Synthesis, Characterization, Crystal and Molecular Structure Analysis of Di-μ-chlorido-bis{[(4-bromobenzoylmethylene) triphenyl-λ5-phosphorane]chloridomercury(II)}

Abstract  

The reaction of phosphorus ylide Ph₃PCHC(O)C6H4–4–Br with HgCl₂ in equimolar ratios using methanol as a solvent is reported. This reaction led to binuclear complex C-Coordination of ylide and trans-like structure of complex [Br–BPPY HgCl₂]₂·2CHCl₃(1) is demonstrated by single crystal X-ray analyses and IR, ¹H and ³¹P NMR spectroscopy. Elemental analyses indicate a 1:1 stoichiometry between the ylide and Hg(II) in the product two Hg atoms are four-coordinate in the form of a tetrahedral. The title molecule [Hg₂Cl₄(C₂₆H₂₉BrOP)₂]·2CHCl₃(1) has a crystallographic inversion centre at the centroid of the four-membered ring formed by the two Hg atoms and two Cl atoms, with one short Hg–Cl(2.393A^°) bond, one Hg–C bond and two asymmetric bridging Hg–Cl (bonds at distances o 2.7345 and 2.2.7090A. The crystal packing is stabilized by C–H…O hydrogen bonds.     

Synthesis and Crystal Structure of Bis-(N,N′-dibenzylethane-1,2-diamine) cobalt(II) acetate

Abstract  

Bis-(N,N′-dibenzylethane-1,2-diamine) cobalt(II) acetate has been synthesized and the crystal structure determined. The compound crystallizes in the space group P2₁/c, a = 8.3212(6) ?, b = 11.8774(8) ?, c = 17.3643(12) ?, β = 98.1850(10)°, V = 1698.7(2) ?³, Z = 2. The complex occupies a crystallographic inversion center. The cobalt is in a distorted octahedral environment likely due to steric influences of the acetate groups.     

Synthesis,Crystal Structure and Characterization of (Z)-2-N′-hydroxyisonicotinamidine

The compound (Z)-2-N′-hydroxyisonicotinamidine, (2) was synthesized and characterized by ¹H NMR, FT-IR, FAB-Mass, UV-Visible Spectra, and elemental Analysis. Its molecular structure was solved by single crystal X-ray diffraction method. The title molecule, C₆H₇N₃O is crystallized in the orthorhombic crystal system with the space group Pna2₁ and with unit cell parameters a = 12.5664(8) Å, b = 8.8622(6) Å, c = 5.7953(4) Å, α = 90°, β = 90°, γ = 90°, and Z = 4. The molecular and crystal structure of the title molecule is stabilized by an intramolecular interaction of the type N—H···O, and the intermolecular interactions of types N—H···N and O—H···N.     

Synthesis and Crystal Structure of a Bulky β-Diketiminato Ytterbium(II) Iodide Complex

Abstract  

The reaction of YbI₂ with [K(THF)₃(^ButNacnac)] (^ButNacnac = [(DipNCBu^t)₂CH]⁻; Dip = C₆H₃Pr₂ⁱ-2,6) has afforded the dimeric complex, [{Yb(η⁵-^ButNacnac)(THF)(μ-I)}₂] 1. The cell parameters of compound 1 are: P-1, a = 10.498(2), b = 13.146(3), c = 16.293(3); α = 88.06(3), β = 79.43(3), γ = 71.10(3). The compound represents a rare example of a structurally characterized complex exhibiting an η⁵-interaction between a β-diketiminate ligand and an ytterbium(II) center.     

Crystal and molecular structure of di-μ-chlorobis[2-[[[(2-hydroxy-1-naphthyl)methyl]-imino]ethanolato]N,O,O′]di-copper(II) dihydrate

The crystal structure of the title compound has been determined from three-dimensional, single crystal X-ray diffraction data. [Cu₂Cl₂(C₁₃H₁₂NO₂)₂]·2H₂O crystallizes in the orthorhombic space group P2₁2₁2₁ with lattice constants,a=11.866(2),b=13.555(3),c=17.380(3) Å. Final full-matrix least-squares refinement of 3735 unique reflections yieldedR=0.054. The structure consists of dimeric C₂₆H₂₄Cl₂Cu₂N₂O₄ molecules and water molecules connected with the dimeric molecules by a hydrogen bond system. Both of the copper(II) centers are five-coordinated by twotrans oxygen atoms and one nitrogen atom from one ligand molecule and two chloride ions. The geometry at each copper(II) center is best described as distorted tetragonal pyramidal. The apical Cu1–Cl2 and Cu2–C11 distances are 2.747(2) and 2.938(3)Å, respectively. The Cu...Cu separation is 3.496(1)Å. The comparison with previously reported crystal structure of [Cu₂Cl₂ (C₁₃H₁₂NO₂)₂]·1/2H₂O is given.     

Synthesis,Crystal Structure and Cytotoxic Property of <Emphasis Type="Italic">catena</Emphasis>-Poly[[{2-[2-(methylamino)ethyliminomethyl]-4-nitrophenolato}Zinc(II)]-μ-acetato]

Abstract  

The acetato-bridged polymeric Schiff base zinc(II) complex [Zn(MENP)(CH₃COO)]_n (MENP = 2-[2-(methylamino)ethyliminomethyl]-4-nitrophenolate) was synthesized and characterized by elemental analysis, IR and single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P2₁/c with a = 14.054(2), b = 11.167(1), c = 9.323(2) ?, β = 92.053(2)°, V = 1462.2(4) ?³, Z = 4, R ₁ = 0.0420 and wR ₂ = 0.1019. The Zn atom is coordinated in a trigonal–bipyramidal manner by one Schiff base ligand and two bridging acetate anions. The adjacent Zn···Zn distance is 4.727(2) ?. The [Zn(MENP)] units are linked through the bridging acetate groups, forming chains running along the c axis. The complex shows slight cytotoxic property to both normal and carcinoma cells.     

Synthesis and Structure of Di-μ-oxo-bistripyrazolylborato Dioxo Vanadium (V) Complex with Lattice of Diacetonitrile

Abstract A novel oxovanadium complex was obtained by the reaction of VOSO₄ · 3H₂O with tripyrazolylborate sodium in MeOH. The complex (1) was characterized by element analysis, IR spectroscopy, ¹HNMR and its crystal for X-ray diffraction recrystallized from saturated CH₃CN solution. The compound crystallizes in the monoclinic, space group Pbca, with cell dimensions of a = 15.531(2) ?; b = 18.007(2) ?; c = 10.725(2) ?; V = 2,999.4(8) ?³ and D _calc = 1.533 g/cm³ for Z = 4. The structure was solved by direct methods and refined to an R-value of 0.0401. Structure analysis show that it is a di-μ-oxo-bistripyrazolylborato dioxo vanadium (V) complex with lattice of diacetonitrile. In addition, the electronic structure and the bonding characters of the complex were analyzed with ab initio calculations. Index Abstract Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Crystal structures of copper(II) nitrate complexes containing 4,4’-bipyridyl and halogen-substituted 2-[(2-hydroxyethylimino)methyl]phenols

The crystal structures of (μ-4,4’-bipyridyl)-di{nitrato-2,4-dibromo-6-[(2-hydroxyethylimino)methyl]phenolo (1-)copper} (I), (μ-4,4’-bipyridyl)-di{nitrato-2,4-dichloro-6-[(2-hydroxyethylimino)methyl]phenolo(1-)copper} (II), and (μ-4,4’-bipyridyl)-{4-chloro-2-[(2-hydroxyethylimino)methyl]phenolo(2-)copper-nitrato-4-chloro-2-[(2-hydroxyethylimino)methyl]phenolo(1-)copper} tetrahydrate (III) are determined. The crystal structures of compounds I and II contain binuclear complexes, in which each copper atom is coordinated by the singly deprotonated tridentate molecule of the corresponding azomethine, the monodentate nitrate ion, and bipyridyl that plays the role of a bridge between the central atoms. In the structures of compounds I and II, the coordination polyhedra of the copper atoms are slightly distorted tetragonal pyramids. The pyramid base is formed by the imine and bipyridyl nitrogen atoms and the phenol and alcohol oxygen atoms. The axial vertices of the pyramids are occupied by the oxygen atoms of the monodentate nitrato groups. The crystal structure of compound III involves tetranuclear complexes in which the coordination polyhedra of the central copper atoms are (4 + 1 + 1) bipyramids. The base of these bipyramids is formed by the imine and bipyridyl nitrogen atoms and the phenol and alcohol oxygen atoms. One apical vertex is occupied by the bridging phenol oxygen atom of the nearest complex. The sixth coordination site of the first copper atom is occupied by the chlorine atom of the salicylidene fragment of the neighboring complex related to the initial complex through the center of symmetry. In turn, the sixth coordination site of the second copper atom is occupied by the oxygen atom of the monodentate nitrato group.     

Synthesis, spectroscopy, and X-ray structure of the polymer catena-[bis(azido-N)-copper(II)-μ-bis(2-benzimidazolyl)butane]

The title compound, catena-[bis(azido-N)-copper(II)-(bis(2-benzimidazolyl)butane), [Cu(C₁₈H₁₈N₄)(N₃)₂]_n, was obtained from the reaction of the ligand bis(2-benzimidazolyl)butane and Cu(N₃)₂. The x-ray crystal structure is reported. The compound crystallizes in the monoclinic space group P2₁/c with a = 8.2524(10), b = 12.765(5), c = 9.1125(15) Å, = 106.423(12)°, Z = 2. The Cu(II) ions are square-planar coordinated with trans-oriented end-on binding azido ligands. The structure is a polynuclear chain with the benzimidazole bridging at each end. In addition a N_(ligand)-H···N_(azido) H-bridge [N_(ligand)···N_(azido) = 2.994(7) Å] is present, resulting in a pseudo 2-dimensional lattice. The characteristic azido infrared vibrations are found at 2060 and 2077 cm^–1 (_as(N₃)) and 1284 and 1297 cm^–1 ((N₃)).     

Synthesis,Crystal Structure and Biological Activity of N′-tert-butyl-N-(3-methoxylbenzoyl)-N-(4-methyl-1,2,3-thiadiazole-5-formylhydrazine

Abstract  

The title compound, N′-tert-butyl-N-(3-methoxylbenzoyl)-N-(4-methyl-1,2,3-thiadiazole-5-formylhydrazine (C₁₆H₂₀N₄O₃S) was prepared from the reaction of 4-methyl-1,2,3-thiadiazole-5-carbonyl chloride with N′-tert-Butyl-3-methoxylbenzohydrazine, and its structure was characterized by ¹Hydrogen Nuclear Magnetic Resonance, High-Resolution Mass Spectrometry, IR spectra, and single crystal X-ray diffraction. The crystal of the title compound belongs to monoclinic system, space group P 21/c with cell parameters a = 17.986(2) ?, b = 8.0180(10) ?, c = 12.0190(14) ?, α = 90°, β = 91.160(5)°, γ = 90°, V = 1732.9(4) ?³, Z = 4, D _c  = 1.335 g/cm³, μ (Mo Ka) = 0.209 mm⁻¹, F (000) = 736, R = 0.0367 and wR = 0.0932. X-ray diffraction analysis indicates that all rings in the title compound are non-planar. The bioassay results indicated that, the title compound had good fungicide activity against Sclerotinia sclerotiorum, certain extent of insecticidal activity against Plutella xylostella L.     

N,N′-Di(pyridine-4-yl)-pyridine-3,5-dicarboxamide,a Pincer-Type Tricationic Compound; Synthesis,Crystal Structure,Hirshfeld Surface Analysis,and Computational Chemistry Studies

Journal of Chemical Crystallography - The synthesis, structure, and spectroscopic characterization of a pincer-type compound; N,N′-di(pyridine-4-yl)-pyridine-3,5-dicarboxamide is described....     

Synthesis and structural characterization of a (N,N′-bis[2(S)-pyrrolidylmethyl]-propane-1,3-diamine) nickel (II) complex

The nickel(II) complex [Ni(C₄H₃NCH=N–(CH₂)₃–N=CHC₄H₃N)], (1) containing the symmetrical N₄ tetradentate Schiff base ligand, which is the 2:1 condensation product of pyrrole-2-carboxaldehyde and 1,3-diaminopropane respectively, was prepared. Structural investigation shows that it is monomeric, having space group P2₁/c, a = 7.989(7), b = 17.406(14), c = 9.193(5) Å, = 90, = 100.39(6), = 90, and Z = 4. The coordination geometry around the nickel atom is slightly distorted square planar and the conformation of the six-membered ring containing the metal,azomethine nitrogens and three carbon atoms of the connecting 1,3-diaminopropane is a symmetric boat.     

Synthesis and Crystal Structure of a Copper(II)–Sodium(I) Coordination Polymer

Abstract  

A new coordination polymer, {[Na₂Cu(Ac)₄(H₂O)]·H₂O} _n (HAc = acetic acid), has been synthesized and structurally characterized by IR spectroscopy and X-ray crystallography. The compound crystallizes in the orthorhombic system, space group Pccn with a = 16.9076(17) ?, b = 11.8375(12) ?, c = 15.7567(16) ?, V = 3153.6(6) ?³. Four oxygen atoms from different Ac⁻ groups coordinate to the copper atom in a square-planar arrangement. Each sodium ion is in a distorted octahedral environment, being coordinated by one aqua ligand and five acetate oxygen atoms from two adjacent [Cu(Ac)₄] units. An alternating arrangement of metal ions and bridging acetate ligands results in the formation of two-dimensional sheets which are further linked into a three-dimensional network by the water molecules between the layers through rich hydrogen bonds.     

Crystal and molecular structure of di-μ-chlorobis[2-[[[(2-hydroxy-1-naphthyl)methyl]imino]-ethanolato]N,O,O′]di-copper(II) hemihydrate

The structure of the title compound [Cu₂Cl₂(C₁₃H₁₂NO₂)₂]·1/2 H₂O has been determined from single crystal X-ray diffraction data by direct methods. Full-matrix least-squares refinement of the structural parameters led to conventionalR factor of 0.037 for 4367 intensities above 3(I). The compound forms a dinuclear complex with distorted tetragonal-pyramidal geometry at each copper center. The unsymmetrical dimers are formed by weak axial coordination to one copper center by chloride ligands which are in the base plane of the adjacent copper atom. The apical Cu1-C12 and Cu2-C11 distances are 2.788(1) and 3.130(1) Å, respectively. The Cu1-Cu2 separation is 3.4995(3) Å in the dimers. A disorder of one five-membered chelate ring has been observed. Two alternative positionsa andb of the C26 atom were found and refined with constrained bond lengths. The geometry of the ligand and hydrogen bonds is discussed.     

Synthesis and Crystal Structure of Nickel(II) Complex with 2,2′-Biimidazole and 4-Aminobenzoic Acid

Abstract  The Ni(II) complex, [Ni(H₂biim)₂(PABA)₂]Cl₂·2H₂O, H₂biim being 2,2′-biimidazole, PABA being 4-aminobenzoic acid has been synthesized and the crystal structure determined using X-ray crystallography. The complex crystallizes in triclinic system, space group P − 1 with unit cell parameters a = 8.3920(9) ?, b = 9.8436(11) ?, c = 9.8874(11) ?, α = 94.862(2)°, β = 109.142(2)°, γ = 90.992(2)°, V = 767.95(15) ?³ and Z = 1. The molecules of the complex in the crystal assemble by way of N–H⋯Cl, O–H⋯Cl, O–H⋯O hydrogen bonds as well as π–π stacking interactions to provide a two-dimensional supramolecular structure. Index Abstract  Synthesis and Crystal Structure of Nickel(II) Complex with 2,2′-Biimidazole and 4-Aminobenzoic Acid Yanping Li and Pin Yang* The molecules of the title complex [Ni(H₂biim)₂(PABA)₂]Cl₂·2H₂O in the crystal assemble by way of N–H⋯Cl, O–H⋯Cl, O–H⋯O hydrogen bonds as well as π–π stacking interactions to provide a two-dimensional supramolecular structure.      

The Crystal Structure and Magnetic Susceptibility of Tetrakis-(μ2-phenylacetato-O,O′)-bis(caprolactam-O)copper(II)

Abstract  

Tetrakis-(μ₂-phenylacetato-O,O′)-bis(caprolactam-O)copper(II) (1) was synthesized and characterized by X-ray crystallography, magnetic susceptibility and FT-IR spectroscopy. The title compound (1) crystallized in the monoclinic space group P2₁/n with unit cell parameters a = 18.2242(4) ?, b = 10.0994(2) ?, c = 23.0696(5) ?, β = 101.117(2)°; V = 4166.37(15) ?³; Z = 4. The molecular structure of (1) consists of a copper dimer bridged by four phenylacetate ligands in the paddlewheel geometry with caprolactam coordinated in both axial sites. The copper dimers of (1) are organized into one-dimensional columns by N–H···O interactions between bound caprolactam ligands. Magnetic susceptibility studies indicate antiferromagnetic coupling between the Cu⁺² ions with a singlet ground-state and triplet excited-state separated by |2J = 319(1) cm⁻¹ |.     

Crystal and molecular structure of 2,6-dimethyl-3-acetyl-5-carbomethoxy-4- (4′-methoxyphenyl)-1,4-dihydropyridine

2,6-Dimethyl-3-acetyl-5-carbomethoxy-4-(4-methoxyphenyl)-1,4-dihydropyridine has been synthesized and characterized by X-ray diffraction analysis. The compound crystallizes in the monoclinic space group P2 ₁/c with cell parameters a=16.085(2) Å, b= 12.332(3) Å, c= 8.479(4) Å, = 99.23(8)°, Z=4. The structure exhibits both intra and intermolecular hydrogen bonds. The structure adopts a flat boat conformation in the dihydropyridine ring.     

Catena-Poly[[[2,4-dichloro-6-{[(2-hydroxyethyl)imino]methyl}phenolato-κ3N,O,O']-copper(II)]-μ-chlorido]monohydrate]: Synthesis,structural, spectroscopic and luminescent properties

A new chloride bridged polymeric Cu(II) complex, [Cu(HL)(μ-Cl).H₂O]_n, 1, (H₂L = 2,4-dichloro-6-{[(2-hydroxyethyl)imino]methyl}phenol) has been synthesized and characterized by elemental-spectral analysis, crystal structure analysis and photoluminescence measurements. The Copper(II) atom is five-coordinate in a slightly distorted square-pyramidal geometry (τ = 0.085), with one N and two O atoms of the Schiff base ligand and one Cl atom defining the basal plane and a symmetry-related Cl atom occupying the apical position. The bridging Cl atom lies in apical position for one Cu(II) ion and basal for the other, and it makes this structural arrangement unusual. The linked moieties form polymeric zigzag chains running along the c axis. This zigzag chains connect each other with intramolecular and intermolecular O–H···O hydrogen bonds, which form 3D structure through π?π interactions. Furthermore, the photoluminescence properties of H₂L and 1 were investigated, they exhibit unique bright green visible emissions in the solid state, under the excitation of 349 nm UV light. The strong luminescence emission of them makes 1 a potentially useful photoactive material in photo-physical chemistry.     

The properties,crystal, and molecular structure of catena-[(μ-acetato-) (μ-phthalazine)silver(I)dihydrate]: {[Ag(μ-O2CCH3) (μ-PHZ) (H2O)2]2}n

The crystal and molecular structure of catena-[(-acetato) (-phthalazine)-silver(I)dihydrate], {[Ag(O₂CCH₃) (C₈H₆N₂)(H₂O)₂]₂}_n, has been determined by single crystal X-ray analysis: the space group is P2₁/n,a=16.150(8) Å,b=3.886(5) Å,c=18.716(9) Å, =96.02(5)°,V=1168 ų. Phthalazine (PHZ) bridges the silver atoms to form {Ag--PHZ]₂ dimeric subunits. These dimeric subunits are planar and stack by bridging acetates to form a polymeric lattice. The acetates also form an asymrnetric chelate ring with the silver atoms which result in a distorted, square pyramidal configuration. The complex is further characterized by its IR and thermal properties.