Synthesis,Crystal Structure and Thermal Properties of <Emphasis Type="Italic">N</Emphasis>-Acetyl-3-(2-furyl)-5-ferrocenyl-2-pyrazoline and <Emphasis Type="Italic">N</Emphasis>-Acetyl-3-(2-thienyl)-5-ferrocenyl-2-pyrazoline

Abstract  

Two novel ferrocenyl substituted N-acetyl-2-pyrazolines, N-acetyl-3-(2-furyl)-5-ferrocenyl-2-pyrazoline (3) and N-acetyl-3-(2-thienyl)-5-ferrocenyl-2-pyrazoline (4), have been synthesized and characterized by FTIR, ¹H-NMR, ¹³C-NMR techniques, elemental analysis and X-ray structure analysis. Thermal properties of these compounds have been determined by TGA, DTA and DSC analysis. Compound 3 (C₁₉H₁₈N₂O₂Fe) crystallizes in the monoclinic space group P21/c and Z = 4, with a = 8.6970(4) ?, b = 18.4725(9) ?, c = 11.0041(5) ?, β = 110.942(3)°. Compound 4 (C₁₉H₁₈N₂OSFe) crystallizes in the orthorhombic space group Fdd2 and Z = 16, with a = 84.242(2) ?, b = 13.5416(5) ?, c = 5.9405(2) ?, β = 90°. In terms of crystal packing, each compound shows different molecular arrangement, which are stabilized by C–H···O intermolecular weak hydrogen bonds, and/or C–H···π interactions.     

Synthesis,Characterization and Antibacterial Activity of <Emphasis Type="Italic">N</Emphasis>-(<Emphasis Type="Italic">N</Emphasis>-Acetic Acid-yl-Phthalimide-5-yl) Maleamic Acid Dihydrate

Abstract  

The compound N-(N-acetic acid-yl-phthalimide-5-yl) maleamic acid (C₁₄H₁₀N₂O₇, M _r  = 318) was synthesized and its structure was characterized by elemental analysis, ¹H NMR and IR spectra. The single crystal of the title compound (C₁₄H₁₄N₂O₉, M _r  = 354.27) was cultured and its structure was determined by single crystal X-ray diffraction. The crystal belongs to monoclinic system, space group P21/c with a = 14.3859(19), b = 12.5835(18), c = 8.6934(15) ?, β = 102.824(2)°, V = 1534.5(4) ?³, Z = 4, D _c  = 1.534 g cm⁻³, μ(Mo Kα) = 0.131 mm⁻¹, F(000) = 736. The final refinement gave R = 0.0652, wR(F ²) = 0.1239 for 2,703 observed reflections with I > 2σ(I). X-ray diffraction analysis reveals that the asymmetric unit of the title compound contains one N-(N-acetic acid-yl-phthalimide-5-yl) maleamic acid molecule and two water molecules. One of the two water molecules is disordered. The phthalimide group is essentially planar. The crystal structure of the title compound is stabilized by N–H…O and O–H…O hydrogen bonds interactions. The compound N-(N-acetic acid-yl-phthalimide-5-yl) maleamic acid possesses moderate antibacterial activity.     

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 and Crystal Structure of Bis(<Emphasis Type="Italic">N</Emphasis>-alkyl-<Emphasis Type="Italic">N</Emphasis>-phenyl dithiocarbamato)mercury(II)

Abstract  

The mixed ligand dithiocarbamate complex was synthesized by the reaction between the ammonium salt of the dithiocarbamate ligands with mercury salt. There are two mercury complexes in the asymmetric unit with a compositional disorder between an ethyl group and a methyl group. A distorted tetrahedral geometry is found for each mercury atom defined by four sulphur atoms derived from two asymmetrically chelating dithiocarbamate ligands. IR spectra show thioureide υ(C–N) bands at 1491 cm⁻¹ which is higher than observed in the simple complexes of the same ligands. The effect of alkyl substituents were observed in the magnetic unequivalence of the thioureide and phenyl units in the NMR spectroscopy. The molecules are related to each other by virtue of the compositional disorder which exists at three positions in the alkyl group across the unit. The compound crystallizes in the triclinic space group P-1 with a = 10.4764(10) ?, b = 11.0433(10) ?, c = 18.5566(17) ?, α = 97.8980(10)^°, β = 95.3340(10)^°, γ = 110.3010(10)^°, and Z = 2.     

Spectral and X-ray Diffraction Studies of <Emphasis Type="Italic">N</Emphasis>-(2-Nitrophenyl)-5-Phenyl-1,3,4-Oxadiazole-2-Amine

Abstract  

Thiosemicarbazides and their derivatives are well known for their use in biological activity and many applications in pharmaceutical and industrial fields. The cyclization of 1-benzoyl-4-(2-nitrophenyl)-3-thiosemicarbazide (BNPTSC) in dimethylformamide (DMF) medium furnished N-(2-nitrophenyl)-5-phenyl-1,3,4-oxadiazole-2-amine (NPPOA). The chemical structure of the above substituted 1,3,4-oxadiazole has been assigned by IR, mass and X-ray diffraction studies. The XRD studies reveal the presence of four types of hydrogen bonds (N–H···O, N–H···N, C–H···O, C–H···N) in the crystal packing. The crystal system was found to be orthorhombic with a space group Pca2(1) and the unit cell dimensions are: a = 26.873(3) ?, b = 6.0827(7) ?, c = 7.8502(10) ?, α = 90°, β = 90°, γ = 90° and Z = 4.     

Synthesis,Characterization and Antibacterial Activity of <Emphasis Type="Italic">N</Emphasis>-(2,3,4-Trimethoxy-6-methylbenzylidene)-2-methyl-benzenamine

Abstract  The title compound N-(2,3,4-trimethoxy-6-methylbenzylidene)-2-methyl-benzenamine (C₁₈H₂₁NO₃, M _r = 299.36) was synthesized and characterized by elemental analysis, IR spectra and single crystal X-ray diffraction. The crystal belongs to monoclinic, space group P2₁/n, with a = 7.2804(5), b = 8.5909(9), c = 26.117(3) ?, β = 92.056(2)°, V = 1,632.4(3) ?³, Z = 4, D _c = 1.218 g cm⁻³, λ = 0.71073 ?, μ(Mo Kα) = 0.083 mm⁻¹, F(000) = 640. The final refinement gave R = 0.0497, wR(F ²) = 0.1157 for 2,879 observed reflections with I > 2σ(I). X-ray diffraction analysis reveals that the dihedral angle between the two phenyl rings is 25.9 (2)°. The molecule adopts a trans configuration about the central C=N functional bond. The crystal structure is stabilized by C–H…O hydrogen bonds and π–π stacking interactions. The title compound possesses moderate antibacterial activity. Graphical Abstract  The title compound N-(2,3,4-trimethoxy-6-methylbenzylidene)-2-methyl-benzenamine (C₁₈H₂₁NO₃, M _r = 299.36) was synthesized and characterized by elemental analysis, IR spectra and single crystal X-ray diffraction. The crystal belongs to monoclinic, space group P2₁/n, with a = 7.2804(5), b = 8.5909(9), c = 26.117(3) ?, β = 92.056(2)°, V = 1,632.4(3) ?³, Z = 4, D _c = 1.218 g cm⁻³, λ = 0.71073 ?, μ(Mo Kα) = 0.083 mm⁻¹, F(000) = 640. The final refinement gave R = 0.0497, wR(F ²) = 0.1157 for 2,879 observed reflections with I > 2σ(I). X-ray diffraction analysis reveals that the dihedral angle between the two phenyl rings is 25.9 (2)°. The molecule adopts a trans configuration about the central C=N functional bond. The crystal structure is stabilized by C–H…O hydrogen bonds and π–π stacking interactions. The title compound possesses moderate antibacterial activity.      

An X-ray Crystallographic Study of 1,4-Di[(<Emphasis Type="Italic">E</Emphasis>)-2-(<Emphasis Type="Italic">p</Emphasis>-tolyl)-1-diazenyl]piperazine

Abstract  

The crystal structure of methyl 1,4-di[(E)-2-(p-tolyl)-1-diazenyl]piperazine (4) has been determined by single crystal X-ray diffraction analysis. The bis-triazene (4) adopts a normal chair conformation in the piperazine ring, with puckering parameters : φ₂ = −29(5)°, Q_T = 0.534(2) ? and θ₂ = 177.0(2)°. The crystal structure of 4 is compared with the structure of the triazene (2a) and the closely related bis-triazenes (3 and 5a). The piperazine ring of 2a and 4 adopt a typical chair conformation, whereas the piperazine ring of 3 adopts an unusual pseudo-boat conformation. Crystal data: 4 C₁₈H₂₂N₆, triclinic, space group P[`1] P\overline{1} , a = 6.8925(2) ?, b = 7.8574(3) ?, c = 16.8856(8) ?, α = 103.103(2)°, β = 90.528(2)°, γ = 101.776(2)° and V = 870.44 (6) ?³, for Z = 2.     

Synthesis and Characterization of <Emphasis Type="Italic">N,N</Emphasis>-di(prop-2-ynyl)-<Emphasis Type="Italic">p</Emphasis>-toluidine

Abstract  

In order to investigate the intramolecular [4 + 2] cycloaddition, we prepared some new tertiary N-(5-substituted-2-furfuryl)-N-prop-2-ynyl-p-toluidines [Hergold-Brundić et al., Acta Cryst C56:e520, 2000; Mance and Jakopčić, Mol Divers 9:229, 2005; Mance, “unpublished results”] by the alkylation of secondary N-(5-substituted-2-furfuryl)-p-toluidines with the propargyl-bromide [Mance and Šindler-Kulyk, Synth Commun 26:923, 1996]. In the course of preparation of N-(5-methoxy-2-furfuryl)-N-prop-2-ynyl-p-toluidine [Mance, “unpublished results”], besides the main product (compound 1) (Scheme 1) we obtained N,N-di(prop-2-ynyl)-p-toluidine (compound 2) as the colourless crystals. The title compound 2, N,N-di(prop-2-ynyl)-p-toluidine, C₁₃H₁₃N, crystallizes in monoclinic C 2/c space group with unit cell parameters: a = 19.5319(9) ?, b = 7.5230(3) ?, c = 15.9000(7) ?, β = 112.554(5)°, V = 2157.64(18) ?³, Z = 8. The crystal structure is dominated by van der Waals forces only. The bond distances around amine N atom correspond to σ dominated bonds (1.467(2), 1.462(2) and 1.419(2) ?). The angles sum around amine N atom is in accord with sp³ hybridization (343°).     

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.     

Structure and Antibacterial Activity of 3-(3,4-Dimethoxyphenyl)furan-2(5<Emphasis Type="Italic">H</Emphasis>)-ones

Abstract  

Crystalline hydrate of the title compound (5), C₁₉H₂₆N₂O₅·2(H₂O), was structurally characterized by single crystal X-ray diffraction. It crystallizes in monoclinic system space group P 21/c with a = 7.3987(7) ?, b = 17.8691(16) ?, c = 17.0022(13) ?, β = 112.944(3)°, V = 2070.0(3) ?³, Z = 4, R ₁ = 0.0592, wR ₂ = 0.1016, and T = 298(2) K. The X-ray structure determination revealed that the center furanone ring is nearly coplanar with 3,4-dimethoxybenzene ring, making a dihedral angle of 0.860(69)°. Two kinds of centrosymmetric tetramers characterized by graph-set motifs of R ₇⁸(36) and R ₄⁶(32) are formed through O–H···O, O–H···N and C–H···O hydrogen bonding interactions, which generate a sheet of edge-fused rings parallel to the (011) plane. These sheets are further linked into a three dimensional network by C–H···π interactions. Nine 3-(3,4-dimethoxyphenyl)furan-2(5H)-ones were synthesized and fully characterized by elemental analysis, MS and ¹H NMR. All of them were evaluated for antimicrobial activities against three Gram-positive organisms and a Gram-negative organism, and compound 5 was the most active against Staphylococcus aureus ATCC 25923.     

Spectroscopic Studies and Crystal Structure of (<Emphasis Type="Italic">Z</Emphasis>)-6-[(2-hydroxyphenylamino)methylene]-2-methoxycyclohexa-2,4-dienone

Abstract  The Schiff base (Z)-6-[(2-hydroxyphenylamino)methylene]-2-methoxycyclohexa-2,4-dienone has been synthesized from the reaction of 2-aminophenol with 2-hydroxy-3-methoxybenzaldehyde. The title compound has been characterized by elemental analysis, FT-IR, ¹H-NMR, ¹³C-NMR and UV–Visible techniques. The structure of the title compound also was determined crystallographically. The crystal structure has been solved by direct methods and refined by full-matrix least squares. The title compound crystallize in the monoclinic space group P2₁/c with a = 10.438(1), b = 8.851(1), c = 12.746(1) ?, β = 95.72(1)°, V = 1171.7(2) ?³, D _x  = 1.379 g cm⁻³, respectively (R1 = 0.0522 and wR2 = 0.126 for 1442 reflections [I > 2σ(I)]). Index Abstract   N-salicylideneaniline derivatives have been shown to exist as tautomeric forms due to intramolecular proton shifts between the phenol-oxygen and the imine-nitrogen, via intramolecular hydrogen bonding O–H···N or O···H–N.      

Synthesis,characterization, and crystal structure of <Emphasis Type="Italic">N</Emphasis>-<Emphasis Type="Italic">p</Emphasis>-nitrobenzoyl-<Emphasis Type="Italic">N</Emphasis>′-<Emphasis Type="Italic">p</Emphasis>-chlorophenylthiourea

N-p-nitrobenzoyl-N′-p-chlorophenylthiourea was synthesized and characterized by elemental analysis, IR and ¹H NMR etc. Single crystal structure of the title compound was determined on X-ray diffraction instrument. It is confirmed that the title compound crystallizes in monoclinic space group P2(1)/c, with a=8.5985(14) ?, b=12.1537(19) ?, c=14.972(2) ?, β=105.886(2)°, and D _calc=1.482 g/cm³ for Z=4. Intermolecular N–H⋯O H-bonds link pairs of two molecules. H-bonds and π-π stacking are the main non-bonding interactions in the molecular structure.     

Synthesis and Crystal Structures of Two Novel Complexes with <Emphasis Type="Italic">N</Emphasis>-[2-(5-Bromo-2-Hydroxybenzylideneamino)Ethyl]-4-Methylbenzenesulfonamide as Ligand

Abstract  

Two novel complexes constructed from the sulfonamide Schiff base ligand H ₂ L, N-[2-(5-bromo-2-hydroxybenzylideneamino)ethyl]-4-methylbenzene-sulfonamide, [Cu(HL)₂] (1) and [CuL(H₂O)] (2) are synthesized and characterized via X-ray single-crystal diffraction, elemental analysis, FT-IR and UV–Vis. 1 and 2 both form 1-D supramolecular architectures by π–π stacking interactions. 1 and 2 both crystallize in monoclinic, with space group C2/c and P2/c for 1 and 2, with unit cell parameters a = 27.640(18) ?, b = 7.907(5) ?, c = 17.945(14) ?, β = 118.27(2)°, V = 3454(4) ?³, Z = 4 for 1, and a = 16.758(5) ?, b = 7.272(2) ?, c = 15.080(4) ?, β = 106.334(5)°, V = 1763.6(9) ?³, Z = 4 for 2.     

Experimental and Semi-Empirical and DFT Calculational Studies on (<Emphasis Type="Italic">E</Emphasis>)-2-[(2,4-Dichlorophenylimino) methyl]-<Emphasis Type="Italic">p</Emphasis>-cresol

Abstract  

The molecular and crystal structure of the title compound, C₁₄H₁₁Cl₂NO, has been determined by X-ray single crystal diffraction technique. The compound crystallizes in the orthorhombic, space group Pbca with unit cell dimensions a = 7.5537(10) ?, b = 11.5518(13) ?, c = 29.760(4) ?, M _r  = 280.14, V = 2596.8(6) ?³, Z = 8, R ₁ = 0.065 and wR ₂ = 0.191. The title compound exists in the enol–imine tautomeric form with a strong intramolecular O–H···N hydrogen bond. The dihedral angle between the two benzene rings is 37.66(15)°. The asymmetric unit in the crystal structure contains only one neutral molecule. Calculational studies were performed by using AM1, PM3, PM6 semi-empirical and DFT methods. Geometry optimizations of compound have been carried out by using three semi-empirical methods and DFT method and bond lengths, bond and torsion angles of title compound have been determined. Dipole moments (Debye) and the energy parameters of compound (kcal/mol) were calculated by using above mentioned calculation methods. Atomic charge distribution has been obtained from AM1, PM3, PM6 and DFT. In order to determine conformational flexibility on the molecule, molecular energy profile of the title compound was obtained with respect to the selected torsion angle T(N1–C7–C1–C2), which is varied from −180° to +180° in every 10 via PM3 semi-empirical method.     

Synthesis and Crystal Structures of Two Metal Complexes Formed in the Solvothermal Decomposition Reactions of <Emphasis Type="Italic">N</Emphasis>-Carboxyphenylenesulfonyl-S-Carboxymethyl-<Emphasis Type="SmallCaps">l</Emphasis>-Cysteine

Abstract  

The reactions of a new compound of N-Carboxyphenylenesulfonyl-S-Carboxymethyl-l-Cysteine (Cs-cmc) with Zn(II) or Co(II) salts in the presence of 4,4′-bipyridine (4,4′-bipy) led to the decomposition of Cs-cmc and produced [Zn(4,4′-bipy)(H₂O)₄]X₂ (X = p-sulfamoylbenzoate) 1 and [Co(4,4′-bipy)(H₂O)₄]Y·H₂O (Y = p-sulfonatobenzoate) 2, in which the decomposition products of Cs-cmc exist as free counter-anions. The single crystal X-ray diffraction analyses revealed that compound 1 crystallizes in monoclinic C2/c space group with a = 18.748(4) ?, b = 11.520(2) ?, c = 12.751(3) ?, β = 90.290(4)°, V = 2753.9(10) ?, Z = 4 and compound 2 crystallizes in orthorhombic Pca2₁ space group with a = 12.114(3) ?, b = 11.369(2) ?, c = 14.770(3) ?, V = 2034.1(7) ?, Z = 4. It was revealed that 1D chains were constructed from metal ions and 4,4′-bipy in both compounds. The 1D chains interact with the counter-anions by hydrogen bonds, forming 3D supramolecular structures.     

Synthesis and Crystal Structure of (<Emphasis Type="Italic">S</Emphasis>)-2-((<Emphasis Type="Italic">S</Emphasis>)-2-(<Emphasis Type="Italic">N</Emphasis>-Ts-Amino)-3-methylbutanoyl)-3-(1H-indol-3-yl)-6-phenyl-3,4-dihydro-1,2,4-triazin-5(2H)-one

Abstract  

The diastereoselective synthesis, NMR and X-ray structure of (S)-2-((S)-2-(N-Ts-amino)-3-methylbutanoyl)-3-(1H-indol-3-yl)-6-phenyl-3,4-dihydro-1,2,4-triazin-5(2H)-one—a potential antivirus agent are reported. The compound crystallizes in the triclinic space group P1 with unit cell parameters: a = 5.9259(6) ?, b = 9.6370(12) ?, c = 12.9541(9) ?, α = 109.210(9)°, β = 90.804(7)°, γ = 105.074(10)° and Z = 1.     

Structure of a New Bioactive Agent Containing Combined Antibacterial and Antifungal Pharmacophore Sites: 4-{[(<Emphasis Type="Italic">E</Emphasis>)-(5-Bromo-2-hydroxyphenyl)methylidene]amino}-<Emphasis Type="Italic">N</Emphasis>-(5-methyl-1,2-oxazol-3-yl)benzenesulfonamide

Abstract  

The title compound (3), C₁₇H₁₄BrN₃O₄S, is a Schiff base compound of 5-bromosalicylaldehyde (1) and sulfamethoxazole (2). The structure of (3) was determined by spectral (IR, ¹H and ¹³C NMR), elemental analyses and X-ray diffraction data. Compound (3) crystallizes in the monoclinic space group C2/c, with a = 31.936(3), b = 6.2571(5), c = 16.903(1) ?, β = 94.867(8), V = 3365.5(5) ?³, Z = 8. In the molecule of compound (3), the molecule is bent at the S atom with a C–SO₂–NH–C torsion angle of −86.3(3)°. Pairs of molecules, related by inversion centres, form intermolecular N–H···N hydrogen bonds to produce a dimer. An intramolecular phenolic O–H···N hydrogen bond is also formed. Intermolecular hydrogen bonding and π–π stacking hold the molecules together. The average distance between stacked benzene ring planes is 3.625(2) ?.     

Crystallographic and conformational analyses of zwitterionic form of (<Emphasis Type="Italic">E</Emphasis>)-2-methoxy-6-[(2-morpholinoethylimino)methyl]phenolate

The single crystal X-ray diffraction analysis of the title compound, C₁₄H₂₀N₂O₃, reveals that the structure is adapted to its zwitterionic form and centrosymmetric dimers are formed by N⁺–H···O⁻ type ionic weak hydrogen bonds in the crystal structure. The title compound crystallizes in the triclinic space group P−1 with a = 5.9255(13) ?, b = 9.853(3) ?, c = 12.248(3) ?, α = 101.793(19)°, β = 94.941(17)°, γ = 104.36(2)°, Z = 2, D_x = 1.308 g/cm³, μ (Mo-K_α) = 0.092 mm⁻¹. The structure was solved by direct methods and refined to a final R = 0.0371 for 2183 reflections with I > 2σ (I). The crystal structure is stabilized by N⁺–H···O⁻ type intra-molecular hydrogen bonds and N⁺–H···O⁻ type packing interactions referred to as weak hydrogen bonds. To elucidate conformational flexibility of the title molecule, the selected torsion angle is varied from −180° to +180° in every 10° separately and then molecular energy profile is calculated and construed. In addition, charge-population analysis of the crystallographically observed structure confirms its zwitterionic form.     

Synthesis and Crystal Structure of One Trinuclear di-<Emphasis Type="Italic">n</Emphasis>-butyltin(IV) Complex with Salicylaldoxime

Abstract   One trinuclear di-n-butyltin(IV) complex with salicylaldoxime (o-HON=CHC₆H₄OH=HONZOH), (Bu₂Sn)(Bu₂SnO)(Bu₂SnOH)(ONZOH)(ONZO), has been synthesized and characterized by elemental analyses, IR spectrum, and single crystal X-ray diffraction. This complex is a small cluster displaying two unequivalent salicylaldoximate with one seven-coordinate pentagonal–bipyramidal tin atom linked two five-coordinate trigonal–bipyramidal tin atoms via a network of oxygen atoms by Sn–O–Sn bridges. The hydrogen bonds (o-HON=CHC₆H₄–O…H–O) are observed in the complex. These hydrogen bonds include intramolecular hydrogen bonds and intermolecular hydrogen bonds. (Bu₂Sn)(Bu₂SnO)(Bu₂SnOH)(ONZOH)(ONZO) belongs to monoclinic: space group P2₁/n, with a = 12.2307(15) ?, b = 17.361(2) ?, c = 20.976(3) ?, β = 94.424(2)°, V = 4440.5(10) ?³, Z = 4, D _c  = 1.500 g/cm³, μ(MoKα) = 1.715 mm⁻¹, F(000) = 2024, and final R ₁ = 0.0426, wR ₂ = 0.1064 for observed reflections 7779(I > 2σ(I)). Index abstract  The title compound, di-n-butyltin(IV) complex with salicylaldoxime, was synthesized and its crystal structure determined. Single crystal X-ray diffraction analysis reveals that the molecular structure of the title compound is trinuclear. The complex is a small cluster displaying two unequivalent salicylaldoximate with one seven-coordinate pentagonal–bipyramidal tin atom linked two five-coordinate trigonal–bipyramidal tin atoms via a network of oxygen atoms by Sn–O–Sn bridges.      

Crystallographic and Conformational Analysis of [(<Emphasis Type="Italic">E</Emphasis>)-2-[(3-Chlorophenylimino)methy])-4-methoxyphenol]

Abstract  The crystal structure of C₁₄H₁₂ClNO₂ was determined by X-ray analysis. It crystallizes in the triclinic space group Pc with a = 12.5346(10) ?, b = 4.5101(3) ?, c = 12.0534(11) ?, α = 90.00o, β = 113.669(6)o, γ = 90.00o, Z = 2, Dx = 1.393 mg/m³, μ (MoK_α) = 0.298 mm⁻¹. The title compound is photochromic and molecule is non-planar. It adopts a phenol–imine tautomeric form with a strong intramolecular O–H···N hydrogen bond and a strong intermolecular C–H···O hydrogen bond. Minimum energy conformations AM1 were calculated as a function of the three torsion angles θ1(C10–C9–N1–C8), θ2(C9–N1–C8–C1) and θ3(N1–C8–C1–C6), varied every 10°. As in the X-ray experiment results, molecule has an angle that makes it non-planar between two aromatic rings in AM1 optimized geometry. Graphical Abstract  Molecular and crystal structure of [(E)-2-[(3-chlorophenylimino)methy])-4-methoxyphenol], C₁₄H₁₂ClNO₂, have been determined by single crystal X-ray diffraction study, and conformational analysis of the title molecule with respect to the selected torsion angle has been achieved by AM1 semi-empirical calculations.