N‐(p‐Chloro­benzyl­idene)­phenyl­amine N‐oxide

The crystal structure of the title compound, C₁₃H₁₀ClNO, confirms that it exists as a nitro­ne. The geometry about C=N is Z. The relevant torsion angles indicate trans and cis conformations around the nitro­ne bond.     

3‐(4‐Chloro­benzoyl)‐7‐(N,N‐di­methyl­amino)‐1‐phenyl­indolizine and 3‐(2,4‐di­chloro­benzoyl)‐7‐(N,N‐di­methyl­amino)‐1‐phenyl­indolizine

In both of the title compounds, C₂₃H₁₉ClN₂O, (I), and C₂₃H₁₈Cl₂N₂O, (II), the molecular packing is influenced by weak intermolecular C—H⋯O and C—H⋯π interactions, but despite the chemical similarity of the compounds, the packing in (II) is entirely different from that observed in (I).     

N‐(3‐Chloro­phenyl)‐α‐phenyl­nitro­ne: association with benzoic acid through hydrogen bonding

The identity of the title complex, C₁₃H₁₀ClNO·C₇H₆O₂, is confirmed to be a hydrogen‐bonded adduct of benzoic acid and N‐(3‐chloro­phenyl)‐α‐phenyl­nitro­ne. The two aromatic rings in the nitro­ne are trans about the C=N bond.     

N‐(o‐Chloro­phenyl)‐2,5‐di­methyl­pyrrole‐3‐carb­aldehyde

Crystal structure analysis of the title compound, C₁₃H₁₂ClNO, reveals three crystallographically independent mol­ecules in the asymmetric unit. The main conformational difference between these mol­ecules is the orientation of the phenyl rings with respect to the pyrrole rings. The coplanar arrangement of the aldehyde groups attached to the pyrrole rings influences the pyrrole‐ring geometry. The C2—C3 and N1—C5 bonds are noticeably longer than the C4—C5 and N1—C2 bonds. Two independent mol­ecules of the title compound form dimers via intermolecular C—H⃛O hydrogen bonds [D⃛A = 3.400 (3) Å and D—H⃛A = 157°]. The perpendicular orientation of the phenyl and pyrrole rings of one independent mol­ecule and its symmetry‐related mol­ecule allows C—H⃛π interactions, with an H⃛centroid distance of 2.85 Å and a C—H⃛π angle of 155°. The distances between the H atom and the pyrrole‐ring atoms indicate that the C—H bond points towards one of the bonds in the pyrrole ring.     

N‐(4‐Cyano­phenyl)‐α‐(4‐methoxy­phenyl)­nitro­ne

In the crystal structure of the title compound, 4‐cyano‐N‐(4‐methoxy­benzyl­idene)­phenyl­amine N‐oxide, C₁₅H₁₂N₂O₂, the 4‐methoxy­phenyl is approximately coplanar with the nitrone moiety but significantly rotated with respect to the 4‐cyano­phenyl moiety. The extent of this rotation is significantly different for the two crystallographically independent mol­ecules of the asymmetric unit [dihedral angles of 19.4 (1) and 26.5 (1)°]. The geometry about the C=N bond is Z. The two mol­ecules are related to one another by a pseudo inversion centre.     

[2‐(Anilino­methyl)­phenyl]­di­phenyl­phosphine and {2‐[(N‐methyl­anilino)­methyl]­phenyl}di­phenyl­phosphine

The title compounds, Ph₂PCH₂N(H)Ph or C₂₅H₂₂NP and Ph₂PCH₂N(CH₃)Ph or C₂₆H₂₄NP, respectively, are isomorphous, with calculated theoretical Tolman angles of 174 and 182°.     

4‐Methyl‐N‐[2‐(p‐tolylsulfanyl)phenyl]benzene­sulfonamide

The title compound, C₂₀H₁₉NO₂S₂, is formed by a palladium–copper‐catalyzed reaction between 4‐methyl‐N‐[2‐(prop‐2‐ynyl­sul­fanyl)­phenyl]­benzene­sul­fon­amide and p‐iodo­toluene. The mol­ecules contain three essentially planar parts, namely an amino­thio­phenol moiety (A), a toluene­sulfone moiety excluding the oxo ligands (B) and a tolyl group (C), approximately orthogonal to each other; the dihedral angles A/B, A/C and B/C are 111.6 (1), 89.3 (1) and 101.4 (1)°, respectively. Intermolecular N—H?O hydrogen bonds link the mol­ecules into infinite one‐dimensional chains.     

N‐Chloro­acetyl‐β‐alanine

The β‐alanine residue of the title compound, C₅H₈ClNO₃, has a ggt folded conformation, which is mainly stabilized through intermolecular N—H⋯O=C (amide–acid) and O—H⋯O=C (acid–amide) hydrogen bonds. In addition, a cis conformation is found for the Cl—CH₂—C(=O)—NH torsion angle, which is associated with the presence of an intramolecular hydrogen bond.     

4‐[2‐(4‐Cyano­phenyl)ethenyl]‐N‐methyl­pyridinium tetra­phenyl­borate

In the title compound, C₁₅H₁₃N₂⁺·C₂₄H₂₀B⁻, the pyridyl ring of the cation makes a dihedral angle of 1.6° with the benzene ring. Each is rotated in the same direction with respect to the central –C—CH=CH—C– linkage, by 3.8 and 5.3°, respectively. The anions have a slightly distorted tetra­hedral geometry. Mol­ecular packing analysis was carried out using the packing energy portioning scheme in the program OPEC. Around each anion in the crystal structure there are eight anions, which inter­act with the central anion through C—H⋯π inter­actions. The cations are hydrogen bonded in a head‐to‐tail fashion, forming chains along [10].     

Synthesis of a new monomer N′‐(β‐methacryloyloxyethyl)‐2‐pyrimidyl‐(p‐benzyloxycarbonyl)aminobenzenesulfonamide and its copolymerization with N‐phenyl maleimide

The new monomer N′‐(β‐methacryloyloxyethyl)‐2‐pyrimidyl‐(p‐benzyloxy‐ carbonyl)aminobenzenesulfonamide (MPBAS) (M₁) is synthesized using sulfadiazine as parent compound. It could be homopolymerized and copolymerized with N‐phenyl maleimide (NPMI) (M₂) by radical mechanism using AIBN as initiator at 60 °C in dimethylformamide. The new monomer MPBAS and polymers were identified by IR, element analysis and ¹H NMR in detail. The monomer reactivity ratios in copolymerization were determined by YBR method, and r₁ (MPBAS) = 2.39 ± 0.05, r₂ (NPMI) = 0.33 ± 0.02. In the presence of ammonium formate, benzyloxycarbonyl groups could be broken fluently from MPBAS segments of copolymer by catalytic transfer hydrogenation, and the copolymer with sulfadiazine side groups are recovered. © 2000 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 38: 2548–2554, 2000     

6‐(1‐Hydro­xy‐2,2‐di­phenyl­ethyl)‐4,4‐di­phenyl‐2‐cyclo­hexen‐1‐one

The crystal structure of the title compound, C₃₂H₂₈O₂, (I), confirms the erythro stereochemistry of the aldol adduct. In the crystal, (I) forms centrosymmetric O—H?O=C hydrogen‐bonded dimers which in turn are connected by C—H?O and C—H?π interactions.     

3‐(p‐Chloro­phenyl)‐4‐phenyl‐4,5‐di­hydro­isoxazole‐5‐spiro‐2′‐1′,2′,3′,4′‐tetra­hydro­naphthalen‐1′‐one

In the title compound, C₂₄H₁₈ClNO₂, the phenyl ring and the tetralone moiety are approximately orthogonal to the isoxazoline ring. The isoxazoline ring adopts an envelope conformation, while the cyclo­hexenone ring of the tetralone moiety has an intermediate sofa/half‐chair conformation. In this structure, one C—H?N intermolecular and two C—H?O intramolecular hydrogen bonds occur; the H?A distances are 2.60, and 2.35 and 2.57 Å, respectively. The mol­ecules are held together by an intermolecular C—H?N hydrogen bond, forming a one‐dimensional chain along the [100] direction.     

4‐(4‐Methoxy­phenyl­amino)‐3‐phenyl­azo‐3‐penten‐2‐one

The title compound, C₁₈H₁₉N₃O₂, was obtained by an azo‐coupling reaction with en­amino­nes and is composed of a planar azoen­amine skeleton which forms a six‐membered ring through a symmetrical intramolecular hydrogen bond. The compound was found to exist as an equilibrium mixture of major hydrazoimino and minor azoen­amine tautomers. Quantification of the relative contribution of the tautomeric forms is obscured by the existence of the hydrogen bond. Comparison of the results with those obtained for a similar structure revealed a substantial effect on the tautomeric equilibria of the nature of the substituent bonded to the amine nitro­gen.     

4‐(4‐Chloro­phen­yl)‐3‐(4‐phenyl­pent‐4‐en­yloxy)‐1,3‐thia­zole‐2(3H)‐thione

The title compound, C₂₀H₁₈ClNOS₂, is a thia­zole‐derived thio­hydroxamic acid O‐ester. The value of Z′ is 3 and the asymmetric unit comprises three mol­ecules of identical helicity along the N—O bond. Two of these show an anti and the third a syn arrangement of substituents attached in positions 3 and 4 to the 1,3‐thia­zole nucleus.     

(4R)‐3‐Allenyl‐4‐(di­phenyl­methyl)­oxazolidin‐2‐one,an unsubstituted allen­amide

The first X‐ray structure of an unsubstituted allen­amide, C₁₉H₁₇NO₂, is reported. The solid‐state phase supports the notion that a key minimum conformation of allen­amides can be invoked to rationalize the observed stereochemical outcomes in many of our methodological studies employing allen­amides. This minimum conformation involves two important factors, i.e. having approximate coplanarity between the planes of the oxazolidinone ring and the internal olefin, and having the allene moiety facing away from the carbamate carbonyl group. The C—N—C=C torsion angle that quantifies this approximate coplanarity between the plane of the oxazolidinone ring and that of the internal olefin, as determined from this crystallographic study, is −19.1 (2)°. A minimized structural calculation, which determined this angle to be −16.1°, is in close agreement. Additional structural features include a probable π–π interaction between the allene moiety and a benzene ring, and non‐classical hydrogen bonding in the form of weak C—H⋯O interactions that are responsible for the formation of two‐dimensional networks.     

Chloro­bis­[N‐ethoxy­carbonyl‐N′‐(p‐methoxy­phenyl)­thio­urea‐κS]copper(I)

The title copper(I) complex, [CuCl(C₁₁H₁₄N₂O₃S)₂], was synthesized by the redox reaction of cupric chloride with the corresponding thio­urea derivative as reducing agent. The Cu^I coordination environment is trigonal planar, involving two S atoms and one Cl atom. The presence of intramolecular hydrogen bonds leads to the formation of a cis conformation and promotes the stability of the complex.     

N‐(4‐Bi­phenyl­yl)­urea

In the crystal structure of the title compound, C₁₃H₁₂N₂O, N—H(anti)?O hydrogen bonds produce the so‐called urea α‐network and the N—H(syn) donor forms an unconventional N—H?π hydrogen bond.     

1‐(4‐Chloro­phenyl­sulfanyl)‐2‐nitro‐4‐(tri­fluoro­methyl)­benzene and 1‐(4‐chloro­phenyl­sulfanyl)‐4‐nitro‐2‐(tri­fluoro­methyl)­benzene

Two chemical isomers of 3‐nitro­benzotrifluoride, namely 1‐(4‐chloro­phenyl­sulfanyl)‐2‐nitro‐4‐(tri­fluoro­methyl)­benzene, C₁₃H₇ClF₃NO₂S, (I), and 1‐(4‐chloro­phenyl­sulfanyl)‐4‐nitro‐2‐(tri­fluoro­methyl)­benzene, C₁₃H₇ClF₃NO₂S, (II), have been prepared and their crystal structures determined with the specific purpose of forming a cocrystal of the two. The two compounds display a similar conformation, with dihedral angles between the benzene rings of 83.1 (1) and 76.2 (1)°, respectively, but (I) packs in P while (II) packs in P2₁/c, with C—H⋯O interactions. No cocrystal could be formed, and it is suggested that the C—H⋯O associations in (II) prevent intermolecular mixing and promote phase separation.     

Bis­[2‐(di­phenyl­phosphinoyl)­benzene] di­sulfide

The title compound, [2‐Ph₂P(O)C₆H₄S]₂ or C₃₆H₂₈O₂P₂S₂, obtained by electrochemical oxidation of 2‐(di­phenyl­phosphino)­benzene­thiol, has twofold crystallographic symmetry. Principal dimensions include S—S 2.0212 (15) Å, S—C 1.786 (3) Å and C—S—S—C 81.34 (14)°.     

Supramolecular structures of 2‐cyano‐3‐di­methyl­amino‐N‐(4‐methyl­phenyl)­acryl­amide and 2‐cyano‐3‐di­methyl­amino‐N‐(2‐methoxy­phenyl)­acryl­amide

In the title compounds, C₁₃H₁₅N₃O, (I), and C₁₃H₁₅N₃O₂, (II), the dihedral angles between the planes of the phenyl ring and the amide group are 4.1 (1) and 20.7 (1)°, respectively. The mol­ecules adopt a fully extended conformation, aided by intramolecular interactions. The molecular structures of (I) and (II) display different crystal packing and hydrogen‐bonding networks.