Synthesis,spectroscopic exploration,biocidal activities,and crystal structures of 3‐(3‐fluorophenyl)‐2‐phenylpropenoic acid and trimethyltin(IV) complex

The ligand, 3‐(3‐fluorophenyl)‐2‐phenylpropenoic acid, [C₁₅H₁₁FO₂] ( I ) was prepared by reacting equimolar amount of phenyl acetic acid with 3‐fluorobenzaldehyde (1:1) using Perkin condensation method. The trimethyltin(IV) carboxylate, [Me₃SnO₂FH₁₀C₁₅] ( II ) was synthesized by refluxing an equimolar (1:1) mixture of trimethyltin chloride and silver salt of the ligand acid, [C₁₅H₁₀FO₂Ag] ( Ia ). The ligand and complex both were characterized by elemental analysis, IR, mass, ¹H NMR, and X‐ray crystallographic data. On the basis of ¹H NMR data, (²J[^117/119Sn, ¹H] and C Sn C bond angle), it is concluded that the environment around the tin atom in solution is tetrahedral. The Infrared spectroscopic results showed that trimethyltin(IV) derivative has 5‐coordinated polymeric structure with bridging carboxylate groups in the solid state, which has been confirmed by the X‐ray crystallographic data. The crystal of ligand acid ( I ) is triclinic with space group Pbar1. However, the crystal of the complex ( II ) is monoclinic with space group C_2/c. The geometry around the tin atom is distorted trigonal bipyramid with O(1) and O(2) atoms in apical positions. The ligand ( I ) and complex ( II ) were also tested for their biocidal activities. © 2004 Wiley Periodicals, Inc. Heteroatom Chem 15:398–406, 2004; Published online in Wiley InterScience (www.interscience.wiley.com). DOI 10.1002/hc.20032     

A 1,2,4‐Triazole‐based Polynuclear Mixed‐valence MnIIMnIII Complex: Synthesis,Characterization, and Magnetic Property

A mixed‐valence Mn complex {[Mn^IIMn^III(HL)₂(4,4′‐bpy)(H₂O)₂] · (ClO₄)(DMF)₃(4,4′‐bpy)_0.5}_n ( 1 ) [H₂L = 3‐(2‐phenol)‐5‐(pyridin‐2‐yl)‐1,2,4‐triazole] was synthesized and characterized by X‐ray single‐crystal structure analysis and magnetic susceptibility. Single‐crystal X‐ray analysis revealed that complex 1 has a dinuclear core, in which adjacent central Mn^III atoms are linked by 4,4′‐bipyridine to form an infinite one‐dimensional (1D) molecular configuration. According to the Mn surrounding bond lengths and bond valence sum (BVS) calculations, we demonstrated that the Mn atom coordinated to the pyridine N atoms is in the +2 oxidation state, while another Mn atom coordinated to the phenolic oxygen atoms is in the +3 oxidation state. Magnetic susceptibility data of the complex 1 indicate that the ferromagnetic interaction dominates in this complex.     

丙酮酸异烟酰腙四核有机锡配合物的合成、表征及{[nBu2Sn(C9H8N3O3)O]SnBu3n}2的晶体结构

The tetranuclear alkyltin(Ⅳ) compounds {[R2Sn(C9H8N3O3)O]SnR3}2 [R=n-Bu (1), 4-CNC6H4CH2 (2),C6H5CH2 (3), 4-ClC6H4CH2 (4)] were prepared by the reaction of Schiff base ligand pyruvic acid isonicotinyl hydrazone with (R3Sn)2O in the corresponding molar ratio of 1:1. All compounds have been characterized by elemental analysis, IR and ^1H NMR spectra. The crystal structure of compound 1 was determined by X-ray single crystal diffractional analysis. This compound exhibits a dimeric structure containing distannoxane units with two types of the tin atoms. For the first tin atom, it appears to be seven-coordinated with a distorted pentagonal bipyramid geometry, and the other is five-coordinated with a distorted trigonal bipyramidal geometry. The molecules are packed in the unit cell in two-dimensional network structure through an interaction between the N atoms of the pyridine and the tin atoms of an adjacent molecule.     

Organotin Carboxylates based on 3‐(1,3‐Dioxo‐2,3‐dihydro‐1H‐phenalen‐2‐yl)benzoic Acid and the Influence of Solvent on the Molecular Structure

Self‐assembly of dibutyltin oxide with 3‐(1,3‐dioxo‐2,3‐dihydro‐1H‐phenalen‐2‐yl)benzoic acid (HL) produces (nBu)₂SnL₂ ( 1 ) when benzene is used as solvent, whereas the reaction generates {[(nBu)₂SnO]₂L}₂ · C₇H₈ ( 2 ) when toluene is the reactive solvent. The novel organotin carboxylate (nBu)₂SnL₂ ( 1 ) was characterized by elemental analysis, as well as IR, ¹H, ¹³C, and ¹¹⁹Sn NMR spectroscopy. Single crystal X‐ray study reveals that 1 is a dialkyltin carboxylate monomer possessing crystallographically imposed twofold symmetry. Ligand HL in 1 chelates with tin atom in bidentate coordination mode. The molecules of 1 build complicate 1D, 2D, and 3D structures via intermolecular hydrogen bonds, and π ··· π interactions can be found in the 3D architecture. The preliminary fluorescence activity and antitumor activity of the complex were also studied.     

Synthesis,Structure and Magnetic Property of an “Adamantane” Type Tetranuclear Iron(III) Complex

A new tetranuclear complex [Fe₄ L ₂(μ‐O)₂(μ‐>OH)₂](ClO₄)₄·H₂O ( 1 ), (H L = N,N,N′,N′‐tetrakis‐[(2‐pyridyl)methyl]‐2‐hydroxypropane‐1,3‐diamine) has been synthesized and its crystal structure and magnetic properties are shown. X‐ray crystallography reveals that complex 1 contains a quadruply‐charged, tetranuclear iron(III) cation and four perchlorate anions. In 1 , the Fe₄O₆ core is composed of a tetrahedron of iron atoms bridged by six oxygen atoms (two oxo, two hydroxo, and two alkoxo groups from L ). This results in an adamantane‐type geometry with the iron atoms occupying the bridgehead positions. Susceptibility data of 1 indicate strong intramolecular antiferromagnetic coupling of high‐spin Fe^III atoms.     

Synthesis,structural characterization and cytotoxic activity of triorganotin 5‐(salicylideneamino)salicylates

Six new triorganotin complexes ( 1a – 1c and 2a – 2c ) of 5‐(salicylideneamino)salicylic acid, [5‐(3‐X‐2‐HOC₆H₃CH═N)‐2‐HOC₆H₃COO]SnR₃ (X = H, 1 ; CH₃O, 2 ; R = Ph, a ; Cy, b ; CH₂C(CH₃)₂Ph, c ), have been synthesized by one‐pot reaction of 5‐aminosalicylic acid, salicylaldehyde and triorganotin hydroxide and characterized using elemental analysis and infrared and NMR (¹H, ¹³C and ¹¹⁹Sn) spectra. The crystal structures of 1a , 1b , 2a ·CH₃OH, 2b ·CH₃OH and 2c ·CHCl₃ have been determined using single‐crystal X‐ray diffraction. In non‐coordinated solvent CDCl₃, the tin atoms in the complexes are all four‐coordinated. In the crystalline state, these compounds adopt a four‐ or five‐coordination mode. Complex 1a exhibits a 44‐membered macrocyclic tetrameric structure with trigonal bipyramidal geometry around the tin atoms in which the axial positions are occupied by the oxygen atom of carboxylate group of the ligand and the phenolic oxygen atom from the adjacent ligand. The coordination geometry of tin atom in 1b and 2c ·CHCl₃ is a distorted tetrahedron shaped by three carbon atoms of alkyl groups and a carboxylate oxygen atom of the ligand. In 2a ·CH₃OH and 2b ·CH₃OH, the tin atom has a distorted trans‐C₃SnO₂ trigonal bipyramidal geometry formed by three alkyl groups, a monodentate carboxylate group and a coordinated methanol molecule. The molecules of 2a ·CH₃OH and 2b ·CH₃OH are linked via O─H···O hydrogen bonds into a one‐dimensional supramolecular chain and a centrosymmetric R₄⁴(22) macrocycle, respectively. Bioassay results against two human tumor cell types (A549 and HeLa) show the complexes are efficient cytostatic agents and may be explored as potential antitumor drugs.     

Synthesis and spectroscopic properties of [N-(4-carboxyphenyl) salicylideneiminato] di- and tri-organotin (IV) complexes and crystal structures of {[Bu2Sn(2-OHC6H4CHNC6H4COO)]2O}2 and Ph3Sn(2-OHC6H4CHNC6H4COO)

Reactions of R₂SnO (R: ⁿBu, Cy, Ph, PhCH₂) and R₃SnCl (R: Ph, Cy, PhCH₂, 2-Cl-PhCH₂, 4-F-PhCH₂, 4-Cl-PhCH₂) with N-(4-carboxyphenyl)-salicylideneimine (LH₂) in 1:1 stoichiometry afford complexes {[R₂Sn(LH)]₂O}₂ and R₃Sn(LH). These complexes have been characterized by elemental analyses, IR, ¹H and ¹¹⁹Sn NMR spectroscopy. The crystal structures of {[ⁿBu₂Sn(LH)]₂O}₂, 1 and Ph₃Sn(L), 5 are determined by single crystal X-ray diffraction. Results showed that in the solid state the complex 1 is a tetranuclear centrosymmetric dimer with six-coordination being assigned to both the endo-cyclic and exo-cyclic tin atoms after consideration of close intermolecular tin oxygen contacts, and study show that the imino nitrogen atom do not participate in coordination to the tin atom. The complex 5 is a monomer, and in the molecule the tin atoms are five-coordinated in trigonal bipyramidal geometries with the two oxygen atom of the carboxylate both coordinating to the tin atoms.     

Synthesis,properties and crystal structural characterization of diorganotin(IV) derivatives of 2‐mercapto‐6‐nitrobenzothiazole

The diorganotin(IV) dichlorides R₂SnCl₂ (R: Ph, PhCH₂ or n‐Bu) react with 2‐mercapto‐6‐nitrobenzothiazole (MNBT) in benzene to give [Ph₂SnCl(MNBT)] ( 1 ), [(PhCH₂)₂Sn(MNBT)₂] ( 2 ) and [(n‐Bu)₂Sn(MNBT)₂] ( 3 ). The three complexes have been characterized by elemental analysis and IR, ¹H, ¹³C and ¹¹⁹Sn NMR spectroscopies. X‐ray studies of the crystal structures of 1 , 2 and 3 show the following. The tin environment for complex 1 is distorted cis‐trigonal bipyramid with chlorine and nitrogen atoms in apical positions. The structure of complex 2 is a distorted octahedron with two benzyl groups in the axial sites. The geometry at the tin atom of complex 3 is that of an irregular octahedron. Interestingly, intra‐molecular non‐bonded Cl…S interactions and S…S interaction were recognized in the crystallographic structures of 1 and 3 respectively. As a result, complex 1 is a polymer and complex 3 is a dimer. Copyright © 2003 John Wiley & Sons, Ltd.     

Coordination polymers based on building blocks of dimethyltin(IV) Chloride iso‐thiocyanate and dimethyltin(IV) di‐iso‐thiocyanate with pyrazine‐2‐carboxylate and 4, 4′‐bipyridine

The reaction of 4,4′‐bipy with dimethyltin(IV) chloride iso‐thiocyanate affords the one‐dimensional (1D) coordination polymer, [Me₂Sn(NCS)Cl·(4,4′‐bipy)]_n ( 1 ), whereas reaction of dimethyltin(IV) dichloride with sodium pyrazine‐2‐carboxylate in the presence of potassium iso‐thiocyanate affords the two‐dimensional (2D) coordination polymer, {[Me₂Sn(C₄H₃N₂COO)₂]₂ [Me₂Sn(NCS)₂]}_n ( 2 ). Both coordination polymers were characterized by elemental analysis and infrared spectroscopy in addition to ¹H and ¹³C NMR spectroscopy of the soluble coordination polymer ( 1 ). A single‐crystal structure determination showed that the asymmetric unit in 1 contains Me₂Sn(NCS)Cl and 4,4′‐bipy moieties and a 1D infinite rigid chain structure forms through bridging of the 4,4′‐bipy ligand between tin atoms and the geometry around the tin atom is a distorted octahedral. Coordination polymer 2 contains two distinct tin atom geometrics in which one tin atom is seven coordinate, and the other is six coordinate. The two tin atom environments are best described as a pentagonal bipyramidal in the former and distorted octahedral in the latter where the carboxylate groups bridge the two tin atoms and construct a 2D‐coordination polymer. The ¹¹⁹Sn NMR spectroscopy indicates the octahedral geometry of 1 retains in solution. © 2011 Wiley Periodicals, Inc. Heteroatom Chem 22:699–706, 2011; View this article online at wileyonlinelibrary.com . DOI 10.1002/.20736     

Synthesis,Characterization and Crystal Structure of Chlorodibenzyltin（Ⅳ） Complex with Dithiomorpholinocarba—mate Ligand

Chlorodibenzyltin (IV) complex with dithiomorpholinocarbamate ligand was synthesized by the reaction of dibenzyltin dichloride with dithiomorpholinocarbamate in 1:1 stoichiometry. The complex was characterized by elementary analysis, UV, BR and ¹H NMR spectra. The crystal structure was determined by X‐ray single crystal diffraction study. The crystallographic data are as follows: triclinic, space group P1 , a = 0.8723 (2) ran, b = 1.099 (2) nm, c = 1.1036 (3) nm, α = 86.498 (4)°, β = 89.697 (5)°, γ = 82.807 (5)°, Z = 2, V = 1.0479 (4) nm³, D_c= 1.580 g/cm^?3, μ = 1.553 mm^?1, F (000) = 500, R₁ = 0.0442, wR₂ = 0.0974. The crystal consists of discrete molecules containing five‐coordinate tin atoms in a distorted tigonal bipyramidal configuration. The molecules are packed in the unit cell in one‐dimensional chain structure through a weak interaction between the chlorine atom and sulfur atom, the sulfur atom and one of the sulfurs of an adjacent molecule.     

A novel dinuclear bismuth(III) coordination compound: bis(μ‐pyridine‐2,6‐dicarboxylato)‐κ4O2,N,O6:O6′;κ4O2:O2′,N,O6‐bis[(azido‐κN)(1,10‐phenanthroline‐κ2N,N′)bismuth(III)] tetrahydrate

A novel dinuclear bismuth(III) coordination compound, [Bi₂(C₇H₃NO₄)₂(N₃)₂(C₁₂H₈N₂)₂]·4H₂O, has been synthesized by an ionothermal method and characterized by elemental analysis, energy‐dispersive X‐ray spectroscopy, IR, X‐ray photoelectron spectroscopy and single‐crystal X‐ray diffraction. The molecular structure consists of one centrosymmetric dinuclear neutral fragment and four water molecules. Within the dinuclear fragment, each Bi^III centre is seven‐coordinated by three O atoms and four N atoms. The coordination geometry of each Bi^III atom is distorted pentagonal–bipyramidal (BiO₃N₄), with one azide N atom and one bridging carboxylate O atom located in axial positions. The carboxylate O atoms and water molecules are assembled via O—H...O hydrogen bonds, resulting in the formation of a three‐dimensional supramolecular structure. Two types of π–π stacking interactions are found, with centroid‐to‐centroid distances of 3.461 (4) and 3.641 (4) Å.     

Synthesis,Structure, and Physical Properties of a Barium Complex with 5‐Sulfoisophthalic Acid Sodium Salt

The complex [Ba₃(sip)₂(H₂O)₉] · H₂O ( 1 ) (NaH₂sip = 5‐sulfoisophthalic acid sodium) was synthesized and characterized by single‐crystal X‐ray diffraction. Structural determination reveals that the asymmetric unit in 1 contains two crystallographically independent Ba^II atoms. The Ba1 atom is eight‐coordinate with distorted monocapped pentagonal bipyramidal arrangement, whereas the Ba2 atom is ten‐coordinated with bicapped tetragonal prismatic arrangement. The two carboxylate groups of sip^3– adopt different coordination modes, μ₂‐η¹:η¹‐bridging, and μ₂‐η²:η¹‐bridging. The sulfonate group coordinates to three different Ba^II atoms in a tridentate μ₃ mode to generate a ladder‐like one‐dimensional chain. The chains are connected by μ₂‐η¹:η¹‐bridging carboxylate groups to form a wave‐like two‐dimensional network, which are further linked by sip^3– anions to generate a three‐dimensional structure. The thermal stability and luminescence properties of complex 1 were also investigated.     

A Novel Proton Transfer Self‐Associated Compound from Dipicolinic Acid and Guanidine and Its Cadmium(II) Complex: Synthesis,Characterization, Crystal Structure,and Solution Studies

A novel 1:2 proton transfer self‐associated compound LH₂ , (GH⁺)₂(pydc^2—), was synthesized from the reaction of dipicolinic acid, pydcH₂, (2, 6‐pyridinedicarboxylic acid), and guanidine hydrochloride, (GH⁺)(Cl^—). The characterization was performed using IR, ¹H and ¹³C NMR spectroscopy and single‐crystal X‐ray diffraction. LH₂ · H₂O crystallizes in the space group C2/c of the monoclinic system and contains eight molecules per unit cell. The unit cell dimensions are: a = 26.480(5)Å, b = 8.055(2)Å, c = 14.068(3)Å. The first coordination complex (GH)₂[Cd(pydc)₂] · 2H₂O, was prepared using LH₂ and cadmium(II) iodide, and characterized by ¹H and ¹³C NMR spectroscopy and X‐ray crystallography. The crystal system is triclinic with space group P1¯ with one molecule per unit cell. The unit cell dimensions are: a = 8.5125(7)Å, b = 11.0731(8)Å, c = 13.2404(10)Å. The cadmium(II) atom is six‐coordinated with a distorted octahedral geometry. The two pydc^2— units are almost perpendicular to each other. The protonation constants of the building blocks of the pydc‐guanidine adduct, the equilibrium constants for the reaction of pydc^2— with guanidine and the stoichiometry and stability of the Cd²⁺ complex with LH₂ in aqueous solution were accomplished by potentiometric pH titration. The solution studies strongly support a self‐association between pydc^2— and GH⁺ with a stoichiometry for the Cd^II complex similar to that observed for the isolated crystalline complex. In fact, the [Cd(pydc)₂]^2— complex was found as the most abundant species in solution (> 90 %) at a pH >5.     

Synthesis, Characterization and Properties of Organotin Complexes Dibutyltin（Ⅳ） Bis（heteroaromatic carboxylate） and Crystal Structure of Dibutyltin（Ⅳ） Bis（2-thiazolylcarboxylate）

The six organotin complexes dibutyltin(IV) bis(heteroaromatic carboxylate) were synthesized by the reaction of (n‐Bu)2SnO with heteroaromatic carboxylic acid in 1:2 molar ratio. These complexes have been characterized by elemental analysis, IR, ¹H, ¹³C and ¹¹⁹Sn NMR. The crystal structure of dibutyltin(IV) bis(2‐thiazolylcarboxylate) was determined by X‐ray single crystal diffraction. This compound is a weakly bridged dimer through weak interaction Sn···O between molecules. The tin atoms took six‐coordinate skew‐trapezoidal bipyramidal geometry. The crystal of complex 3 belongs to monoclinic symmetry with space group P2₁/c, a=1.863(2) nm, b=2.220(3) nm, c=1.0395(10) nm, β=90.275(16)°, Z=8, V=4.292(8) nm³, D_c=1.514 Mg/m³, μ=1.406 mm^‐1, F(000)=1968, S=0.999, R=0.0549, wR=0.1011.     

A Novel Proton Transfer Compound Containing 2, 6‐Pyridinedicarboxylic Acid and Creatinine and its Zinc(II) Complex — Synthesis,Characterization, Crystal Structure,and Solution Studies

The 1:1 proton transfer compound LH₂, (creatH)⁺ (pydcH)^?, has been prepared from the reaction of creatinine, creat, and dipicolinic acid, pydcH₂, (2, 6‐ pyridinedicarboxylic acid) and characterized using IR, ¹H and ¹³C NMR spectroscopy. The first coordination complex (creatH)[Zn(pydc)(pydcH)]·4H₂O, was prepared using LH₂ and zinc(II) nitrate, and characterized using IR, ¹H and ¹³C NMR spectroscopy and single crystal X‐ray crystallography. The crystal system is triclinic with space group with two molecules per unit cell. The unit cell dimensions are a = 8.085(2) Å, b = 10.802(4) Å, c = 13.632(4) Å, α = 104.98(2)°, β = 90.31(2)° and γ = 92.55(3)°. The structure has been refined to a final value for the crystallographic R factor of 0.0381 based on 3003 reflections. The zinc atom is six‐coordinated with a distorted octahedral geometry. The (pydc)^2? and (pydcH)^? units are almost perpendicular to each other. Extensive hydrogen bondings between carboxylate groups, (creatH)⁺ and water molecules throughout the zinc(II) complex as well as π–π stacking and ion pairing play important roles in stabilizing the corresponding lattices. The protonation constants of the building blocks of the pydcH₂‐creat adduct, the equilibrium constants for the reaction of (pydc)^2? with creat and the stoichiometry and stability of the Zn^II complex with LH₂ in aqueous solution were accomplished by potentiometric pH titration. The solution studies support a self‐associated (creatH)⁺(pydcH)^? as the most abundant species at pH = 3.4. The stoichiometry of the crystalline complex (i.e. (creatH) [Zn(pydc)(pydcH)])and that of the most abundant species detected in solution were found the same.     

Synthesis, Properties and Crystal Structure of Seven-coordinated Organotin Complex [~nBu_2Sn(OOCC_5H_4N-2)_2(H_2O)]

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A Three—Dimensional Lead(II) Polymer with Bridging Saccharinate and Unusually Coordinated Acetate Ligands — Synthesis,IR Spectra,and Crystal Structure of [Pb(H2O)(μ‐OAc)(μ‐sac)]n

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.     

Diorganotin(IV) complexes of polyaromatic azo‐azomethine ligand derived from salicylaldehyde and ortho‐aminophenol: Synthesis,characterization, and molecular structures

The diorganotin(IV) complexes of methyl 2‐{4‐hydroxy‐3‐[(2‐hydroxy‐phenylimino)‐methyl]‐phenylazo}‐benzoate (H2L) were obtained by the reaction of ortho‐aminophenol, R₂SnO (R = Me, ⁿBu, or Ph) and methyl 2‐[(E)‐(3‐formyl‐4‐hydroxy)diazenyl]benzoate (H2PL²) in ethanol, which led to diorganotin(IV) compounds of composition [Me₂SnL]₂ ( 1 ), ⁿBu₂SnL ( 2 ), and Ph₂SnL ( 3 ) in good yield. The ¹H, ¹³C, and ¹¹⁹Sn NMR, IR, the mass spectrometry along with elemental analyses allowed establishing the structure of ligand (H2L) and compounds 1–3 . In all the three cases, ¹¹⁹Sn chemical shifts are indicators of five‐coordinated Sn atoms in a solution state. The crystal structures of ligand H2L and complexes 1 and 2 were determined by a single crystal X‐ray diffraction study. In the solid state, the ligand H2L exists as a keto‐enamine tautomeric form. The molecular structure of complex 1 in the solid state shows a distorted octahedral geometry around a tin atom due to additional coordination with an oxygen atom from a neighboring molecule leading to a four‐membered ring with Sn‐O···Sn‐O intermolecular coordination, leading to a dimeric species. On the other hand, complex 2 is a monomer with trigonal bipyramidal geometry surrounding the tin atom. © 2012 Wiley Periodicals, Inc. Heteroatom Chem 23:457–465, 2012; View this article online at wileyonlinelibrary.com . DOI 10.1002/hc.21037     

Synthesis,Characterization, and Magnetic Properties of Novel Cobalt(II) and Copper(II) Complexes with 5‐(Isonicotinamido)isophthalate Ligand

Two new complexes, {[Co(INAIP) · H₂O] · 2H₂O}_n ( 1 ), and {[Cu(INAIP)] · H₂O}_n ( 2 ) [H₂INAIP = 5‐(isonicotinamido)isophthalic acid] were synthesized under hydrothermal conditions, and characterized by single‐crystal X‐ray structure determination, thermogravimetric analysis, X‐ray powder diffraction, and magnetic studies. In complex 1 both Co^II atoms and INAIP^2– ligands act as four‐connected node, whereas in 2 both Cu^II atoms and INAIP^2– ligands act as three‐connected node.     

Synthesis,spectra, crystal structures and anticancer studies of 26‐membered macrocyclic dibutyltin(IV) dithiocarbamate complexes: Single‐source precursors for tin sulfide nanoparticles

Four new macrocyclic dinuclear dibutyltin(IV) dithiocarbamate complexes of the type [Bu₂Sn(dtc)]₂, where dtc = hexane‐1,6‐diylbis(4‐fluorobenzyldithiocarbamate) anion ( 1 ), hexane‐1,6‐diylbis(4‐chlorobenzyldithiocarbamate) anion ( 2 ), hexane‐1,6‐diylbis(furfuryldithiocarbamate) anion ( 3 ) and hexane‐1,6‐diylbis(pyrrole‐2‐ylmethyldithiocarbamate) anion ( 4 ), have been prepared. The dithiocarbamate ligands efficiently self‐assemble with Bu₂Sn(IV) to form bimetallic 26‐membered macrocycles. All the complexes have been characterized using elemental analysis, infrared and NMR (¹H and ¹³C) spectroscopies and X‐ray crystallography. Single‐crystal X‐ray diffraction analysis of all the complexes confirms the formation of the dinuclear metallomacrocycles in which dithiocarbamate ligands are asymmetrically bound to the tin atoms. The coordination sphere around the tin atom in 1 – 4 can be described as a skew trapezoidal bipyramid. The dimensions of the cavity of the macrocycles of 1 – 4 are ca 8.0 × 9.0 Å². Complexes 1 – 4 were evaluated for their in vitro anticancer activity against MCF‐7 and HL‐60 cells. Complexes 1 and 2 are more active against MCF‐7 and HL‐60. Thermal decomposition of 1 and 4 yielded tin sulfides. They were characterized using powder X‐ray diffraction (PXRD), high‐resolution transmission electron microscopy and UV diffuse reflectance and energy‐dispersive X‐ray spectroscopies. PXRD studies reveal that the as‐prepared tin sulfides are composed of orthorhombic phase of SnS.