Synthesis and Crystal Structure of Dibromido{2-[(4-tert-butylmethylphenyl) iminomethyl]pyridine-κ<Superscript>2</Superscript><Emphasis Type="Italic">N</Emphasis>,<Emphasis Type="Italic">N'}</Emphasis>Zinc

The title compound [Zn(dip)Br₂] was synthesized using the Schiff base bidentate ligand (E)-4-tert-butyl-N-(pyridine-2-ylmethylene)benzeneamine (dip) and zinc(II) bromide salts. It has been characterized by elemental analysis, X-ray diffraction, and optical spectroscopy. The X-ray diffraction analysis demonstrates that in this structure, the zinc(II) ion is located on an inversion center and exhibits a ZnN₂Br₂ tetrahedral geometry. In this structure the dip ligand is coordinated with zinc(II) ion in a cyclic-bidentate fashion forming a five-membered metallocyclic ring. The compound crystallizes in the monoclinic sp. gr. P2₁/m with a = 9.2700(13) Å, b = 7.6128(11) Å, c = 12.3880(17) Å, and β = 97.021(3)°.     

Synthesis and Crystal Structure of Di-μ-chlorido-bis{chlorido[4-ethyl-<Emphasis Type="Italic">N</Emphasis>-(pyridin-2-ylmethylidene-κ<Emphasis Type="Italic">N</Emphasis>)aniline-κ<Emphasis Type="Italic">N</Emphasis>]mercury(II)}

The centrosymmetric dinuclear title complex [Hg₂Cl₄(dip)₂] was synthesized using the Schiff base bidentate ligand (E)-4-ethyl-N-(pyridine-2-ylmethylene)benzeneamine (dip) and mercury(II) chloride salts. It has been characterized by elemental analysis, X-ray diffraction, and UV-Visible and infrared spectroscopic techniques. The X-ray analysis shows that the title compound crystallizes in the monoclinic sp. gr. P2₁/n, Z = 2 with a = 7.8233(17) Å, b = 15.178(3) Å, c = 12.559(3) Å, β = 97.021(3)°. The Hg(II) ion has a distorted trigonal–bipyramidal coordination environment formed by the bischelating N-heterocyclic ligands, two bridging Cl atoms and one terminal Cl atom.     

Synthesis,Characterization, and Crystal Structure of <Emphasis Type="Italic">N</Emphasis>-<Emphasis Type="Italic">p</Emphasis>-Bromophenyl-<Emphasis Type="Italic">N</Emphasis>′-Phenylacetylthiourea

Abstract   N-p-bromophenyl-N′-phenylacetylthiourea was characterized by elemental analysis, IR and ¹H NMR etc. Single crystal structure of the title compound was determined on X-ray diffraction instrument. The title compound crystallizes in monoclinic space group c2/c, with a = 21.442(5) ?, b = 12.208(2) ?, c = 11.955(2) ?, β = 109.375(4)°, and D _calc = 1.571 g/cm³ for Z = 8. An intermolecular hydrogen bond N–H···S which links two thiourea molecules as a dimer and an offset face-to-face π–π stacking interaction were observed in the title compound. The strong non-covalent interaction influences the conformation and property of thiourea derivatives. Index Abstract  The title compound, N-p-bromophenyl-N′-phenylacetylthiourea, was synthesized by the treatment of phenylacetyl chloride with 4-bromoaniline and its crystal structure determined. Single crystal X-ray diffraction analysis reveals that hydrogen bonds and face-to-face π–π stacking interactions have strong influence on the conformation and molecular stacking of the title compound.      

Synthesis and crystal structure of <Emphasis Type="Italic">N</Emphasis>-(6methoxylbenzothiazol-2-yl)-1-(4-fluorophenyl)<Emphasis Type="Italic">O</Emphasis>,<Emphasis Type="Italic">O</Emphasis>-dipropyl-<Emphasis Type="Italic">α</Emphasis>-aminophosphonate

Molecular and crystal structure of N-(6-methoxybenzothiazol-2-yl)-1-(4-fluorophenyl)-O,O-dipropyl-α-aminophosphonate, C₂₁H₂₆FN₂O₄PS, have been determined by single-crystal X-ray diffraction study. The title compound is tetragonal, with a = 21.35(3) Å, c = 20.16(5) Å, Z = 16, D _x = 1.308 Mg/m³, μ(MoKα) = 0.247 mm^?1, and space group is I4₁/a. The structure was solved by direct method and refined to a final R = 0.0687 for 2370 reflections with I > 2σ(I). The compound shows a fully delocalized benzothiazole system with a sp² hybridization of the N(2). There is a strong intermolecular hydrogen bond between P=O and NH. The crystal structure is stabilized by a strong intermolecular N–H?sO hydrogen bond.     

Synthesis and Crystal Structure of New <Emphasis Type="Italic">N</Emphasis>,<Emphasis Type="Italic">N</Emphasis>′-Bis[1-(4-methoxyphenyl)-5-methyl-1<Emphasis Type="Italic">H</Emphasis>-1,2,3-triazole-4-carbonyl]hydrazide

Abstract  The N,N′-bis[1-(4-methoxyphenyl)-5-methyl-1H-1,2,3-triazole-4-carbonyl]hydrazide 6 was synthesized from aryl triazole acids and its structure is established by MS, IR, and ¹H NMR spectral data. Compound 6, C₂₂H₂₂N₈O₄, Mr = 462.48, crystallizes in the monoclinic space group P2(1)/c with unit cell parameters a = 15.3451(8), b = 8.6486(4), c = 16.8502(9) ?, α = 90.00, β = 95.731(2), γ = 90.00o, V = 2225.1(2) ?³, Z = 4, and Dx = 1.381 mg m⁻³. The final R was 0.0450. The four aromatic rings are close to linear because of N···H–N hydrogen bonds. Index Abstract  Synthesis and crystal structures of N,N′-bis[1-(4-methoxyphenyl)-5-methyl-1H-1,2,3-triazole-4-carbonyl]hydrazide Heng-Shan Dong, Yan-Fei, Wang, Hong-Ru Dong, Bin, Wang, Bin Quan N,N′-Bis[1-(4-methoxyphenyl)-5-methyl-1H-1,2,3-triazole-4-carbonyl]hydrazide was synthesized.      

Synthesis,Characterization and Crystal Structure of <Emphasis Type="Italic">N,N</Emphasis>′-di[(<Emphasis Type="Italic">E</Emphasis>)-1-(2-hydoxyphenyl)methylidene]-2,6-naphthalenedicarbohydrazide

Abstract  

A new bishydrazone compound, N,N′-di[(E)-1-(2-hydoxyphenyl)methylidene]-2,6-naphthalenedicarbohydrazide (1), has been prepared by condensation reaction of 2,6-naphthalenedicarbohydrazide with salicylaldehyde in ethanol, and characterized by elemental analysis, FT-IR, ¹H- and ¹³C-NMR, ESI–MS and single-crystal X-ray diffraction analysis. The crystal of 1·2DMF belongs to monoclinic, space group P2(1)/n with a = 10.454(1), b = 7.711(1), c = 18.801(2) ?, β = 93.364(1)°, V = 1512.9(3) ?³, Z = 2, D _c  = 1.314 g cm⁻³, μ = 0.093 mm⁻¹, F(000) = 632, Mr = 598.65, the final R ₁ = 0.0861 and wR ₂ = 0.2279 for 7243 observed reflections with I > 2σ(I). The structural analysis reveals that compound 1·2DMF contains one N,N′-di[(E)-1-(2-hydoxyphenyl)methylidene]-2,6-naphthalenedicarbohydrazide molecule and two N,N-dimethylformamide solvent molecules. A 2D supramolecular structure of 1·2DMF was constructed by multiple intermolecular N–H···O and C–H···O hydrogen bonds.     

Synthesis and Crystal Structure of Bis (<Emphasis Type="Italic">N</Emphasis>,<Emphasis Type="Italic">N</Emphasis>,<Emphasis Type="Italic">N</Emphasis>′,<Emphasis Type="Italic">N</Emphasis>′-tetramethylethylendiammonium) Octaiodo Pentachloroantimonate (III)

Abstract  

The synthesis and Crystal structure are given for the bis (N,N,N′,N′-tetramethylethylendiammonium) octaiodo pentachloroantimonate (III) salt. An X-ray investigation has shown that the title compound crystallizes in a monoclinic system, space group P2₁/m with the following lattice parameters a = 9.786(2) Ǻ, b = 14.024(5) Ǻ, c = 14.336(3) Ǻ, β = 91.35(2)° and Z = 2. The structure was solved from 3085 independent reflections with R ₁ = 0.0402 and wR ₂ = 0.0952 and refined with 152 parameters. The structure shows a layer arrangement perpendicular to the [(b)\vec] \vec{b} -axis: planes of [SbCl₅]²⁻, I₃ ⁻ and I₅ ⁻ anions alternate with planes of [(CH₂)₂(NH(CH₃)₂)₂]²⁺ cations. The [SbCl₅]²⁻ square pyramids present an active lone electron pair (LEP) on the Sb atoms and they are interconnected by means of N–H···Cl hydrogen bond originating from [(CH₂)₂(NH(CH₃)₂)₂]²⁺ entities. The polyiodides (I₃ ⁻ and I₅ ⁻) anions form a planer zigzag polymeric chains via I···I linking interactions. These chains are linked to the [SbCl₅]²⁻ anions by a long range contact.     

Synthesis and crystal structure of <Emphasis Type="Italic">catena</Emphasis>-bis(nicotinamide)aqua(μ-phthalato)copper(II) hemihydrate

The copper(II) phthalate complex with nicotinamide [CuL ₂(μ-Pht)(H₂O)] · 0.5H₂O(I) (where L is nicotinamide and Pht ^2? is an anion of phthalic acid) is synthesized and investigated using IR spectroscopy and X-ray diffraction. The crystals of compound I are monoclinic, a = 13.368(2) Å, b = 7.891(3) Å, c = 20.480(2) Å, β = 108.69(2)°, Z = 4, and space group P2₁/c. The structural units of crystal I are linear chains formed by bridging phthalate anions and crystallization water molecules. The copper atom is coordinated by two pyridine nitrogen atoms of two nicotinamide ligands (Cu-N, 2.001 and 2.045 Å), two oxygen atoms of different phthalate anions (Cu-O, 1.964 and 2.235 Å), and the oxygen atom of the H₂ O molecule (Cu-O, 2.014 Å). The coordination polyhedron of the copper atom is completed to an elongated (4 + 1 + 1) tetragonal bipyramid by the second (chelating) oxygen atom of the carboxyl group (Cu-O, 2.587 Å), which is one of the anions of phthalic acid. The linear polymer molecules are joined into complex macromolecular dimers with the closest internal contacts of the specific type. The macromolecular dimers are the main supramolecular ensembles of the crystal structure.     

Crystal Structure of a Novel One-dimensional Chain-like Compound,Catena(μ<Subscript>2</Subscript>-4,4′-Bipyridyl)-bis(Formato-<Emphasis Type="Italic">O</Emphasis>,<Emphasis Type="Italic">O′</Emphasis>)-Copper(II)

Abstract  

The title compound, [Cu(C₁₀H₈N₂)(HCO₂)₂]_n, in which the asymmetric unit contains one crystallographically independent copper(II) ions, one formate and half of 4, 4′-bipy molecules, has a linear polymeric structure, with the bridging ligand 4, 4′-bipyridine connecting the Cu^II ions. Each ion lies on an inversion center and has a distorted octahedral environment, being coordinated by two bipy ligands and four oxygen atoms from two formate groups. The O1 in the formate group is disordered over two sites with occupancy of 0.55 and 0.45. In the crystal structure, the linear polymeric chains are linked by intermolecular C–H···O hydrogen bonds, resulting in a two-dimensional supramolecular network.     

Intermolecular Hydrogen Bonds and the Supramolecular Structure of <Emphasis Type="Italic">N</Emphasis>,<Emphasis Type="Italic">N</Emphasis>′-Bis(<Emphasis Type="Italic">p</Emphasis>-tolylsulfonyl)diethylenetriamine

Abstract  The title compound N,N′-bis(p-tolylsulfonyl)diethylenetriamine (1) was synthesized and its crystal structure determined by X-ray diffraction. Adjacent molecules of 1, symmetrically related through a c-glide, are linked by alternating hydrogen bonds that form molecular chains along [0 0 1]. Two molecular chains occur in each unit cell and pack to form alternating layers in a three-dimensional supramolecular structure. The compound crystallizes in the Pca2₁ space group stabilized by the inclusion of solvent dichloromethane molecules in structural voids between molecules of 1. The dichloromethane molecules are related through a twofold screw rotation axis and are not disordered. Index Abstract  Intermolecular hydrogen bonds involving sulfonamide moieties of title compound afford a supramoleular structure that accommodates the inclusion of dichloromethane in alternating layers.      

Synthesis,Crystal Structure and Bioactivities of <Emphasis Type="Italic">N</Emphasis>-(2,6-Difluorobenzoyl)-<Emphasis Type="Italic">N</Emphasis>′-[5-(Pyrid-4-yl)-1,3,4-Thiadiazol-2-yl]Urea

Abstract N-(2,6-difluorobenzoyl)-N′-[5-(pyrid-4-yl)-1,3,4-thiadiazol-2-yl]urea, 3, has been synthesized by reaction of 2-amino-5-(pyrid-4-yl)-1,3,4-thiadiazole with 2,6-difluorobenzoyl isocyanate, and its structure was characterized with X-ray crystallographic, NMR, MS and IR techniques. It crystallizes in the triclinic space group P − 1, with a = 7.0821(9) ?, b = 9.4896(13) ?, c = 11.6594(15) ?, α = 82.311(2)°, β = 82.328(2)°, and γ = 87.641(2)°. In the title compound, the urea scaffold in each molecule is essentially planar due to the presence of intramolecular N–H···O hydrogen bond. The molecules are linked by intermolecular complementary N–H···O hydrogen bonds into centrosymmetric R ₂²(8) dimers. Intermolecular π–π stacking interactions are also present. The preliminary bioassay shows that the title compound exhibits excellent fungicidal activities against Rhizoctonia solani, Botrytis cinerea and Dothiorella gregaria. Index Abstract N-(2,6-difluorobenzoyl)-N′-[5-(pyrid-4-yl)-1,3,4-thiadiazol-2-yl]urea has been synthesized and characterized with X-ray crystallographic, NMR, MS and IR techniques. The preliminary bioassay shows that the title compound exhibits excellent fungicidal activities.      

Crystal structure of Сu<Subscript>2–<Emphasis Type="Italic">m</Emphasis></Subscript>Te (<Emphasis Type="Italic">m</Emphasis> = 0.25)

The Сu₂Te compound has been synthesized by alloying Сu and Te taken in stoichiometric ratios. A Сu₂Te sample has been homogenized by annealing at 773 K for 100 h. A pure copper phase in the form of thin filaments is found to segregate from the synthesized product (4 g) by the end of annealing. It is established by X-ray diffraction analysis that the copper-deficient sample is crystallized into the trigonal system with lattice parameters а = 8.328(1) Å, с = 7.196(1) Å, V = 432.2(1) ų, sp. gr. \(P\overline 3 m1\), Z = 8. The crystal structure is determined and the sample composition Сu_2–m Te (m = 0.25) is refined by the Rietveld method. The three independent copper atoms in the lattice are found to have different coordination numbers: 3, 4, and 5.     

Crystal structure of [<Emphasis Type="Italic">N</Emphasis>-(2-aminoethyl)iminodiacetato](1,10-phenanthroline)copper(II) tetrahydrate, [Cu(<Emphasis Type="Italic">Aeida</Emphasis>)(<Emphasis Type="Italic">Phen</Emphasis>)] · 4H<Subscript>2</Subscript>O

Crystals of [N-(2-aminoethyl)iminodiacetato](1,10-phenanthroline)copper(II) tetrahydrate, [Cu(Aeida)(Phen)] · 4H₂O (I), are obtained, and their structure is determined. Crystals I are triclinic, and the unit cell parameters are as follows: a = 8.341(1) Å, b = 9.424(1) Å, c = 13.864(2) Å, α = 74.23(1)°, β = 79.25(1)°, γ = 82.67(1)°, Z = 2, and space group P1. The structural units of the crystal are [Cu(Aeida)(Phen)] molecular complexes and crystallization water molecules. The coordination polyhedron of the copper atom is a tetragonal bipyramid with four nitrogen atoms in the equatorial plane (mean Cu-N, 2.05 Å) and two oxygen atoms of the acetate groups in axial positions (Cu-O, 2.264 and 2.426 Å; O-Cu-O angle, 148.8°). The Aeida and Phen ligands fulfill the tetradentate (2N + 2O) chelate and bidentate (2N) chelate functions, respectively. The complexes are joined into dimer associates in which the interplanar spacing between Phen molecules is equal to 3.54 Å and the Cu?Cu distance is 7.02 Å.     

Synthesis and Structure Determination of <Emphasis Type="Italic">S</Emphasis>,<Emphasis Type="Italic">S</Emphasis>′-(Naphthalen-2-ylmethyl sulfanyl (1-<Emphasis Type="Italic">p</Emphasis>-tolyl-ethylidene) Hydrazine

Abstract  

S,S′-(Naphthalen-2-ylmethyl sulfanyl (1-p-tolyl-ethylidene) hydrazine (SNM4MA) was prepared by the condensation of S-napthalen-2-ylmethyldithiocarbazate (SNMDTC) and 4-methylacetophenone. Yellow needles of SNM4MA were obtained upon slow evaporation of a 50:50 mixture of acetonitrile and DMSO over a period of weeks. The compound crystallizes in the monoclinic system with the space group C 2/c and Z = 4. The unit cell parameters are a = 7.0221(2) ?, b = 22.8428(6) ?, c = 23.5127(6) ? with β = 94.0222(13)°. Single crystal X-ray analysis shows that the molecule has crystallographic two-fold rotational symmetry coincident with the S–S bond. The title compound exists as a trans–cis conformer in which the naphthalene group is trans with respect to the thione sulfur while the benzyl group adopts a cis geometry. ¹³C and ¹H spectra confirm that the dimeric nature is retained in DMSO solution.     

Synthesis,Crystal Structure Properties of {μ-Nitrato-[<Emphasis Type="Italic">N</Emphasis>,<Emphasis Type="Italic">N</Emphasis>′-ethylene-bis(3-methoxysalicylideneimin) diaqua nitrato Cu(II)La(III)]nitrat}

Abstract  

The [μ-NO₃-LCuLa(NO₃)·(H₂O)₂]NO₃ (I) complex has been prepared and characterized by single crystal X-ray diffraction properties. The title compound crystallizes in the monoclinic system, space group P 2₁/c, with a = 9.1699(4), b = 21.6796(8), c = 13.7068(6) ?, α = γ = 90o, β = 111.308(3)°, V = 2538.63 (18) ?³ and Z = 4. The unit cell contains four discrete the title compounds. The central region is occupied by Cu^II and La^III ions which are brigged by two phenolato oxygen atoms of ligand. The intramolecular La–Cu distance is 3.5016 (3) Ǻ. The copper (II) ion is in a distorted square pyramidal geometry with the imino nitrogen atoms N1 and N2, and the phenolic oxygen atoms O2 and O3 forming the square base. The La^III ion is deca coordinated.     

Crystal Structure of Trinuclear Nickel(II) Complex with Schiff Base Ligand of <Emphasis Type="Italic">N</Emphasis>,<Emphasis Type="Italic">N</Emphasis>′-Bis(Salicylidene)-1,3-Diiminopropane

Abstract  

A linear trinuclear nickel complex containing the ligand, N,N′-bis(salicylidene)-1,3-diiminopropane(H₂Salpn), is synthesized and characterized by elemental analysis, thermogravimetric analysis, IR spectroscopy and X-ray diffraction techniques. The title complex contains two different molecules, [Ni₃(Salpn)₂(CH₃COO)₂(DMF)₂](1) and [Ni₃(Salpn)₂(CH₃COO)₂(CH₃OH)₂]·2CH₃OH(2). Both molecules are constructed by two mononuclear NiSalpn units linked by a central Ni(II) ion and two bridging acetate anions, the difference between them is: molecule (1) contains two coordinated DMF molecules, while molecule (2) contains two coordinated methanol molecules and two hydrogen bond linked methanol molecules. All the Ni(II) ions are coordinated in disorted octahedral geometry. The crystal of the title complex(formula C₈₆H₁₀₆N₁₀Ni₆O₂₂, M _r 1,984.07) belongs to triclinic system, space group Pī(2) with the following crystallographic parameters: a = 12.1506(11) Å, b = 13.3601(12) Å, c = 14.8600(13) Å, α = 84.894(2)°, β = 70.101(2)°, γ = 81.899(2)°, V = 2243.9(3) ų, Z = 1, Dc = 1.468 g cm⁻³, μ = 1.310 mm⁻¹, F(000) = 1,036, and the final R indices[[I > 2σ(I)]: R ₁ = 0.0545, wR ₂ = 0.1052.     

X-ray Structure of <Emphasis Type="Italic">mer</Emphasis>-[Mo(CO)<Subscript>3</Subscript>(PPh<Subscript>3</Subscript>)(<Emphasis Type="Italic">κ</Emphasis><Superscript>2</Superscript>-dppm)]

Abstract  

Treatment of [Mo(CO)₃(NCMe)₃] with bis(diphenylphosphino)methane (dppm) and triphenylphosphine (PPh₃) at 50 °C afforded mer-[Mo(CO)₃(PPh₃)(κ ²-dppm)] (1) in 55% yield which has been characterized by single crystal X-ray diffraction studies and spectroscopic measurements. Compound 1 crystallizes in the triclinic space group P−1 with a = 10.3449(6), b = 11.1570(6), c = 17.8961(10) ?, β = 80.8400(10)°, Z = 2 and V = 1959.8(2) ?³.     

Synthesis,Crystal Structures and Physicochemical Properties of Poly[bis(<Emphasis Type="Italic">N</Emphasis>,<Emphasis Type="Italic">N</Emphasis>-Dimethylformamide)tetra(thiocyanato)metal(II) Mercury(II)] (Metal = Cadmium and Manganese)

Abstract  

Two novel single crystals, poly[bis(N,N-dimethylformamide)tetra(thiocyanato)metal(II)mercury(II)] (metal = cadmium and manganese, abbreviated as DTCM and DTMM, respectively) were prepared. The characterizations of DTCM and DTMM were performed by elemental analyses, infrared, X-ray single crystal diffraction. The two title complexes crystallized in the same monoclinic crystallographic system and P2₁/n space group with unit cell parameters: a = 9.2515(2) Å, b = 14.1670(3) Å, c = 16.5898(3) Å, β = 93.0320(10)°, z = 4, D _x  = 2.115 g/cm³ for DTCM, and a = 9.24580(10) Å, b = 14.1110(2) Å, c = 16.4937(2) Å, β = 92.9120(10)°, z = 4, D _x  = 1.960 g/cm³ for DTMM, respectively. The two structures are isostructural. The thermal decomposition processes of the two crystals were investigated by means of thermogravimetric analysis and differential thermal analysis measurements in air.     

Solid-state Spectroscopic and Structural Investigation of <Emphasis Type="Italic">cis</Emphasis>-(CH<Subscript>3</Subscript>)<Subscript>2</Subscript>Au(<Emphasis Type="Italic">O</Emphasis>,<Emphasis Type="Italic">O</Emphasis>′-acac)

Abstract  The structure of cis-(CH₃)₂Au(O,O′-acac) was investigated by single-crystal X-ray diffraction. It crystallizes in the orthorhombic space group Cmca with unit cell dimensions a = 6.7831(13) ?, b = 15.080(3) ?, c = 18.073(3) ? and α = β = γ = 90°. The molecule is planar but lacks a C₂ axis in the solid-state, with two Au–C bond lengths that differ by 0.078(21) ? due to crystal packing effects. The inequivalence of the crystallographic carbon positions is evident in the solid-state ¹³C CP-MAS NMR spectrum, which was recorded at low temperature due to the thermal sensitivity of the compound during magic-angle spinning. Head-to-tail stacking, which creates short intermolecular paths, was reproduced computationally in a dimer model. Graphical Abstract   Solid-state Spectroscopic and Structural Investigation of cis -(CH ₃ ) _Au 2 ( O , O ′-acac) Miyako Hisamoto • Swarup Chattopadhyay • Juergen Eckert • Guang Wu • Susannah L. Scott In the solid state, cis-(CH₃)₂Au(O,O′-acac) has no C₂ axis, two different Au–C bond lengths (1.960, 2.038 ?; Δd = 0.078(21) ?) and a close Au–C…C–Au contact; these features give rise to additional features in the ¹³C CP-MAS NMR spectrum.     

X-ray Structure Investigation of 20-<Emphasis Type=\"Italic\">O</Emphasis>-β-<Emphasis Type=\"SmallCaps\">d</Emphasis>-glucopyranosyl-20(<Emphasis Type=\"Italic\">S</Emphasis>)-protopanaxadiol

Abstract  20-O-β-d-glucopyranosyl-20(S)-protopanaxadiol (I) has been isolated as a metabolite of ginseng saponins by Paecilomyces bainier. The crystal structure of (I) was also investigated by single crystal X-ray diffraction analysis. It crystallizes in the monoclinic space group P2₁, with a = 15.99 2 (3) ?, b = 11.960 (19) ?, c = 20.127 (3) ?, β = 101.85 (4)°, and V = 3767.5 (11) ?³, Z = 4, R _int = 0.1129, ωR(F ²) = 0.1749, F(000) = 1,448. The title compound is a dammarane-type triterpenoid, and the four rings of this compound connect with each other in trans characteristics,with the three-six-membered rings in chair conformation and the five-membered ring adopting envelope one. A β-d-glucopyranosyl group and a 2-methyl-2-pentenyl group connect to C20 of S configuration. The space symmetrical motif is adopted and each packing unit-cell contains two symmetrical compound (I) molecules and four H₂O molecules. The hydrogen-bonding (both intra- and inter-molecular) interactions play a major role in this structural association. Index Abstract  In the present paper, the single-crystal structure of 20-O-β-d-glucopyranosyl-20(S)-protopanaxadiol was determined by X-ray analysis