Synthesis and crystal structure of a novel 3D supramolecular complex [Na(DC18C6-B)][Ni(mnt)<Subscript>2</Subscript>]

A supramolecular complex [Na(DC18C6-B)][Ni(mnt)₂] (1) (DC18C6-B = cis-anti-cis-dicyclohexyl-18-crown-6, isomer B; mnt = maleonitriledithiolate) has been prepared and characterized by elementary analysis, FT-IR spectroscopy and X-ray single crystal diffraction. It crystallizes in triclinic, space group P1 with crystallographic data: a = 7.974(4) Å, b = 14.343(7) Å, c = 15.559(8) Å, α = 96.230(8)^∘, β = 100.361(8)^∘, γ = 93.849(9)^∘, V = 1733.2(15) ų, Z = 2, D_calcd = 1.408 g/cm³, F(000) = 766, R₁ = 0.0491, wR₂ = 0.1018. The formula unit contains one [Na(DC18C6-B)]⁺ complex cation and one [Ni(mnt)₂]⁻ complex anion, which are constructed into an infinite chain-like structure through Na–N bonds. The resulting chains crisscross on the [Ni(mnt)₂]⁻ complex anions and further assemble into an unusual 3D supramolecular framework via the weak interactions.     

Crystal structure of two brom containing aza-tetracyclic fused-ring N-heterocycles including isoxazolidine ring

Crystal structure of two brom containing aza-tetracyclic fused N-heterocycles including isoxazolidine ring compounds have been determined in single-crystal X-ray diffraction studies. The compound, C₁₄H₁₉BrN₂O₃, (1), and C₁₂H₁₅BrN₂O₃, (2), were obtained from a stereospecific[3+2] 1,3-cycloaddition of oxime based tandem nitrone generation reactions. The envelope conformation of the isoxazolidine rings are different, leading the substituents to be pseudoaxial in (1) and pseudoequatorial in (2). The stereochemistry of these fused compounds are exo- and endo-stereoisomer geometry contributed by exo and endo transition state of nitrone 1,3-dipolar cycloaddition reactions. The title compound (1) crystallizes in the monoclinic space group P2 ₁/n with a = 12.6221(5)Å, b = 7.5917(4) Å, c = 16.2350(9) Å, = 112.254(5)°, V = 1439.81(12) ų, and D _calc = 1.583 Mg/m³ for Z = 4 and compound (2) crystallizes in the monoclinic space group P2 ₁/c with a = 11.6906(9) Å, b = 6.4255(7) Å, c = 17.2070(10) Å, = 109.264(5)°, V = 1220.2(2) ų, and D _calc = 1.716 Mg/m³ for Z = 4. The antibacterial activity of both compounds were investigated for three Gram (+) and two Gram (–) bacteria by employing broth microdilution method and subsequently inhibitory activity against yeast-like fungi was also determined.     

Solid-state structure of a 1:1 adduct of 2-<Emphasis Type="Italic">t</Emphasis>-butylphenol and 3-<Emphasis Type="Italic">t</Emphasis>-butylsalicylaldehyde

The co-crystal structure of 2-t-butylphenol with 3-t-butylsalicylaldehyde (1) was obtained by single-crystal X-ray diffraction. 2-t-Butylphenol was co-crystallized with 1 equivalent of 3-t-butylsalicylaldehyde. The phase crystallizes in the monoclinic system with P2₁/c space group. The unit cell dimensions are a = 12.351(3) Å, b = 15.253(3) Å, c = 10.377(2) Å, β = 97.58(3)^∘, V = 1937.8(7) ų and Z = 4. The structure of the crystal layered by nonpolar group includes strong intramolecular and weak intermolecular hydrogen bonds. The aldehyde oxygen O2 accepts a three-centered bond through intramolecular O1–H1A⋅sO2 and intermolecular O3–H3A⋅sO2 interactions. In addition, the crystal consists of right-handed helical (P) and left-handed helical (M) chains linked by hydrogen bonding.     

Synthesis and crystal structure of an infinite double- stranded chain manganese(II) coordination polymer bridged through 1,2-bis(imidazol-1-yl)ethane ligand

The manganese complex [Mn(bim)₂(NCO)₂]_n (1) (bim = 1,2-bis(imidazol-1-yl)ethane) has been synthesized and structurally characterized by X-ray diffraction analysis. It crystallizes in the monoclinic space group C2/c, a = 9.896(3) Å, b = 15.383(4) Å, c = 13.949(4) Å, β = 98.966(5)^∘, V = 2097.5(9) ų, Z = 4. The coordination geometry of Mn(II) atom is distorted octahedral; it is coordinated equatorially by four nitrogen atoms from the imidazole rings of four symmetry-related bim ligands, and axially by two nitrogen atoms from two symmetry-related cyanate anions. The structure is polymeric, with 18-membered spiro-fused rings and each 18-membered ring involving two inversion-related bim molecules.     

Crystal structure of (Ph<Subscript>4</Subscript>P)[Hg(SPh)<Subscript>2</Subscript>Br]: Synthesis,characterization and structural analysis

The complex (Ph₄P)[Hg(SPh)₂Br] has been prepared and the crystal structure has been determined. The complex crystallized in the triclinic space group P with a = 9.607(5), b = 10.120(5), c = 17.071(8) Å, α = 96.00(3), β = 100.36(2), γ = 90.42(3)^∘, V = 1623(2) ų, D_c = 1.71 g cm⁻³, μ = 6.153 cm⁻¹, F(000) = 816 and Z = 2. The anionic complex [Hg(SPh)₂Br]⁻ is the monomer with distorted trigonal planar geometry. It contains relatively strongly bonded two thiolate ligands with a weaker bonding bromide ion. The crystal structure demonstrates a supramolecularity represented by nonconventional Br⋅sH–C(π) hydrogen bonds as well as aryl⋅saryl [C(π)–H⋅sC(π)] interactions. The Ph₄P⁺ cations are forming recognized extended supramolecular motifs of phenyl embraces.     

Crystal structures of mollugin and lucidin

Mollugin was isolated from the extract of Rubia tinctorum roots. Lucidin was obtained by semisynthesis from xanthopurpurin. Mollugin crystallises in space group P-1 (No. 2), a = 8.5857(7), b = 11.473(4), c = 15.024(1) Å, α = 77.64(2)^∘, β = 89.36(1)^∘, γ = 89.71(2)^∘, and V = 1445.5(5) ų, lucidin crystallises in space group P2₁/c (No.14), a = 16.800(6), b = 9.637(2), c = 7.073(7) Å, β = 98.01(5)^∘, and V = 1134(1) ų.     

Crystal structures of 2,4,9-trimethyl-(3ar,4c,9c,9ac)-3a,4,9,9a-tetrahydro-benzo[?] isoindole-1,3-dione(endo), C15H17NO2 (1), and 2-methyl-(3ac,9ac)-3a,4,9,9a-tetrahydro-4r,9c-ethano-benzo[?]isoindole-1, 3-dione(endo), C15H15NO2 (2)

The title compounds crystallize in the space group P-1 (compound 1), with a = 7.198(2) Å, b = 7.965(2) Å, c = 12.707(2) Å, α = 72.05(1)^∘, β = 87.65(2)^∘, γ = 65.18(2)^∘ and Pbca (compound 2), with a = 8.156(3) Å, b = 13.177(3) Å, c = 22.742(4) Å. The chiral centers in both compounds C3a, C4, C9, C9a are either R, S, R, S or S, R, S, R (compound 1) and either R, R, S, S or S, S, R, R (compound 2) because of the centric space group.     

Reactivity of 1,2,4,5-tetracarboxylatebenzene with cobalt(II)

The complexes [Co(H₂O)₆][Co(BTCA)(H₂O)₄]⋅7.2H₂O (1) and [Na₂Co(H₂O)₄(μ-H₂O)₂ (μ-BTCA)] (2) (BTCA = 1,2,4,5-tetracarboxylatebenzene) have been synthesized and characterized by single crystal X-ray diffraction. Compound (1) crystallizes in the triclinic space group P-1 with a = 6.8591(9) Å, b = 9.9691(13) Å, c = 10.9231(11) Å, α = 93.021(2)^∘, β = 104.883(2)^∘, and γ = 103.702^∘ with Z = 1. This compound exhibits a 1-dimensional structure of two alternating layers. A chain of cobalt ions and BTCA constitute one layer. Cobalt complex ions and solvent water molecules occupy the other. Compound (2) crystallizes in the monoclinic space group C 2/m with a = 8.8647(6) Å, b = 10.5247(7) Å, c = 21.2265(14) Å, and β = 92.525(2)^∘, with Z = 2. This compound consists of a 3-dimensional network of cobalt and sodium ions linked by BTCA. The sodium complex moiety is disordered around a center of inversion.     

Bis(2,2′-biimidazoline)bis(isothiocyanato)Metal(II) compounds. Synthesis,characterization and lattice hydrogen bonding for Metal = Mn(II) and Ni(II)

The synthesis, characterization and X-ray structures of two compounds with the general formula trans-M(biz)₂(NCS)₂ (in which biz = 2,2′-biimidazoline and M = Mn(II) for compound 1 and Ni(II) for compound 2) are reported. Both compounds crystallize in the triclinic space group P-1 with a = 8.393(5), b = 8.946(5), c = 7.659(5) Å, α = 104.440(5), β = 106.880(5), γ = 66.180(5)^∘, V = 497.7(5) ų, Z = 1 for compound 1 and a = 8.155(2), b = 8.8190(10), c = 7.480(2) Å, α = 102.259(15), β = 106.135(13), γ = 67.706(14)^∘, V = 474.7(2) ų, Z = 1 for compound 2.Both metal ions show octahedral coordination with the four nitrogen atoms of two biz ligands in the equatorial plane and the two nitrogen atoms of two isothiocyanate anions in the axial positions. The M–N≡C angles are 166.5(2) and 167.7(2) for compounds 1 and 2, respectively. These values are in the usually obtained range for trans-isothiocyanate coordinated compounds. The sulfur atom of each isothiocyanate anion acts as acceptor for the hydrogen bond with the NH group of the biz ligands. In the IR spectrum the vibrations of the thiocyanate anion are observed at 2090 and 776 cm⁻¹ for compound 1 and at 2108 and 778 cm⁻¹ for compound 2, and these values are typical for linear-bond isothiocyanate complexes of transition metals.     

Structure and magnetic properties of a dinuclear complex [Cu<Subscript>2</Subscript>(TPA)<Subscript>2</Subscript>(<Emphasis Type="Italic">o-</Emphasis>phth)](ClO<Subscript>4</Subscript>)<Subscript>2</Subscript>

A new dinuclear complex, [Cu₂(TPA)₂(o-phth)](ClO₄)₂ (TPA = tris(2-pyridylmethyl) amine, o-phth = terephthalato dianion), was synthesized and characterized by X-ray crystallography. The unit of dinuclear Cu(II) was bridged by terephthalato dianion. The complex crystallizes in triclinic space group P1, with a = 8.287(3) Å, b = 10.623(4) Å, c = 13.818(5) Å; α = 92.077(7)^∘, β = 94.768(7)^∘, γ = 90.352(6)^∘; V = 1211.4(8) ų; Z = 2; R₁ = 0.0604, wR₂ = 0.1707. In the temperature range 4–300 K, magnetic measurement shows that the exchange interaction of the two metal ions is weak ferromagnetic with J = 1.20 cm⁻¹, g = 1.97.     

Crystal structure and conformation of methionyl dipeptides: Structure of <Emphasis Type="SmallCaps">L</Emphasis>-methionyl-<Emphasis Type="SmallCaps">L</Emphasis>-asparagine: Preferred conformations of peptides containing methionyl and asparaginyl residues

Crystals of L-methionyl-L-asparagines (C₉N₃H₁₇O₄S) are orthorhombic, space group P2₁2₁2₁, with cell parameters at 294 K of a = 5.248(1), b = 13.251(2), c = 18.028(2) Å, V = 1251.6(4) ų, Z = 4, D_m = 1.40 Mg/m³, and D_x = 1.397 Mg/m³. The crystal structure was solved by direct methods and refinded by full-matrix least-squares method to a final R value of 0.059 for 1804 reflections. The peptide is slightly nonpalnar [ω = 172.0(5)^∘]; the other torsion angles ψ₁, ϕ₂, ψ₂¹, and ψ₂² are 155.6(5), −95.8(5), 152.5(5), and −29.4(6)^∘ respectively. The methionyl side chain is disordered with two possible position for its C^γ, S^δ, and C^ε atoms. The methionly side chain is twisted with χ¹ = −86.4(7), χ² = 177.5(9), and χ³ = 116.6(2)^∘ for the major conformer A. The asparaginyl side chain is also twisted with χ¹ = −76.3(5) and χ² = 102.3(6)^∘. The crystal structure is stabilized by an intermolecular network of hydrogen bonds involving the N-terminal amino group and the ε-terminal amino group of asn residue as donors and the carboxyl oxygens of the C-terminal and the peptide carbonyl oxygens as acceptor atoms.     

Synthesis and crystal structures of two copper(I) π-complexes with 1-allyloxybenzotriazole of CuBr?C6H4N3(OC3H5) and 2CuCl?C6H4N3(OC3H5) compositions

Both compounds of CuBr⋅C₆H₄N₃(OC₃H₅) (sp. gr. P1, a = 7.633(1) Å, b = 9.987(1) Å, c = 14.898(2) Å, α = 104.75(1)^∘, β = 94.76(1)^∘, γ = 106.90(1)^∘) (I) and 2CuCl⋅C₆H₄N₃(OC₃H₅) (sp. gr. Cc, a = 11.2483(4) Å, b = 16.7076(6) Å, c = 7.2948(3) Å, β = 118.612(2)^∘) (II) composition were prepared by alternating-current electrochemical synthesis. In I due to a bridging function of organic moieties 16-membered cycles appear which are combined into ribbons {Cu₂Br₂[(C₆H₄N₃(OC₃H₅)]₂}_n. Each of two crystallographically independent copper atom possesses a trigonal-pyramidal arrangement with different degree of tetrahedral distortion. Distinctive numbers of hydrogen bonds around Br1 and Br2 atoms cause rather appreciable distinctions in copper–olefinic bond interaction effectiveness for each metal atom. In II Cu₂Cl₂ rhombs are joined to infinite chains oriented along [010] direction. Each ligand molecule is also coordinated through the C=C—bond of the allylic group to copper atom of one inorganic chain and through the nitrogen atom to a metal atom belonging to another copper-halide chain. Cu1 atoms is tetrahedrally surrounded by three chlorine atoms and nitrogen one, whereas a trigonal-planar arrangement of Cu2 atom is formed by two halogen atoms and slightly disordered olefinic group.     

Synthesis and crystal structure of 2-benzoyl-4-methyl phenyl benzoate

The crystal structure of the title compound, C₂₁H₁₆O₃, has been determined. The compound crystallizes in triclinic space group PĪ with cell parameters a = 9.2240(9) Å, b = 9.8050(8) Å, c = 10.1610(11) Å, α = 94.749(6)^∘, β = 112.544(4)^∘, γ = 102.145(6)^∘ and Z = 2. The structure exhibits both intra and intermolecular interactions of the type C–H ⋅s O. The intermolecular interaction between the molecules form centrosymmetric dimers.     

C–H⋅<Emphasis Type="Italic">s</Emphasis>O hydrogen bond networks in <Emphasis Type="Italic">E</Emphasis>- and Z-unsaturated esters of C-glycosides

Methyl E(Z)-4,7 anhydro-5-benzamido-6,8-di-O-benzoyl-2,3,5-trideoxy-d-allo-oct-2-enoate have been synthesized like intermediates and isolated as single crystals during the synthesis of pyrazole-related C nucleosides as synthetic product with cytotoxic activity.¹ Crystal structures of E(Z) isomers were determined by X-ray analysis. E isomer crystallizes in the triclinic crystal system, space group P1, a = 5.319(1) Å, b = 10.758(2) Å, c = 12.229(2) Å, α = 72.38(2)^∘, β = 89.97(2)^∘, γ = 87.07(2)^∘, D_x = 1.320 Mgm⁻³ and Z isomer in the orthorhombic crystal system, space group P2₁2₁2₁, a = 5.1297(13) Å, b = 19.667(5) Å, c = 25.871(6) Å, D_x = 1.348 Mgm⁻³. The molecular structure was solved by direct method on the basis of 2609 and 2727 unique reflections recorded at the temperature 293 K (E-isomer) and 173 K (Z-isomer) up to the final R-factor 0.0378 and 0.0435, respectively. C–H⋅sO contact networks were analyzed and the correlation established between the existence of the weak C–H⋅sO hydrogen bonds and the melting point of the single crystals.     

Synthesis,spectroscopic and X-ray structural study of [<Emphasis Type="Italic">trans</Emphasis>-di(4-aminobenzoato)bis(ethylenediamine) cobalt(III)] 4-aminobenzoate tetrahydrate

The title compound was synthesized by mixing the separately dissolved trans-dichlorobis(ethylenediamine)cobalt(III) chloride and sodium 4-aminobenzoate in aqueous medium in 1:3 molar ratio and recrystallizing the product obtained, from hot water. Elemental analyses and spectroscopic techniques (IR, UV/visible, ¹H and ¹³C NMR) were used for characterizing the complex salt. X-ray structure determination revealed an ionic structure consisting of [Co(en)₂(C₇H₆NO₂)₂]⁺ cation, (C₇H₆NO₂)⁻ anion and four lattice water molecules. The complex salt crystallizes in the triclinic space group P with cell dimensions a = 9.985(1) Å, b = 11.522(1) Å, c = 14.233(1) Å, α = 80.20(1)^∘, β = 72.80(1)^∘, γ = 86.43(1)^∘, Z = 2, V = 1541.3(2) ų, R₁ = 0.0291, and wR₂ = 0.0751.     

Synthesis and Crystal Structures of 3,3,6,6-tetramethyl-9-(2,4-dichlorophenyl)-3,4,6,7,9,10-hexahydro-2H,5H-acridine-1,8-dione and 3,3,6,6-tetramethyl-9,10-di(4-methoxyphenyl)-3,4,6,7,9,10-hexahydro-2H,5H-acridine-1,8-dione

The title compounds 3,3,6,6-tetramethyl-9-(2,4-dichlorophenyl)-3,4,6,7,9,10-hexahydro-2H,5H-acridine-1,8-dione 1 (C₂₃H₂₅Cl₂NO₂, Mr = 418.34) and 3,3,6,6-tetramethyl-9,10-di(4-methoxy-phenyl)-3,4,6,7,9,10-hexahydro-2H,5H-acridine-1,8-dione 2 (C₃₁H₃₅NO₄, Mr = 485.60) were synthesized and crystallized. The crystals of compound 1 are monoclinic, space group P2₁/c, a = 9.826(3), b = 19.866(5), c = 11.471(3) ?, β = 111.929(4)°, Z = 4, V = 2077(1) ?³; The compound 2 crystallizes in space group P2₁/c, with cell parameters a = 12.089(2), b = 11.447(2), c = 19.742(3) ?, β = 101.00(1)°, V = 2681.8(8) ?³ and D _calc = 1.203 g/cm³ for Z = 4. X-ray analysis reveals that atoms C(1), C(6), C(7), C(8), C(13) and N(1) form a 1,4-dihydropyridine ring in compound 1, which adopts half-chair conformation. In compound 2 the atoms C(1), C(6), C(7), C(8), C(13) and N form a 1,4-dihydropyridine ring which adopts boat conformation. In addition, the two outer six-membered rings display half-chair conformations in the crystal structures 1 and 2.     

Crystal structure of [RuCl2[N-(2,4,6-trimethyl-benzyl)N-(n-butyl)]-imidazolidin-2-ylidene] and [RuCl2[N-(2,4,6-trimethyl-benzyl)-N-(2-methoxyethyl)]-imidazolidin-2-ylidene]

Two imidazolidin ruthenium complexes, [RuCl₂{[N-(2,4,6-trimethyl-benzyl)-N-(n-butyl)]-imidazolidin-2-ylidene}], 1, and [RuCl₂{[N-(2,4,6-trimethyl-benzyl)-N-(2-methoxyethyl)]-imidazolidin-2-ylidene}], 2, have been synthesised and their crystal structures have been determined from single crystal X-ray diffraction data. Compound 1 is monoclinic, of space group C2/c with a = 18.466(4) Å, b = 14.816(3) Å, c = 15.413(3) Å, β = 118.067(2)^∘, and V = 3720.9(12) ų with Z = 8 for d_calc = 1.536 g/cm³. Compound 2 is monoclinic, of space group P2₁/c with a = 8.1800(5) Å, b = 14.344(8) Å, c = 14.809(9), β = 91.604(10)^∘, and V = 1736.7(18) ų with Z = 4 for d_calc = 1.653 g/cm³. In each complex the ligand functions as an arene and carbene, occupying four coordination sites. The two chlorines in each compound complete a distorted octahedron.     

Investigation of 4-acetyl-2,6-dibenzyl-1,5-dihydroxy-2-methylcyclohexa-4,6-dien-3-one by X-ray crystallography and 1H-NMR spectroscopy

Benzylation of 3-methylphloracetophenone [1-(2,4,6-trihydroxy-3-methylphenyl)ethanone] (3) with benzyl chloride gave 4-acetyl-2,6-dibenzyl-1,5-dihydroxy-2-methylcyclohexa-4,6-dien-3-one (5). Compound 5 crystallizes in the orthorhombic space group Fdd2 with a = 17.586(2), b = 42.891(5), c = 10.279(2) Å, V = 7753(2) Å,³ and Z = 16. When crystals of 5 were dissolved in [D₆]acetone the compound underwent tautomerization and a mixture of 5 and its keto form 4 was obtained (keto form/enol form ratio 1:4).     

Preparation,spectral studies,and X-ray crystal structures of (16S, 17R, 20S)-3-oxo-16-hydroxy-25-nor-lanostan-24-oic lactone (II) and (16S, 17R, 20S)-4,16-dihydroxy-25-nor-3,4-seco-lanostan-3,24-dioic acid dilactone (III)

The crystal and molecular structures of the title compounds have been determined by direct methods, and refined to a finalR of 0.059 forII and 0.046 forIII. Both molecules crystallize in space group P2₁2₁2₁. The cell dimensions forII area=10.096(5),b=11.255(3),c=20.300(7) Å;Z=4,D _x=1.188 g cm^–3, (MoK)=0.70 cm^–1, while the cell dimensions forIII area=7.346(1),b=10.470(3),c=30.546(5) Å;Z=4,D _x=1.212 g cm^–3, (MoK)=0.74 cm^–1. The rings of the triterpene skeletons aretrans-cis-trans-cis connected. The conformations of both molecules are discussed. Also the preparation and the spectral data of (17R, 20S)-3,16-dioxo-25-nor-lanostan-24-oic acid (V) and (17R, 20S)-3,16,24-trioxo-25-hydroxy-16,24-seco-lanostan-25-acetate (VI) are given.     

Crystal structures of 1,1-di(p-substituted phenyl)-2,2-dinitroethylenes

The X-ray crystal structures of 1,1-di(p-methylphenyl)-2,2-dinitroethylene (2), 1,1-di(p-methoxylphenyl)-2,2-dinitroethylene (3), 1,1-di(p-fluorophenyl)-2,2- dinitroethylene (4), 1,1-di(p-chlorophenyl)-2,2-dinitroethylene (5), and 1-phenyl-1- (p-nitrophenyl)-2,2-dinitroethylene (6) are reported and compared with that of 1,1-diphenyl-2,2-dinitroethylene (1). Owing to steric repulsion between the aryl rings, the single bond lengths between C(1) and the two ring carbons atoms are longer than the normal sp²–sp² bond distance of 1.46 Å. For 4–6 in which the aryl rings contain electron-withdrawing substituents (F, Cl, NO₂), the double bonds between C(1) and C(2) are shorter than those in 2 and 3, whose aryl rings containing electron-donating substituents. Furthermore, the steric repulsion between the aryl rings and C NO₂ fragments results in an appreciable twist about the central double bond. The two aryl rings of compounds 1–6 make dihedral angles of 77.7, 66.6, 62.8, 80.9, 82.0, and 71.2°, and the two C NO₂ fragments make dihedral angles of 68.5, 67.8, 65.9, 76.9, 73.0, and 71.9°, respectively.