Synthesis and X-ray analysis of (RS)-N-tert-butyl-2-anilino-

The crystal and molecular structure of (RS)-N-Tert-butyl-2-anilino-3,3-dimethylbutanamide, a derivative of an amino acid that was obtained by highly selective cleavage of 1,3-di-tert-butylaziridinone by aniline, is described. The racemic mixture of the amide crystallizes in the space groupP 2₁/n with four molecules per unit cell. Crystal Data:a=10.483(2) Å,b=6.206(1) Å,c=24.767(5) Å,β=90.39(3),V=1611.5(6) A³,R(F)[I>2σ(I)]=0.0679.wR(F ²) [I>2σ(I)]=0.1148.     

X-ray diffraction analysis of (Ph2PO)2

The title compound (Ph2PO)2 is analyzed by single crystal X-ray diffraction analysis. The crystals are monoclinic, space group P2(1)/n with a = 9.5112(19) Å, b = 11.161(2) Å, c = 9.5487(19) Å, α = 90°, β = 91.65(3)°, γ = 90°, V = 1013.2(3) ų, Z = 2, F(₀₀₀) = 420, Dc = 1.319 g cm^–3, μ = 0.232 mm^?1, the final R = 0.0818, and wR = 0.2259. A total of 7954 reflections were collected, of which 1758 were independent (R_int = 0.0542). In the crystal packing diagram, intermolecular C—H···O hydrogen bonds stabilize the solid state of the title compound.     

Synthesis and Crystal Structure of bis [2-(3-(2-((2-Hydroxybenzylidene) Amino)Ethyl)Oxazolidin-2-yl)Phenol]Cerium (IV) 1,4-Dioxane Monosolvate

The metal complex, bis [2-(3-(2-((2-hydroxybenzylidene)amino)ethyl) oxazolidin-2-yl)phenol]cerium(IV) 1,4-dioxane monosolvate was synthesized and characterized by infrared, ¹H NMR, elemental analysis, single-crystal, and powder X-ray diffraction. The coordination polyhedra of cerium shows a distorted square-antiprismatic geometry. No classical hydrogen bonds were observed. The crystal packing was influenced by weak C-H···O (intermolecular) and van der Waals interactions.     

Crystal structure of 2-{(R)-1-hydroxy-1-[(2S)-1-tritylaziridin-2-yl] methyl}acrylate and spectroscopic properties of the (R,S) and (S,S) stereoisomers

The crystal and molecular structure of 2-{(R)-1-Hydroxy-1-[(2S)-1-tritylaziridin-2-y1] methy1}acrylate is described. Crystal data: C₂₆H₂₅NO₃, orthorhombic, space group P2₁2₁2₁, a = 9.6954(5), b = 13.1458(5), c = 16.7885(7) Å, V = 2139.8(2) ų, Z = 4. The (R,S) diastereomer shows an intramolecular hydrogen bonding N···H—O under formation of a five-membered ring with N···O distance of 2.664 Å. IR, ¹H NMR and ¹³C NMR data are discussed. The ¹H NMR of the (R,S) diastereomer shows a singlet- whereas the (S,S) diastereomer exhibits a doublet-pattern for the hydroxyl proton.     

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.     

Synthesis and Crystal Structure of [2-(4-chlorobenzoyloxy)-5-methylphenyl]-(4-methylphenyl)methanone

[2-(4-Chlorobenzoyloxy)-5-methylphenyl]-(4-methylphenyl)methanone was synthesized and characterized by spectroscopic and X-ray diffraction methods. The molecule crystallizes in the monoclinic space group P2₁/c with cell parameters a = 13.7530(19) Å, b = 10.0560(19) Å, c = 13.469(3) Å, β = 100.630(7)° and Z = 4. There is a large discrepancy between the carbonyl group bond lengths of ketone and the ester. The structure exhibits intermolecular hydrogen bonds of the type C–H···O.     

Synthesis and Crystal Structure of 4,6-dihydroxy-2-[2-(4-hydroxy-phenyl)-vinyl]-benzene-1,3-dicarbaldehyde

Abstract The title compound, 3, 6-dihydroxy-2-[2-(4-hydroxy-phenyl)-vinyl]- benzene-1,3-dicarbaldehyde was synthesized by Vilslmeier reaction from resveratrol (trans-3,4′,5-trihydroxystilbene). Its structure was determined by X-ray single crystal diffraction. The crystal belongs to monoclinic, space group P2₁/n with crystallographic parameters: a = 7.2950(15) ?, b = 14.781(3) ?, c = 12.202(2) ?, β = 96.57(3)°, μ = 0.108 mm⁻¹, V = 1307.1(5) ?, Z = 4, Dx = 1.445 g/cm³, F(000) = 592, T = 293(2) K, 2.17°≤ θ ≤ 26.00°. The X-ray results demonstrated that the Vilslmeier reaction of resveratrol with DMF, POCl₃ and CH₃CN yielded 4,6-dhydroxy-2-[2-(4-hydroxy-phenyl)-vinyl]-benzene-1,3-dicarbaldehyde. Graphical Abstract In this article, a resveratrol derivative was prepared and structurally characterized by single crystal X-ray diffraction.      

Crystal and molecular structure of (2E,4S,10R)-4-hydroxy-2-undecen-10-olide (nor-patulolide C), C11H18O3

The stereogeometry and absolute configuration of the title compound has been proved by an X-ray diffraction analysis. Crystal data: monoclinic, P2₁,a=7.7976(2),b=7.8288(2),c=8.9791(4) Å, =90.331(4)^o, Z=2. The crystal structure has been solved by vector search methods and refined toR=0.042 for 1798 observed reflections.     

Structure of Organic Compound (E)-3-((S)1-Phenylethylamine)methylene R (+) Camphor

Crystallography Reports - The synthesis and crystal structure of (E)-3-((S)-1-phenylethylamine)methylene R-(+) camphor are discussed. The 1H NMR spectrum in a chloroform solution indicates the...     

Synthesis, crystal structure, and molecular modeling (AM1) of Methyl 6-chloro-4-(2-chlorophenyl)-5-formyl-2-methyl-1, 4-dihydropyridine-3-carboxylate

The synthesis and structural characterization of Methyl 6-chloro-4-(2-chlorophenyl)-5-formyl-2-methyl-1,4-dihydropyridine-3-carboxylate is described. The structure was refined to R₁ = 0.0470 for 2665 reflections (with I > 2(I)). Crystal data: C₁₅H₁₃C₁₂NO₃, monoclinic,space group P2₁/c, a = 11.163(9), b = 14.484(8), c = 9.422(7) Å, V = 1512.9(19) ų, Z = 4. The results of crystallographic and molecular modeling (AM1) were compared. The Cl atom attached to the phenyl group has two possible orientations, having 75% (sp) and 25% (ap) occupancy, respectively. The molecules in the crystal are held together by means of intermolecular hydrogen bonds of the type N=H...O and by C=H...O interactions.     

X-ray structure analysis of 1-(4-bromophenyl)-3-(4-chlorophenyl)-prop-2-en-1-one

The title compound crystallizes in the monoclinic space group P2₁/c with unit cell parameters a = 15.6239(15) ?, b = 14.0537(14) ?, c = 5.8396(5) ?, β = 92.666(3)°, V = 1280.8 (2) ?³, and Z = 4. The final reliability index is 0.0538 for 2921 observed reflections. Two phenyl rings of the title molecule are not coplanar, with a dihedral angle of 46.3(0)°. The molecular planarity of this substituted chalcone is strongly affected by the 4′-bromo group. The crystal cohesion is accentuated by π···π, C–H···Br interactions and R₃ ¹ (11) hydrogen bond.     

Synthesis,Characterization and Crystal Structure of Ethyl 2-amino-4-(4-fluorophenyl)-6-phenylcyclohexa-1,3-diene-1-carboxylate

Ethyl 2-amino-4-(4-fluorophenyl)-6-phenylcyclohexa-1,3-diene-1-carboxylate was synthesized from ethyl 6-(4-bromophenyl)-4-(4-fluorophenyl)-2-oxocyclohex-3-ene-1-carboxylate and ammonium acetate in glacial acetic acid. The synthesized compound was characterized by elemental analysis, FT-IR, thermogravimetric analysis (TGA), differential thermal analysis (DTA), UV-Visible, and single-crystal X-ray diffraction. The title compound, ethyl 2-amino-4-(4-fluorophenyl)-6-phenylcyclohexa-1,3-diene-1-carboxylate, C₂₁H₂OFNO₂, crystallizes in the orthorhombic space group Pbca with the following unit-cell parameters: a = 17.417(2), b = 9.7287(9), c = 21.014(2) Å, and Z = 8. The crystal structure was solved by direct methods using single-crystal X-ray diffraction data collected at room temperature and refined by full-matrix least-squares procedures to a final R-value of 0.0644 for 1616 observed reflections. An intramolecular N–H…O hydrogen bond generates an S(6) graph-set motif. In the crystal, molecules are linked by N–H…O hydrogen bonds, forming a two-dimensional network.     

Synthesis and crystal structures of complexes of Ni (II) to chiral Schiff bases of (R)- and (S)-serine with (S)- and (R)-2-N-(N′-benzylprolyl)-aminobenzophenone

The three-dimensional molecular and crystal structures of a pair of enantiopure mirror complexes of Ni (II) to chiral Schiff bases of (R)- and (S)-serine with (S)- and (R)-2-N-(N′-benzylprolyl)-aminobenzophenone (BPB), denoted as (S,R)-BPB-Ser-Ni and (R,S)-BPB-Ser-Ni, respectively, have been determined by X-ray diffraction. The complexes crystallize in the orthorhombic space group P2 ₁ 2 ₁ 2 ₁ with unit cell parameters: a = 10.050(2) Å, b = 10.100(2) Å, c = 26.514(5) Å, V = 2691.3(9) ų, and Z = 4 for (S,R)-BPB-Ser-Ni; and a = 9.878(2) Å, b = 10.130(2) Å, c = 26.304(5) Å, V = 2632.1(9) ų, and Z = 4 for (R,S)-BPB-Ser-Ni. The Ni atom is square-planar-coordinated to N(1), N(2), O(4), and N(3) of the Schiff base with minor distortion. The hydroxymethyl group on the serine moiety is axial to the coordination plane and parallel to the neighboring phenyl group.     

Synthesis, characterization, and structural analysis of ethyl (2Z)-3-(4-chlorophenyl)-2-cyano-3-(methoxyamino)prop-2-enoate

Ethyl (2Z)-3-(4-chlorophenyl)-2-cyano-3-(methoxyamino)prop-2-enoate was prepared by reacting the lithium salt of ethyl cyanoacetate with (Z)-O-methyl-4-chloroben-zohydroximoyl fluoride. This compound crystallizes in space group Pbca,with lattice constants a=7.5740(15) ?, b=11.337(2) ?, and c=30.424(5) ? at 110 K. Characterizations include spectrometric identifications employing IR, UV, and ¹H and ¹³C NMR. The compound exists in the solid as the enamine tautomer, with the cyano group cis to the 4-chlorophenyl group (the Z configuration). The C=C and C–N bond distances are 1.3930(16) ? and 1.3278(16) ?, respectively. The N–H group forms a bifurcated hydrogen bond with acceptors C=O (intramolecular) and C≡N (intermolecular).Supplementary material CCDC-289444 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge via www.ccdc.cam.ac.uk/data_request/cif, by e-mailing data_request@ccdc.cam.ac.uk, or by contacting The Cambridge Crystallographic Data Centre, 12 Union Road, Cambridge CB2 1EZ, UK; Fax: +44(0)1223-336033.     

Synthesis and X-ray crystal structure studies of 1-ethyl-3-(2-chlorophenyl)-1,2,3-triazolium perchlorate

The isolation of stable carbenes of the Arduengo (1a) and Wanzlick (2a) type has prompted us to look for stable nitrenium ions of the related structural type 1-ethyl-3-(2-chloropenyl)-1,2,3-triazolium perchlorate (6⁺ClO₄ ^–). The title compound was synthesized and the structure was investigated by X-ray crystallography. It crystallizes in the monoclinic space group P2 ₁/n with cell parameters a = 7.066(4) Å, b = 27.680(6) Å, c = 7.486(2) Å, = 111.22(3)°, and Z = 4. The structure exhibits arrangement of the molecules with intermolecular hydrogen bonds within the layers.     

Metal complexes of chiral pyridine ligands. X-ray structure of nitratobis {2-(2S)-2-pyrrolidinyl]pyridine} copper (II) nitrate

Cobalt(II), nickel(II), and copper(II) complexes of 2-[(2S)-2-pyrrolidinyllpyridine (L) have been synthesized and characterized. The crystal structure of the complex [Cu(L)₂(NO₃)]NO₃ has been determined by X-ray diffraction. Crystals are monoclinic, space groupP2+, witha=10.766(3).b=7.525(2),c=13.447(4) Å. =104.64(2)°. and Z=2. The structure consists of [Cu(L)₂(NO₃)]⁺ cations and NO ₃ ^t- anions. The copper atom has a distorted trigonal bipyramidal coordination geometry with the two pyrrolidine nitrogens and one nitrate oxygen occupying the equatorial positions and the two pyridine nitrogens at the apices. The crystalline cohesion is ensured by a network of hydrogen bonds involving the pyrrolidine groups as donors and both coordinate and uncoordinate nitrates as acceptors.     

Crystal structures of 3-[1-Benzenesulfonyl-3-phenylsulfanyl-1H-indol-2-yl]-1-[4-(methyl (I)/methoxy (II) phenyl)]-2-phenyl-propane-1-one

The compounds 3-(1-Benzenesulfonyl-3-phenylsulfanyl-1H-indol-2-yl)-1-[4-methyl (I)/methoxy (II)phenyl)]-2-phenyl-propane-1-one crystallize in triclinic space group P . The details are: compound I a = 11.941(6) ?, b = 12.154(7) ?, c = 13.006(7) ?, α = 63.124(8)°, β = 84.464(9)°, γ = 64.810(8)°, V = 1519.7(14) ?³, Z = 2, D _cal = 1.284 Mg m⁻³, and R = 0.0382 (wR = 0.0978); compound II a = 11.897(6) ?, b = 12.268(6) ?, c = 13.001(7) ?, α = 61.919(8)°, β = 83.480(8)°, γ = 64.676(7)°, V = 1504.0(14) ?³, Z = 2, D _cal = 1.333 Mg m⁻³, and R = 0.0422 (wR = 0.1049). The indole ring system in both the molecules I and II are not strictly planar and the dihedral angles formed by the pyrrole and benzo planes are 4.0(7)° and 3.5(8)°, respectively. The C–HO, C–Hπ and ππ types of interactions stabilize the molecules in the unit cell in addition to van der Waal's forces in I and II.     

The crystal structure and absolute configuration of(S)-((S)-1-chloroethyl)-methyl-1-naphthalenylphenylsilane

Recrystallization from hexane of diastereomeric (S)-((R/S)-1-chloroethyl)-methyl-1-naphthalenylphenylsilane, C₁₉H₁₉ClSi, initially yields crystals composed of only one stereoisomer, whose crystal structure has been determined. The crystals are orthorhombic, space groupP2₁2₁2₁ (No. 19), with four formula units in a cell of dimensionsa=7.729(4),b=11.239(1), andc=19.214(3) Å. Intensities were measured (Mo radiation) for all reflections having 2θ<43°, but only part of the data were collected from 43 to 60° due to crystal decomposition. The structure was solved by direct methods and refined by full-matrix least-squares calculations to a finalR of 0.0378 for 2074 reflections havingI>3σ(I). The crystal structure is composed of discrete molecules having theS configuration at both Si and alpha-C(2) asymmetric centers, and in which the naphthalenyl group bonded to Si is juxtaposed to the Cl bonded to C(2). The plane of the naphthalenyl group almost eclipses the Si-C(methyl) bond, and a similar relationship exists between the phenyl group and the Si-C(2) bond.     

Synthesis and Crystal Structure of Heptyl 3-(3,4-dihydroxyphenyl)-2-propenoate

Abstract  The title compound, C₁₆H₂₂O₄, synthesized by modified Knoevenagel condensation of protocatechualdehyde with monoheptyl-malonate and recrystallized from benzene, was confirmed by single-crystal X-ray diffraction (CCDC 272827). The compound crystallizes in triclinic space group Pī with cell parameters a = 5.296(3) ?, b = 10.711(13) ?, c = 13.870(4) ?, α = 98.84(7)°, β = 90.97(4)°, γ = 96.77(7)° and Z = 2. The structure is the E isomer and its packing is stabilized by intermolecular O–H···O and C–H···O hydrogen bonds. Index Abstract  The title compound, C₁₆H₂₂O₄, synthesized by modified Knoevenagel condensation, was confirmed by single-crystal X-ray diffraction showing its structure is in E isomer and its packing is stabilized by hydrogen bonds.      

Synthesis and X-ray Crystal Structures of Two Luminescent Imidazopyridinium Derivatives from the Corresponding N-(aryl)-Pyridine-2-aldimines

Syntheses and X-ray structural characterizations of two new luminescent imidazopyridinium derivatives, 2-(phenyl)-N(3)-(4(methyl)phenyl)-imidazo[1,5a] pyridinium perchlorate (1) and 2-(pyridyl)-N(3)-(4-(chloro)phenyl)-imidazo[1,5a] pyridinium perchlorate (2) are reported. The compounds are prepared in one step from N-(4-(methyl)phenyl) pyridine-2-aldimine and N-(4-(chloro)phenyl) pyridine-2-aldimine respectively in a transformation mediated by Mn(OAc)₂-KMnO₄ mixture. It is found that the molecular structures of the two compounds are similar. In the solid state, 1 forms a three-dimensional network through a series of hydrogen bonds between the cations and anions in the lattice while 2 forms a similar but less extensively linked network. The substitution of hydrogen at the 2-position of the imidazopyridinium ring by phenyl or 2-(pyridyl) affects the nature of their first excited states as detected by changes in their emission and absorption spectra.