Crystal structure of palladium(II) complex with 2,2′-dipyridylamine and 4-toluenesulfonyl-L-serine

The [Pd(dpa)(tsser)] complex (1) is prepared from the reaction of PdCl₂ and 2,2′-dipyridylamine (dpa) with 4-toluenesulfonyl-L-serine (tsserH₂). This complex is characterized by spectral methods (IR, UV-Vis, ¹H NMR, and luminescence), elemental analysis, thermal analysis (TG, DTA), and single crystal X-ray diffraction. X-ray structure determinations show that in this complex, Pd^II atoms are four-coordinated in a distorted square-planar configuration by two N atoms from a bidentate 2,2′-dipyridylamine ligand and one N atom and one O atom from a bidentate tsser^2– ligand.     

Nickel(II) complex containing 5,5′-dimethyl-2,2′-bipyridine: Crystal structure and luminescent properties

[Ni(5,5′-dmbipy)₂Cl₂]·3H₂O (1) complex was obtained from the reaction of NiCl₂·6H₂O with 5,5′-dimethyl-2,2′-bipyridine (5,5′-dmbipy) in a mixture of CH₃OH/CH₃CN. This complex was characterized by elemental analysis, IR, UV-Vis and luminescence spectroscopy, and its structure was determined by the single-crystal diffraction method. The Ni atom has a distorted octahedral coordination by four N atoms from two 5,5′-dmbipy ligands and two Cl^– anions.     

Synthesis and characterization of palladium(II) complexes [PdX2(p-diben)] (X = Cl,Br, I,N3, or NCO; p-diben = N,N′-bis(4-dimethylaminobenzylidene)ethane-1,2-diamine): crystal structure of [Pd(N3)2(p-diben)]

Five new complexes of general formula [PdX₂(p-diben)], where p-diben = N,N′-bis(4-dimethylaminobenzylidene)ethane-1,2-diamine) (1) and X = Cl (2), Br (3), I (4), N₃ (5), or CNO (6), were synthesized and characterized by physicochemical and spectroscopic methods. The crystal structure of compound (5) was determined by single-crystal X-ray diffraction. Complexes 2–6 were characterized as N,N-chelated products. The crystal structure confirmed this formulation for [Pd(N₃)₂(p-diben)], besides showing the isomerism inversion of one of the C=N bonds, caused by Pd(II) coordination.     

Synthesis and Crystal Structure of [Zn(FcCOO)2(2,2′-bipy)(H2O)]2·H2O

A novel complex [Zn(FcCOO)2(2,2′-bipy)(H2O)]2·H2O (Fc = (η5-C5H5)Fe(η5-C5H4), 2,2′-bipy = 2,2′-bipyridine) has been synthesized and characterized by elemental analysis, IR and X-ray diffraction. It crystallizes in monoclinic system, space group P21/c with a = 6.8187(4), b = 21.7155(13), c = 19.7411(12) (A), α = 90, β = 97.7420(10), γ = 90°, C64H58Fe4Zn2N4O11, Mr = 1413.28, V = 2896.4(3) (A)3, Dc = 1.620 g/cm3, Z = 2, F(000) = 1444, μ(MoKα) = 1.857 mm-1, R = 0.0523 and wR = 0.0982 for 3219 observed reflections (I ＞ 2σ(I)). Structural analysis shows that the zinc atom is coordinated with three oxygen atoms from two ferrocenemonocarboxylates and one water molecule together with two nitrogen atoms from 2,2′-bipyridine, giving a distorted square-pyramidal coordination geometry. The complex molecules are linked to form an infinite one-dimensional chain by both intermolecular hydrogen bonds and π-π stacking interactions of the bipyridine rings.     

Synthesis and Crystal Structure of [Zn(FcCOO)2(2,2′-bipy)(H2O)]2·H2O

A novel complex [Zn(FcCOO)2(2,2′-bipy)(H2O)]2·H2O (Fc = (η5-C5H5)Fe(η5-C5H4), 2,2′-bipy = 2,2′-bipyridine) has been synthesized and characterized by elemental analysis, IR and X-ray diffraction. It crystallizes in monoclinic system, space group P21/c with a = 6.8187(4), b = 21.7155(13), c = 19.7411(12) (A), α = 90, β = 97.7420(10), γ = 90°, C64H58Fe4Zn2N4O11, Mr = 1413.28, V = 2896.4(3) (A)3, Dc = 1.620 g/cm3, Z = 2, F(000) = 1444, μ(MoKα) = 1.857 mm-1, R = 0.0523 and wR = 0.0982 for 3219 observed reflections (I ＞ 2σ(I)). Structural analysis shows that the zinc atom is coordinated with three oxygen atoms from two ferrocenemonocarboxylates and one water molecule together with two nitrogen atoms from 2,2′-bipyridine, giving a distorted square-pyramidal coordination geometry. The complex molecules are linked to form an infinite one-dimensional chain by both intermolecular hydrogen bonds and π-π stacking interactions of the bipyridine rings.     

Molecular structure of compounds containing a 2,2′-bithienyl fragment (review)

The results of X-ray crystallographic investigations of compounds containing a 2,2-bithienyl fragment are summarized and analyzed. The structural characteristics of unsubstituted bithiophene, 5-monosubstituted, 5,5-, 3,3-, 4,4-, and 3,4-disubstituted, and more highly substituted bithiophenes and also the structure of -conjugated oligothiophene derivatives are considered.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 6, pp. 725–760, June, 2000.     

Crystal and molecular structure of cyano(ethylenediamine) [Ethylenediamine-N,N′-Diacetato(1-)]Cobalt(III) Trichloromercurate(II) [Co(HEdda)En(CN)]HgCl3

An X-ray diffraction analysis of [Co(HEdda)En(CN)]HgCl₃ crystals (a = 6.664(4), b = 16.613(13), c = 16.684(7) å, space group P2₁2₁2₁, Z = 4) showed that the crystals contain distorted tetrahedra HgCl₄ linked by one of their vertices into infinite chains [HgCl₃] _n ^n- . In isolated complex cations, three donor atoms of the HO₂CCH₂NHCH₂CH₂NHCH₂CO ₂ ^- (HEdda) ion occupy a face of the coordination octahedron around the cobalt atom; the opposite face is occupied by the cyanide ion and the nitrogen atoms of the ethylenediamine (En) molecule; the latter are in trans positions relative to the terminal donor atoms of the HEdda ligand.     

Synthesis and crystal structure of platinum(II) acetamidates [Pt(2,2′-bipy)(NHCOCH3)2] and [enPt(μ-NHCOCH3)(μ-OH)Pten](NO3)2

The diamines PtbipyCl₂, and PtenCl₂ and their aqua and hydroxy derivatives react with acetonitrile to give the Pt(II) acetamidates [Pt(2,2′-bipy)(NHCOCH₃)₂] · 4.125 H₂O (I) and [enPt(μ-NHCOCH₃(μ-OH)Pten](NO₃)₂ · H₂O (II), which are characterized by X-ray diffraction. The crystals of I are triclinic, a = 7.137(10) Å, b = 12.655(3) Å, c = 21.914(6) Å, α = 81.82(2)°, β = 82.12(2)°, γ = 77.72(2)°, V = 1908.6(7) ų, space group P $\overline 1 $ , Z = 4, R = 0.033 for 3700 reflections. Complex I is a mononuclear acetamidate with terminal (NHCOCH₃)^? ligands. The crystals of II are monoclinic, a = 11.413(2) Å, b = 10.981(2) Å, c = 14.385(3) Å, β = 105.90(3)°, V = 1733.8(6) ų, space group P2₁/n, R = 0.028 for 2797 reflections. Complex II is a dimer with bridging (NHCOCH₃)^? and (OH)^? groups. The Pt-Pt distance is 3.1667(7) Å.     

Mixed neutral compounds of palladium(II) and platinum (II) chelated by diolato(2−) and di-imine ligands

The synthesis and characterization are described for compounds abbreviated (a) 1–5: [Pd(phen)(OO)], where OO = the dianion from 1,2-ethanediol (1), (+)-1,2-propanediol (2), (±)-2,3-butanediol (3), (−)-1,2-butanediol (4), catechol (5); (b) the sulphur analogue (6) [Pd(phen)(SCH₂CH₂S)], from ethane-1,2-dithiol; (c) the platinum analogue (7) [Pt(phen)(OCH₂CH₂O)]; (d) the 2,2′-bipyridyl analogue (8), [Pd(bipy)(OCH₂CH₂O)] (phen = 1,10-phenanthroline and bipy = 2,2′-bipyridyl).     

Synthesis,characterization and crystal structure determination of iron(III) complexes containing 4,4′-dimethyl-2,2′-bipyridine,dimethyl sulfoxide and chloride, [Fe(dmbipy)Cl4][dmbipyH] and [Fe(dmbipy)Cl3(DMSO)]

[Fe(dmbipy)Cl₄][dmbipyH], 1 (dmbipy is 4,4′-dimethyl-2,2′-bipyridine), was prepared from reaction of FeCl₃ · 6H₂O with 4,4′-dimethyl-2,2′-bipyridine in 0.1 molar aqueous HCl. Treatment of 1 with dimethyl sulfoxide in methanol produced [Fe(dmbipy)Cl₃(DMSO)], 2 (DMSO is dimethyl sulfoxide). Both complexes were characterized by IR, UV-vis, and ¹H-NMR spectroscopies and their structures were studied by single crystal diffraction. Compounds 1 and 2 are high-spin with spin multiplicity of six.     

Synthesis of molybdenum complexes containing η3-bonded trans-butadienyl ligands: crystal structure of[Mo(2,2′-bipyridine)(CO)2-

Reaction of Ph₄P[Mo(2,2′-bipyridine)Cl(CO₃] with 1,4-dichlorobut-2-yne in the presence of primary or secondary aliphatic amines gives high yields of neutral molybdenum complexes containing 2-substituted η³-bonded trans-butadienyl ligands. The crystal structure of the perfluorocarboxylate derivative [Mo(2,2′-bipyridine)(CO)₂(η³-CH₂C(CONHMe)CCH₂) (O₂CC₃F₇] has been determined.     

一维链状配位聚合物[Ni(p-CPOA)(2,2′-bipy)(H2O)]n的合成与晶体结构

合成了一个新的配位聚合物[Ni(p-CPOA)(2,2′-bipy)(H2O)]n(p-CPOA2-= 4-羧基苯氧乙酸根,2,2′-bipy= 2,2′-联吡啶),并对其进行了元素分析、红外和单晶X-射线的表征.结果表明:配合物的化学式为C19H16N2O6Ni,晶体属单斜晶系,空间群为C2/c,晶胞参数a = 14.254(3),b = 13.085(3),c = 19.372(4)A,β = 104.89(3)°,V = 3491.8(12)A3,Z = 8,Mr = 427.05,Dc = 1.625 g/cm3,μ = 1.153mm－1,F(000) = 1760,最终R = 0.0345,wR = 0.0565。Ni原子为扭曲的六配位八面体构型,每个p-CPOA2－配体桥联2个Ni原子形成一维折叠链状结构,Ni…Ni原子之间的距离为9.675A,且通过分子间氢键将一维链连接成双链结构.     

Copper(II) and palladium(II) complexes of N,N′-bis(2-hydroxyethyl)stilbenediamine

A new 1,2-diamine ligand, N,N-bis(2-hydroxyethyl)stilbenediamine (L), has been prepared by reduction of the condensation product of benzaldehyde with 2-aminoethanol with Al amalgam. Mononuclear complexes of the [CuL(H₂O)]X₂ type where X=Cl^– or AcO^– with Cu^II and PdLCl₂ with palladium(II) have been prepared and characterized by elemental analysis and i.r., u.v.–vis. or ¹H-n.m.r. spectroscopy.     

Synthesis, Characterization and Crystal Structure of (2,2′-Bipyridine)(μ-maleato)copper(II) Dihydrate

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Ruthenium(III) mono (2,2′-bipyridine) complexes containing O,O-donor ligands and their oxidation properties for organic compounds

The new complexes [Ru^IIIbpyL₂](PF₆) and [Ru^IIIbpyLCl₂] [bpy = 2,2-bipyridine; HL = acetylacetone, trifluoroacetylacetone, benzoylacetone (Hbac), tropolone or maltol; HL = Hbac or dibenzoylmethane) have been prepared and characterized by spectroscopy. Their redox behaviour was studied by cyclic voltammetry. They effectively catalyze the oxidation of alcohols, alkanes and primary aromatic amines.     

Manganese(II) complexes with edta-type ligands. The molecular structure of aquo-dihydrogen(1,2-propanediamine-N,N,N′,N′-tetraacetate)manganese(II) trihydrate, [Mn(H21,2-pdta)(H2O)] · 3H2O

New manganese(II) complexes with ethylenediamine-N,N,N,N-tetra-3-propionate (edtp) and 1,2-propanediamine-N,N,N,N-tetraacetate (1,2-pdta) were prepared and characterized by elemental analysis, i.r. spectroscopy and magnetic measurements. The structure of [Mn(H₂1,2-pdta)(H₂O] · 3H₂O was determined by the single crystal X-ray diffraction technique. The complex crystallizes in the space group P2₁/n(#14) of the monoclinic crystal system with unit cell parameters a = 10.993(2) Å, b = 14.092(2) Å, c = 11.753(1) Å, = 96.302(9)⁰, V = 1809.7(3) ų, Z = 4 and R = 0.051. The complex contains seven-coordinated Mn^II ion with H₂1,2-pdta ion acting as hexadentate ligand and one water molecule.     

Comparative analysis of physicochemical properties of dinuclear zinc(II) helicates with 2,2′-, 2,3′-, and 3,3′-bis(dipyrromethenes)

The effect of the attachment position of a methylene spacer in 2,2′-, 2,3′-, and 3,3′-bis(dipyrromethene) N₄-ligands (H₂L) on physicochemical properties of their dinuclear homoleptic helicates [Zn₂L₂], such as specific features of their molecular structure, luminescence spectral characteristics, lability in acid solutions, and thermal stability in an argon atmosphere, has been examined. It has been shown that the substitution of the biladiene-type helicand by its 2,3- and especially 3,3′-analogues leads to a considerable enhancement of the chromophoric properties, an increase (up to 30-fold) of the fluorescence quantum yield, and an increase in the stability of corresponding dinuclear helicates [Zn₂L₂].     

Fluorine-substituted β-diketonate PbII complexes, [Pb(phen)(TFPB)2] and [Pb(2,2′-bipy)(TFPB)2]

Lead(II) 4,4,4-trifluoro-1-phenyl-1,3-butandionate (TFPB^?) complexes with 1,10-phenanthroline (phen) and 2,2′-bipyridine (2,2′-bipy), [Pb(L)(TFPB)₂], have been synthesized and characterized by elemental analysis, IR-, ¹H NMR spectroscopy and studied by X-ray crystallography. The self-assembly of [Pb(L)(TFPB)₂] complexes, (L?=?phen or 2,2′-bipy) is caused by C–H?···?F–C, C–H?···?O–C and π–π stacking interactions. The thermal stabilities of compounds were studied by thermal gravimetric (TG) and differential thermal analyses (DTA).     

A trinuclear bis(dioximate)(chloro)(nitrosyl)ruthenium(II) complex containing two (2,2′-bipyridine)copper(II) groups

A trinuclear bis(cyclohexanedioximate)(chloro)(nitrosyl)ruthenium(II) complex containing two (2,2-bipyridine)-copper(II) groups has been synthesized and its electronic and electrochemical properties investigated. According to ZINDO/S calculations, the electronic structure of the ruthenium(dioximate)(nitrosyl) moiety is strongly delocalized. The electrochemical behavior has been interpreted with the aid of spectroelectrochemical measurements. In the trinuclear complex, it has been shown that the copper(II) ions can promote the oxidation of the NO species generated electrochemically, and also mediate the redox reactions of the complex, under a dioxygen atmosphere.