Synthesis and X-ray structure of 3-(4-methyl phenyl)-2-(4-biphenyl)-1,3-thiazolidin-4-one

The title compound (C₂₂H₁₉NOS) was synthesized, characterized and structure was determined by X-ray diffraction method. It crystallizes in the monoclinic space group P2₁/c with cell parameters a = 22.181(2) Å, b = 6.0760(4) Å, c = 13.349(3) Å, = 95.615(3)^, and {Z = 4}. The final residual factor is 0.0625 for 1724 reflections with I > 2(I). 4-thiazolidinone ring moiety shows twisted conformation.     

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.     

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.     

Synthesis of homoleptic lanthanide amides and the crystal structure of [Li(THF)4][Y(NPh2)4]

Anhydrous LnCl₃ reacted with three equivalents of LiNPh₂ in THF to give the unexpected homoleptic lanthanide amides [Li(THF)₄][Ln(NPh₂)₄] (Ln = Sm (1), Y (2)) in high yield. The crystal structure of complex 2 has been determined by X-ray diffraction methods. It crystallizes in the orthorhombic space group Pbcn with a = 17.522(3) Å, b = 16.321(3) Å, c = 19.947(3) Å, V = 5704.4(17) ų, and D _calc = 1.231 mg/m³ for Z = 4. Complex 2 is composed of discrete [Li(THF)₄]⁺ cations and [Y(NPh₂)₄]^– anions, both of which have crystallographically imposed two-fold symmetry. To achieve steric saturation of the metal center, there are interactions between the yttrium atom and one -carbon atom of each amide ligand. The yttrium and lithium atoms both exhibit distorted tetrahedral coordination geometry.     

The crystal and molecular structure of (−)—Crinine (C16H17NO3)

(–)—Crinine, C₁₆H₁₇NO₃, is an alkaloid extracted from the bulbs of Pancratium maritimum L. (Amaryllidaceae). The compound crystallizes in the space group P2₁2₁2₁ with cell dimensions a = 6.040(1), b = 12.382(1), c = 17.861(2) Å, with Z = 4. The molecule has five rings and an OH group. The N-containing, five-membered ring and the D ring have envelope conformations. The A and B rings have distorted chair and half-chair conformations, respectively.     

X-ray crystal structure and1H-NMR chiral shift reagent study of a crown trimer

3,4,5-Trimethoxybenzyl alcohol was cyclooligomerized with a bentonite clay used as a catalyst. Results of the crystal structure analysis of the racemic (±) nonamethoxy[1,1,1]orthocyclophane trimer, C₃₀H₃₆O₉, are described. The structure was determined by X-ray diffraction at 293 K and shown to belong to the triclinic space group P . The compound possesses a distorted crown conformation with unusual C–H...O intermolecular interactions, and with a crystal packing not observed before in other related derivatives. The racemic mixture was also discriminated in its two enantiomeric isomers, using proton NMR and Eu(III) as a chiral shift reagent.     

Molecular structure and crystal packing of uncomplexed 1,6-bis(N-cyano-p-methoxy-anilino)-2,4-hexadiyne, C22H18N4O2

The X-ray crystal structure of 1,6-bis(N-cyano-p-methoxy-anilino)-2,4-hexadiyne, C₂₂H₁₈N₄O₂, is determined. The crystal packing is dominated by phenyl stacking interactions. Weak C–H···N hydrogen bonds help align the molecules. C–H··· hydrogen bonding is not apparent.     

Synthesis and crystal structure of Bi(mpo)3 (Hmpo = 2-mercaptopyridine N-oxide)

The synthesis as well as crystal and molecular structure of [Bi(C₅H₄NOS)₃] are reported. The complex crystallizes in the monoclinic system, space group P2₁/n with lattice parameters a = 9.6521(3) Å, b = 10.0659(4) Å, c = 18.4484(7) Å, = 102.13(6)°, and D _calc = 2.227 Mg · m^–3 for Z = 4. It is clear from the packing diagram that the title compound is a dimer via the secondary coordination. Surrounding Bi atom, three five-membered ring planes (Bi,O,N,C,S) make a dihedral angle of 55.91, 54.72, and 26.13° respectively. The whole crystal presents a three-dimensional network structure as each molecule produces four weak C–H O hydrogen bonds and a weak C–H S hydrogen bond.     

Synthesis and crystal structure of tripeptide fragment of elastin

Boc-Gly-Val-Pro-OBzl, a protected tripeptide fragment of repeating sequences of mammalian elastic protein elastin was synthesized and characterized by X-ray diffraction method. The sequence C₂₄ H₃₅ N₃ O₆ crystallizes in the orthorhombic space group P2₁2₁2₁ with the parameters a = 9.4700(11) Å, b = 9.8980(8) Å, c = 26.721(3) Å, V = 2504.7(4) ų and Z = 4. The final residual factor is 0.0670. The structure exhibits intra and intermolecular hydrogen bonds.     

Syntheses and crystal structures of two soybean isoflavone derivatives

Two soybean isoflavone derivatives, 7-methoxy-4′-hydroxyisoflavone (1) and 4′, 7-diethoxyl-5-hydroxyisoflavone (2) were synthesized and their crystal structures were determined by single-crystal X-ray diffraction. Two derivatives crystallize in the monoclinic crystal system, space group P2₁/c. The cell dimensions of 1 are a = 8.696(4) Å, b = 11.947(5) Å, c = 12.078(5) Å, β = 93.594(7)^∘, D_c = 1.423 Mg/m³, V = 1252.3(10) ų, Z = 4, and those of 2 are a = 37.672(12) Å, b = 11.228(4) Å, c = 7.582 (3) Å, β = 94.150(6)^∘, D_c = 1.355 Mg/m³, V = 3198.6(18) ų and Z = 8. They have the same isoflavone skeleton which is composed of a benzopyranone moiety and a phenyl moiety. Hydrogen bonding and π < eqid1 > π stacking interactions assemble 1 into supramolecule with a three-dimensional network. And in the crystal structure of 2, hydrogen bonding and C–H ⋅s π stacking interactions lead to the formation of a two-dimensional network.     

Synthesis and crystal structure of 4,5-(cis-cyclohexylenedithio)-1,3-dithiole-2-one

The x-ray crystal structure of 4,5-(cis-cyclohexylenedithio)-1,3-dithiole-2-one has been determined. Yellow block shaped crystals of C₉H₁₀OS₄ crystallize in the space group P with cell dimensions a = 8.872(4), b = 9.330(8), c = 14.333(12) Å, = 95.23(7), = 91.09(5), = 107.60(5)°, V = 1124.8(14) ų, and Z = 4. This compound has two S---S contacts [3.574, 3.610 Å] shorter than 3.70 Å and the usual disordered ethylene moiety [C(3)—C(8)] of the six-membered ring is fixed by the cis-cyclohexylene subsitituent. This means that it may be a new precursor for conducting and strong near-IR absorbing nickel-dithiolenes. Also, it provides the first example of polymorphism of the dmit derivatives and contains two independent molecules I and II in the asymmetric unit.     

Ortho-metalation and carboxylate coordination in the reaction between the dipotassium salt of phthalic acid and Cp*Ir(PMe3)Cl2: X-ray diffraction structure of Cp*Ir(PMe3)[C6H3(CO2)(CO2H)]

The cyclopentadienyl complex Cp*Ir(PMe₃)Cl₂ reacts with the dipotassium salt of phthalic acid in the presence of AgPF₆ via chloride substitution to give the ortho-metalated compound Cp*Ir(PMe₃)[C₆H₃(CO₂)(CO₂H)]. This new compound has been isolated by recrystallization and has been characterized in solution by ¹H and ¹³C NMR spectroscopies, and the solid-state structure has been verified by X-ray crystallography. Cp*Ir(PMe₃)[C₆H₃(CO₂)(CO₂H)] crystallizes in the monoclinic space group P2₁/c, a = 9.1010(6) Å, b = 16.715(1) Å, c = 14.3965(9) Å, = 108.24(1)°, V = 2080.0(2) ų, Z = 4, and d _calc = 1.813 mg/m³; R = 0.0276, R _w = 0.0810 for 2730 reflections with I > 2(I). Coordination of the benzene ring to the iridium center via one of the carboxylate groups and ortho-metalation of the C–H moiety that was to the iridium-bound carboxylate group is confirmed.     

Synthesis and crystal structure of 2-acetylnaphthalen-6-yl 4-methylbenzosulfonate

The title compound has been synthesized by the reaction of 1-(6-hydroxy-2-naphthyl)-1-ethanone (2) with p-toluenesulfonyl chloride. Its structure was determined by single crystal X-ray diffraction. 2-Acetylnaphthalen-6-yl 4-methylbenzosulfonate (3) crystallizes in the orthorhombic space group Pbca with a = 12.727(3) Å, b = 14.560 (3) Å, c = 17.688 (4) Å, V = 3277.8 (11) ų, and Z = 8. The results demonstrate that the dihedral angle between the benzene ring and the naphthalene ring is 116.5^°, and the length (1.417 Å) of single C–O bond of 3 is longer than that of single C–O bond in the relative compounds.     

Synthesis and crystal structure of hexakis(N-methylimidazole) iron(II) pyridine-2-sulfonate

The compound [Fe(C₄H₆N₂)₆][C₅H₄NSO₃]₂ crystallized in the monoclinic space group, P2₁/n with unit cell parameters: a = 13.676(3), b = 8.345(2), c = 18.663(4) Å, = 106.40(3)° and Z = 2. The title compound consists of a [Fe(C₄H₆N₂)₆]⁺² hexacoordinated iron(II) cation and two C₅H₄NSO^– ₃ anions. In the cation the iron atom is coordinated to six N-methylimidazole imine nitrogen atoms in a distorted octahedral arrangement. The N1,N5,N1ⁱ,N5ⁱ atoms are coplanar and the iron lies in this plane.     

Preparation and crystal structure of a quadruply bonded dimolybdenum complex with trans-crotonate ligands

A quadruply bonded dimolybdenum complex with trans-crotonate ligands, Mo₂(O₂CC₃H₅)₄, was synthesized and characterized by UV–VIS, IR, and NMR spectra. The crystal structure was determined by an X-ray single crystal diffraction analysis. The title complex (C₁₆H₂₀O₈Mo₂, M _w = 532.2) crystallized in the triclinic space group P-1 with the following crystallographic parameters: a = 10.236(2) ?, b = 10.393(2) ?, c = 10.524(2) ?, α = 89.59(1)°, β = 73.34(1)°, γ = 70.78(2)°, V = 1008.1(3) ?³, Z = 2, D _c = 1.753 Mg m⁻³, μ(Mo Kα = 0.71073 ?, F(000) = 528, and final R ₁ = 0.041, wR ₂ = 0.114 for observed reflections 2889 (I > 2σ(I)). The Mo₂ ⁴⁺ unit was surrounded by four trans-crotonate ligands resulting in a paddle wheel structure with one disordered trans-crotonate ligand. Molecules are bonded together by means of interactions consisting of the donation of lone pairs of electron on carboxylate O atoms on one molecule to the Mo atom on an adjacent complex. A new pattern of intermolecular bonding is observed.     

Synthesis and crystal structure characterization of (E)-2,2,2-Trifluoro-N-[2-(2-nitrovinyl)phenyl]acetamide

The title compound, (E)-2,2,2-trifluoro-N-[2-(2-nitrovinyl)phenyl]acetamide, was synthesized and characterized by ¹H and ¹³C NMR and HRMS spectroscopy. Its molecular configuration was investigated by X-ray crystallography. The crystal structure analysis revealed that the structure exhibits intermolecular hydrogen bonds of the type N–H…O and intermolecular hydrogen bonds of the type N–H…F, and molecules are linked by weak C–H…O contacts. Furthermore, the two oxygen atoms of nitro group are disordered over two positions, respectively, with site occupancy factors of 0.8:0.2 and 0.6:0.4. Three fluorine atoms are also disordered over two positions, respectively, one fluorine atom with site occupancy factors of 0.6:0.4 and the other two fluorine atoms with site occupancy factors of 0.5:0.5.     

Synthesis and crystal structure of cyanohydrin trimethylsilyl ether of o-chlorobenzoylferrocene

The cyanohydrin trimethylsilyl ether of o-chlorobenzoylferrocene has been synthesized by the addition of trimethylsilyl cyanide (TMSCN) in methylene chloride in the presence of zinc iodide. Its structure was determined by X-ray single crystal diffraction. The crystal belongs to monoclinic, space group P2₁/n with the following crystallographic parameters: a = 9.480(3) ?, b = 22.319(6) ?, c = 9.783(3) ?, β = 101.197(4)°, μ = 0.943 mm^− 1, V=2030.5(10) ?³, Z=4, F(0 0 0) = 880, D _calc=1.386 mg/m³, T=293(2) K, 1.82° ≤ θ ≤ 26.40°, the final R factor: R ₁=0.0366, wR ₂=0.0802.     

Synthesis and crystal structure of [Nd(H2O)2]2(C2O4)3

Some crystals of [Nd(H₂O)₂]₂(C₂O₄)₃ were synthesized hydrothermally by heating at 200°C for 8 days an aqueous suspension of neodymium oxalate decahydrate in presence of terephthallic acid and guanidinium carbonate. They crystallize in the orthorhombic system, space group P2₁2₁2₁, with a = 8.6702(7) Å, b = 9.558(2) Å, and c = 17.009(2) Å. The structure of this complex is built up by two independent neodymium atoms, three bischelating oxalate ligands, and four water molecules forming a rectangle building unit of 6-membered ring, [Ln(H₂O)₂(C₂O₄)]₆. The packing of these units leads to a layer parallel to the plane (001). However, the neodymium atoms of two neighbor layers share an edge of oxalato oxygen atoms thus giving a double-layer. The three dimensionality between these double-layers is insured by hydrogen bonds of water molecules which are bound to the neodymium atoms. There is no zeolitic water molecule. The two neodymium atoms are nine-coordinated. In both cases, the coordination polyhedron can be described as a distorted tricapped trigonal prism.     

Synthesis and crystal structure of 3,5,9,11-tetraacetyl-14-oxo-1,3,5,7,9,11-hexaazapentacyclo[5.5.3.02,6.04,10.08,12]pentadecane

Crystals of 3,5,9,11-tetraacetyl-14-oxo-1,3,5,7,9,11-hexaazapentacyclo[5.5.3.0^2,6.0^4,10 .0^8,12]pentadecane, a new hexaazaisowurtzitane derivative, were obtained from a condensation reaction of 2,6,8,12-tetraacetyl-2,4,6,8,10,12-hexaazatetracyclo[5.5.0.0^5,9.0^3,11] dodecane with aqueous formaldehyde and subsequent crystallization of the product from aqueous acetone. X-ray diffraction analysis at room temperature indicates that the compound crystallizes in monoclinic system, space group P2₁/n with a = 9.4564(15), b = 14.184(2), c = 13.334(2) ?, β = 107.671(4)°, V = 1704.1(5) ?³, Z = 4, D _calc = 1.475 g/cm³, F(000) = 800, μ(MoK) = 0.112 mm⁻¹, and final R ₁ = 0.0505, wR ₂ = 0.1215 for observed reflections 2641 (I > 2σ(I)). The ether link (C–O–C) forms two heptacyclic rings with the N, C atoms in the cage respectively. The results of elemental analysis, IR and NMR spectroscopy are included.     

Synthesis and crystal structure of K3Sb4BO13

K₃Sb₄BO₁₃, Mr = 823.11 g.mol^–1, crystallizes in the triclinic system, space group P , Z = 2. The lattice parameters are a = 7.133(1) Å, b = 7.232(1) Å, c = 13.259(2) Å, = 82.00 (1)°, = 99.77(1)° and = 117.08(1)°, V = 598.7(2) ų, D_x = 4.566 Mg m^–3. The final R index and weighted R_w index are 0.0251 and 0.0623, respectively. The three-dimensional network of the title compound is constituted by layers (Sb₃O₉)_n, similar to that of hexagonal bronze of Magneli. These layers are linked together, in the c direction, alternatively by edge-sharing pairs of SbO₆ octahedra and BO₃ triangles. This framework has interconnected tunnels, running approximately along the a and b directions, in which the K⁺ ions are located.