Crystal and molecular structure of (2R,3R)-2-exo-((1R)-1-hydroxy-2-methyl-propyl)-3-exo-hydroxymethyl-bicyclo[2.2.1]-hept-5-ene,C12H20O2

The stereogeometry of the title compound which was prepared by a stereoselective addition reaction, has been proved by an X-ray diffraction analysis. Crystal data: monoclinic, P2₁,a=10.495(16),b=8.392(16),c=13.209(20) Å, =93.80(8),Z=4. The crystal structure has been solved by vector search methods and refined toR=0.05 for 782 observed reflections.     

Crystal structure of methyl trans-3-[(2-(methoxycarbonyl)phenyl)sulfinyl]acrylate: a product resulting from trapping of a sulfenic acid by methyl propiolate

Evidence for the formation of unstable sulfenic acids (RSOH) as reaction intermediates is commonly provided by trapping these compounds with methyl propiolate. The crystal structure of a vinyl sulfoxide derived from the trapping of a sulfenic acid with methyl propiolate is reported here. The title compound C₁₂H₁₂O₅S crystallized in the triclinic space group,P1¯ with unit cell parameters: a = 6.1600(4), b = 9.7286(7), c = 11.3698(8) Å, = 112.024(1), = 94.662(1), = 95.429(1)°, and Z = 2.     

Tautomeric properties and crystal structure of N-[2-hydroxy-1-naphthylidene]2,5-dichloroaniline

The title compound has been synthesised by the reaction of 2-hydroxy-1-naphthaldehyde with 2,5-dichloroaniline. The compound was characterized by elemental analysis, IR and UV-Visible techniques. The UV-Visible spectra of the Schiff base with OH group in ortho position to the imino group was studied in polar and nonpolar solvents in acidic and basic media. The structure of compound has been examined cyrstallographically. It crystallizes in the orthorhombic space group P2₁2₁2₁ with a = 6.059(1), b = 12.105(2) c = 20.006(2) Å, V = 1467.4(3) ų, D_x = 1.431 g.cm^-3 and Z = 4. The crystal structure was solved by direct methods and refined by full-matrix least squares. Molecule of the title compound N-[2-hydroxy-1-naphthylidene]2,5-dichloroaniline is nearly planar. The molecule contains a strong intramolecular N…H-O hydrogen bond between the imine and hydroxyl group [O1 and N1 = 2.540(4) Å]. (© 2006 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and Crystal Structure of 3-[(Naphthalen-2-yl)methyl]Isocoumarin

Abstract 3-[(Naphthalen-2-yl) methyl]isocoumarin was synthesized by the reaction of homophthalic acid with 2-(naphthalen-2-yl)acetyl chloride at elevated temperature and its crystal structure has been determined (C₂₀H₁₄O₂), Mr = 286.31, a = 13.704(3), b = 7.356(4), c = 7.042(7) ?, β = 99.21(3)°, space group Pc, Z = 2, and V = 700.7(8) ?³. The isocoumarin and the naphthalene ring systems are individually planar and the dihedral angle between the mean planes of these two ring systems is 70.05(8)°. Graphical Abstract Synthesis and crystal structure of 3-[(Naphthalen-2-yl)methyl]isocoumarin Aamer Saeed, Junmei Liang, Masood Parvez The synthesis and crystal structure of a novel isocoumarin, 3-[(naphthalen-2-yl)methyl]isocoumarin has been presented.      

Crystal structures and spectroscopic properties of copper(II) and zinc(II) complexes with the macrocycle 1,4,7-tris(2-pyridylmethyl)-1,4,7-triazacyclononane

Two novel transition-metal copper and zinc complexes [(CuL)₂]·(ClO₄) (1) and [(ZnL)]·(ClO₄)₂ (2) (L = 1,4,7-tris(2-pyridylmethyl)-1,4,7-triazacyclononane) have been synthesized and structurally determined. The two complexes are both crystallized in monoclinic space group P2(1)/c with a = 14.318(4), b = 17.214(5), c = 22.403(7) Å, = 93.096(6)°, V = 5522(3) ų, and Z = 4 for 1 and a = 9.371(2), b = 17.615(4), c = 17.579(4) Å, =104.070(4)°, V = 2814.6(11) ų, and Z = 4 for 2. The center metal ions are coordinated to six nitrogen atoms, three of which are from triazacyclononane and other three from the pendant-arms 2-pyridylmethyl, forming a slightly distorted octahedral geometry. Two complexes have been characterized by element analysis, infrared spectroscopy, and the UV–Vis and ESR spectra for 1 have also been determined.     

Synthesis,characterization and crystal structure of bis{2-methoxy-6-[(2-diethylaminoethylimino)methyl]phenolato}thiocyanatocobalt(III) perchlorate

Brown block-shaped crystals of bis{2-methoxy-6-[(2-diethylaminoethylimino)methyl]phenolato}thiocyanatocobalt(III) perchlorate, the first cobalt(III) complex derived from the Schiff base ligand HL, [Co^III(L)(HL)(NCS)].ClO₄ (HL=2-methoxy-6-[(2-diethylaminoethylimino)methyl]phenol) have been obtained and characterized by elemental analysis and X-ray single crystal determination. The complex crystallizes in the monoclinic space group P2₁/c with unit cell dimensions a=16.087(3) ?, b=12.354(3) ?, c=16.762(3) ?, β=93.77(3)°, V=3324.1(12) ?³, Z=4, R ₁=0.0741 and wR2=0.1366. X-ray structure determination revealed that the complex consists of a [Co^III(L)(HL)(NCS)]⁺ cation and a disordered perchlorate anion. The Co atom in the cation is six-coordinate in an octahedral coordination. In the crystal structure, the perchlorate anions are linked to the cations through intermolecular C–H⋯O hydrogen bonds, forming zigzag chains running along the caxis. It is the first cobalt(III) complex derived from the Schiff base ligand HL.     

Crystal structures of (I) 2-(9,9-dipropylfluorene-2-yl)-9,9- dipropylfluorene and (II) 2-(1,1-dimethylpropyl)-7- {4-[(1,1-dimethylpropyl)-9,9-diethylfluoren-2-yl]phenyl}-9,9-diethylfluorene and (III) 2-(4-ethylphenyl) -7-[7-(ethylphenyl)-9,9-dipropylfluoren-2-yl]-9,9-dipropylfluorene

The crystal structures of the three fluorene related molecules, (I) 2-(9,9-dipropylfluorene-2-yl)-9,9-dipropylfluorene, [Exalite 384, C₃₈H₄₂], (II) 2-(1,1-dimethylpropyl)-7-{4-[(1,1-dimethylpropyl)-9,9-diethylfluoren-2-yl] phenyl}-9,9-diethylfluorene, [Exalite 404, C₅₀ H₅₈], and (III) 2-(4-ethylphenyl)-7-[7-(ethylphenyl)-9,9-dipropylfluoren-2-yl]-9,9-dipropylfluorene, [Exalite 416, C₅₄H₅₈], have been determined. Structural details reveal a novel new bonding arrangement at the C2 atoms of symmetry-related fluorene moieties in all three molecules producing a linear type array with an inversion center connecting adjacent asymmetric units within each molecule. Exalite 384 is monoclinic, space group P2₁/c with a = 9.002(2) Å, b = 16.275(4) Å, c = 10.525(1) Å, = 103.05(1), and V = 1502.1(5) ų with Z = 4, for d _calc = 1.103 g/cm³. Exalite 404 is triclinic, space group P1 with a = 10.383(1) Å, b = 13.404(2) Å, c = 7.7007(9) Å, = 105.296(9), = 104.23(1), = 73.707(9), and V = 974.9(2) ų with Z = 2, for d _calc = 1.141. Exalite 416 is monoclinic, space group P2₁/c with a = 15.99(10) Å, b = 11.178(8) Å, c = 23.766(4) Å, = 104.21(4), and V = 4117(4) ų with Z = 4, for d _calc = 1.141 g/cm³.     

Spectroscopic studies, antimicrobial activities, and crystal structure of N-[2-hydroxy-1-naphthylidene]3, 5-bis(trifluoromethyl)aniline

A new Schiff base compound has been synthesized by the reaction of 2-hydroxy-1-naphthaldehyde with 3,5-bis(trifluoromethyl)aniline.The title compound was characterized by elemental analysis, IR,¹H NMR,¹³C NMR, and UV–Visible techniques.Its UV–Vis spectra was examined in polar and nonpolar solvents and in acidic and basic media. The crystal structure of the compound showed the OH group to be ortho to the imine group. It crystallizes in the monoclinic space group P2₁ with a = 11.328(2), b = 6.125(1), c = 11.937(2) ?, V = 825.1(2) ?³, D _x = 1.543 g cm⁻³and Z = 2. An intramolecular O1- H⋯N1 [2.558(7) ?] hydrogen bond stabilizes the molecule. The compound has also been characterized by its antimicrobial activities. The ligand has been screened in vitro against the organisms Escherichia coli ATCC 11230, Staphylococcus aureus ATCC 6538, Klebsiella pneumoniae UC57, Micrococcus luteus La 2971, Proteus vulgaris ATCC 8427, Pseudomonas aeruginosa ATCC 27853, Mycobacterium smegmatis CCM 2067, Bacillus cereus ATCC 7064, and Listeria monocytogenes ATCC 15313, the yeast cultures Candida albicans ATCC 10231, Kluyveromyces fragilis NRRL 2415, Rhodotorula rubra DSM 70403, Debaryomyces hansenii DSM 70238, and Hanseniaspora guilliermondii DSM 3432.     

Methyl 4-((E)-2-{3-[(3-{ (E)-2-[4-(methoxycarbonyl)phenyl]- 1-diazenyl}-5,5-dimethylhexahydro-1-pyrimidinyl)methyl]-5,5-dimethylhexahydro-1-pyrimidinyl-1-diazenyl) benzoate. X-ray crystal structure

Methyl 4-((E)-2-{3-[(3-{(E)-2-[4-(methoxycarbonyl)phenyl]-1-diazenyl}-5, 5-dimethyl hexahydro-1-pyrimidinyl)methyl]-5, 5- dimethylhexahydro-1- pyrimidinyl}-1- diazenyl) benzoate (1) has been synthesized by reaction of a mixture of formaldehyde and 2,2-dimethyl-1,3-propanediamine with p-methoxycarbonylbenzenediazonium chloride. The crystal structure of 1 has been determined by single crystal X-ray diffraction analysis. The crystals of 1 displayed problems of disorder; the asymmetric unit is built up by two independent molecules, which display disorder within a methoxycarbonyl group. The two independent molecules in the asymmetric unit are very similar, differing only slightly about the mutual orientation of the aryltriazenyl groups. With respect to the N–C–N bridge between the hexahydropyrimidinyl rings, the two equivalent fragments containing the triazene moieties are in a cis orientation. The N–N single bonds, in the range 1.319(4)–1.348(4) Å, and the N=N double bonds, in the range 1.255(5)–1.275(4) Å, indicate significant conjugations within the triazene moieties. All the hexahydropyrimidine six-membered rings adopt a chair conformation as shown by their puckering parameters. The crystal packing is determined only by simple van der Waals interactions. The crystal structure of 1 is compared with the previously reported structure of the unbranched hexahydropyrimidine analogue 2. Crystal data: 1 C29H40N8O4, triclinic, space group P-1, a = 13.9652(2), b = 14.2908(3), c = 16.6129(4) Å, = 97.279(1), = 90.872(1), = 107.385(1), V = 3133.6(1) ų, for Z = 4.     

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 structures of bis{4-bromo-2-[(2-hydroxyethylimino)methyl]phenolato}copper and bis{4-chloro-2-[(2-hydroxyethylimino)methyl]phenolato}copper

The crystal structures of bis{4-bromo-2-[(2-hydroxyethylimino)methyl]phenolato}copper (I) and bis{4-chloro-2-[(2-hydroxyethylimino)methyl]phenolato}copper (II) are determined. Crystals I are monoclinic, space group P2₁/c, Z = 2, and R = 0.0732 (for all reflections). Crystals II are likewise monoclinic, space group P2₁/n, Z = 2, and R = 0.1106. In the structures of compounds I and II, the metal atom is situated at the center of symmetry and coordinated by two singly deprotonated bidentate 4-bromo-or 4-chloro-2-[(2-hydroxyethylimino)methylphenol molecules, respectively, through phenol oxygen and azomethine nitrogen atoms, which form a distorted planar square. In the structures of compound II, the coordination polyhedron of the central atom is completed to an elongated tetragonal bipyramid by the amino alcohol oxygen atoms of the adjacent complexes.     

Crystal structure of [WI2(CO)3{P(OMe)3}2]

[WI₂(CO)₃{P(OMe)₃}₂]crystallizes in the orthorhombic space group Pca2₁, with a = 26.924(5), b = 10.726(2), c = 14.136(3) Å, and Z = 8. There are two molecules in the asymmetric unit, the metal atoms in each case being seven-coordinate with a capped fac-(CO)₃ octahedral geometry. The molecular dimensions in the two molecules are nearly identical. The W–P distance to the capping atom 2.397 Å (average) is significantly shorter than the other W–P distance, 2.525 Å (average).     

Synthesis and structure of chiral ligand [(<Emphasis Type="Italic">S</Emphasis>)-1-(((<Emphasis Type="Italic">S</Emphasis>)-1-methylpyrrolidin-2-yl) methyl) pyrrolidin-2-yl] diphenylmethanol

The title compound (C₂₃H₃₀N₂O), a chiral ligand, has been successfully synthesized from a natural proline. FTIR spectrum has been discussed. DFT (B3LYP) method has been used to determine the structure. With the basis set of the 6–311G^* quality, the DFT calculated bond parameters and harmonic vibrations are predicted in very good agreement with experimental data.

Synthesis,characterization and crystal structure of a mononuclear iron(III) complex derived from 4-bromo-2-[(pyridin-2-ylmethylimino)methyl]phenol

A nitrate salt of bis[4-bromo-2-(pyridin-2-ylmethyliminomethyl)phenolato]iron(III), [Fe(C₁₃H₁₀BrN₂O)₂].NO₃, has been obtained and characterized by elemental analysis and X-ray single crystal determination. The complex crystallizes in the tetragonal space group P4₂/n with unit cell dimensions a = b = 17.608(3) ?, c = 17.199(3) ?, V = 5332.4(15) ?³, Z = 8, R ₁ = 0.0444 and wR2 = 0.0902. The complex consists of a [Fe(C₁₃H₁₀BrN₂O)₂]⁺ cation and a nitrate anion. The Fe atom in the cation is six-coordinated in an octahedral geometry. In the crystal structure, molecules are linked through weak C–H⋯O intermolecular hydrogen bonds, forming chains running along the c axis. Supplementary material CCDC-607149 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge at http://www.ccdccam.ac.uk/const/retrieving.html or from the Cambridge Crystallographic Data Centre (CCDC), 12 Union Road, Cambridge CB2 1EZ, UK; fax: +44(0)1223-336033 or e-mail: deposit@ccdc.cam.ac.uk.     

Crystal structure of 25,27-bis[(2-cyanophenyl)methoxy] calix[4]arene

The crystal structure of 25,27-bis[(2-cyanophenyl)methoxy] calix[4]arene (C₄₄H₃₄N₂O₄) was determined by X-ray crystallographic analysis. It possesses space group R , with a = b = 35.993(8) Å, c = 13.842(3) Å, = = 90°, = 120°, and D _calc = 1.260 mg/cm³ for Z = 18. Crystal data indicate that Compound 1 exists in a pinched-cone conformation with intramolecular hydrogen bonds.     

Synthesis and molecular structure of 4,4,5,5-tetramethyl-2-(1-(phenylsulfonyl)propan-2-yl)-1,3,2-dioxaborolane

The compound 4,4,5,5-tetramethyl-2-(1-(phenylsulfonyl)propan-2-yl)-1,3,2-dioxabo- rolane has been prepared by the rhodium catalyzed hydroboration of allyl phenyl sulfone and characterized by a single crystal X-ray diffraction study. The title compound crystallized in the monoclinic space group P2₁/c, with cell parameters a=16.0728(8) ?, b=9.8884(5) ?, and c=10.1926(5) ?, β=92.067(1)°, Z=4, and V=1618.90(14) ?³. The structure was solved by direct methods and refined to a final R=0.0449 for 3627 reflections with I>2σ(I). No significant intramolecular or intermolecular interaction is observed with the Lewis acidic boron atom.     

Crystal structure of 1,3-di-2-[(4-methoxyphenyl)-1-diazenyl]imidazolidine

The crystal and molecular structure of 1,3-di-2-[(4-methoxyphenyl)-1-diazenyl]imidazolidine (1) has been determined by single crystal X-ray diffraction analysis. This novel bis-triazene assumes a close-to planar structure with the aryltriazene moieties aligned in diametrically opposed directions, unlike many other previously reported bis-triazenes, which assume a folded structure. The structure of 1 is compared with the closely related, non-cyclic bis-triazene analogue (2), and also compared with the structure of the simple mono-triazene (3). Crystal data: 1 C₁₇H₂₀N₆O₂, monoclinic, space group C2/c, a = 34.948(3), b = 5.925(5), c = 8.1225(6) Å, = 100.8420(10)°, and V = 1652.0(2) ų, for Z = 4.     

Crystal structure of a nucleoside analog: 1-(R)-[6-(R)-hydroxymethyl-1,4-dioxan-2-yl] uracil

The title compound (C₉H₁₂N₂O₅,M _r =228.2) crystallizes in the trigonal space groupP3₁,21 witha=b=9.438(3) andc=19.775(3) Å,V=1525.5 ų,D _x =1.490 gm cm^–3,Z=6,=0.12 mm^–1,F(000)=720.0,T=293 K. The structure was solved by direct methods and refined by full-matrix least-squares calculations to anR value of 0.044 on 843 unique observed reflections. The dioxane ring adopts a chair conformation. The crystal structure is stabilized by N-HO hydrogen bonds and C-HO close contacts.     

Crystal and molecular structure of 2-[(4-nitrophenyl)carbonyl]cyclohex-1-ene-1-yl 4-nitrobenzoate

The crystal structure of 2-[(4-nitrophenyl)carbonyl]cyclohex-1-ene-1-yl 4-nitrobenzoate is studied (T = 173 K, R1 = 0.0354 for 2713 observed reflections). This crystal is orthorhombic, a = 7.8367(8) Å, b = 9.6082(10) Å, c = 23.856(3) Å, V = 1796.3(3) ų, space group P2₁2₁2₁, and Z = 4. The molecule has a folded configuration, which is stabilized by π-π interactions between its two parts. A system of intermolecular C-H...O hydrogen bonds (H...O, 2.44–2.67 Å; CHO angles 122°–169°) and intramolecular C-H...O contacts closing five-membered cycles (H...O, 2.42–2.59 Å; CHO angles 96°–102°) are formed in the structure.