Di­chloro­bis(1,2‐phenyl­enedi­amine)­nickel(II)

The title compound, [NiCl₂(C₆H₈N₂)₂], contains centrosymmetric mol­ecules with two phenyl­ene­di­amine ligands coordinated in a bidentate fashion. The Ni—N distances are 2.088 (1) and 2.096 (1) Å, and the Ni—Cl distance of 2.4635 (4) Å. The plane of each phenyl­enedi­amine mol­ecule makes a dihedral angle of 26.53 (7)° with the NiN₄ plane. Extensive hydrogen bonding leads to distinct cleavage in the bc plane.     

Tris­(ethyl­enedi­amine‐N,N′)cobalt(III) oxalate perchlorate dihydrate

The crystallization behavior of the title compound, [Co(C₂H₈N₂)₃](C₂O₄)(ClO₄)·2H₂O, has been studied in order to evaluate the effect of the counter‐anion on the crystalline structures of [Co(en)₃](C₂O₄)·X (en = ethyl­enedi­amine). Two‐dimensional intermolecular hydrogen‐bonding networks are formed between the amine protons of the [Co(en)₃]³⁺ cations and the O atoms of the oxalate anions. Perchlorate and water mol­ecules fill in the channels between the two‐dimensional networks and form hydrogen‐bonding interactions with the two‐dimensional layers, thus constructing a three‐dimensional hydrogen‐bonding network.     

Bis­(acetone‐κO)­bis(N,N′‐di­methyl­ethyl­enedi­amine‐κ2N,N′)copper(II) diperchlorate

The title compound, [Cu(C₄H₁₂N₂)₂(C₃H₆O)₂](ClO₄)₂, is the first structurally characterized Cu^II complex having acetone as axial ligands. The complex adopts an elongated octahedral trans‐[CuN₄O₂] coordination geometry, with the Cu atom having 222 site symmetry. The axial Cu—O(acetone) and in‐plane Cu—N bond lengths are 2.507 (5) and 2.041 (3) Å, respectively.     

[N′‐Benzoyl‐N,N‐bis(2‐pyridylmethyl‐κN)­ethyl­enedi­amine‐κN]chloro­copper(II) hexa­fluoro­phosphate

The title mononuclear copper(II) complex, [CuCl(C₂₁H₂₂­N₄O)]­PF₆, shows a distorted square‐planar coordination and the benzoyl­amino N atom does not coordinate to the Cu atom.     

(1R*,2R*)‐1,2‐(2,3‐Di­methoxy­butane‐2,3‐dioxy)cyclo­hexane

The title compound, 2,3‐di­methoxy‐2,3‐di­methyl‐5,6,7,8‐tetra­hydro‐4‐oxa­chroman, C₁₂H₂₂O₄, was synthesized as a model compound for substituted diequatorial fixed vicinal trans‐cyclo­hexane­diols.     

Chloro­[N′,N′‐diethyl‐N,N‐bis(2‐pyri­dyl­methyl)­ethyl­enedi­amine‐κ4N]copper(II) perchlorate

The title mononuclear copper(II) complex, [CuCl(C₁₈H₂₆N₄)]ClO₄, shows a square‐pyramidal coordination with the diethyl­amino N atom at the apical position. Large anisotropies in the displacement parameters of the non‐H atoms of the ligand seem to be due to rotational disorder of the ClO₄^? anion.     

Bis­(ethyl­enedi­amine)copper(II) bis(O,O′‐diethyl di­thio­phosphate)

In the structure of the title compound, [Cu^II­(en)₂][(EtO)₂P(S)S]₂ (en is ethyl­ene­di­amine) or [Cu(C₂H₈N₂)₂](C₄H₁₀O₂PS₂)₂, the Cu atom lies on a center of inversion and is coordinated in a slightly distorted square coordination geometry by four N atoms from two ethyl­enedi­amine mol­ecules. The diethyl di­thio­phosphate moieties, (EtO)₂P(S)S^?, act as counter‐anions.     

trans‐Chloro­bis­(ethyl­enedi­amine‐N,N′)­nitro­cobalt(III) perchlorate

In the title compound, trans‐[CoCl(NO₂)(C₂H₈N₂)₂]ClO₄, there are two independent Co^III complexes with a distorted octahedral coordination, and they show an orientational disorder such that the positions of the nitro and chloro ligands are exchanged. As a result, the averaged structure has inversion centres at the Co atoms. The perchlorate‐O atoms are disordered over two sites.     

(1R,2R,3S,4S)‐2‐[(2R,3S)‐2,3‐Di­methyl­oxiran‐2‐yl]‐3,4‐bis(4‐methoxy­benzyl­oxy)­cyclo­hexanol

The relative configuration was determined for the title com­pound, C₂₆H₃₄O₆, which was prepared in a synthetic study on immunosuppressant FR­65­814. There is an intra­mol­ecular hydrogen bond between the hydroxy and epoxy groups.     

Tris[(1‐methylimidazol‐2‐yl)methyl]amine–boric acid (1/1)

Cocrystallization of a poly­imidazole compound with boric acid results in the formation of the title compound, C₁₅H₂₁N₇·B(OH)₃, which has an extensive hydrogen‐bonding network. The O?N(im) separations (im is imidazole) range from 2.6991 (15) to 2.7914 (14) Å, with O—H?N angles ranging from 170.6 (18) to 175 (2)°. In addition, symmetry‐related boric acid mol­ecules form intermolecular hydrogen bonds, with an O?O distance of 2.7582 (14) Å, and symmetry‐related imidazole groups form π–π stacks, with a centroid‐to‐centroid separation of 3.533 Å.     

(1R,8R,11R)‐3,3,11‐Tri­methyl‐6,6‐ethyl­ene­dioxy­bi­cyclo­[6.3.0]­undecan‐2‐one and (1R,2R,8R,11R)‐3,3,11‐tri­methyl‐6,6‐ethylenedioxybicyclo[6.3.0]undecan‐2‐ol

The reduction of (1R,8R,11R)‐3,3,11‐tri­methyl‐6,6‐ethyl­ene­dioxy­bi­cyclo­[6.3.0]­undecan‐2‐one, C₁₆H₂₆O₃, (I), gave exclusively an alcohol, C₁₆H₂₈O₃, (II). The stereochemistry of the hydroxyl group in (II) was shown as R. The conformation around the eight‐membered carbocycle in (I) differs markedly from that in (II).     

trans‐Chloro­bis­(ethyl­enedi­amine‐N,N′)­nitro­cobalt(III) nitrate

In the title compound, trans‐[CoCl(NO₂)(C₂H₈N₂)₂]NO₃, a distorted octahedral Co^III complex shows an orientational disorder such that the positions of the nitro and chloro ligands are exchanged. The occupation factors of the major and minor orientations are 84 and 16%, respectively. The O atoms of the nitrate ion are disordered over two sites.     

5,8‐Di­methoxy‐2,3‐bis(2‐pyridyl)­quinoxaline

In the crystal structure of the title compound, C₂₀H₁₆N₄O₂, the two pyridine rings subtend dihedral angles of 39.0 (1) and 43.4 (2)° with the mean quinoxaline plane and 67.6 (1)° with each other. The orientation of the pyridine rings is such that their N‐donors face each other (cis–cis conformation) with a separation of 3.169 (2) Å. There exist significant π–π interactions responsible for the formation of stacks along the crystallographic a axis of the crystal.     

4‐Pyridone–terephthalic acid–water (2/1/2) and bis(3‐hydroxypyridinium) terephthalate

4‐Hydroxypyridine and terephthalic acid cocrystallize as a hydrate, 4‐pyridone–terephthalic acid–water (2/1/2), 2C₅H₅NO·C₈H₆O₄·2H₂O, from a methanol–water solution. The molecules form a two‐dimensional hydrogen‐bonded network resulting in sheets of hydrogen‐bonded molecules that lie parallel to the (10) plane. In contrast, 3‐hydroxypyridine and terephthalic acid form the salt bis(3‐hydroxypyridinium) terephthalate, 2C₅H₆NO⁺·C₈H₄O₄²⁻, giving rise to two‐dimensional hydrogen‐bonded sheets extending through the lattice parallel to the (10) plane.     

Bis­[N,N′‐bis­(di­phenyl­methyl­ene)ethyl­enedi­amine‐κ2N,N′]copper(I) di­chloro­cuprate(I)

The 1:1 adduct of N,N′‐bis­(di­phenyl­methyl­ene)­ethyl­enedi­amine (bz₂en) with copper(I) chloride, viz. [Cu(C₂₈H₂₄N₂)₂][CuCl₂], has been synthesized. The structure contains cationic moieties of Cu^I ions (Cu on a twofold axis) coordinated to four N atoms of two bz₂en mol­ecules (in a distorted tetrahedron) and linear di­chloro­cuprate(I) anions (with Cu on an inversion centre). These cations and anions are packed in columns along b. The packing of the cation and anion columns involves a significant C—H⋯Cl interaction and four short intermolecular C—H⋯π contacts, two of which are between cation columns.     

Bis­(ethyl­enedi­amine‐N,N′)(pyrimidine‐2‐carboxyl­ato‐N1,O)­cobalt(III) bis­(tri­fluoro­methane­sulfonate) dihydrate

In the title compound, the coordination geometry of the Co^III atom is only slightly distorted from regular octahedral, and the racemic nature of the material was confirmed by X‐ray structure analysis.     

(1E)‐2‐(Di­acetyl­amino)‐1‐methyl­prop‐­1‐enyl acetate

The analysis of the title compound, C₁₀H₁₅NO₄, firmly establishes the configuration of the double bond as E, a stereochemistry that had been assigned tentatively by other methods. The di­acetyl­amine and acetate substituents are approximately coplanar to one another, but approximately perpendicular to the planar ethene core. H atoms of the ethene methyl substituents are found within the ethene plane, indicating that hyperconjugation does not play an important role in stabilizing the double bond.     

(1R,2R)‐2‐(4‐Methylenecyclohex‐2‐enyl)propyl (1R,4S)‐camphanate

Esterification of a single diastereomer of 2‐(4‐methylene­cyclohex‐2‐enyl)propanol, (II), with (1R,4S)‐(+)‐camphanic acid [(1R,4S)‐4,7,7‐trimethyl‐3‐oxo‐2‐oxabicyclo[2.2.1]heptane‐1‐carboxylic acid] leads to the crystalline title compound, C₂₀H₂₈O₄. The relative configuration of the camphanate was determined by X‐ray diffraction analysis. The outcome clarifies the relative and absolute stereochemistry of the naturally occurring bisabolane sesquiterpenes β‐turmerone and β‐sesquiphellandrene, since we have converted (II) into both natural products via a stereospecific route.     

Two seven‐membered heterocycles with 1,2‐diaza ring N atoms: 3,5,7‐triphenyl‐1,2‐diazacyclohepta‐1(7),2‐diene and 3,7‐bis(2‐hydroxyphenyl)‐5‐phenyl‐1,2‐diazacyclohepta‐1(7),2‐diene

The title compounds, 3,5,7‐triphenyl‐1,2‐diazacyclohepta‐1(7),2‐diene, C₂₃H₂₀N₂, (I), and 3,7‐bis(2‐hydroxyphenyl)‐5‐phenyl‐1,2‐diazacyclohepta‐1(7),2‐diene, C₂₃H₂₀N₂O₂, (II), constitute the first structurally characterized examples of seven‐membered heterocycles with 1,2‐diaza ring N atoms. Compound (I) crystallizes in the space group P, with two independent molecules in the asymmetric unit that differ in the conformation of one of the phenyl rings, while (II) crystallizes in the space group C2/c. The C₅N₂ ring in each of (I) and (II) adopts a twist‐boat conformation. Compound (I) exhibits neither C—H...π interactions nor π–π stacking interactions, whereas (II) shows both intramolecular O—H...N hydrogen bonds and a C—H...π interaction that joins the molecules into an infinite chain in the [010] direction.     

[N‐(Carboxyl­ato­methyl)­aspartato(3–)](ethyl­enedi­amine)­cobalt(III) trihydrate

The mononuclear title complex, [Co(C₆H₆NO₆)(C₂H₈N₂)]·3H₂O, contains an octahedrally coordinated Co^III atom. The N‐(carboxy­methyl)­aspartate moiety is coordinated as a tetradentate ligand, providing an OONO‐donor set and forming two trans five‐membered chelate rings and one six‐membered chelate ring. A seven‐membered chelate ring is also formed, which consists of part of the six‐membered chelate ring and part of one of the five‐membered chelate rings. The crystal structure of the complex is stabilized by hydrogen bonds with three water mol­ecules.