(H2O)(ClO4)](ClO4) (1) and [Cd(dps)2](ClO4)2 (2). The crystal structure of 1 exhibits a distorted square pyramidal geometry, coordinated by one sulfur and two nitrogen atoms from the dps ligand, one water molecule and one perchlorate oxygen atom. For 2, the environment around cadmium atom is in a distorted octahedron with four nitrogen and two sulfur atoms from the dps ligand. Cyclic voltammetric data show that complexes undergo two waves of a one-electron transfer corresponding to M(II)/M(III) and M(II)/M(I) processes. Spectral and electrochemical behaviors of the complexes are also discussed.  相似文献   

3.
Two new lead(II) complexes containing nitrite, [Pb(L)2(NO2)2], L?=?1,10-phenanthroline (phen) or 2,2′-bipyridine (bpy), have been synthesized and characterized. The crystal structure of [Pb(phen)2(NO2)2] shows monomeric units. The coordination number is eight (four from “phen” ligands and four nitrite anions), weak interaction of lead(II) with oxygen atoms of adjacent molecules produce dimer units in the solid state. The arrangement of ligands exhibits a coordination hole around the lead(II), occupied possibly by a stereoactive lone pair of electrons on lead(II), and the coordination around lead is hemidirected. There is a π–π stacking interaction between the parallel aromatic rings that may help to increase the “gap” around lead(II).  相似文献   

4.
[Cu(L)(NO3)2] (1) and [Cu(L)(H2O)2](SCN)2 (2) [L?=?3,14-diethyl-2,6,13,17-tetraazatricyclo(16.4.0.07,12)docosane] have been prepared and structurally characterized by single-crystal X-ray diffraction at 100?K. For these constrained macrocycle complexes, copper(II) exists in a tetragonally distorted octahedral environment with the four nitrogen atoms of the macrocyclic ligands and two oxygen atoms from either nitrate or water in axial positions. The macrocyclic ligands in both complexes adopt the most stable trans-III conformation. The Cu–N distances are 2.021(2)–2.047(2)?Å and typical but the axial ligands are weakly coordinating, with Cu–O bond lengths, 2.506(2)?Å for 1 and 2.569(2)?Å for 2, due to the pseudo Jahn–Teller effect. The crystals are stabilized by a 3-D network by intra and intermolecular hydrogen bonds that are formed among the secondary nitrogen hydrogen atoms and nitrate in 1, and intermolecular hydrogen bonds are formed by water and thiocyanates in 2. The electronic absorption and IR spectral properties are also discussed.  相似文献   

5.
Three new copper(II) complexes with isonicotinic acid N-oxide (HL) and 1,10-phenanthroline (phen) as ligands, [Cu(L)(phen)(H2O)]2(NO3)2···2H2O (1), [Cu(L)(phen)(H2O)]2(ClO4)2···2H2O (2), and [Cu(L)(phen)Br]2- [Cu(L)(phen)(H2O)]2Br2···6H2O (3) have been synthesized and structurally characterized. The structures of all three complexes feature a Cu2 dimer formed by two Cu(II) ions interconnected by two bridging ligands. Each copper(II) ion has a distorted square pyramidal coordination geometry with elongated axial coordination by an aqua ligand or halogen anion. The isonicotinic acid N-oxide anion is bidentate, being coordinated to two Cu(II) ions through its N-O oxygen and one of its carboxylate oxygen atoms. Magnetic susceptibility measurements show a Curie–Weiss paramagnetic behavior characteristic of one unpaired electron for a copper(II) ion for all three complexes.  相似文献   

6.
Several Cu(II) complexes with 1,2,4-triazolo[1,5-a]pyrimidine (tp) and its 5,7-dimethyl derivative (dmtp) have been isolated and structurally characterized. Five of them are mononuclear and contain 1,10-phenanthroline (phen) or ethylenediamine (en) as auxiliary ligands, their formula being [Cu(H2O)(phen)(tp)2](ClO4)2 · H2O, [Cu(H2O)(phen)(dmtp)2](ClO4)2, [Cu(NO3)(H2O)(phen)(tp)](NO3), [Cu(H2O)2(en)(tp)2](ClO4)2 and [Cu(H2O)2(en)(dmtp)2](ClO4)2. In all these compounds the tp or dmtp ligand is monodentately coordinated via the nitrogen atom in position 3. The auxiliary ligand influences the coordination number, which is five when this ligand is phen and six when it is en whereas the number of triazolopyrimidine ligands linked to the metal seems to be influenced by the nature of the counteranion. A dinuclear compound with tp has also been isolated, its formula being [Cu2(OH)(H2O)2.5(tp)5](ClO4)3·(H2O)1.5, with both metal atoms linked by an hydroxydo group and by a tp bridging ligand, coordinated to one of the copper atoms via N3 and to the other via N4. This compound has several unusual features among the metal complexes with triazolopyrimidine derivatives: the presence of two different kinds of bridging moieties, the coexistence of bridging and terminal ligands and the formation of a N3–N4 bridge for a Cu(II) dinuclear compound for a derivative without exocyclic oxygen atoms.  相似文献   

7.
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   

8.
The syntheses and crystal structures of four new divalent transition metal complexes of the types [Cu2(dien)2(nic)](ClO4)3 · MeOH (nic = anion of nicotinic acid; dien = diethylenetriamine), 1; [Cu(dien)(nic)]2(nic)2, 2; [Cu(dien)(nic)]2(BF4)2 · 2MeOH, 3 and [Ni(dien)(nic)(H2O)]4(NO3)4 · 2MeOH, 4, are reported, which were prepared by the reactions of diethylenetriamine and nicotinic acid with Cu(ClO4)2 · 6H2O, Cu(OAc)2 · H2O, Cu(BF4)2 · 6H2O and Ni(NO3)2 · 6H2O in MeOH, respectively. These complexes were characterized by single-crystal X-ray diffraction method and elemental analyses. In the cation of complex 1, one nicotinate ligand bridges two Cu(II) metal centers through the pyridyl nitrogen atom and one of the carboxylate oxygen atoms. The cations of complexes 2 and 3 form the twelve-membered metallocycles, involving two Cu(II) ions that are bridged by two nicotinate ligands. The cation of complex 4 forms a tetranuclear cage with the four Ni(II) metal centers bridged by four nicotinate ligands and each Ni(II) metal center adopts the distorted octahedral geometry. Their thermal properties have been investigated by using differential scanning calorimetry (DSC) and thermogravimetric analyses (TGA).  相似文献   

9.

Reaction of the ligand 2,2′-diphenyl-4,4′-bithiazole (DPBTZ) with Hg(SCN)2, Tl(NO3)3, CuCl, and PdCl2 gives complexes with stoichiometry [Hg(DPBTZ)(SCN)2], [Tl(DPBTZ)(NO3)3], [Cu(DPBTZ)(H2O)Cl], and [Pd(DPBTZ)Cl2]. The new complexes were characterized by elemental analyses and infrared spectroscopy. The crystal structure of [Hg(DPBTZ)(SCN)2] determined by X-ray crystallography. The Hg atom in the title monomeric complex, (2,2′-diphenyl-4,4′-bithiazole)mercury(II)bisthiocyanate, [Hg(C18H12N2S2)(SCN)2], is four-coordinate having an irregular tetrahedral geometry composed of two S atoms of thiocyanate ions [Hg-S 2.4025(15) and 2.4073(15) Å] and two N atoms of 2,2′-diphenyl-4,4′-bithiazole ligand [Hg-N 2.411(4) and 2.459(4) Å]. The bond angle S(3)-Hg(1)-S(4) of 147.46(5)° has the greatest derivation from ideal tetrahedral geometry. Intermolecular interaction between Hg(1) and two S atoms of two neighboring molecules, 3.9318(15) and 3.9640(18) Å, make the Hg(1) distort from a tetrahedron to a disordered octahedron. The attempts for preparation complexes of Tl(I), Pb(II), Bi(III), Cd(II) ions with 2,2′-diphenyl-4,4′-bithiazole ligand were not successful and also the attempts for preparation complexes of 4,4′,5,5′-tetraphenyl-2,2′-bithizole ligand with Cu(II), Ni(II), Co(II), Co(III), Mn(II), Mn(III), Fe(II), Fe(III), Cr(III), Zn(II), Tl(III), Pb(II), Hg(II), Cu(I), Pd(II) were not successful. This point can be regarded as the initial electron withdrawing of phenyl rings and also their spatial steric effects.  相似文献   

10.
Summary The reaction of monochloropentaphenoxycyclotriphosphazene with 3-(aminomethyl)pyridine yields 3-(aminomethyl)pyridylpentaphenoxycyclotriphosphazene (1), a new N-donor ligand with five nitrogen atoms as potential coordination centers. Complex formation with copper(II) nitrate yields compound2 with the general structure Cu(1)2(NO3)2. The X-ray structure analysis shows that the copper ion is coordinated by two nitrogen atoms of the pyridine rings and four oxygen atoms of the unsymmetrical bidentate nitrate groups in aJahn-Teller distorted octahedral arrangement.
Synthese von 3-(Aminomethyl)pyridylpentaphenoxycyclotriphosphazen und seine Komplexibildung mit Kupfer(II)nitrat. Molekülstruktur von {Cu[N3P3(OC6H5)5(NHCH2(3-C5H4N))]2(NO3)2}
Zusammenfassung Die Reaktion von Monochlorpentaphenoxycyclotriphosphazen mit 3-(Aminomethyl)pyridin ergibt 3-(Aminomethyl)pyridylpentaphenoxycyclotriphosphazen (1), einen neuen N-Donor Liganden mit fünf Strickstoffatomen als potentielle Metallkoordinationszentren. Bei der Umsetzung von1 mit Kupfer(II)nitrat entsteht der Metallkomplex2 mit der Zusammensetzung Cu(1)2(NO3)2. Die durch Röntgenstrukturanalyse ermittelte Molekülstruktur zeigt, daß das Kupferion von zwei Stickstoffatomen der Pyridinringe sowie vier Sauerstoffatomen der unsymmetrisch zweizähnigen NitratgruppenJahn-Teller-verzerrt oktaedrisch umgeben ist.
  相似文献   

11.
To investigate the effect of different imidazole-containing ligands on the structure of coordination polymers, two new Zn(II) coordination polymers based on 1,4-cyclohexanedicarboxylic acid (H2cda) and two different imidazole-containing ligands, [Zn(cda)(bib)0.5]n (1) and [Zn(cda)(bmib)0.5]n (2) (bib = 1,4-bis(imidazol-1-yl)benzene and bmib = 1,4-bis(2-methylimidazol-3-ium-yl)benzene), have been synthesized and characterized by single-crystal X-ray diffraction. Complex 1 shows a 3-D structure with point symbol (4.82.103).(4.82). Complex 2 displays a 2-D layer structure with an –AB– stacking sequence.  相似文献   

12.
Three coordination polymers [Zn(μ3-HNIDC)(CH3OH)]n (H3NIDC = 2-(2-naphthyl)-1H-imidazole-4,5-dicarboxylic acid) (1), [Mn(μ2-HNIDC)(4,4′-bipy)]n (4,4′-bipy = 4,4′-bipyridine) (2) and [Mn22-HNIDC)2(phen)2]n (phen = 1,10-phenanthroline) (3) have been solvothermally synthesised and structurally characterised by single-crystal X-ray diffraction, elemental analyses, thermal analyses and IR spectra. Polymer 1 displays a three-dimensional open architecture with one-dimensional (1D) channels. Polymer 2 exhibits a sheet structure containing infinite rectangles. Polymer 3 presents a 1D wave chain structure. The solid-state photoluminescence of 1 has been investigated as well.  相似文献   

13.
Deprotonation of the tridentate isoindoline ligand 1,3-bis[2-(4-methylpyridyl)imino]-isoindoline, 4'-MeLH, and reaction with hydrated zinc(II) perchlorate produces an unexpected trinuclear Zn(II) complex, [Zn(3)(4'-MeL)(4)](ClO(4))(2).5H(2)O (1), whereas reaction with hydrated copper(II) perchlorate in methanol produces the expected mononuclear product, [Cu(4'-MeL)(H(2)O)(2)]ClO(4) (2). X-ray diffraction shows that the trinuclear Zn(II) complex (1) contains a linear zinc backbone, and the arrangement of ligands about the outer chiral zinc(II) atoms is helical. The two terminal zinc ions exhibit approximate C(2) site symmetry, with tetrahedral coordination by two pyrrole and two pyridyl nitrogen atoms of the potentially tridentate isoindoline ligands. The central zinc ion exhibits approximate tetrahedral symmetry, with coordination by four pyridyl nitrogen atoms of four different isoindoline ligands. Pyridyl-pyrrole intramolecular pi-stacking interactions contribute to the stability of the trinuclear cation. The structure of the mononuclear copper(II) complex cation in 2 is best described as a distorted trigonal bipyramid. The isoindoline anion binds Cu(II) in both axial positions and one of the equatorial positions; water molecules occupy the other two equatorial positions.  相似文献   

14.
A new crystalline complex salt, 4,7,13,16,21,24-hexaoxa-1,10-diazaniabicyclo[8.8.8]hexacosane tetra(nitrato-O)copper(II) [H2(Crypt-222)]2+ · [Cu(NO3)4]2?(I), is synthesized and studied using X-ray diffraction analysis (space group P21/c, a = 10.264 Å, b = 14.798 Å, c = 19.516 Å, β = 100.20°, Z = 4). The structure is solved by a direct method and refined by the full-matrix least-squares method in the anisotropic approximation to R = 0.032 for 4050 independent reflections (CAD-4 automated diffractometer, λMoK α radiation). Salt I exist in crystals as individual ions: the [Cu(NO3)4]2? complex anion and the slightly disordered dication of 2.2.2-cryptand with two protonated nitrogen atoms. The Cu2+ cation has a square coordination somewhat distorted toward a flattened tetrahedron with four coordination bonds with the O atoms of the four NO 3 ? ligands. Trifurcate hydrogen bonds of the [H2(Crypt-222)]2+ type are observed in the N-H(? O)3 dication.  相似文献   

15.
Li  Baolong  Xu  Zheng  Cao  Zhengbai  Zhu  Liming  Yu  Kaibei 《Transition Metal Chemistry》1999,24(6):622-627
The reaction of diethylenetriamine (dien) and 1,2-bis(1,2,4-triazole-1-yl)ethane (btrz) with Cu(ClO4) · 6H2O forms [Cu(dien)(btrz)(ClO4)2] (1), and the reaction of [Cu(en)2(ClO4)2] (en = ethylenediamine) with btrz forms [Cu(en)2(btrz)(ClO4)2] (2). Complexes (1) and (2) were characterized by elemental analysis, i.r., electronic spectroscopy, e.s.r. and magnetic susceptibility. Their crystal structure was determined by X-ray diffraction. In complex (1), Cu is coordinated by a dien and two btrz, forming a distorted CuN5 square pyramid with one btrz bound at the apical position. In complex (2), Cu is coordinated by two en and two nitrogen atoms of btrz forming an elongated octahedron. Both complexes have a one-dimensional chain structure in which btrz ligands bridge between pairs of Cu atom.  相似文献   

16.
In the title complex, [Ru(bpy)(dppy)2(CO)2](PF6)2 (bpy = 2,2′‐bipyridine, dppy = 2‐(diphenylphosphino)pyridine), the ruthenium atom exhibits a slightly distorted octahedral coordination with the carbonyl ligands in cis positions. In addition, two dppy ligands coordinate to the ruthenium center through the phosphorus atoms in mutually trans positions and two pyridyl nitrogen atoms of the dppy direct toward two carbonyl ligands. Copyright © 2004 John Wiley & Sons, Ltd.  相似文献   

17.
Two copper(I) complexes [Cu(Cin2bda)2]ClO4 (I) and [Cu(Ncin2bda)2]ClO4 (II) have been prepared by the reaction of the ligands N2,N2′-bis(3-phenylallylidene)biphenyl-2,2′-diamine (L1) and N2,N2′-bis[3-(2-nitrophenyl)allylidene]biphenyl-2,2′-diamine (L2) and copper(I) salt. These compounds were characterized by CHN analyses, 1H NMR, IR, and UV-Vis spectroscopy. The C=N stretching frequency in the copper(I) complexes shows a shift to a lower frequency relative to the free ligand due to the coordination of the nitrogen atoms. The crystal and molecular structure of II was determined by X-ray single-crystal crystallography. The coordination polyhedron about the copper(I) center in the complex is best described as a distorted tetrahedron. A quasireversible redox behavior was observed for complexes I and II. The article is published in the original.  相似文献   

18.
Two Co(II) coordination polymers, [Co(Hbtc)(bix)] n , (1) and [Co(1,4-bdc)(bix)H2O] n (2) (bix = 1,4-bis(imidazole-1-ylmethyl)benzene; H3btc = benzene-1,3,5-tricarboxylic acid; 1,4-H2bdc = benzene-1,4-dicarboxylic acid) have been synthesized under hydrothermal conditions and structurally characterized. X-ray structure analysis reveals that in polymer 1, 2D infinite grid-like frameworks are interconnected by hydrogen-bond interactions to result in a 3D supramolecular architecture, in which the three carboxylate groups of the H3btc molecule adopt three different coordination modes. In polymer 2, 1,4-bdc ligands with cobalt atoms construct 1D zigzag chains which are bridged by bix ligands to form a 3D framework.  相似文献   

19.
The hydrazone (E)-3-hydroxy-N’-(1-(2-oxo-2H-chromen-3-yl)ethylidene)-2-naphthohydrazide (H2L) was synthesized from the reaction of 3-acetylcoumarin and 3-hydroxy-2-naphthoic hydrazide in methanol. Compounds [Mn(H2L)(NO3)2(CH3OH)]·CH3OH (1a), [Mn(HL)(NO3)(CH3OH)]n (1b), [Co(HL)(NO3)(CH3OH)]n (2), and [Cu(HL)(NO3)] (3) were obtained by reaction of an equimolar amount of H2L with nitrate salts of Mn(II), Co(II), or Cu(II) in methanol. The reaction of ligand and Mn(NO3)2·4H2O was also carried out in the presence of sodium azide which led to the 1-D coordination polymer, [Mn(HL)(N3)(CH3OH)]n (4). All of the synthesized compounds were characterized by elemental analyses and spectroscopic methods. Single-crystal X-ray analysis of 1–4 indicated that H2L is neutral (in 1a) or mononegative ligand (in 1b, 2, 3 and 4). In 1b, 2 and 4 the 1-D polymeric chain is found by a rare coordination mode of this kind of hydrazone ligand since the naphtholic oxygen is coordinated to the neighboring metal ions while the NH moiety of hydrazone remains intact, also confirmed by FT-IR spectroscopic studies. The thermal stability of 2 and 4 were also studied from 30–1000 °C.  相似文献   

20.
[{CuCl(dm4bt)}2 μ-Cl)2] (1) (dm4bt = 2,2′-dimethyl-4,4′-bithiazole) was prepared from the reaction of CuCl2 · 2H2O with 2,2′-dimethyl-4,4′-bithiazole in methanol; [Cu(dm4bt)2NO3](NO3) (2) was prepared from the reaction of Cu(NO3)2 · 3H2O with 2,2′-dimethyl-4,4′-bithiazole in methanol. Both complexes were characterized by IR, UV–Vis spectroscopy, and single-crystal structure. The structure of 1 consists of centrosymmetric dimeric [{CuCl(dm4bt)}(μ-Cl)], in which two chloro ligands bridge the coppers forming a four-membered ring; a terminal chloride and a bidentate chelating bithiazole complete five coordination at each Cu(II) in a highly distorted trigonal-bipyramidal geometry. The mononuclear structure 2 consists of a Cu(II), two 2,2′-dimethyl-4,4′-bithiazoles, one monodentate nitrate and one uncoordinated nitrate in a highly distorted square pyramid.  相似文献   

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