Tris(2‐cyanoethyl) isocyanurate

The title compound, 1,3,5‐tris(2‐cyano­ethyl)‐1,3,5‐triazine‐2,4,6(1H,3H,5H)‐trione, C₁₂H₁₂N₆O₃, forms a layered structure stabilized by C—H?O and C—H?N hydrogen bonds.     

Tris(2‐cyano­ethyl)­amine

In the title compound, N(CH₂CH₂CN)₃, (I), the three cyano­ethyl groups adopt a conformation with the CN groups oriented in the same direction, suggesting the compound may behave as a potential tripodal ligand.     

Molecular dynamics of cis‐1‐(2‐hydroxy‐5‐ methylphenyl)ethanone oxime and N‐(2‐hydroxy‐4‐methylphenyl)acetamide in solution studied by NMR spectroscopy

The formation of hydrogen bonds and molecular dynamics for the molecules cis‐1‐(2‐hydroxy‐5‐methylphenyl)ethanone oxime ( I ) and N‐(2‐hydroxy‐4‐methylphenyl)acetamide ( II ) have been investigated in solution using NMR. The results confirm the formation of O? H···O, O? H···N and O···H? N type inter‐ and intramolecular hydrogen bonds. Spin‐lattice relaxation times (T₁), activation energy of molecular dynamics and energy of intramolecular hydrogen bonds have been determined. Copyright © 2010 John Wiley & Sons, Ltd.     

1,3,5‐Tris(bromomethyl)benzene

The asymmetric unit of the title compound, C₉H₉Br₃, is composed of a single molecule. Two bromo substituents are located on one side of the plane of the aromatic ring and the third is on the opposite side, with the molecular unit exhibiting an approximate noncrystallographic C_s point group. The crystal structure is rich in Br...Br, CH₂...Br and CH...π weak intermolecular contacts which mediate the crystal packing of individual molecules. These interactions promote a red‐shift of a handful of vibrational modes (associated with the pendant –CH₂Br groups) compared with values from theoretical density functional theory (DFT) calculations.     

Tris(2‐methyl­quinoline‐8‐seleno­lato‐κ2N,Se)antimony(III)

The title complex, [Sb(C₁₀H₈NSe)₃], has a 3Se+3N distorted octa­hedral geometry at the Sb atom. The structure is stabilized by weak inter­molecular C—H⋯π(arene) inter­actions.     

Bis(2,5‐dimethoxy‐4‐methylphenyl)methane and bis(2,5‐dimethoxy‐3,4,6‐trimethylphenyl)methane

Bis(2,5‐di­methoxy‐4‐methyl­phenyl)­methane, C₁₉H₂₄O₄, (IIa), was obtained and characterized as a minor product from the reaction of tolu­hydro­quinone di­methyl ether (1,4‐dimethoxy‐2‐methylbenzene) with N‐(hydroxy­methyl)­tri­fluoro­acet­amide. Similarly, bis(2,5‐di­methoxy‐3,4,6‐tri­methyl­phenyl)­methane, C₂₃H₃₂O₄, (IIb), was prepared from the corresponding reaction of tri­methyl­hydro­quinone di­methyl ether (2,5‐dimethoxy‐1,3,4‐trimethylbenzene). The mol­ecules of (IIa) and (IIb) each lie on a twofold axis passing through the methyl­ene group. The dihedral angle between the planar phenyl rings is 73.4 (1)° in (IIa) and 77.9 (1)° in (IIb). The external bond angles around the bridging methyl­ene group are 116.6 (2) and 117.3 (2)° for (IIa) and (IIb), respectively. In (IIa), the methoxy substituents lie in the plane of the ring and are conjugated with the aromatic system, whereas in (IIb), they are almost perpendicular to the phenyl ring and are positioned on opposite sides.     

A short synthesis of the parp inhibitor 2‐(4‐trifluoro‐methylphenyl)benzimidazole‐4‐carboxamide (NU1077)

A four‐step synthesis of the PARP inhibitor 2‐(4‐trifluoromethylphenyl)benzimidazole‐4‐carboxamide (1, NU1077) is presented. Condensation of 2,3‐diaminotoluene and 4‐trifluoromethylbenzaldehyde afforded 4‐methyl‐2‐(4‐trifluoromethylphenyl)benzimidazole. Oxidation of the methyl group with potassium permanganate in warm t‐butanol afforded the carboxylic acid that was converted to the corresponding carboxamide via,/ the acid chloride.     

trans‐1,2,3‐Tris(1‐hydroxycyclo­propyl)cyclopropane

The central three‐membered ring in the title compound, trans‐1,1′,1′′‐cyclo­propane‐1,2,3‐triyl­tris­(cyclo­propanol), C₁₂H₁₈O₃, shows pronounced asymmetry of the bond lengths, which is induced by the different orientations of the substituents. A network of hydrogen bonds links the mol­ecules into sheets.     

Structural investigation of 5,10‐A2B2‐type porphyrins: palladium(II) and zinc(II) complexes of 5,10‐dibromo‐15,20‐bis(4‐methylphenyl)porphyrin

The analysis of [5,10‐dibromo‐15,20‐bis(4‐methylphenyl)porphyrinato]palladium(II), [Pd(C₃₄H₂₂Br₂N₄)], and [5,10‐dibromo‐15,20‐bis(4‐methylphenyl)porphyrinato](methanol)zinc(II), [Zn(C₃₄H₂₂Br₂N₄)(CH₄O)], reveals a small but localized influence of the bromine residues on the conformation of the macrocycle. A comparison of the 5,10‐dibromo substituent pattern with literature data for 5,15‐dibromoporphyrins shows similar in‐plane distortions in both but a different mix of out‐of‐plane distortion modes for the different regiochemical arrangements.     

2‐[(E)‐(4‐Hydroxy‐3‐methoxybenzylidene)amino]‐N‐(2‐methylphenyl)‐4,5,6,7‐tetrahydro‐1‐benzothiophene‐3‐carboxamide

The title compound, C₂₄H₂₄N₂O₃S, exhibits antifungal and antibacterial properties. The compound crystallizes with two molecules in the asymmetric unit, with one molecule exhibiting `orientational disorder' in the crystal structure with respect to the cyclohexene ring. The o‐toluidine groups in both molecules are noncoplanar with the respective cyclohexene‐fused thiophene ring. In both molecules, there is an intramolecular N—H...N hydrogen bond forming a pseudo‐six‐membered ring which locks the molecular conformation and eliminates conformational flexibility. The crystal structure is stabilized by O—H...O hydrogen bonds; both molecules in the asymmetric unit form independent chains, each such chain consisting of alternating `ordered' and `disordered' molecules in the crystal lattice.     

Tris(1,9‐diethyl­adeninium) triiodide diiodide

X‐ray analysis of the title compound reveals three crystallographically distinct cations of 1,9‐diethyl­adeninium, two iodide anions and one triiodide anion in the asymmetric unit, giving six residues and the formula 3C₉H₁₄N₅⁺·I₃⁻·2I⁻. Standard purine nomenclature is used to identify the atoms of each adenine moiety. Hydrogen bonding is observed between atoms N6 and N7 of a pair of cations [N⋯N = 2.885 (4)/2.902 (3) and 2.854 (3)/2.854 (3) Å], with additional hydrogen bonding to I⁻ anions via the other N6 H atom [N⋯I = 3.708 (3), 3.738 (3) and 3.638 (3) Å]. The triiodide anion is not involved in hydrogen bonding. The bond lengths and angles of the 1,9‐diethyl­adeninium cations are compared with literature values and confirm the formation of the imine tautomer.     

An enantiomerically pure P‐stereogenic bisphosphine: (S,S)‐ethylenebis[(2‐methylphenyl)phenylphosphine] (o‐tolyl‐DiPAMP)

In connection with a research program involving the synthesis, structure determination, reactivity and ability to coordinate to metal centres of chiral bisphosphine ligands, we have synthesized and structurally characterized, by means of single‐crystal X‐ray diffraction analysis, the title compound {systematic name: (S,S)‐(ethane‐1,2‐diyl)bis[(2‐methylphenyl)phenylphosphane], abbreviated as o‐tolyl‐DiPAMP}, C₂₈H₂₈P₂. So far, neither the free bisphosphine (DiPAMP) nor analogues that incorporate the ethylenebisphosphine frame have had their crystal structures reported. The investigated compound forms crystals which are isostructural with the bisphosphine dioxide analogue [King et al. (2007). Acta Cryst. E 63 , o3278], despite the involvement of the dioxide in C—H...O(=P) hydrogen bonds and the lack of similar hydrogen bonds in the investigated crystal structure. In both molecules, the P—C—C—P chain is in a trans conformation, extended further at both ends by one of the two P—C_ipso bonds. The planes of the phenyl and o‐tolyl rings attached to the same P atom are nearly perpendicular to one another. Both crystal structures are mainly stabilized by dispersive interactions.     

Tris[2‐(morpholin‐4‐ylmethyl)phenyl‐κ2C1,N]antimony(III)

The title compound, [Sb(C₁₁H₁₄NO)₃], is monomeric with the Sb atom located on a threefold axis. The complex exhibits distorted trigonal–antiprismatic geometry around the Sb atom, owing to the presence of intramolecular N→Sb interactions. H...phenyl intermolecular interactions lead to the formation of dimers stacked along the c axis. The morpholine rings exhibit almost ideal chair conformations. No intermolecular interactions between the morpholine rings of neighbouring molecules were observed.     

Tris(1,10‐phenanthroline‐κ2N,N′)cobalt(III) tris(trifluoromethanesulfonate) dihydrate

The title compound, [Co(C₁₂H₈N₂)₃](CF₃SO₃)₃·2H₂O, crystallizes to form infinite chains of complex cations that are connected through offset face‐to‐face and edge‐to‐face interactions between their phenanthroline ligands. The chains are themselves interconnected through weak offset face‐to‐face ligand interactions. The three trifluoromethanesulfonate anions of the asymmetric unit are connected with one another through the two water molecules by hydrogen bonds. One of the trifluoromethanesulfonate anions is described by a disorder over three positions, with occupancies of 0.35, 0.35 and 0.3 in the refined model.     

2‐{[Tris(hydroxymethyl)methyl]aminomethylene}cyclohexa‐3,5‐dien‐1(2H)‐one and its 6‐hydroxy and 6‐methoxy derivatives

The title compounds, 2‐{[tris­(hydroxy­methyl)­methyl]­amino­methyl­ene}cyclo­hexa‐3,5‐dien‐1(2H)‐one, C₁₁H₁₅NO₄, (I), 6‐hydroxy‐2‐{[tris­(hydroxy­methyl)­methyl]­amino­methyl­ene}­cyclo­hexa‐3,5‐dien‐1(2H)‐one, C₁₁H₁₅NO₅, (II), and 6‐methoxy‐2‐{[tris­(hydroxy­methyl)­methyl]­amino­methyl­ene}­cyclo­hexa‐3,5‐dien‐1(2H)‐one, C₁₂H₁₇NO₅, (III), adopt the keto–amine tautomeric form, with the formal hydroxy H atom located on the N atom, and the NH group and oxo O atom display a strong intramolecular N—H⋯O hydrogen bond. The N—H⋯O hydrogen‐bonded rings are almost planar and coupled with the cyclo­hexa­diene rings. The carbonyl O atoms accept two other H atoms from the alcohol groups of adjacent mol­ecules in (I), and one from the alcohol and one from the phenol group in (II), but from only one alcohol H atom in (III).     

1,4,7‐Tris(2‐cyano­ethyl)‐4,7‐tri­aza‐1‐azonia­cyclo­nonane perchlorate

There are three independent mol­ecules in the asymmetric unit of the title compound, C₁₅H₂₅N₆⁺·ClO₄⁻. The cations are linked to form an (30) ring with two arms and are then linked into columns in the [010] direction by C(11) chains formed via C—H⃛N hydrogen bonds.