Structural investigation of five N-arylsulfonyloxazolidines

The crystal structures of (1R,5R,8S)-8-[(2R,4R)-4-ethyl-3-(2,4,6- trimethyl-benzenesulfonyl)-oxazolidin-2-yl]-1-hydroxy-bicyclo[3.3.1]nonan-3-one (1), formic acid (1S,2R)-2-{2-[(2R,4R)-4-ethyl-3-(toluene-4-sulfonyl)-oxazolidin-2-yl]-cyclohexylidene}-1-trimethylsilanyl-ethyl ester (2), (2R,4R)-2-{(4S,5R,6S)-6-tertbutyl-2,2,4,5-tetramethyl-[1,3]dioxan-4-yl}-4-ethyl-3-(toluene-4-sulfonyl)-oxazolidine (3), (2S)-2-[(2R,4R,5R)-4-methyl-5-phenyl-3-(toluene-4-sulfonyl)-oxazolidin-2-yl]-3,4-dihydro-2H-naphthalen-1-one (4) and (1R)-1-[(2R,4R,5R)-4-methyl-5-phenyl-3-(toluene-4-sulfonyl)-oxazolidin-2-yl]-3,4-dihydro-1H-naphthalen-2-one (5) have been determined: (1) crystallizes in the orthorhombic space group P2₁2₁2₁ with cell dimensions a = 11.120(1), b = 13.809(1), c = 14.676(1) Å, (2) crystallizes in the monoclinic space group P2₁ with cell dimensions a = 12.577(3), b = 9.589(1), c = 13.971(3) Å, = 95.77(1) °, (3) crystallizes in the monoclinic space group P2₁ with cell dimensions a = 7.990(4), b = 11.282(9), c = 14.473(4) Å, = 96.31(3)°, (4) crystallizes in the orthorhombic space group P2₁2₁2₁ with cell dimensions a = 7.674(1), b = 14.647(1), c = 20.620(1) Å, (5) crystallizes in the monoclinic space group P2₁ with cell dimensions a = 7.890(2), b = 11.319(1), c = 13.493(3) Å, = 104.12(1)°.     

Diels-Alder reactions of 2,3-bis-(phenylthio)-1,3-butadiene: X-ray and NMR structural investigations ofcis andtrans-1,2-bis-(phenylthio)-4,5-dimethoxycarbonyl-1-cyclohexene

The Diels-Alder reaction of 2,3-bis-(phenylthio)-1,3-butadiene (4), derivedin situ by thermal extrusion of sulfur dioxide from 3,4-bis-(phenylthio)-2,5-dihydrothiophene-1,1-dioxide (3), with dimethyl fumarate gavetrans-1,2-bis-(phenylthio)-4,5-dimethoxycarbonyl-1-cyclohexene (1). Similarly, the reaction of4 with maleic anhydride gavecis-4,5-bis-(phenylthio)-4-cyclohexene-1,2-dicarboxylic anhydride(5), which was converted intocis-1,2-bis-(phenylthio)-4,5-dimethoxycarbonyl-1-cyclohexene (2). The characterization of1 and2 included a single-crystal X-ray diffraction study of 1, simulations of portions of their¹H NMR spectra, and homonuclear decoupling experiments. The cyclohexene rings of1 and2 are in half-chair conformations with diequatorial and axial-equatorial diester groups, respectively.     

Crystal structure of (E)-5-hydroxypyrrolizidin-3-one and (Z)-5-thioketalpyrrolizidin-3-one

The crystal structures of (E)-5-hydroxypyrrolizidin-3-one (2) and (Z)-5-thioketalpyrrolizidin-3-one (3) have been determined by single-crystal x-ray diffraction techniques and refined by full-matrix least squares. Molecule2 crystallizes in the monoclinic space groupP2₁/a(No. 14) witha=7.887(3) Å,b=9.788(5) Å,c=9.316(4) Å,=100.6(1), andZ=4. Molecule 3 crystallizes in the monoclinic space groupP2₁/c witha=12.947(14) Å,b=10.553(14) Å,c=9.629(14) Å,=101.4(1), andZ=4. The calculated density for both molecules is 1.33 g cm^–1. FinalR-factors were 5.1% for2 and 8.59% for3. The x-ray results showed that a change in configuration occurred in the reaction going from2 to3.     

Synthesis and Crystal Structures of Methyl 3-(Benzoylamino)-6-methyl-2-oxo-2<Emphasis Type="Italic">H</Emphasis>-pyran-5-carboxylate and <Emphasis Type="Italic">N</Emphasis>-[5-(3,4-Dimethoxyphenyl)-6-methyl-2-oxo-2<Emphasis Type="Italic">H</Emphasis>-pyran-3-yl]benzamide

Abstract  

The compounds methyl 3-(benzoylamino)-6-methyl-2-oxo-2H-pyran-5-carboxylate (1), C₁₅H₁₃NO₅, and N-[5-(3,4-dimethoxyphenyl)-6-methyl-2-oxo-2H-pyran-3-yl]benzamide (2), C₂₁H₁₉NO₅, crystallize as a centrosymmetric hydrogen-bonded dimer facilitated by N–H···O interactions involving the amide and carbonyl moiety of the lactone group of adjacent molecules. Supramolecular aggregation in 1 is controlled by a combination of π–π interactions [centroid–centroid distance = 4.0745(11) ?] and weak C–H···O hydrogen bonding between the phenyl ring of the benzoylamino group and the carbonyl atom of the methoxycarbonyl group and in 2 by a combination of π–π interactions [centroid–centroid distance = 4.0699(8) and 4.1556(10) ?], weak C–H···O interactions between the methoxy substituents of the adjacent dimethoxyphenyl group and weak C–H··· π 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.     

Synthesis and crystal structures of two novel 3,4,5- trimethoxyphenyl derivatives from (Z)-1-[(2′,3′-dinitro-4′-methoxy)-phenyl]-2-[(3″,4″,5″-trimethoxy)-phenyl] ethene

The title compounds, (Z)-1-[(2′,4′-dimethoxy-3′-nitro)-phenyl]-2-[(3″,4″,5″-trimethoxy)-phenyl]ethene, C₁₉H₂₁O₇N (I), and 2-amino-4-methyl-6-(3,4,5-trimethoxy-phenyl)-pyrimidine, C₁₄H₁₇O₃N₃ (II), were obtained unexpectedly from a reaction involving (Z)-1-[(2′,3′-dinitro-4′-methoxy)-phenyl]-2-[(3″,4″,5″-trimethoxy)-phenyl]ethene (IV). The molecular structures of these compounds were obtained by single-crystal X-ray diffraction. Crystallization of I occurs in the centrosymmetric monoclinic space group P2₁/c (No. 14) with a=7.7311(5), b=19.9239(13), c=11.5725(8); and β=92.193(3) and Z=4. Crystallization of II occurs in the centrosymmetric monoclinic space group C2/c (No. 15) with a=21.296(2), b=6.8963(7), c=20.001(2); and β=114.121(6) and Z=8. Details of the synthesis and the structural characterization of the title compounds are presented and discussed.     

Structure of 4-(2-chloro-4,5-dimethoxybenzylidene)-2-methyl-5-oxazolone. X-ray and NMR study

The azlactone of 6-chloroveratraldehyde 3 (4-(2-chloro-4,5-dimethoxybenzylidene)-2-methyl-5-oxazolone) was synthesized from 6-chloroveratraldehyde 2 and its structure investigated using X-ray crystallographic and nuclear magnetic resonance methods. Compound 3 crystallized in the P2₁/c (#14) space group (Z = 4) with cell dimensions a = 9.148(2), b = 22.938(2), c = 6.707(1) Å, and = 111.50(2)°. The X-ray study shows that azlactone 3 exists as the Z-isomer and crystallizes as a planar structure, i.e., both the phenyl and azlactone ring systems, as well as the functional groups attached to them, lie in the same plane. The ¹H and ¹³C NMR spectral values also support the formation of the Z-isomer only, during the synthesis of 4-(2-chloro-4,5-dimethoxybenzylidene)-2-methyl-5-oxazolone.     

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.     

X-ray diffraction, DFT, and spectroscopic study of N , N ′-difluoroboryl-5-(2-thienyl)dipyrrin and fluorescence studies of related dipyrromethanes, dipyrrins and BF2-dipyrrins and DFT conformational study of 5-(2-thienyl)dipyrrin

To explore the characteristics of potential fluorescent probes that could be used to screen prospective HDS catalysts, new 5-thienyl dipyrromethene derivatives have been prepared. 5-(2-thienyl)- (1a), 5-(3-thienyl)- (1b), and 5-(3-(2,5-dibromothienyl))-dipyrromethane (1c), were oxidized with DDQ (2,3-dichloro-5,6-dicyano-1,4-benzoquinone) separately to give the corresponding dipyrrins 2a–2c. These were subsequently treated with F₃B·OEt₂ to afford the respective N,N′-difluoroboryl-5-(thienyl)dipyrrin compounds, 3a–3c; the latter two may serve as polymer precursors. Significant fluorescence signal enhancement is achieved with 3a–3c over 2a–2c. Orange fluorescence is observed for 3a whereas its isomer 3b gives green fluorescence (365 nm). An X-ray diffraction study of 3a was performed (orthorhombic, P2₁2₁2₁, a=10.684(10) ?, b=15.208(13) ?, c=7.256(6) ?, V=1179.0(17) ?³, Z=4, R ₁=0.0428, wR ₂=0.0686) and its geometry was studied by way of DFT (Gaussian 03; B3LYP/6-31G^*) to give a HOMO/LUMO energy level difference of 414 nm, and a 2-thienyl group rotational barrier of ∼6 kcal/mol, compared to that of ∼12 kcal/mol for the phenyl derivative. Theoretical modeling of 2a demonstrated that the [N–H⋯N] interaction is favored by ca. 10 kcal/mol, whereas [N–H⋯S] bonding is sterically unattainable.     

Synthesis, Crystal Structure and Conformational Studies of Schiff-Base Compound 2-{[4-(Phenyldiazenyl)Phenyl]Iminomethyl}-5-Bromophenol

Abstract  

Schiff-base compound 2-{[4-(Phenyldiazenyl)phenyl]iminomethyl}-5-bromo phenol (1), containing an azo group was synthesized from the reaction of p-aminoazobenzene with 5-bromosalicylaldehyde and characterized by elemental analyses, FT-IR spectroscopy and X-ray single-crystal diffraction analysis. Molecular orbital calculation has been carried out using density functional method (B3LYP) at 6-31G basis set. Compound 1 crystallizes in the orthorhombic system, space group Pca2₁, with a = 12.1781(2) ?, b = 4.4894(10) ?, c = 27.7841(5) ?, V = 1519.02(5) ?³, and Z = 4. Compound 1 displays a trans configuration with respect to the C=N and N=N double bonds.     

Synthesis and crystal structure of 1-phenyl-3-methylthio-4-imino-5-allyl-pyrazolo[3,4-d]pyrimidine

The title compound 1-phenyl-3-methylthio-4-imino-5-allyl-pyrazolo[3,4-d]pyrimidine, C₁₅H₁₅N₅S, has been synthesized and characterized by x-ray diffraction: orthorhombic, space group Pbca, with a = 17.3480(9), b = 8.5022(5), c = 19.8132(11) Å. Z = 8, V = 2922.4(3) ų. The compound shows a fully delocalized pyrazolo[3,4-d]pyrimidine system with a sp² hybridization of the N(4) atom.     

Syntheses,Structural, and Biological Studies of Two New Peptide Compounds, 2(s)-(5-fluorouracil-1-aceto)amino-2-isopropyl Acetate Hemihydrate and 2(s)-(5-fluorouracil-1-aceto)amino-2-isopropyl Acetic Acid

Abstract  Two new peptide compounds, 2(s)-(5-fluorouracil-1-aceto)amino-2-isopropyl acetate hemihydrate (1:1/2H ₂ O) and 2(s)-(5-fluorouracil-1-aceto)amino-2-isopropyl acetic acid (2), have been synthesized and characterized by elemental analysis, IR, ¹H- and ¹³C NMR spectroscopy. Two new compounds were structurally characterized by single-crystal X-ray diffraction. The thermal stabilities of compounds 1:1/2H ₂ O and 2 were studied by DSC-TGA techniques. The result of the biological test showed that the compounds 1:1/2H ₂ O and 2 have certain antitumor activities. Index Abstract  Two new peptide compounds, 2(s)-(5-fluorouracil-1-aceto)amino-2-isopropyl acetate hemihydrate (1:1/2H2O) and 2(s)-(5-fluorouracil-1-aceto)amino-2-isopropyl acetic acid (2), have been synthesized and characterized by elemental analysis, IR, 1H-, and 13C NMR spectroscopy. Two new compounds were structurally characterized by single-crystal X-ray diffraction. The thermal stabilities of compounds 1:1/2H2O and 2 were studied by DSC-TGA techniques. The result of the biological test showed that the compounds 1:1/2H2O and 2 have certain antitumor activities.      

Synthesis,Crystal Structure and Thermodynamic Calculations of 1,3-Diethyl-5-(diethylaminium)methylene-2-thiobarbituric Acid Adduct

Abstract  

5-[(Diethylammonio)methyl]-1,3-diethyl-6-oxo-2-thioxo-1,2,3,6-tetrahydro-4-pyrimidinolate (3) was obtained in good yield from the reaction of 1,3-diethyl-6-oxo-5-(1-pyridiniumylmethyl)-2-thioxo-1,2,3,6-tetrahydro-4-pyrimidinolate (2) and diethylamine. The crystal structure of 3 and thermodynamic calculations pertaining to that structure are discussed. The obtained product was characterized using different techniques including single crystal X-ray diffraction, NMR spectroscopy and uni (bi)-molecular systems in gaseous phase. Compound 3 crystallizes in the monoclinic space group P2₁/c with unit cell dimensions a = 13.3701(11) ?, b = 10.9983(7) ?, c = 20.8855(15) ?, β = 105.448(6)°, V = 2960.2(15) ?, Z = 8.     

Hydrogen Bonding in Proton-Transfer Compounds of 5-Sulfosalicylic Acid with a Series of Aliphatic Nitrogen Lewis Bases

Abstract  

The crystal structures of the proton-transfer compounds of 5-sulfosalicylic acid (3-carboxy-4-hydroxybenzenesulfonic acid) with the aliphatic nitrogen Lewis bases, hydroxylamine, triethylamine, pyrrolidine, morpholine, N-methylmorpholine and piperazine, viz. hydroxyammonium 3-carboxy-4-hydroxybenzenesulfonate (1), triethylaminium 3-carboxy-4-hydroxybenzenesulfonate (2), pyrrolidinium 3-carboxy-4-hydroxybenzenesulfonate monohydrate (3), morpholinium 3-carboxy-4-hydroxybenzenesulfonate monohydrate (4), N-methylmorpholinium 3-carboxy-4-hydroxybenzenesulfonate monohydrate (5) and piperazine-1,4-diium bis(3-carboxy-4-hydroxybenzenesulfonate) hexahydrate (6) have been determined and their comparative structural features and hydrogen-bonding patterns described. Crystals of 4 are triclinic, space group P-1 while the remainder are monoclinic with space group either P2₁/c (1–3) or P2₁/n (5, 6). Unit cell dimensions and contents are: for 1, a = 5.0156(3), b = 10.5738(6), c = 18.4785(9) ?, β = 96.412(5)^o, Z = 4; for 2, a = 8.4998(4), b = 12.3832(6), c = 15.4875(9) ?, β = 102.411(5)^o, Z = 4; for 3, a = 6.8755(2), b = 15.5217(4), c = 12.8335(3) ?, β = 92.074(2)^o, Z = 4; for 4, a = 6.8397(2), b = 12.9756(5), c = 15.8216(6) ?, α = 90.833(3), β = 95.949(3), γ = 92.505(3)^o, Z = 4; for 5, a = 7.0529(3), b = 13.8487(7), c = 15.6448(6) ?, β = 90.190(6)^o, Z = 4; for 6, a = 7.0561(2), b = 15.9311(4), c = 12.2102(3) ?, β = 100.858(3)^o, Z = 2. The hydrogen bonding generates structures which are either two-dimensional (2 and 5) or three-dimensional (1, 3 , 4 and 6). Compound 6 represents the third reported structure of a salt of 5-sulfosalicylic acid having a dicationic piperazine species.     

Synthesis and crystal structure of 2-anilino-6<Emphasis Type="Italic">H</Emphasis>-5-(1-phenyl-3-methyl-5-pyrazolone-4-ylene)-1,3,4-thiadiazine

A novel pyrazolone derivative 2-anilino-6H-5-(1-phenyl-3-methyl-5-pyrazolone-4-ylene)-1,3,4-thiadiazine (PMCP-PTSC) containing NNS hexa-atomic heterocycle has been obtained and characterized by means of single crystal X-ray diffraction, IR and ¹H NMR spectroscopies. It is interesting that when grown from two different solvents, two different crystalline structures are formed. The monoclinic crystal A belongs to a P2₁/c space group. The unit cell parameters are a = 16.414(4) Å, b = 12.530(3) Å, c = 8.432(1) Å, = 91.75(2) Å, and Z = 4. The triclinic crystal B belongs to a P space group. The unit cell parameters are a = 11.386(2) Å, b = 12.326(2) Å, c = 12.411(3) Å, = 83.07(1)°, = 87.76(2)°, = 86.52(2)°, and Z = 4. The structure analyses show the title compound is the keto-form. Dimers in crystal packing of A and supramolecular one-dimensional (B) concatenate structures were assembled by the intermolecular hydrogen bonds.     

The Synthesis and Crystal Structure of 5-(4-Bromophenylamino)-2-methylsulfanylmethyl-2<Emphasis Type="Italic">H</Emphasis>-1,2,3-triazol-4-carboxylic Acid Ethyl Ester

Abstract  The 5-(4-bromophenylamino)-2-methylsulfanylmethyl-2H-1,2,3-triazol-4-carboxylic acid ethyl ester 6 was synthesized from p-bromoaniline. The yielded product 6 was investigated with X-ray crystallographic, NMR, MS, and IR techniques. Compound 6, C₁₃H₁₅BrN₄O₂S, Mr = 371.26, crystallizes in the monoclinic space group P2₁/n with unit cell parameters a = 5.5220(1), b = 26.996(5), c = 10.596(2) ?, β = 103.83(3). V = 1533.8(5) ?³, Z = 4, Dx = 1.608 mg m⁻³. The final R ₁ was 0.0844; wR ₂ was 0.1560. H-bond is discussed. Index Abstract  The structure of 5-(4-bromophenylamino)-2-methylsulfanylmethyl-2H-1,2,3-triazol-4-carboxylic acid ethyl ester from 5-amino-1-(4-bromophenyl)-1,2,3-triazol-4-carboxylic acid ethyl ester is studied. H-bond is discussed.      

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.     

The Synthesis and Crystal Structure of 5-Methyl-1-(1-naphthyl)-1,2,3-triazol-4-carboxyl Acid

Abstract  5-Methyl-1-(1-naphthyl)-1,2,3-triazol-4-carboxyl acid 3 was synthesized from 1-aminonaphthalene. The yielded product 3 was investigated with X-ray crystallographic, NMR, MS and IR techniques. Compound 3, C₁₄H₁₁N₃O₂, Mr = 253.26, crystallizes in the orthorhombic space group Pbca with unit cell parameters a = 10.068(2), b = 12.353(2), c = 20.102(4) ?, V = 2500.1(8) ?³, Z = 8, Dx = 1.346 Mgm^-3. The final R was 0.0474. The molecular packing is stabilized by intermolecular O–H···N interactions. Index Abstract  5-Methyl-1-(1-naphthyl)-1,2,3-triazol-4-carboxyl acid 3 was synthesized from 1-aminonaphthalene. The yielded product 3 was investigated with X-ray crystallographic, NMR, MS and IR techniques. Compound 3, C₁₄H₁₁N₃O₂, Mr = 253.26, crystallizes in the orthorhombic space group Pbca with unit cell parameters a = 10.068(2), b = 12.353(2), c = 20.102(4) ?, α = β = γ = 90.00o. V = 2,500.1(8) ?³, Z = 8, Dx = 1.346 Mgm⁻³. The final R was 0.0474. The molecular packing is stabilized by intermolecular O–H···N interactions.      

Synthesis and crystal structure of 5-allyl-5<Emphasis Type="Italic">H</Emphasis>dibenzo[b,f]azepine

The crystals 5H-dibenzo[b,f]azepine 2 and 5-allyl-5H-dibenzo[b,f]azepine 3 were synthesized and characterized by X-ray crystallography. The compound 3 is a novel synthon for the construction of unusual isoxazoli(ne)dine rings bearing at the 5th position of dibenzo[b,f]azepine moiety. The compound 2 (C₁₄H₁₁N) crystallizes in the orthorhombic space group P2₁2₁2₁ with the parameters a = 6.036(1) Å, b = 8.250(7) Å, c = 20.528(4) Å, Z = 4 and the final R factor is R1 = 0.0544. The compound 3 (C₁₇H₁₅N) crystallizes in the Hexagonal space group P6₁ with the parameters a = 11.043(9) Å, c = 18.575 Å, Z = 6 and the final R factor is R1 = 0.0373.     

Synthesis,Characterization and Crystal Structure of 1-Phenyl-3-methyl-4-(salicylidene hydrazide)-phenylethylene-pyrazolone-5

Abstract A new compound 1-phenyl-3-methyl-4-(salicylidene hydrazide)-phenylethylene-pyrazolone-5 (PMPeP-SHZ) has been synthesized and characterized by elemental analysis, IR spectrum, MS and single crystal X-ray diffraction. The compound crystallizes in a monoclinic, space group P2(1)/c with cell parameters: a = 10.8275(19) ?, b = 24.689(4) ?, c = 9.7167(16) ? and β = 95.127(4)°, Z = 4, S = 1.097. In the crystal structure, the compound presents in the diketo form. The structure exhibits both intra- and intermolecular hydrogen bonding and the molecules are interlinked through hydrogen bonds forming an infinite 2D network. The fluorescent result shows blue emission at room temperature in solid state. Graphical Abstract Synthesis, Characterization and Crystal Structure of 1-Phenyl-3- methyl-4-(salicylidene hydrazide)-phenylethylene-pyrazolone-5 Li Zhang, Guan-Cheng Xu, Lang Liu, Guang-Fei Liu, and Dian-Zeng Jia* Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users.