Synthesis and Crystal Structure of 1,3-Bis(p-nitrophenoxy)propane

Abstract  The title compound 1,3-bis(p-nitrophenoxy)propane was synthesized by nucleophilic substitution of p-nitrophenol and 1,3-dibromopropane. Single crystal X-ray diffraction analysis reveals that the molecule in the solid state packs in the monoclinic P2/n space group with crystal cell parameters a = 17.465(5) ?, b = 4.8433(13) ?, c = 17.610(5) ?, β = 100.290(6)o, V = 1465.6(7) ?³, D_calc = 1.442 g/cm⁻³. Two half-molecules are located in the asymmetric unit which are each completed by twofold symmetry making Z = 4, Z′ = 1. Index Abstract  The title compound 1, 3-bis (p-nitrophenoxy) propane was prepared from p-nitrophenol and 1, 3-dibromopropane, crystallized from an ethanolic solution, and the structure was obtained by single crystal X-ray diffraction: monoclinic, P2/n, a = 17.465(5) ?, b = 4.8433(13) ?, c = 17.610(5) ?, β = 100.290(6)°, V = 1465.6(7) ?³.      

Structures of Bis(1-ethylbenzimidazol-2-yl)alkyl Copper(II) Dichlorides: An Unusual Cocrystallization

Abstract  Two structures containing pseudo-tetrahedral Cu(II)N₂Cl₂ coordination complexes are reported. The first molecular structure (A) of the compound, 1,1′bis(1-ethylbenzimidazol-2-yl)propane copper(II) dichloride (triEtBBIM)Cu(II)Cl₂, 1, is reported. The complex crystallized in the triclinic space group P-1 with a = 8.616(3) ?, b = 9.302(3) ?, c = 14.314(4) ?, α = 85.613(6)°, β = 85.170(6)°, γ = 66.117(6)° and V = 1044.1(5) ?³ with Z = 2. The second structure (B) contains 1 and (3,3′bis(1-ethylbenzimidazol-2-yl)pentane) copper(II) dichloride (tetEtBBIM)Cu(II)Cl₂, 2, both of which, cocrystallize in an equal molar ratio with a nitromethane solvate molecule. The complex crystallized in the monoclinic space group P2₁/c with a = 18.876(4) ?, b = 14.975(3) ?, c = 18.344(4) ?, β = 116.75(3)°, and V = 4630.3(16) ?³ with Z = 4. The cocrystallization of such discrete complexes has been coined a chemical Janus. Graphical Abstract  The title complexes contain pseudo-tetrahedral Cu(II)N₂Cl₂ coordination. One of the structures is the result of an unusual cocrystallization, in which two different discrete Cu(II) molecules cocrystallize in an equimolar ratio with a nitromethane solvate molecule.      

Phenylamido and Diphenylamido Complexes of Chromium(II)

Abstract  Addition LiNHPh to a [(NacNac)Cr(μ-I)]₂ [NacNac = 2,4 pentane-N-N′-bis(2,6-diisopropylphenyl) ketiminato] in THF yields a dimeric anilido complex, 1, that crystallizes in P2₁/n with unit cell parameters a = 13.390(2) ?, b = 26.298(5) ?, c = 21.326(4) ?, β = 93.905(4)°, V = 7492(2) ?³ and Z = 4. The same reaction in the presence of aniline yields a monomeric anilido complex, 2, with a coordinated aniline molecule. Complex 2 crystallizes in P2 ₁ /c with unit cell parameters a = 28.530(5) ?, b = 10.8116(18) ?, c = 26.492(5) ?, β = 115.685(3)°, V = 7364(2) ?³ and Z = 8. Addition of aniline to isolated 1 yields 2. Addition of LiNPh₂ to [(NacNac)Cr(μ-I)]₂ in THF yields a monomeric complex that crystallizes in P2₁/n with the unit cell parameters a = 11.152(6) ?, b = 23.820(12) ?, c = 17.915(9) ?, β = 106.223(9)°, V = 4569(4) ?³ and Z = 4. All complexes have been spectroscopically and structurally characterized. Graphical Abstract  Addition of LiNHPh or LiNPh₂ to [(NacNac)Cr(μ-I)]₂ yields a dimeric or a monomeric complex whereas addition of LiNHPh in the presence of aniline yields the monomeric anilido complex.      

Crystal Structures of a Series of 1,1-Spiro-bis(1,2,3,4-tetrahydronaphthalene)-Based Derivatives

Abstract  

The structures of four spirobisnaphthalenes based monomers 1, 2, 3a and 3b are reported. Each compound represents a methoxylated precursor which after deprotection led to the formation of a monomer successfully used for the synthesis of Polymers of intrinsic microporosity. The spiro-centre represents the site of contortion that, since its rigidity, leads to inefficient packing in the solid state inducing microporosity in the final polymer. Compound 1 crystallized in the monoclinic P2/c space group with unit cell parameters a = 8.1659(19) ?, b = 7.5298(18) ?, c = 19.130(5) ?, β = 97.935(4)°, V = 1165.0(5) ?³, Z = 2, D = 1.210 Mg m⁻³. Compound 2 crystallized in the monoclinic P2₁/n space group with unit cell parameters a = 12.6940(9) ?, b = 7.7267(6) ?, c = 19.9754(15) ?, β = 97.220(1)°, V = 1943.7(3) ?³, Z = 4, D = 1.355 Mg m⁻³. Compound 3a crystallized in the monoclinic P2₁/c space group with unit cell parameters a = 16.8137(14) ?, b = 10.5577(9) ?, c = 31.344(3) ?, β = 103.618(1)°, V = 5407.5(8) ?³, Z = 8, D = 1.308 Mg m⁻³. Compound 3b crystallized in the monoclinic Pc space group with unit cell parameters a = 15.594 ?, b = 12.564 ?, c = 18.339 ?, β = 90.224(1)°, V = 3593.0 ?³, Z = 4, D = 1.236 Mg m⁻³.     

Crystal Structure of 4,7-Dichloro-1,2,3,5,6,8-hexakis-(4-methoxy-phenylsulfanyl)-acenaphthylene

Abstract  The title compound was prepared from the reaction of perchloroacenaphthylene with an excess of sodium salt of 4-methyloxythiophenol in toluene/ethanol (1:1) solvent and structurally characterized by single-crystal X-ray diffraction. The compound crystallizes in the Monoclinic space group P2(1) with the parameters: a = 10.351(1) ?, b = 20.453(3) ?, c = 12.1837(16) ?, β = 105.584(3)°, V = 2484.5(6) ?³, with Z = 2 formula units. Graphical Abstract   The title compound 4,7-dichloro-1,2,3,5,6,8-hexakis-(4-methoxy-phenylsulfanyl)-acenaphthylene was synthesized from perchloroacenaphthylene C ₁₂ Cl ₈ with an excess of 4-methoxybenzene thiolate in toluene/ethanol (1:1) .     

The Crystal Structures of Some 1-Aryl-5-methyl-1,2,3-triazole Derivatives

Abstract  The two 1-aryl-5-methyl-1,2,3-triazole derivatives were prepared by the 1-aryl-5-methyl-1,2,3-triazol-4-carboxylic acids 3. The yielded products 4a–b were confirmed by NMR, MS, IR spectra. We investigated the crystalline structure of compounds 4a and 4b. Compound 4a, C₉H₈BrN₃, Mr = 238.09, crystallizes in the monoclinic space group P2(1)/n with unit cell parameters a = 11.660(2), b = 7.668(2), c = 11.818(2) ?, α = 90.00, β = 116.01(3), γ = 90.00o. V = 949.6(3) ?³, Z = 4, Dx = 1.665 Mg m⁻³. The final R was 0.0477. Compound 4b, C₁₃H₁₁N₃, Mr = 209.25, crystallized in the orthorhombic space group Pbca with unit cell parameters a = 10.373(2) ?, b = 11.691(2) ?, c = 17.579(4) ?, α = 90.00o, β = 90.00o, γ = 90.00o, V = 2131.8(7) ?³, Z = 8, D _m = 1.304 Mg m⁻³. The final R was 0.0565. Index Abstract  The two 1-aryl-5-methyl-1,2,3-triazole derivatives were prepared by the 1-aryl-5-methyl-1,2,3-triazol-4-carboxylic acids 3. The yielded products 4a–b were confirmed by NMR, MS, IR spectra. We investigated the crystalline structure of compounds 4a and 4b. Compound 4a, C9H8BrN3, Mr = 238.09, crystallizes in the monoclinic space group P2(1)/n with unit cell parameters a = 11.660(2), b = 7.668(2), c = 11.818(2)  ?, α = 90.00, β = 116.01(3), γ =90.00o. V = 949.6(3) ?³, Z = 4, Dx = 1.665 Mg m⁻³. The final R was 0.0477. Compound 4b, C13H11N3, Mr = 209.25, crystallized in the orthorhombic space group Pbca with unit cell parameters a = 10.373(2) ?, b = 11.691(2) ?, c = 17.579(4) ?, α = 90.00o, β = 90.00o, γ = 90.00o, V = 2131.8(7) ?³, Z = 8, D _m = 1.304 Mg m⁻³. The final R was 0.0565.      

Structural, Spectroscopic and Thermal Characterisation of bis (dibenzoylmethanato)Cd(II) Adducts with Dimethylsulfoxide and Water

Abstract  Adducts of cadmium(II) dibenzoylmethate, Cd(dbm)₂X₂ (X = DMSO, H₂O) were synthesized and analyzed by thermogravimetric analysis (TGA), differential-scanning calorimetry (DSC), hot-stage microscopy (HSM), single crystal X-ray diffraction, FTIR and Raman spectroscopy, and elemental analysis. Products obtained by thermal decomposition of the two Cd(II) complexes in oxygen, were used for quantitative analysis of cadmium in the adduct molecules. Single-crystal X-ray diffraction analysis of the DMSO adduct revealed that it has cis configuration. The DMSO adduct crystallizes in P2₁/a space group, a = 17.2494(6) ?, b = 8.3251(4) ?, c = 22.2746(9) ?, β = 93.836(3)°, V = 3191.53(7) ?³, Z = 4. Graphical abstract   Structural, Spectroscopic and Thermal Characterisation of bis (dibenzoylmethanato)Cd(II) Adducts With Dimethylsulfoxide and Water Ivan Halasz, Michaela Horvat, Tomislav Biljan, Ernest Meštrović Two adducts of bis(dibenzoylmethanato)Cd(II), Cd(dbm)₂X₂ (X = DMSO, H2O) have been synthesized and characterized.      

Pentacarbonyl(trimethylamine)chromium and Pentacarbonyl(trimethylamine)Molybdenum

Abstract  

Pentacarbonyl(trimethylamine)chromium (1) and pentacarbonyl(trimethylamine)molybdenum (2) are isomorphous and crystallize in the space group P2₁/n, a = 6.8267(14) ?, b = 11.269(2) ?, c = 14.692(3) ?, β = 102.89(3)°, V = 1,101.8(4) ?³, Z = 4 for 1 and a = 6.949(5) ?, b = 11.362(5) ?, c = 14.927(5) ?, β = 102.639(5)°, V = 1,150.0(10) ?³, Z = 4 for 2; both compounds possess distorted octahedral molecular geometries that result from the steric influence of the coordinated amine ligand.     

The Synthesis and Structure of Two Novel <Emphasis Type="Italic">N</Emphasis>-(Benzothiazol-2-yl)benzamides

Abstract  Two novel benzothiazoles 2-chloro-N-(benzothiazol-2-yl)benzamide (1) and 2-chloro-N-(6-cyanobenzothiazol-2-yl)benzamide (2) were obtained in multistep synthesis. They were characterised by means of IR, ¹H- and ¹³C-NMR spectroscopy and also by single-crystal X-ray diffraction. The compound 1 crystallises with triclinic space group P , a = 9.5923(8) ?, b = 9.8583(8) ?, c = 13.8962(10) ?, α = 89.162(6)°, β = 77.741(7)°, γ = 80.064(7)°, V = 1264.5(2) ?³, Z = 4 and compound 2 crystallises as methanol solvate with monoclinic space group P 2₁/n, a = 7.5093(9) ?, b = 13.0211(14) ?, c = 16.032(2) ?, β = 92.717(10)°, V = 1565.9(3) ?³, Z = 4. Both crystal structures consist of discrete dimers connected into a three-dimensional network by intermolecular C–H···O and C–H···X (X = Cl or S) hydrogen bonds and by face-to-face π–π stacking interactions. Index Abstract  The synthesis and structure of two novel N-(benzothiazol-2-yl)benzamides. Irena Ćaleta, Dominik Cinčić, GraceKarminski-Zamola and Branko Kaitner. Hydrogen bonds and π–π interactions in N-(benzothiazol-2-yl)benzamides N-(benzothiazol-2-yl)benzamides.      

Synthesis,Characterization and Crystal Structure of Iridium(III)bis(2-<Emphasis Type="Italic">p</Emphasis>-tolyl-benzothiazolato-N,C<Superscript>2</Superscript>)(acetylacetonate)

Abstract  A novel thiazole-based iridium (III) complex (iridium(III)bis(2-p-tolyl-benzothiazolato-N,C²)(acetylacetonate)) has been prepared and fully characterized by EA, IR, ¹H-NMR and MS. The molecular structure of the complex has been determined by single crystal X-ray diffraction analysis. The iridium (III) center adopts a distorted octahedral geometry with cis-O–O, cis-C–C, and trans-N–N chelate disposition. The complex crystallizes in the orthorhombic Pbca space group with cell parameters a = 10.1388(7) ?, b = 18.3565(12) ?, c = 31.021(2) ?, α = β = γ = 90 ° and Z = 8. The electronic absorption and emission spectra of this complex have been investigated. Index Abstract  A novel thiazole-based phosphorescent iridium (III) complex (iridium(III) bis (2-p-tolyl-benzothiazolato-N,C²)(acetylacetonate)) has been prepared and fully characterized by EA, IR, ¹H-NMR, MS and X-ray diffraction analysis.     

Synthesis and Crystal Structure Analysis of Thiourea-Pendant Pyridines

Abstract  The crystal structures of pyridine containing thiourea moieties as substituents, (1) and (2), have been determined. The ortho-substituted pyridine (1) crystallized in monoclinic space group P2₁/c with a = 16.091(3) ?, b = 11.368(2) ?, c = 7.4364(14) ?, β = 100.489(4)o, V = 1337.5(4) ?³, z = 4. In this structure an intramolecular N–H···N hydrogen bond forms a pseudo-seven-membered ring. The meta-substituted pyridine (2) crystallized in monoclinic space group P2₁/c with a = 14.5408(15) ?, b = 8.8508(9) ?, c = 10.7959(11) ?, β = 106.435(2)o, V = 1332.6(2) ?³, z = 4. Crystal packing revealed that compounds (1) and (2) can form dimeric structures via intermolecular H-bonding using N–H···S and N–H···N interactions, respectively. Graphical Abstract  Varying the substituent position on the pyridine ring using thiourea moieties gave unique molecular aggregations in solid state structures.      

Synthesis and Structure of cis-Dioxo(3-Methoxysalicylaldehyde 4-Methylthiosemicarbazonato-N,O,S)(γ-Picoline-N)Molybdenum(VI)

Abstract  Red crystals of cis-dioxo(3-methoxysalicylaldehyde 4-methylthiosemicarbazonato-N,O,S)(γ-picoline-N)molybdenum(VI), [MoO₂L(γ-pic)], [L²⁻=CH₃OC₆H₄(O)CH=NN=C(S)NHCH₃, 3-methoxysalicylaldehyde 4-methylthiosemicarbazonato] were prepared by the reaction of [MoO₂L] _n with γ-picoline in dry methanol. The title compound crystallized in the monoclinic space group P2₁/n, a = 6.7984(7) ?, b = 15.9760(12) ?, c = 17.1466(14) ?, β = 93.613(8)°, V = 1858.6(3) ?³, Z = 4. The coordination geometry around the molybdenum center is distorted octahedral with the tridentate thiosemicarbazonato ligand (L²⁻) bonded meridionally to the [MoO₂]²⁺ core. The sixth coordination site is occupied by a weakly bound γ-picoline molecule. The adjacent molecules are joined by the N–H···O hydrogen bonds between their amino and methoxy groups thus forming infinite molecular chains. The three-dimensional solid-state structure is achieved by the additional C–H···O, C–H···π and van der Waals interactions. Graphical Abstract  In the title compound, [MoO₂L(γ-pic)], the tridentate thiosemicarbazonato ligand (L²⁻) is meridionally bound to the [MoO₂]²⁺ core, while a molecule of γ-picoline completes the distorted octahedral coordination around the metal atom.      

Structures of Eight Thio(semi)carbazones Derived from 2-Acetylpyrazine, 2-Acetythiazole and Acetophenone

Abstract  The structures of eight related thio(semi)carbazones are described. These are syn,1E-2-acetylpyrazine-3-thiosemicarbazone (1), syn,1E,4Z-2-acetylpyrazine-4-ethyl-3-thiosemicarbazone, (2) and syn,1Z-2-acetylpyrazine-4,4-dimethyl-3-thiosemicarbazone (3), syn,1E,4Z-2-acetylthiazole-4-phenyl-3-thiosemicarbazone (4), syn,1Z-phenyl-4,4-dimethyl-3-thiosemicarbazone (5), syn,1E,4Z-phenyl-4-methyl-3-thiosemicarbazone (6), syn,1E,4Z-phenyl-4-ethyl-3-thiosemicarbazone (7), syn,1E,4Z-2-acetophenone-5-(N-aminothionyl)-3-thiocarbazone (8). Crystal data: for 1: triclinic, P-1, a = 5.4053(10) ?, b = 7.435(3) ?, c = 11.772(4) ?, α = 81.70(3)°, β = 82.59(2)°, γ = 77.38(2)°, and Z = 2: for 2: triclinic, P-1, a = 7.322(3) ?, b = 7.8239(16) ?, c = 9.783(4) ?, α = 87.73(2)°, β = 79.46(3)°, γ = 80.41(2)°, and Z = 2; for 3: orthorhombic, Pnma, a = 13.5210(15) ?, b = 6.6914(5) ?, c = 11.7214(10) ?, and Z = 4; for 4: triclinic, P-1, a = 5.7058(7) ?, b = 9.8776(15) ?, c = 11.869(2) ?, α = 76.389(12)°, β = 86.364(13)°, γ = 88.322(12)°, and Z = 2; for 5: triclinic, P-1, a = 7.5362(3) ?, b = 8.6331(4) ?, c = 9.8753(4) ?, α = 91.401(4)°, β = 102.532(4)°, γ = 110.540(4)°, and Z = 2; for 6: monoclinic, P2(1)/c, a = 10.7178(4) ?, b = 5.5866(2) ?, c = 18.7647(9) ?, β = 104.392(5)°, and Z = 4; for 7: monoclinic, P2(1)/c, a = 8.9557(3) ?, b = 9.7418(4) ?, c = 13.6864(5) ?, β = 94.044(4)°, and Z = 4; for 8: triclinic, P-1, a = 9.8091(5) ?, b = 10.6173(4) ?, c = 16.4691(7) ?, α = 75.540(4)°, β = 80.305(4)°, γ = 65.192(4)°, and Z = 4. Structures 1, 2, 4, 5, 7, and 8 form intramolecular N4–H···N1 hydrogen-bonds. Structures 3 and 5 exist in the tautomeric form in which N1 is protonated. Graphical Abstract  Structures of thio(semi)carbazones were found to fall into two categories: those with intramolecular N4-H…N1 hydrogen-bonds, and those which show a tautomeric form in which N1 is protonated.      

Interesting Reactivity in the Thermolysis and Photolysis of 2,3-Diphenyl-1-naphthol

Abstract  2,3-Diphenyl-1-naphthol (1) undergoes two unexpected reactions under different conditions. Compound (1) was heated in DMSO-d₆ and underwent a Pummerer type thermal reaction to give two isomeric products, 1-(methylthio)methoxy-2,3-diphenyl naphthol-d₅ which crystallized in the space group with a = 7.1610(9) ?, b = 11.2795(15) ?, c = 12.8905(17) ?, α = 114.049(2)°, β = 96.589(2)°, and γ = 102.945(2)°, and 2-(methylthio)methyl-2,3-diphenyl 1(2H)-naphthalenone-d₅ which crystallized in the space group with a = 8.5981(5) ?, b = 10.4374(6) ?, c = 11.1078(6) ?, α = 78.748(2)°, β = 67.709(2)°, and γ = 83.184(2)°. Photolysis (254 nm) of (1) resulted in 2,2′,3,3′-tetraphenyl-1,1′-bi-2-naphthol which crystallized in the space group P2₁/c with a = 26.3616(11) ?, b = 10.1707(4) ?, c = 23.3376(9) ?, and β = 99.034(2)°. Graphical Abstract  When 2,3-diphenyl-1-naphthol was heated in DMSO-d₆ two unexpected isomers, 1-(methylthio)methoxy-2,3-diphenyl naphthol-d₅ and the racemate 2-(methylthio)methyl-2,3-diphenyl 1(2H)-naphthalenone-d₅ were produced. Photolysis in THF at 254 nm led to the unexpected product 2,2′,3,3′-tetraphenyl-1,1′-bi-2-naphthol. All structures were elucidated by X-ray crystallography.      

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

Abstract  The synthesis and crystal structure of 1,7-bis(4-chlorophenyl)-4-(1,3-dithiolan-2-ylidene)-1,6-heptadiene-3,5-dione is described. This compound is a curcuminoid analogue, configurationally symmetric about the C4–C5 atoms and also retains the two fold axis in the crystal phase. This compound crystallizes in the space group C2/c with unit cell parameters a = 19.203(1) ?, b = 13.147(1) ?, c = 8.801(1) ?, β = 112.99(1)°, with half a molecule in the asymmetric unit. The ketenedithioacetal functionality present between the carbonyl groups prevents the possibility of keto-enol tautomerization in this compound. The push-pull nature of the ketenedithioacetal functionality organizes the cinnamoyl groups parallel to each other. Index Abstract  The details regarding synthesis and crystal structure of the title compound which is a curcuminoid analogue is reported in this paper.      

A Facile Synthesis and Crystallographic Analysis of Seven Trityl Phosphorus Compounds and Two Nickel(II) Phosphine Side-Products

Abstract  The syntheses and X-ray analyses of triphenylmethyl (trityl=Tr) phosphorus compounds are reported and the structural similarities, differences and ³¹P chemical shifts compared. A series of seven trityl-substituted phosphorus-containing compounds have been characterized by single crystal X-ray diffraction. Ph₃CPPh₂, 1, a bulky P(III) compound crystallizes in the triclinic space group , a = 7.5624(6) ?, b = 9.5470(8) ?, c = 16.9722(14) ?, α = 83.4720(10)°, β = 80.541(2)°, γ = 68.1580(10)°, the borane complex of 1, 2, Ph₃CPPh₂(BH₃) crystallizes as monoclinic colorless crystals, P2₁/c, a = 10.0972(12) ?, b = 9.6955(12) ?, c = 25.197(3) ?, β = 90.258(2)°. The analogous methyl substituted, 3, Ph₃CPMe₂(BH₃) is monoclinic, C₂/c, a = 15.628(3) ?, b = 12.770(3) ?, c = 18.406(4) ?, β = 103.968(3)°. Compounds 4–7 are trityl substituted P(V) compounds: Ph₃CP(Ph)(O)(OH), 4, crystallizes in the triclinic space group , a = 8.9847(18) ?, b = 9.7443(19) ?, c = 12.786(3) ?, α = 72.045(3)°, β = 72.031(3)°, γ = 78.769(3)°. Esterification of 4 affords TrCP(O)(Ph)OBn 5, space group, P2₁/c, a = 7.9196(5) ?, b = 31.701(2) ?, c = 19.8062(13) ?, β = 99.7750(10)°. A phosphonate diester was also characterized, Ph₃CP(O)(OEt)₂, 6, triclinic, , a = 7.9521(17) ?, b = 9.2205(19) ?, c = 14.471(3) ?, α = 85.906(4)°, β = 83.031(4)°, γ = 68.283(4)°. Treatment of the trityl H-phosphinic acid, Ph₃CPO₂H_2, with elemental selenium yields yellow crystals of 7, [Ph₃CP(O)(OH)Se]_2, P2₁/c, a = 9.0603(4) ?, b = 22.3652(11) ?, c = 16.9134(7) ?, β = 107.035(2)°. In our efforts to isolate a nickel-phosphine complex, two Ni(II) complexes were crystallographically analyzed, [Ni(OP(H)Ph₂)₆]₂BF₄ ⁻ 8 and 9. Complex 8 with an uncoordinated BF₄ ⁻ ion crystallizes as yellow orthorhombic crystals, Pbca, a = 18.8247(12) ?, b = 18.5518(12) ?, c = 21.0976(14) ?, while crystals of 9 are trigonal, , a = b = 13.1545(12) ?, c = 68.461(9) ?. Graphical Abstract  The syntheses and X-ray analyses of triphenylmethyl (trityl=Tr) phosphorus compounds are reported and the structural similarities, differences and ³¹P chemical shifts compared.      

3-Methyl-3a,4-Dihydro-3H-Thiochromeno[4,3-c]isoxazol

Abstract  The crystal structure of the title compound, C₁₁H₁₁NOS, was determined by an X-ray diffraction analysis. The compound crystallizes in the monoclinic space group P2₁/c with cell parameters a = 10.533(2) ?, b = 12.7826(19) ?, c = 7.6491(17) ?, β = 107.997(17)^°, V = 979.5(3) ?³ and Z = 4. The S containing heterocycle adopts a sofa conformation, whereas the 5-membered ring adopts an envelope conformation. The crystal packing is characterized by weak C–H···N contacts and π-stacking interactions. Graphical Abstract  The title compound, 3-methyl-3a,4-dihydro-3H-thiochromeno[4,3-c]isoxazol was synthesized by an 1,3 dipolar cycloaddition reaction and its crystal structure determined. Single crystal X-ray diffraction analysis reveals that the aromatic 6-membered ring is planar, whereas the ring containing the S atom adopts a sofa conformation and the 5-membered ring an envelope conformation. The methyl group is in an equatorial position.      

Methoxyflavone Inhibitors of Cytochrome P450

Abstract  Cytochrome P450 enzymes are a superfamily of enzymes involved in the metabolism of endogenous compounds as well as xenobiotics. Due to the large number of reactions catalyzed by these enzymes and their importance in drug metabolism and carcinogenesis, they have been the focus of many studies over the years. Based on the knowledge that flavones are natural substrates of certain P450 enzymes (such as P450 1A2) involved in carcinogenesis, we have synthesized and studied a number of flavonoids as potential inhibitors of these enzymes. These compounds are structurally very similar to the natural flavone substrates of these enzymes but have methoxy substituents at various positions. Here we are reporting the synthesis, structural analysis, X-ray crystal structures, and preliminary inhibition studies of four methoxyflavones from this series. Crystallographic data: 2′-methoxyflavone, P-1, a = 7.2994(8) ?, b = 8.3322(7) ?, c = 10.8240(10) ?, α = 97.905(8)°, β = 92.779(10)°, γ = 111.105(8)°, V = 604.9(1) ?³; 3′-methoxyflavone, P2₁/n, a = 15.1313(16) ?, b = 3.9699(4) ?, c = 19.9454(16) ?, β = 91.673(8)°, V = 1197.6(2) ?³; 4′-methoxyflavone, P2₁/n, a = 16.451(12) ?, b = 3.881(1) ?, c = 19.529(16) ?, β = 106.65(1)°, V = 1195.1(4) ?³; 3′,4′-dimethoxyflavone, C2/c, a = 30.819(5) ?, b = 4.0857(7) ?, c = 26.100(3) ?, β = 124.21(1)°, V = 2717.6(7) ?³. Index Abstract  Methoxyflavone Inhibitors of Cytochrome P450 Michael McKendall, Tasha Smith, Kien Anh, Jamie Ellis, Terri McGee, Maryam Foroozesh, Naijue Zhu and Cheryl L. Klein Stevens* This paper is a report of the synthesis, structural analysis, X-ray crystal structures, and preliminary inhibition studies of 2′-methoxyflavone, 3′-methoxyflavone, 4′-methoxyflavone, and 3′,4′-dimethoxyflavone.

Spectroscopic Studies and Crystal Structure of 1-[(2,5-dioxopyrrolidin-1-yl)(phenyl) methyl] Thiourea

Abstract  A new mannich base 1-[(2,5-dioxopyrrolidin-1-yl)(phenyl)methyl] thiourea formed by the direct condensation of thiourea, succinimide and benzaldehyde has been synthesized. The structure of this mannich base has been elucidated on the basis of micro elemental analysis, IR, ¹H NMR, ¹³C NMR, Mass and UV–Visible Techniques. The crystal structure of the title compound C₁₂ H₁₃ N₃ O₂ S was determined. It crystallizes in the monoclinic system, space group P2₁/c with a = 10.8234 (7) ?, b = 6.0355 (5) ?, c = 19.3692 (14) ?, β = 100.540(3)°, Z = 4 and V = 1243.94 (16) ?³. The structure was solved by the full-matrix least squares on F ² and had a refined R value of 0.0465 for 1,964 observed reflections. The crystal structure is stabilized by strong intramolecular C–H···O, C–H···S interactions and inter molecular N–H···O and S···S interactions. Graphical Abstract  This paper describes the spectroscopic and crystallographic studies of the title compound which is essential in ascertaining the structure of this new compound.      

Crystal Structure of 2-{1-[(1-(2-Pyridinio)ethylidene)hydrazono]ethyl}pyridinium diperchlorate,the Product of Template Condensation in the Presence of Cr(III)

Abstract  In an attempt to synthesize a Cr(III) complex of 2′-[1-(2-pyridinyl)ethylidene]oxamohydrazide an azine product 2-{1-[(1-(2-pyridinio)ethylidene)hydrazono]ethyl}pyridinium diperchlorate was obtained by an electrophilic acyl substitution catalyzed by Cr(III). Its structure was determined by X-ray crystal analysis and showed significant changes in comparison to the corresponding unprotonated compound. The 2-{1-[(1-(2-pyridinio)ethylidene)hydrazono]ethyl}pyridinium diperchlorate crystallizes in the space group P2₁/n of the monoclinic crystal system with unit cell parameters a = 14.3809(3) ?, b = 24.1516(5) ?, c = 15.4471(3) ?, β = 99.930(2)°, V = 5284.74(19) ?³ and Z = 12, i.e. three molecules per asymmetric unit. Graphical Abstract  In the template condensation of the 2′-[1-(2-pyridinyl)ethylidene]oxamohydrazide in presence of the chromium(III) ion the 2-{1-[(1-(2-pyridinio)ethylidene)hydrazono]ethyl}pyridinium diperchlorate was obtained and characterized by NMR spectroscopy and X-ray crystallography. Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users.