Synthesis and Extended 3D Hydrogen-bonded Structure of Complex Tris(violurato-N,O) Cobalt(III) Hexahydrate

1 INTRODUCTION The study of cobalt complexes plays an important role in pharmacology, coordination chemistry and bio- inorganic chemistry. The recent work on organoco- baloximes shows that it has outgrown its initial rele- vance of Vitamin B12 model and acquired an indepen- dent research field because of its rich chemistry[1~4]. At the same time, research on the complexes with oxime ligands has considerable interest owning to their special catalytic, electric, magnetic properties and bio…     

Synthesis and Crystal Structure of Cobalt(Ⅲ) Tris(diethyldithiocarbamato) Complex

1INTR0DUCTI0NRecently,thedesignandsynthesisofdinuclearcomplexeshavebeenafascinat-ingareaofresearchowingt0theirimportanceinbasicandappliedchemistry"'.Par-ticularintersthasdevelopedindinuclearcomplexesasmodelsformeta1loproteins"'.Inanattempttosynthesizethetypeof[Ln(S,CN(C2H,)2)3j[Co(S2CN(C2H5)2)2jdinuc1earcomplex,thepurefinecrystalsofCo[S2CN(C2H5)2)2)3were0btained.2EXPERIMENTAL2'1Preparation0fC0[S,CN(C,H,),j,TotheclearsolutionoftheanhydrousSmCl3(0.5mmol)in5mLanhydrousethanolw…     

Synthesis and Crystal Structure of a New Mononuclear Cobalt(Ⅲ) Complex with 2,2′-Dipyridylamine and Glycine as Ligands

A new mononuclear cobalt(III) complex [Co(dpa)2(Gly)](ClO4)2′4H2O was synthesized by the reaction of Co2+, glycine (gly) and 2,2′-dipyridylamine (dpa) in a methanol-water solution, and its structure was characterized by IR, EA, ES-MS and X-ray structure analysis. The compound crystallizes in the monoclinic system, space group P21/n with a = 12.8795(2), b = 13.2904(2), c = 19.1104(2) , β = 109.378(1)°, V = 3085.89(8) 3, Z = 4, Mr = 746.36, Dc = 1.606 g/cm3, μ = 0.808 mm-1, F(000) = 1536, the final R = 0.0543 and wR = 0.1306 for 5393 independent reflections. The magnetic measurement of the compound at room temperature shows that it is diamagnetic and the cobalt ion is in low spin +3 oxidation state. ES-MS experiments show that the [Co(dpa)2(Gly)]2+ cation is very stable in the methanol solution.     

Synthesis and Crystal Structure of Bis(2,2′-Bipyridine-N,N′)Dichloromanganese(II) Complex with Free 2,2′-Bipyridine

The title complex [Mn(bipy)₂Cl₂]·0.5bipy·2.5H₂O, where bipy = 2,2'-bipyridine, has been prepared and its crystal structure has been determined by X-ray diffraction methods. The complex crystallizes in the triclinic space group P-1, with a = 8.814(2), b = 11.335(2), c = 13.347(3) Å, α = 76.85(2), β = 89.55(2), γ = 86.52(2)°. Two chloride and two bipy ligands cis-coordinate to a Mn(II) atom with a distorted octahedral geometry. The crystal consists of Mn(II) complex, free bipy and crystalline water. The complex crystalline water link to each other by H-bonding to form supra-molecular chains, and free bipy molecules locate between parallel chains with a van der Waals contact distance of 3.58(1) Å. A π-π interaction is also observed between adjacent bipy rings. The chelating bipy and free bipy showed different IR absorptions.     

Synthesis,Crystal Structure and Magnetic Properties of a Cobalt(Ⅱ) Complex with Quinoxaline-substituted Nitronyl Nitroxide Radicals

A new complex with the formula [Co(acac)_2(NITQ)_2]×2CH_2Cl_2 1(acac = acetylacetone, NITQ = 2-(2′-quinoxalinyl)-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide), was synthesized and elucidated structurally as well as magnetically in detail. The crystal belongs to the monoclinic system, space group P2_1/c with a = 9.6896(1), b = 20.539(4), c = 12.147(2) ?, β = 93.84(3)°, M_r = 997.65, V = 2412.1(8) ?~3, Z = 2, Dc = 1.374 g/cm, F(000) = 1038, m = 0.635 mm~(-1), the final R = 0.0539 and w R = 0.1289 for 5998 observed reflections(I 2σ(I)). The Co(Ⅱ) ion is coordinated by two nitrogen atoms of quinoxaline rings from two NITQs and four oxygen atoms from two acac ions to complete a distorted octahedral coordination environment. Compound 1 is further linked into a three-dimensional(3D) supramolecular network by hydrogen-bonding, Cl×××O weak contact and π···π stacking interactions. The magnetic measurements show compound 1 exhibits weak ferromagnetic interactions.     

Synthesis,Crystal Structure and Bioactivity of a Pd(Ⅱ) Complex with Demethylcantharate and 2,2′-Bipyridine

A novel crystal with the molecular formula [Pd(DCA)(bipy)]2 [Pd(bipy)Cl2 ]·6.75H2O was formed by PdCl2 with disodium demethylcantharate (Na2 (DCA),DCA2= 7-oxa-bicyclo[2.2.1]heptane-2,3-bicarboxylate) and 2,2-bipyidine (bipy) through the hydrothermal method.The complex was characterized by elemental analysis and infrared spectroscopy.The structure of the complex was determined by single-crystal X-ray diffraction,which is of triclinic system,space group P1 with a=13.6818(7),b=14.8426(8),c=15.0043(8),α=97.319(3),β=92.521(3),γ=105.776(2)°,V=2898.4(3) 3,Dc=1.545 g·cm-3,Z=1,F(000)=1420,S=0.852,the final R=0.0525 and wR=0.1777 for 13634 observer reflections (I>2σ(I)).The binding reaction of the complex with ct-DNA and bovine serum albumin (BSA) was studied by fluorescence spectroscopy.The results indicated that the complex binds to ct-DNA via the partial intercalation.The binding constant K A of the complex interaction with BSA was 3.98×10 5 L·mol-1 and one binding site would be formed.The antiproliferative activity of the complex against human hepatoma cells (SMMC7721) in vitro is much higher than that of Na 2 (DCA).     

Synthesis,crystal structure and reactivity of trans-diaquo N,N′-ethylenebis-(3-methoxysalicylideneiminato)chromium(III)

A new chromium(III) Schiff base complex, [Cr(3-methoxysalen)(H₂O)₂]ClO₄, where salen=N,N-ethylenebis- (salicylideneimine), has been synthesized and characterized by spectroscopic techniques. Single crystal X-ray data reveals that the complex assumes a trans-diaquo structure with formulation [Cr(C₁₈H₂₂N₂O₆)]ClO₄ but, unlike in Cr (salen)(H₂O)₂ ⁺, the two trans-water molecules are equidistant from Cr^III. The effect of the substituent on the phenyl ring in respect of redox reactivity has been investigated. The kinetics of the oxidation of [Cr(Schiff base)- (H₂O)₂]ClO₄, where Schiff base=salen, (1) and 3-OMe-salen, (2) by PhOI has been studied. The bimolecular rate constant for the formation of the O=Cr^v Schiff base in case of (2) was four times faster than that of (1). The introduction of the OMe group substituent on the phenyl ring influences not only the structure and crystal packing, but also the reactivity of the complex and the electronic environment around the metal ion.     

Cobalt(III), nickel(II) and copper(II) complexes of N,N′-didodecildithiooxamide

The complexes of N,N′-didodecildithiooxamide (L): CoL₃(ClO₄)₃, NiL₂X₂ (X = Cl, Br, I, ClO₄, HSO₄), CuL₂X₂ (X = ClO₄, HSO₄) and CuLX₂ (X = Cl, Br) were prepared. The cobalt and nickel complexes are diamagnetic, with octahedral and planar coordination respectively. The copper complexes are paramagnetic with normal magnetic moments corresponding to a tetragonal coordination. The i.r. and far i.r. spectra are discussed.     

Synthesis and Crystal Structure of Copper(Ⅱ)Complex with N-Acetoxyl-picolinamide

Using Cu(Ⅱ) as the template, a complex {[Cu2L2(H2O)2] 4H2O}n (L = N-acetoxyl- picolinamide) has been successfully synthesized and characterized by single-crystal X-ray diffrac tion. The crystal is of monoclinic, space group C2/c, with a = 24.144(5), b = 7.1622(14), c = 17.283(4) (A), C16H24Cu2N4O12, Mr = 591.47, β = 131.73(3)°, V = 2230.3(8) (A)3, Z = 4, Dc= 1.761 g/cm3, F(000) = 1208,μ = 1.978 mm-1, R = 0.0400 and wR = 0.1099. The copper (Ⅱ) ion is five coordinated with a distorted square pyramidal geometry. The complex can be viewed as a one dimensional chain structure by carboxylic bridges among copper atoms. In the complex there exist hydrogen bonding interactions to stabilize the structure.     

Synthesis, Crystal Structure and Properties of a Europium Complex with 3-Iodobenzoic Acid and 2,2′-Bipyridine

The complex [Eu(3-IBA)3·2,2'-bipy]2 was synthesized from 3-iodobenzoic acid (3-HIBA), 2,2'-bipyridine (2,2'-bipy) and EuCl3·6H2O by hydrothermal synthesis, and its crystal structure was determined by X-ray single-crystal diffraction. It is of triclinic, space group P, with a = 10.958(2), b = 12.311(3), c = 12.556(3) (A), α = 81.549(3), β = 82.404(4), γ = 78.348(3)°, Mr = 1049.15, V = 1631.7(6) (A)3, Z = 1, Dc = 2.135 g/cm3, F(000) = 980, λ(MoKα) = 0.71073 A, μ(MoKα) = 4.804 mm-1, the final R = 0.0329 and wR = 0.0723 for 4640 observed reflections with I ＞ 2σ(I). The Eu(Ⅲ) ion is eight-coordinated and two Eu(Ⅲ) ions are held together by four 3-iodobenzoate groups in the bidentate bridging mode. The complex was characterized by DTA-TG, IR, UV and fluorescence spectra.     

Synthesis, Crystal Structure and Magnetic Properties of Cobalt(II) Complex Involving Imino Nitroxide Radicals

1 INTRODUCTION The synthesis and study of transition metal com-plexes incorporating organic free radicals have arou-sed great interest in the field of molecular magne-tism[1]. Nitronyl nitroxide radicals (NITR), stable or-ganic radicals, have been widely used as molecularunits in the design and construction of magnetic ma-terials[2～5]. These radicals are especially attractivedue to that their donor atoms can assemble an exten-ded coordination geometry with changing magneticcoupling. A…     

Synthesis and Crystal Structure of Copper(II) Complex with N-Acetoxyl-picolinamide

1 INTRODUCTION The picoloylhydrazide compounds are close to thebiologic environment and can react with microele-ments in organism so as to have antitubercular andantineoplastic activities. However, owing to the exis-tence of amino group, this kind of compounds aretoxic to some extent[1]. In order to decrease theirtoxicity, hydrazone or hydrazide compounds synthe-sized by the condensation reaction of amino and car-bonyl groups have been well studied in recentyears[1～7]. Herein we report t…     

A Novel Cobalt(III) Mixed-polypyridyl Complex: Synthesis, Characterization and DNA Binding

ＩｎｔｒｏｄｕｃｔｉｏｎＴｈｅｔｒａｎｓｉｔｉｏｎｍｅｔａｌｐｏｌｙｐｙｒｉｄｙｌｃｏｏｒｄｉｎａｔｉｏｎｃｏｍ ｐｏｕｎｄｓａｓｔｈｅｐｒｏｂｅｏｆＤＮＡｓｔｒｕｃｔｕｒｅａｎｄｃｏｎｆｉｇｕｒａｔｉｏｎｈａｖｅｂｅｅｎｅｘｔｅｎｓｉｖｅｌｙｓｔｕｄｉｅｄｉｎｔｈｅｐａｓｔｆｅｗｙｅａｒｓ .ＴｈｅｙｉｎｔｅｒａｃｔｅｆｆｅｃｔｉｖｅｌｙｗｉｔｈＤＮＡｂｙｃｈａｎｇｉｎｇｔｈｅｔｙｐｅｏｆｈｅｔ ｅｒｏａｒｏｍａｔｉｃｌｉｇａｎｄｏｒｍｅｔａｌｃｅｎｔｅｒ.Ｔｈｏｓｅｗｉｔｈｐｈｅｎ(ｐｈｅｎａｎｅ…     

Synthesis and Crystal Structure of a Novel Copper (II) Complex with Acetylenedicarboxylate and 2, 2′-Bipyridine

The construction of molecular-based crystalline solids using coordination polymer has become a very active research field in recent years,not only due to their intriguing structural motifs,but also due to their potential applications in optical,electronic and magnetic materials1,2.Many of the most interesting coordination polymers are based on polycarboxylate ligands,such as maleate3,malonate4,1,4-benzenedicarboxylate5,1,3,5-benzenetricar-boxylate6and1,2,4,5-benzenetetracarboxylate7,which have …     

Synthesis and Structure of Zinc Complex of N, N-bis ( benzimidazol-2-yl-methyl ) amine

Histidine is known to be an important biological ligand present at the active site of superoxide dismutases (SOD)1-2 and other metalloproteins. It appears to play a crucial role in the coordination chemistry of numerous metalloproteins. The ligand of di(2-benzimidazolyl-methyl)amine (L3) was chosen as the model compound of histidine. This paper reports the synthesis and crystal structure of Zn-L3 complex which is as the model compound of SOD.The complex, Zn(L3)2((ClO4)2(C2H5OH(C32H30N1…     

Synthesis of a New Cobalt (II) Complex and its Interaction with DNA

The interaction of metal complexes with DNA has been widely studied by differentmethods such as spectrophotometry, light scattering technique, fluorometry1-3. Manycomplexes such as Co(phen)2 ,Co(en)2 ,Fe(EDTA)2- etc.4,5 have been synthesized and 3+ 3+their effect on DNA has been studied in order to further explain the mechanism of genemutation, anti-cancer or cancer-induced reason and DNA targeted drugs. In this paper,a new cobalt complex was synth…     

Synthesis and Crystal Structure of Tetra Benzoates Bridged Binuclear Sm(III) Complex

１ＩＮＴＲＯＤＵＣＴＩＯＮＩｔｉｓｗｅｌｋｎｏｗｎｔｈａｔｌａｎｔｈａｎｉｄｅｅｌｅｍｅｎｔｓｔｅｎｄｔｏｂｅｃｏｏｒｄｉｎａｔｅｄｗｉｔｈｐｏｌｙｃａｒ ｂｏｘｙ ｏｒｍａｃｒｏｃｙｃｌｉｃ ｃｏｎｔａｉｎｉｎｇｓｐｅｃｉｅｓｔｏｆｏｒｍｐｏｌｙｎ...     

Synthesis and Crystal Structure of a New Lanthanum(III) 4-Cyanobenzoate Complex

A new dinuclear La(III) complex [La2(4-cba)4[H(4-cba)2]2(phen)2(H2O)4] (4-Hcba = 4-cyanobenzoic acid and phen = 1,10-phenanthroline) 1 has been synthesized by solvothermal reaction in an ethanol/water mixed solution at 100 ℃ and structurally characterized by single- crystal X-ray diffraction. Crystallographic data: C88H58La2N12O20, Mr = 1881.28, triclinic P1, a = 7.518(3), b = 17.033(6), c = 17.551(6), α = 115.333(4), β = 92.9910(10), γ = 99.366(5)°, V = 1985.3(12)3, Z = 1, Dc = 1.574 g/cm3, F(000) = 944 μ = 1.145 mm–1, the final R = 0.0281 and wR = 0.0686 for 6708 reflections with I > 2σ(I). In 1, two nine-coordinated La(III) ions are connected by two 4-cba ligands in a syn-syn bidentate coordination mode, and the other six 4-cba ligands terminate the La(III) ions, resulting in an isolated dinuclear structure. Two different types of intramolecular hydrogen bonds, asymmetrical O-H…O and symmetrical O…H…O, exist in the crystal. The title complex molecules are connected through hydrogen bonds and weak π-π stacking interactions to generate a 2-D layered network. The thermogravimetric analysis of 1 has also been discussed.     

Synthesis and Structure of a Novel Cobalt(Ⅱ)Complex with the Tertiary Carbinol Derivative of Di-4-pyridinylmethanone

The title complex [Co[(4-C5H4N)2C(OH)(NHC3H7)]2(NO3)2]∞ was obtained and characterized through elemental analysis, FT-IR and X-ray crystallography. The complex crystallizes in space group P3(2)21 with a=10.2480(11), b=10.2480(11), c=26.943(6), β=120.00°, [Co[(4-C5H4N)2C(OH)(NHC3H7)]2(NO3)2]∞, C28H34CoN8O8 , Mr=669.56, Z=3, V=2450.5(7)3 , Dc=1.361 g·cm-3 , μ=0.584 mm-1 , F(000)=1047, R=0.0498 and wR=0.1301. The Co(Ⅱ) center exhibits a N4O2-octahedral coordination geometry surrounded by a pair of nitrates at the axial positions and four pyridyl N atoms at the equatorial sites. An infinite double-bridged chain structure with μ2-bridging (4-C5H4N)2C(OH)(NHC3H7) ligands is formed, which is the in situ product of metal-promoted nucleophilic addition reaction of propan-1-amine with di-4-pyridinylmethanone ((4-C5H4N)2CO) in the presence of Co(NO3)2·6H2O. It is the first tertiary carbinol metal complex derived from di-4-pyridinylmethanone so far, and also the rare example of tertiary carbinol derivative of dipyridylmethanone family. The nucleophilic reaction at the carbonyl of dipyridylmethanone in the presence of metal salt will be discussed.