Synthesis and Crystal Structure of 1,7-Bis(4-methoxyphenyl)-4-(1,3-dithiolan-2-ylidene)-1,6-heptadiene-3,5-dione

Abstract  

The synthesis and crystal structure of 1,7-bis(4-methoxyphenyl)-4-(1,3-dithiolan-2-ylidene)-1,6-heptadiene-3,5-dione is described. This compound crystallizes in the space group P2₁ with unit cell parameters a = 14.207 ?, b = 7.752(1) ?, c = 19.473(1) ?, β = 91.00(3)°, with two molecules in the asymmetric unit. The ketenedithioacetal functionality present between the carbonyl groups prevents the possibility of keto-enol tautomerization in this compound. The cinnamoyl groups are organized parallel to each other due to the push–pull nature of the ketenedithioacetal functionality.     

Crystal Structure of 2-(2,2-Dibromovinyl)-1-methyl-1<Emphasis Type="Italic">H</Emphasis>-imidazole-4,5-dicarbonitrile

Abstract  

The crystal structure of 2-(2,2-dibromovinyl)-1-methyl-1H-imidazole-4,5-dicarbonitrile (C₈H₄Br₂N₄, Mr = 315.92) has been determined by single crystal X-ray diffraction analysis. The compound crystallizes in the monoclinic crystal system with space group P2₁/c and unit cell parameters: a = 15.144(2), b = 16.382(3), c = 8.267(1) ?, β = 95.76(2)^o and Z = 8. The final reliability index is 0.0297 for 2505 observed reflections. The two molecules of 2-(2,2-dibromovinyl)-4,5-dicyano-1-methylimidazole are localized in independent part of unit cell. The crystal packing is stabilized by C–H···N hydrogen bonds and Br···N intermolecular interactions.     

Novel Methyl 4,6-O-benzylidene-3-ketoglucopyranosid-fused γ-lactam: Synthesis and Crystal Structure

Abstract  

The title compound methyl 4,6-O-benzylidene-3-ketoglucopyranosid-fused γ-lactam was synthesized from 2-oxoglucopyranoside in one pot via multi-step reaction sequence under mild conditions. It was characterized by HRMS, ¹H and ¹³C-NMR, IR, elemental analysis and single crystal X-ray diffraction. The crystal belongs to orthorhombic P2(1)2(1)2(1) space group with unit cell parameters a = 6.1840 (12) ?, b = 10.372 (2) ?, c = 25.702 (5) ?, V = 1648.5 (6) ?³, Z = 4, D_c = 1.343 Mg/m³, λ = 0.71073 ?, μ(Mo Kα) = 0.102 mm⁻¹, F(000) = 704. X-ray diffraction analysis reveals that the compound adopts chair-chair conformation. The newly formed γ-lactam moiety is fused to glucopyranoside ring by C2 to form spirosugar. The crystal structure is stabilized by N–H···O2 hydrogen bond.     

Synthesis and Structure of a One-Dimensional Copper(II)–Potassium(I) Complex of (<Emphasis Type="Italic">S</Emphasis>)-2-Hydroxy-3-Phenylpropanoic acid

Abstract  

Evaporation of the mixture solution of Cu(ClO₄)₂·6H₂O, KOH and (S)-2-hydroxy-3-phenylpropanoic acid affords a Cu(II)–K(I) coordination compound 1. Single-crystal X-ray diffraction analysis reveals that 1 is a one-dimensional comb-like coordination polymer in the P2₁2₁2₁ space group with crystal cell parameters a = 10.989(2) ?, b = 15.939(3) ?, c = 22.511(5) ?, V = 3943(1) ?³ and Z = 4.     

Crystal and Molecular Structure of Rhaponticin from Rheum hotaoense

Abstract  

Rhaponticin was isolated from the rhizome and root of Rheum hotaoense C.Y. Cheng et C.T. Kao and its crystal structure was determined by single crystal X-ray diffraction. The compound compactly packs in a triclinic unit cell in the P1 space group with unit cell dimensions a = 5.1240(12) ?, b = 7.0453(17) ?, c = 14.535(4) ?, α = 83.182(3)°, β = 89.212(3)°, γ = 68.956(3)°, V = 1486.0(2) ?³, Z = 1, D _calcd = 1.436 Mg m⁻³ and F(000) = 222. The atoms of the stilbene moiety are nearly coplanar, and the dihedral angle between ring (C2–C7) and ring (C10–C15) is 9.0°. The O–H⋯O hydrogen bonding interactions link the molecules into a complicated 3D framework.     

Synthesis and Molecular Structure of Sulfur Containing Cobalt Compounds

Abstract  

The reaction of cobalt (II) chloride hexahydrate and N-tert-butyl-2-thioimidazole (tm^t-Bu) yielded products [k²-(tm^t-Bu)₂]CoCl₂ (1) and [(tm^t-Bu)₂Co₂(μ-tm^t-Bu)₂Cl₂]·CH₃CN (2) at different reaction time. The single crystal X-ray diffraction analysis was carried out for 1 and 2 {Bruker Kappa Apex-II CCD diffractometer, MoK_α radiation}. Crystal data for 1: orthorhombic P212121 unit cell a = 8.195(6) ?, b = 13.778(10) ?, c = 17.354(11) ? and V = 1960(2) ?³ whereas the compound 2 crystallizes in monoclinic system P21/c with unit cell a = 10.069(7) ?, b = 11.181(7) ?, c = 18.156 ?, β = 95.322(4)° and V = 2035.4(2) ?³. The complex 1 contains one dimensional chain running along the a-axis and the complex 2 contains one dimensional chain running along the b-axis due to existence of different types of intermolecular interaction. The change in structure of the product is directly related to the reaction time i.e. reaction for lesser time produces mononuclear product and for longer time produces binuclear compound.     

Synthesis, Crystal and Molecular Structure of 1-(2-Chlorobenzyl)-2-methylthio-1H-benzimidazole

Abstract  

1-(2-Chlorobenzyl)-2-methylthio-1H-benzimidazole compound has been synthesized and characterized by elemental analysis, IR and ¹H-NMR spectroscopy and single crystal X-ray diffraction. The compound crystallizes in the triclinic space group P-1 with unit cell parameters a = 17.201 ?, b = 5.873 ?, c = 24.791 ?, α = 67.410(10)°, β = 74.083(11)°, γ = 81.858(12)°. In the crystal packing, no classic hydrogen bonds are founded, but C–H···π interactions are being between the molecules. The molecular geometry and vibrational frequencies of (C₁₅H₁₃ClN₂S) in the ground state have been calculated by using Hartree–Fock (HF) and Density Functional Method (DFT/B3LYP) with 6-31G(d) basis set. The optimized geometric bond lengths and bond angles obtained by using HF and DFT (B3LYP) show the best agreement with the experimental data.     

Novel Assembly of a Cyanide-Bridged Copper(II)–Nickel(II) Binuclear Complex with a Copper(II) Macrocyclic Ligand

Abstract  

A mononuclear fragment [Cu(L)Cl]ClO₄ (1) and a cyano-bridged Cu^II–Ni^II binuclear complex [CuL][Ni(CN)₄]·0.25H₂O (2) (L = 1,3,6,8,11,14-hexaazatricyclo[12.2.1.18,11]-octadecane), have been prepared and characterized. X-ray single crystal analyses indicate that the both complexes crystallize in the monoclinic crystalline system. The complex of 1 in P1n1 space group with unit cell constants a = 6.1176(6) ?, b = 11.9147(10) ?, c = 12.2041(12) ?, β = 98.816(5)° and 2 in the P2₁/n space group with unit cell constants a = 8.1419(13) ?, b = 14.695(2) ?, c = 16.863(3) ?, β = 98.375(2)° have been revealed. The complex 2 assumes a binuclear structure in which the nickel(II) ion is in a square planar environment and the copper(II) is in a square-prism geometry environment.     

2,4-Pentane <Emphasis Type="Italic">N</Emphasis>,<Emphasis Type="Italic">N</Emphasis>′-Bis(2,6-Diisopropylphenyl) ketiminato cobalt (II) (trimethylsilyl)methylene

Abstract  

The title compound [^MeL^iPrCoCH₂Si(CH₃)₃ ^MeL^iPr = 2,4-pentane-N,N′-bis(2,6-diisopropylphenyl) ketiminato] possesses trigonal planar geometry and crystallizes in monoclinic space group P2₁/n with crystal cell parameters a = 10.6155(14) ?, b = 21.279(3) ?, c = 14.8057(19) ?, β = 97.196(2)°, V = 3,318.1(7) ?³, and Z = 4. The title compound is the second reported three coordinated 13 valence electron Co(II) alkyl complex and the first such complex reported with an asymmetrically bonded alkyl group. The steric effects are discussed in comparison of known similar structures of Fe, Co, and Zn.     

Synthesis and Crystallographic Study of <Emphasis Type="Italic">N</Emphasis>′-(1-benzylpiperidin-4-yl)acetohydrazide

Abstract  

As part of a study into new Fentanyl-derived opioid compounds with potent analgesic activity and reduced side effects the starting material title compound, C₁₄H₂₁N₃O (1), was synthesized and characterized by NMR spectroscopy and single-crystal X-ray diffraction. The crystal structure is monoclinic Cc with unit cell parameters a = 14.1480(3) ?, b = 14.1720(4) ?, c = 27.6701(7) ?, β = 96.956(1)°, α = γ = 90°. The compound has crystallized with four crystallographically unique molecules in the asymmetric unit; each molecule has a very similar conformation and an analysis of the structure shows that although all four unique molecules overlay very well there is no evidence of pseudo-symmetry which would relate the molecules in the higher symmetry space group C2/c. The crystal packing consists of two separate hydrogen bonded chains which are linked together to form a thick 2D structure in the ab plane.     

Crystal Structure of Tetraphenylarsonium Diisothiocyanatodichlorocobaltate(II)

Abstract  

Tetraphenylarsonium diisothiocyanatodichlorocobaltate(II) was synthesized by metathetic pathway. It crystallizes in the monoclinic space group C 2/c with unit cell parameters, a = 13.510(4) ?, b = 15.873(5) ?, c = 22.809(7) ?, β = 105.743(6)°, V = 1,618(5) ?³ and Z = 4. X-ray crystal structure analysis reveals that the asymmetric unit contains one {(C₆H₅)₄As}⁺ cation and one half {Co(NCS)₂Cl₂}²⁻ anion, the latter lying on a crystallographic twofold axis. While each {Co(NCS)₂Cl₂}²⁻ anion exhibits hydrogen bonding interactions with eight arsonium cations; CH···π interactions between phenyl rings of arsonium cations is restricted to two such centers in the crystal structure.     

Syntheses,Characterization and Crystal Structures of <Emphasis Type="Italic">N′</Emphasis>-(5-Chloro-2-Hydroxybenzylidene)-4-Dimethylaminobenzohydrazide and <Emphasis Type="Italic">N′</Emphasis>-(2,4-Dichlorobenzylidene)-4-Dimethylaminobenzohydrazide

Abstract  

The hydrazone compounds, N′-(5-chloro-2-hydroxybenzylidene)-4-dimethylaminobenzohydrazide (1) and N′-(2,4-dichlorobenzylidene)-4-dimethylaminobenzohydrazide (2), have been synthesized by the condensation reaction of equimolar quantities of 4-dimethylaminobenzohydrazide with 5-chlorosalicylaldehyde and 2,4-dichlorobenzaldehyde, respectively, in methanol. The compounds were characterized by elemental analysis, IR, ¹HNMR spectra, and single crystal X-ray diffraction. Compound 1 crystallizes in the monoclinic space group C2/c with unit cell dimensions a = 35.014(3) ?, b = 10.407(2) ?, c = 18.505(2) ?, β = 112.046(2)°, V = 6250.0(15) Ǻ³, Z = 16, R ₁ = 0.0624, and wR ₂ = 0.1187. Compound 2 crystallizes in the triclinic space group P-1 with unit cell dimensions a = 12.625(2) ?, b = 12.688(3) ?, c = 13.005(2) ?, α = 101.271(2)°, β = 112.945(1)°, γ = 104.966(2)°, V = 1747.6(6) Ǻ³, Z = 2, R ₁ = 0.0523, and wR ₂ = 0.1138. In the asymmetric unit of each compound, there exists two hydrazone molecules linking together by an N–H⋯O hydrogen bond. Furthermore, compound (2) contains one methanol molecule and one water molecule of crystallization.     

Synthesis, Crystal Structures and Fluorescence Property of Bis(benzimidazol-2-yl)methane Dichloride

Abstract  

The title compound, a salt of C₁₅H₁₃N₄ ²⁺2Cl⁻, was synthesized and determined by X-ray crystallography. It crystallizes in the orthorhombic system, space group Pbcn, with lattice parameters a = 9.973(2) ?, b = 9.5012(19) ?, c = 15.574(3) ?, V = 1475.8(5) ?³, Z = 4, C₁₅H₁₃Cl₂N₄, Mr = 320.19, Dc = 1.441 g/cm³. In the crystal structure, the Cl⁻ anion interact with the same benzimidzaole through two kinds of hydrogen bonds forming a 1D hydrogen-bonded chain, two 1D hydrogen-bonded chain cross with each other and form 2D layer structure. The EA, UV, IR and TG-DTG were studied and the possible structures of the title compound were speculated. Moreover, the fluorescence of the title compound was studied. The results reveal that it can emit purple fluorescence in DMF solvent.     

Structural Characterization of New Compound from the Ring-Opening Reaction of 3-(1H-1,2,4-triazol-1-yl)-1,5-Benzothiazepine with Phenylonitrile Oxide

Abstract  

The crystal structure of the product (Z)-2-((Z)-((Z)-1,3-diphenyl-2-(1H-1,2,4-triazol-1-yl)allylidene)amino)phenyl N-hydroxybenzimidothioate (4) was obtained by single crystal X-ray diffraction. The title compound, C₃₀H₂₃N₅OS (4), crystallizes in the triclinic space group, P-1, with unit cell parameters a = 8.3306(17) ?, b = 11.394(2) ?, c = 14.560(3) ?, α = 78.75(3)o, β = 89.96(3)o, γ = 70.56(3)o, Z = 2. In the crystal structure, adjacent molecules are linked by O–H···N hydrogen bonds. H-bonds and π–π stacking are the main non-bonding interactions in the molecular structure and give support to molecular packing stability. In addition, the structure is supported by a weak intermolecular C–H···Cg π-ring interaction. Detail of the synthesis, structures, and spectroscopic properties of the title compound is discussed.     

Syntheses, Crystal Structures and Antibacterial Activities of Two Antipyrine Derivatives

Abstract  

Two new antipyrine derivatives, 4-{[1-(5-bromo-2-methoxyphenyl)methylidene]amino}-1,5-dimethyl-2-phenyl-2,3-dihydro-1H-pyrazol-3-one (C₁₉H₁₈BrN₃O₂, 1) and 4-{[1-(2-hydroxy-3-ethoxyphenyl)methylidene]amino}-1,5-dimethyl-2-phenyl-2,3-dihydro-1H-pyrazol-3-one (C₂₀H₂₁N₃O₃, 2), were synthesized and structurally characterized by elemental analysis, IR and single crystal X-ray diffractions. Compound 1 crystallizes in the monoclinic space group P2₁/n with unit cell dimensions a = 6.987(1) ?, b = 27.930(2) ?, c = 9.483(1) ?, β = 109.36(2)°, V = 1745.9(4) ?³, Z = 4, R ₁ = 0.0430, and wR ₂ = 0.0870. Compound 2 crystallizes in the monoclinic space group P2₁/c with unit cell dimensions a = 19.523(2) ?, b = 7.466(1) ?, c = 12.954(2) ?, β = 108.797(1)°, V = 1787.5(4) ?³, Z = 4, R ₁ = 0.0421, and wR ₂ = 0.1032. X-ray structure determinations revealed that the molecules of both compounds display trans configurations about the C=N double bonds. In the crystal structures, molecules are linked together by intermolecular C–H···O hydrogen bonds. Both compounds show strong antibacterial activities.     

Synthesis,Structure, and Two Polymorphs of 4-((1,3-Dioxoisoindolin-2-yl)methyl)-1-methoxypyridinium tetrafluoroborate

Abstract  

4-((1,3-Dioxoisoindolin-2-yl)methyl)-1-methoxypyridinium tetrafluoroborate, C₁₅H₁₃BF₄N₂O₃, 1, was obtained by alkylation of the corresponding N-oxide and has been characterized by ¹H and ¹³C NMR, IR, UV spectroscopy and by X-ray crystallography. The crystal undergoes a reversible phase transition between 173 and 293 K. At room temperature, crystals are orthorhombic, space group Pna2₁ with a = 7.2487(3) ?, b = 17.8359 (8) ?, c = 12.4077(6) ?, V = 1604.16(12) ?³, and Z = 4. At 173 K, cations adopt four conformations in monoclinic space group Cc with a = 24.7076(29) ?, b = 14.4145(9) ?, c = 21.8765(25) ?, β = 126.249(17)°, V = 6283.3(7) ?³, and Z = 16. The compound is photostable in the crystal and does not undergo homolytic N–O bond cleavage as observed in solution.     

Hydrogen Bonding Patterns in Trimethoprimium Cinnamate 1.52 Hydrate

Abstract  

In the title compound, [C₁₄H₁₉N₄O₃ ⁺, C₉H₅ O₂ ⁻, H₂O, O0.52] the asymmetric unit contains a protonated trimethoprim cation and a cinnamate anion and two water molecules. The crystal structure was determined by single crystal X-ray diffraction. This compound crystallized in the triclinic system; space group P−1 with the unit cell parameters a = 10.010(2) ?, b = 10.339(3) ?, c = 13.486(8) ?, α = 105.32(3)°, β = 109.88(3)°, γ = 100.89(3)°, V = 1204.6(10) ?³, Z = 2. The cinnamate group is disordered. The trimethoprim (TMP) molecule is protonated at one of the pyrimidine nitrogen atoms. The carboxylate group of the cinnamate anion interacts with the protonated pyrimidine atom N1 and the 2-amino group via a pair of N–H···O hydrogen bonds, generating the R₂²(8) ring motif. The inversion related TMP cations are paired via N–H···N hydrogen bonds. In addition to the base pairing, the O1W atom bridges the 2-amino and 4-amino groups on either side of the paired bases, resulting in a self complementary DADA array. Two inversion related TMP cations and water molecules (O1W) are linked via N–H···O and O–H···O hydrogen bonds, forming a 22 membered ring with graph-set R₄⁴(22).     

Structural Consequences of Anomeric Effect in 1,3,6,8-tetraazatricyclo[4.3.1.13,8]undecan-1-ium pentachlorophenolate monohydrate

Abstract  

The asymmetric unit of the crystal structure contains one molecule of the title compound and one molecule of water. X-ray diffraction spectrum of the ammonium salt of title compound exhibits deviations from the ideal molecular geometry which is explained on the basis of anomeric effect. This conclusion is consistent with the natural bond orbital analysis at the B3LYP/6-311+G** level of the anomeric effect. The molecules are linked via N–H···O hydrogen bonds. This compound crystallizes in monoclinic symmetry, in space group P2 _1/n , with lattice constants: a = 12.3850(2) ?, b = 6.8123(1) ?, c = 19.6208(4) ?, α = 90°, β = 94.864(2)°, γ = 90°, V = 1649.45(5) ?³, Z = 4, F(000) = 896, R ₁ = 3.3%, wR ₂ = 10.6%.     

Synthesis and Crystal Structure of [Te{S(C<Subscript>6</Subscript>H<Subscript>3</Subscript>S)<Subscript>2</Subscript>O}]: A Tetracyclic Tellurium(II) Compound Displaying a Boat–Chair Conformation

Abstract  

The synthesis and molecular structure of (phenoxathiin-4,6-dithiolate)tellurium(II) is described. [Te{S(C₆H₃S)₂O}] was synthesized from the reaction of 4,6-dimercaptophenoxatiin and TeCl₄ in 36% yield. The crystal structure was determined by single crystal X-ray diffraction analysis. Crystal data: [Te{S(C₆H₃S)₂O}], formula weight = 389.95, crystallized in monoclinic system, space group P2(1)/n with a = 7.7898(10) ?, b = 18.513(2) ?, c = 8.9898(11) ?, β = 105.974(2)°, V = 1246.4(3) ?³ and Z = 4. The tetracyclic compound is non-planar with a di-coordinate Te^II atom. The eight-membered central ring is in a boat–chair conformation. The title compound displays weak intermolecular contacts Te–S, S–S and C–H⋯S.     

Synthesis and Crystal Structures of Two Polymorphs of Trilanthanum Iridium Septaoxide (La<Subscript>3</Subscript>IrO<Subscript>7</Subscript>)

Abstract  

Two polymorphs of trilanthanum iridium septaoxide, La₃IrO₇, were prepared as single crystals using a molten cesium hydroxide flux and were structurally characterized using single-crystal X-ray diffraction. Polymorph A crystallizes in the orthorhombic space group Cmcm with unit cell dimensions of a = 11.2103(3) ?, b = 7.4982(2) ?, and c = 7.6110(2) ?. Polymorph B crystallizes into the monoclinic space group P2₁/n with the unit cell dimensions of a = 8.8512(5) ?, b = 5.7167(3) ?, c = 24.4454(13) ?, and β = 95.542(2)°. The crystal structure of polymorph A is isostructural to the family of compounds with formula Ln₃MO₇ (M = Nb⁵⁺, Mo⁵⁺, Ru⁵⁺, Ta⁵⁺, Re⁵⁺, Os⁵⁺, and Ir⁵⁺) while the crystal structure of polymorph B has no known corollaries.