Synthesis and Structural Characterization of (2,4-Diamino-5-(3′,4′,5′-Trimethoxybenzyl)Pyrimidine Copper (II)) Complex

Abstract  The reaction of Cu(OOCCH₃)₂·H₂O with (2,4-diamino-5-(3′,4′,5′-trimethoxybenzyl) pyrimidine (trimethoprim) in ethanolic solution at 80 °C affords the title complex which has been characterized by elemental, IR, and NMR (¹H and ¹³C).The crystal structure has been determined by single crystal X-ray diffraction. Compound 1 (C₃₆H₄₈Cu₂N₈O₁₄) is triclinic, space group P-1 with a = 7.2676(4) ?, b = 11.6721(7) ?, c = 12.8279(8) ?, α = 95.839(1)°, β = 93.456(1)°, γ = 105.541(1)°, Z = 1. Two copper atoms are coordinated directly to each other as well as are held together by four bridging aceto groups. Each copper atom is also bonded opposite the Cu–Cu vector to a trimethoprim molecule through the N(1) atom of the pyrimidine ring. Trimethoprim acts as a monodentate ligand through the pyrimidine nitrogen N(1) atom. The complex was screened for the activity against several bacteria, showing more activity against bacteria as compared to trimethoprim. Graphical Abstract  To enhance the activity of trimethoprim, its derivative was prepared and there bacterial activity against several bacteria was analyzed.      

Synthesis and Crystal Structures of Ternary Copper(II) Complex Containing Salicylaldehyde Schiff Base and 4,4′-Bipyridine

Abstract  A new ternary mixed-ligand complex [Cu₂(sal-glu)₂(bipy)(H₂O)₂] · (H₂O) (bipy = 4,4′-bipyridine and sal-glu = salicylaldehyde l-glutamic Schiff base) has been synthesized and characterized by X-ray diffraction. It crystallizes in the triclinic system, space group P-1 with a = 9.6199(13) ?, b = 9.9111(13) ?, c = 9.9167(13) ?. The amino acid Schiff base coordinates to the Cu(II) ion in a tridentate mode including phenol-hydroxyl oxygen, carboxyl oxygen and amide nitrogen atom, while the bipy coordinates in bidentate bridging mode linking two Cu(II) ions. The [Cu₂(sal-glu)₂(bipy)(H₂O)₂] units are linked into 1-D chain structure and the bipy molecules are interspersed into parallel sheets via intermolecular hydrogen bonds. The carboxyl oxygen atoms, phenolic oxygen atoms and water oxygen atoms are involved in the extensive intermolecular hydrogen bond network between the water molecules and phenol-hydroxyl oxygen atoms from salicylaldehyde derived ligand. Graphical Abstract  A new ternary mixed-ligand complex [Cu₂(sal-glu)₂(bipy)(H₂O)₂]·(H₂O) (bipy = 4, 4′-bipyridine and sal-glu = salicylaldehyde l-glutamic Schiff base) crystallizes in the triclinic system, space group P-1 with a = 9.6199(13) ?, b = 9.9111(13) ?, c = 9.9167(13) ?. The amino acid Schiff base coordinates to the Cu(II) ion in a tridentate mode including phenol-hydroxyl oxygen, carboxyl oxygen and amide nitrogen atom, while the bipy coordinates in bidentate bridging mode linking two Cu(II) ions. The [Cu₂(sal-glu)₂(bipy)(H₂O)₂] units are linked into 1-D chain structure and the bipy molecules are interspersed into parallel sheets via intermolecular hydrogen bonds. The carboxyl oxygen atoms, phenolic oxygen atoms and water oxygen atoms are involved in the extensive intermolecular hydrogen bond network between the water molecules and phenol-hydroxyl oxygen atoms from salicylaldehyde derived ligand.      

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.      

Synthesis and crystal structure of 1-(1′,3′-dimethyl-5′-chloropyrazol-4′-carbonyl′-3-(2′-chlorophenyl)-5-amino-4-cyanopyrazole

The title compound 1-(1,3-dimethyl-5-chloropyrazol-4-carbonyl)-3-(2-chlorophenyl)-5-amino-4-cyanopyrazole (C₁₆H₁₂Cl₂N₆O) has been synthesized and characterized by X-ray diffraction: Triclinic, space group P1, with a = 8.6712(8) Å, b = 9.5091(10) Å, c = 11.2170(11) Å = 71.531(2)°, = 84.683(2)°, = 74.099(2)° Z = 2; V = 843.7(14) ų. C(10), O(1), C(11), and N(2) atoms are coplanar with the average deviation of 0.0071 Å, which form 11.03° and 43.93° dihedral angles with pyrazole planes (I) and (II), respectively.     

Synthesis of 7,4′-Bis-(hydroxyl)-8,3′,5′-tris-(hydroxymethyl)isoflavone and Crystal Structure of its Ester

Abstract 7,4′-bis-(hydroxyl)-8,3′,5′-tris-(hydroxymethyl)isoflavone (I) and its ester were synthesized and examined by IR, element analysis and ¹H NMR. The crystal of 7,4′-bis-(acetyl oxide)-8,3′,5′-tris-(acetoxymethyl)isoflavone (II) was studied by X-ray diffraction. (II) crystallizes in the monoclinic with space group P2 ₁ /c. a = 17.987(3) ?, b = 17.972(3) ?, c = 8.4087(11) ?, β = 97.703(3)°, V = 2693.7(6) ?³ and Z = 4. The molecular structure of the ester consists of a benzopyranone moiety, a phenyl moiety, two acetyl oxides and three acetoxymethyl groups. Hydrogen bonds and aromatic stacking interactions link the ester into a two-dimensional structure. Index Abstract 7,4′-bis-(hydroxyl)-8,3′,5′-tris-(hydroxymethyl)isoflavone and its ester were synthesized and examined by IR, element analysis and ¹H NMR. The result of the ester’s crystal structure showed that hydrogen bonding and aromatic π–π stacking assemble the ester into a two-dimensional networking structure.      

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.     

Spectroscopic, Thermal and Structural Studies of Cocrystals of 2,2′-Diamino-4,4′-bis(1,3-thiazole) with 2,5-Bis(4-pyridyl)-3,4-Diaza-2,4-Hexadiene and 1,2-Bis(4-pyridyl)Ethylenediamine

Abstract  

Two cocrystals of 2,2′-diamino-4,4′-bis(1,3-thiazole) (DABTZ) with 2,5-bis(4-pyridyl)-3,4-diaza-2,4-hexadiene (bpdh) and 1,2-bis(4-pyridyl)ethylenediamine (bpen) {[(DABTZ)(bpdh)] and [(DABTZ)(bpen)], respectively} have been synthesized and characterized by elemental analysis, IR-, ¹H NMR-, ¹³C NMR spectroscopy and were studied by thermal analysis and X-ray crystallography. Self-assembly of these compounds in the solid state is likely caused by hydrogen bonding with minor contributions from π–π stacking, C–H···π and possibly charge transfer interactions.     

Synthesis,Characterization and Structural Conformation Studies of 2-Amino-3-ethoxycarbonyl-4-(4′-methoxy Phenyl)-4H-pyrano-[3,2-c]-chromene-6-methyl-5-one

2-amino-3-ethoxycarbonyl-4-(4′-methoxy Phenyl)-4H-pyrano-[3,2-c]-chromene-6-methyl-5-one was synthesized by the two-component reaction of 6-methyl-4-hydroxy coumarin with 4′-methoxy-2-cyano cinnamate, which was synthesized by Knoevenagel reaction with 88% yield. The compound obtained was characterized by spectroscopic techniques and confirmed by X-ray crystallographic studies. The crystallographic data analysis reveals that the title compound crystallizes in the triclinic space group \(P\overline{1}\) with cell parameters a = 7.7750(8) Å, b = 9.0310(6) Å, c = 15.6120(17) Å, α = 77.249(7)°, β = 115.860(3)°, γ = 70.139(7)°, V = 1,003.0(16) Å³ for Z = 4. The structure has been solved by direct methods and refined to R1 = 0.0552 for 3,164 observed reflections with I > 2 σ(I). The pyran ring is in a flattened boat conformation. The carbonyl group is oriented in a -synperiplanar(cis) conformation.

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A Cobalt(II) Polymer Constructed by N,N '-Bis(3-Pyridinecarboxamide)-1,4-Benzene: Synthesis and Structural Characterization

Crystallography Reports - Cobalt coordination polymer [Co(btec)0.5(3-bpcb)]n (H4btec is benzene-1,2,4,5-tetracarboxylic acid, 3-bpcb is N,N?'-bis(3-pyridinecarboxamide)-1,4-benzene) has...     

Synthesis and Structural Characterization of Dibromidobis(N,N′-dimethylthiourea-κS)cadmium(II) and Diiodidobis(N,N′-dimethylthiourea-κS)cadmium(II)

Abstract  

Cadmium(II) complexes, dibromidobis(N,N′-dimethylthiourea-S)cadmium(II), [Cd(Dmtu)₂Br₂] (1) and diiodidobis(N,N′-dimethylthiourea-S)cadmium(II), [Cd(Dmtu)₂I₂] (2), have been prepared and their structures have been determined by X-ray crystal structure analysis. Compound 1 crystallized in the monoclinic space group C2/c, and the metal ion is situated on a twofold rotation axis. Compound 2 also crystallized in a monoclinic space group, P2₁/c, but here the molecules have no crystallographic symmetry. In both compounds the cadmium atom is bonded to two halide ions and to two dimethylthiourea molecules through the sulfur atoms in a tetrahedral environment. The molecules are linked via N–H⋯Halide hydrogen bonds to form infinite one-dimensional chains in 1 and infinite two dimensional networks in 2. The complexes were also characterized by IR and NMR spectroscopy and the data are consistent with the structures of the compounds.     

Crystal structure of 2,5-cyclohexadien-4-one-spiro-3′-(2′-methylthio-5′,5′-dimethyl-1′-pyrroline)

The crystal structure of the pyrrole derivative 2,5-cyclohexadien-4-one-spiro-3′-(2′-methylthio-5′,5′-dimethyl-1′-pyrroline) is determined by X-ray diffraction. Two independent molecules have similar structures and close geometric parameters but differ in configuration of the pyrrole ring and orientation of the thiomethyl group with respect to the pyrrole ring.     

Synthesis,Spectral, Thermal and Structural Study of Monoaquabis(Acetylsalicylato-κO)bis(Nicotinamide-κN)Copper(II)

Abstract  

The compound has been formed by mononuclear [Cu(C₉H₇O₄)₂(C₆H₆N₂O)₂(H₂O)] units in which the metal ion as well as the water ligand lies on a twofold symmetry axis, so that only one acetylsalicylate ligand and one nicotinamide ligand are independent. The distortion from ideal five-coordinate geometries can be described best by the degree of trigonality τ. For a regular square-pyramidal (SQP) geometry the trigonality parameter is 0 and for a trigonal–bipyramidal (TBP) structure it increases to 1. The copper coordination geometry is that of a square pyramid (τ = 0.23), with the N atoms from nicotinamide ligands and the bonded carboxylate O atoms from acetylsalicylate ligands defining the quasi-planar square base. The apical site is occupied by the aqua ligand, a bond which coincides with the twofold symmetry axis and is thus exactly perpendicular to the basal plane. The thermal decomposition takes place in four steps: removing of moisture, dehydration of aqua ligand, the elimination of the nicotinamide (na) ligand and the decomposition of acetyl-groups and oxidation of salicylate ion ligands. In complex, all ligands are coordinated to the metal ion as monodendate. The IR spectra of the intermediate products showed similar results.     

Synthesis and mesomorphic properties of 2,4-bis(4′-n-pentyloxybenzoyloxy)- benzylidine-4″- n-alkoxyaniline

The synthesis and mesomorphic properties of a new series of 2,4-bis(4′-npentyloxybenzoyloxy)- benzylidine-4″ -n-alkoxyaniline (DC5An) are reported. The molecular structure of compounds was confirmed by FTIR, ¹H-NMR, ¹³C-NMR, mass spectroscopy and elemental analysis. The mesomorphic properties were studied by differential scanning calorimetry (DSC) and polarizing optical microscopy (POM) measurements. All compounds of the series exhibit nematic (N) and smectic C (SmC) phases. The first four homologues (DC5A1-DC5A4) display a N mesophase, whereas the highest homologues (DC5A5-DC5A10) exhibit an enantiotropic dimorphism N and SmC phases. The mesomorphic properties of the present series are compared and discussed with other structurally related series.     

5(2′Carboxy)phenylazo barbiturate diaqua copper(II) trihydrate: Characterization and crystal structure

The title compound has been synthesized and characterized by standard spectroscopic techniques and magnetic susceptibility measurements and its structure has been determined by monocrystal X-ray diffraction. The complex crystallizes in the monoclinic space groupP2₁/c in a cell of dimensionsa=11.432(3),b=6.927(2),c=21.289(8)Å,=106.54(4)°,V=1616.1(9)ų,D _c =1.758 Mg m^–3,D(flotation)=1.76 Mg m^–3,M _w =427.8, (CuK)=2.47 mm^–1,F(000)=876. The structure refined to a finalR of 0.041 for 1290 observed independent reflections. The copper atom is coordinated by the nitrogen atom of the azo group next to the phenyl ring, the oxygen atom of one of the carbonyl groups of the barbituric moiety and one of the oxygen atoms of the carboxylate, closing two six-member chelate rings. Two water molecules complete a typical 4+1 square-based pyramidal environment.     

Synthesis and Characterization of Two Pb(II) Complexes of 2,2′-dihydroxy,Dimethoxy-1,1′-binaphthyl-3,3′-dicarboxylic Acid

Two new complexes {[Pb(L¹)(DMSO)₂(H₂O)]·DMF}_n (1, L¹ = 2,2′-dihydroxy-l,l′-dinaphthyl-3,3′-dicarboxylate) and {[Pb(L²)(DMS O)·DMSO}_n (2, L² = 2,2′-dimethoxy-l,l′-dinaphthyl-3,3′-dicarboxylate) have been synthesized under mild conditions and structurally characterized. Crystal structural analysis reveals that complex 1 adopts a 1D infinite chain structure which forms 2D sheet by hydrogen bonds interactions. Complex 2 possesses a 2D sheet structure, which was further assembled into a 3D supramolecular network through the π-π weak interactions. IR spectra indicates the carboxyl group coordinates with the Pb²⁺ ion. TGA shows that complex 2 is highly thermally stable up to 120°C.     

Structural study of nitrovinylindoles: (I) 2-methyl-3-(2′-methyl-2′-nitrovinyl)indole and (II) 3-(2′-nitrovinyl)indole

Compound (I) is 2-methyl-3-(2-methyl-2-nitrovinyl)indole, C₁₂H₁₂N₂O₂,M _r=216.24, monoclinic,P2₁/n,a=16.710(1),b=7.627(1),c=17.646(1) Å,=104.8(1)°,V=2174.7(1) ų,Z=8.D _x=1.321 g cm^–3, MoK, =0.71073 Å,=0.858 cm^–1,F(OOO)=912, room temperature,R=0.061 for 1956 observed reflections. Compound (II) is 3-(2-nitrovinyl)indole, C₁₀H₈N₂O₂,M _r=188.18, monoclinic,P2₁/n,a=10.178(1),b=10.608(1),c=8.411(1) Å,=105.5(2)°,V=875.0(1) ų,Z=4,D _x=1.4284 g cm^–3, CuK, =1.5418 Å,=8.068 cm^–1,F(000)=392, room temperature,R=0.040 for 1330 observed reflections. Compounds (I) and (II) have a similar geometry, the only significant difference lying in the rotation of the nitrovinyl chain. This feature could be responsible for the difference in biological activity. In both compounds, the molecules are associated, forming charge-transfer complexes.     

Synthesis and Structural Characterization of Bis(μ2-Iodo)-Bis(Diethyl Ether)-(N-N′-(Bis(2,6-Diisopropylphenyl)Pentane-2,4-Diketiminato)-Lithium-Chromium, a Cr(II) (β-Diketiminato) Complex with a Coordinated LiI Salt

Abstract  Addition of CrI₂ to the lithium salt of N-N′-bis(2,6-diisopropylphenyl)-2,4-diketiminate in diethylether yields a Cr(II) iodide complex with a coordinated, solvated LiI salt. This complex is the intermediate in the synthesis of a bridging iodide complex that is itself a precursor to a side-on bridging dinitrogen complex. This complex crystallizes in the P2₁/n space group with the crystal cell parameters a = 12.3160(19) ?, b = 21.067(3) ?, c = 15.837(3)?, β = 96.767°, V = 4080.6(11) ?³ and Z = 4. Graphical Abstract  Addition CrI2 to the lithium salt of N-N′-bis(2,6- diisopropylphenyl)-2,4-diketiminate in diethylether yields a Cr(II) iodide complex with a coordinated, solvated LiI salt. Herein we report the spectroscopic and structural characterization. An erratum to this article can be found at