Two triclinic polymorphs of 2,3,5,6‐tetrakis­(naphthalen‐2‐yl­sulfanyl­methyl)­pyrazine

The title compound, C₄₈H₃₆N₂S₄, can be crystallized as two polymorphic structures, (I) and (II), both of which are in the triclinic space group P and possess C_i symmetry. In the crystal structure of polymorph (I), the adjacent naphthalene moieties are orientated towards one another and are inclined to one another by 78.7 (1)°, resulting in weak C—H⋯π interactions. In polymorph (II), the adjacent substituents are orientated away from one another, enclosing the pyrazine N atoms. In this way, the S atom of one substituent sits below the plane of the naphthalene ring of the other substituent.     

[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°.     

Halocarbon and arene coordination of lithium(I) in (1‐anilino‐3‐phenyl­imino­propenyl)chloro(methyl)­aluminium bis{[tetrakis(pentafluoro­phenyl)­borato]­lithium} benzene solvate

The crystal structure of the title compound, [AlCl(CH₃)‐(C₁₅H₁₃N₂)]­[Li(C₂₄BF₂₀)]₂­·C₆H₆, is reported. The unusual coordination features of the lithium(I) cation, including Li‐atom coordination to six organohalogen atoms and the shortest Li—F(C) distances so far observed, are discussed.     

(–)‐(S)‐2‐(Fluoro­di­phenyl­methyl)­pyrrolidinium chloride

The title compound, C₁₇H₁₉FN⁺·Cl^?, has an ionic structure, and cations and anions are linked into infinite chains by Cl?H—N—H?Cl hydrogen bonds. The absolute configuration (S) was confirmed.     

Redetermination of bis{[(2‐hydroxy­phenyl­methyl)­bis(2‐pyridyl­methyl)­aminato]copper(II)} diperchlorate

The structure of the title compound, [Cu₂(C₁₉H₁₈N₃O)₂](ClO₄)₂, was reported with insufficient accuracy because of a twinning problem by Adams, Bailey, Campbell, Fenton & He [J. Chem. Soc. DaltonTrans. (1996), pp. 2233–2237]. The dinuclear phenolate‐bridged Cu^II complex has an inversion centre.     

(E)‐5‐[(4‐Nitro­phenyl­hydrazono)­phenyl­acetyl]‐3‐phenyl­isoxazole

The title compound, C₂₃H₁₆N₄O₄, can be considered as consisting of two connected fragments: a nitro­phenyl­hydrazone moiety, which assumes an E configuration, and an isoxazole moiety. In this latter fragment, the weak π‐electron delocalization shortens the carbonyl–isoxazole O?O distance [2.643 (2) Å] to less than the van der Waals radii sum.     

Racemic 3,5‐di­chloro‐2‐{[(1‐phenyl­ethyl)­imino]­methyl}phenol

The title compound, (RS)‐3,5‐di­chloro‐2‐{[(1‐phenyl­ethyl)­imino]­methyl}phenol, C₁₅H₁₃Cl₂NO, was synthesized from racemic 1‐phenyl­ethyl­amine and 3,5‐di­chloro­salicyl­aldehyde. The π‐conjugate system around the imine group is essentially planar in the phenol–imine tautomer. Intramolecular O⋯N hydrogen‐bond and intermolecular C—H⋯π interactions are present in the crystal structure.     

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.     

5‐(2‐Chloro­phenyl­diazenyl)­salicyl­aldehyde and 4‐(2‐chloro­phenyl­diazenyl)‐2‐{[tris­(hydroxy­methyl)­methyl]­amino­methyl­ene}cyclo­hexa‐3,5‐dien‐1(2H)‐one

The mol­ecule of the former title compound, C₁₃H₉ClN₂O₂, (I), is nearly planar, with an intramolecular O⋯O hydrogen bond of 2.692 (2) Å. The latter title compound, C₁₇H₁₈ClN₃O₄, (II), exists in the keto–amine tautomeric form, with a strong intramolecular hydrogen bond of 2.640 (2) Å between the O and N atoms, the H atom being bonded to the N atom. The azo­benzene moieties of both mol­ecules have trans configurations, and the dihedral angle between the planes of the two aromatic rings is 4.1 (1)° in (I) and 9.9 (1)° in (II). The N—H⋯O hydrogen‐bonded rings are almost planar and coupled with the cyclo­hexa­diene rings in (II).     

4‐(2,4‐Dinitro­phenyl­sulfanyl)­morpholine

In the title compound, C₁₀H₁₁N₃O₅S, the 2,4‐dinitro­phenyl fragment is connected by an S atom to the morpholine ring, which is in a chair conformation. The ortho‐ and para‐nitro groups are slightly twisted out of the plane of the benzene ring. The mol­ecules are linked into C(7) and C(10) chains by two inter­molecular C—H⋯O hydrogen bonds.     

Diisopropyl­ammonium 2‐[(2,4‐dinitro­phenyl)­sulfanyl­amino­carbonyl]­benzoate

The structure of title compound, C₆H₁₆N⁺·C₁₄H₈N₃O₇S⁻, comprises discrete ions which are inter­connected by N—H⋯O⁻ and N—H⁺⋯O⁻ hydrogen bonds, leading to a neutral one‐dimensional network along [100]. These hydrogen bonds appear to complement the Coulombic inter­action and help to stabilize the structure further.     

Tetra­aqua(2,2′‐bi­pyridine)­nickel(II) terephthalate

The reaction of nickel(II) nitrate with terephthalic acid and 2,2′‐bi­pyridine in di­methyl­form­amide solution gives the title complex, [Ni(C₁₀H₈N₂)(H₂O)₄](C₈H₄O₄). The Ni^II ion is octahedrally coordinated to one 2,2′‐bi­pyridine and four water mol­ecules and does not coordinate to the terephthalate anion. Hydro­gen bonds between the terephthalate anions and the [Ni(2,2′‐bipy)(H₂O)₄]²⁺ cations produce a two‐dimensional hydrogen‐bonding architecture with double sheets.     

trans‐Tetra­chloro­bis(4‐methyl­pyridine)­germanium(IV)

The structure of the title compound, [GeCl₄(C₆H₇N)₂], (I), is the first example of an addition compound of GeCl₄ with two aromatic nitro­gen bases. The mol­ecule, with essential D_2h symmetry, has crystallographic C_2h symmetry. The environment around the Ge atom can be described as a slightly distorted octahedron with the 4‐methyl­pyridine ligands occupying axial positions and the four chloro ligands in the equatorial plane. The structure of (I) is isomorphous with the corresponding silicon halides.     

[Tris(4‐tolyl)­methyl]­benzene

The crystal structure of the title compound, C₂₈H₂₆, in the monoclinic space group C2/c has a columnar packing arrangement with a 7.20 Å axis, a feature common to several tetra­phenyl­methanes.     

1,1‐Bis­(phenyl­sulfonyl)‐1‐(pyridinio)­methanide

The title di­sulfonyl‐stabilized pyridinium yl­ide, C₅H₅N⁺–C⁻(SO₂C₆H₅)₂ or C₁₈H₁₅NO₄S₂, contains a near planar NCS₂ core. The structure suggests that the formal negative charge of the yl­ide C atom is delocalized to the S atoms rather than the N atom. Structural features of pyridinium yl­ides are briefly discussed.     

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.     

2,6‐Di­methyl‐4‐(phenyl­diazenyl)­phenol

The crystal structure of the title compound, C₁₄H₁₄N₂O, determined at 293 K, shows that the mol­ecule is approximately planar in the solid state and that the aromatic rings have a trans configuration with respect to the azo double bond, as found for other diazene derivatives. The packing can be described as a polymeric arrangement of mol­ecules linked through O—H⋯N and C—H⋯O hydrogen bonds and close contacts. These intermolecular interactions result in the formation of infinite chains parallel to the b axis.     

(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.     

3‐Methoxy‐5‐(4‐methyl­phenyl­diazenyl)­salicyl­aldehyde and 3‐methoxy‐5‐(2‐methyl­phenyl­diazenyl)­salicyl­aldehyde

The two title mol­ecules, both C₁₅H₁₄N₂O₃, are roughly planar and display a trans conformation with respect to the –N=N– double bond, as found for other diazene derivatives. In both compounds, there are intramolecular O—H⋯O hydrogen bonds and the crystal packing is governed by weak intermolecular C—H⋯O hydrogen bonds and π–π stacking.     

Bis­[(R)‐1‐phenyl­ethyl isocyanido](5,10,15,20‐tetrakis{2,6‐bis[(S)‐2,2‐di­methyl‐1,3‐dioxolan‐4‐yl­methyl­oxy]­phenyl}­porphyrin)­ruthenium(II) at 110 K

The geometry about the Ru atom in the title compound, [Ru(C₉H₉N)₂(C₉₂H₁₀₈N₄O₂₄)], is approximately tetragonal and the porphyrin ring is nearly planar, while the C—N—R angles [169.3 (3) and 163.9 (3)°] of the isocyanide ligands in the complex are different from the value of 180° expected in the free ligand.