Acta Crystallographica Section E: Crystallographic Communications最新文献

In the four main structures, the anions and cations are connected by aurophilic contacts, hydrogen bonds C—H⋯halogen and (in two cases) C—H⋯Au contacts. In the by-product without pyridinic N coordination a N—H⋯N bond dominates the packing pattern supported by Br⋯Br, H⋯Br, and Au⋯Br contacts.

Bis(2-methyl­pyridine)­gold(I) di­bromido­aurate(I), [Au(C₆H₇N)₂][AuBr₂], (1), crystallizes in space group C2/c with Z = 4. Both gold atoms lie on twofold axes and are connected by an aurophilic contact. A second aurophilic contact leads to infinite chains of alternating cations and anions parallel to the b axis, and the residues are further connected by a short H⋯Au contact and a borderline Br⋯Br contact. Bis(3-methyl­pyridine)­gold(I) di­bromido­aurate(I), [Au(C₆H₇N)₂][AuBr₂], (2), crystallizes in space group C2/m with Z = 2. Both gold atoms lie on special positions with symmetry 2/m and are connected by an aurophilic contact; all other atoms except for one methyl hydrogen lie in mirror planes. The extended structure is closely analogous to that of 1, although the structures are formally not isotypic. Bis(3,5-di­methyl­pyridine)­gold(I) di­chlor­ido­aurate(I), [Au(C₇H₉N)₂][AuCl₂], (3) crystallizes in space group P

3-Phenyl-2-(thio­phen-3-yl)-2,3-di­hydro-4H-pyrido[3,2-e][1,3]thia­zin-4-one (C₁₇H₁₂N₂OS₂, 1) and 2-(1H-indol-3-yl)-3-phenyl-2,3-di­hydro-4H-pyrido[3,2-e][1,3]thia­zin-4-one 0.438-hydrate (C₂₁H₁₅N₃OS·0.438H₂O, 2) crystallize in space groups P2₁/n and C2/c, respectively. The asymmetric unit in each case is comprised of two parent mol­ecules, albeit of mixed chirality in the case of 1 and of similar chirality in 2 with the enanti­omers occupying the neighboring asymmetric units. Structure 2 also has water mol­ecules (partial occupancies) that form continous channels along the b-axis direction.

3-Phenyl-2-(thio­phen-3-yl)-2,3-di­hydro-4H-pyrido[3,2-e][1,3]thia­zin-4-one (C₁₇H₁₂N₂OS₂, 1) and 2-(1H-indol-3-yl)-3-phenyl-2,3-di­hydro-4H-pyrido[3,2-e][1,3]thia­zin-4-one 0.438-hydrate (C₂₁H₁₅N₃OS·0.438H₂O, 2) crystallize in space groups P2₁/n and C2/c, respectively. The asymmetric unit in each case is comprised of two parent mol­ecules, albeit of mixed chirality in the case of 1 and of similar chirality in 2 with the enanti­omers occupying the neighboring asymmetric units. Structure 2 also has water mol­ecules (partial occupancies) that form continuous channels along the b-axis direction. The thia­zine rings in both structures exhibit an envelope conformation. Inter­molecular inter­actions in 1 are defined only by C—H⋯O and C—H⋯N hydrogen bonds between crystallographically independent mol­ecules. In 2, hydrogen bonds of the type N—H⋯O between independent mol­ecules and C—H⋯N(π) type, and π–π stacking inter­actions between the pyridine rings of symmetry-related mol­ecules are observed.

In the title compound, the dihedral angle between the coumarin ring system and the penta­noate ring is 36.26 (8)°. A short intra­molecular C—H⋯O contact is observed.

In the title compound, C₁₄H₁₄O₄, the dihedral angle between the coumarin ring system (r.m.s deviation = 0.016 Å) and the penta­noate ring is 36.26 (8)°. A short intra­molecular C—H⋯O contact of 2.40 Å is observed. Hirshfeld surface analysis reveals that 46.1% of the inter­molecular inter­actions are from H⋯H contacts, 28.6% are from H⋯O/O⋯H contacts and 14.7% are from H⋯C/C⋯H.

The crystal structures of the title compounds, which arose from the same reaction, consist of discrete complexes in which the cobalt cations are either in a CoN₂O₃ trigonal–bipyramidal or a CoN₂O₄ octa­hedral coordination.

The reaction of CoBr₂, KNCSe and 2-methyl­pyridine N-oxide (C₆H₇NO) in ethanol leads to the formation of crystals of [Co(NCSe)₂(C₆H₇NO)₃] (1) and [Co(NCSe)₂(C₆H₇NO)₄] (2) from the same reaction mixture. The asymmetric unit of 1 is built up of one Co^II cation, two NCSe⁻ iso­seleno­cyanate anions and three 2-methyl­pyridine N-oxide coligands, with all atoms located on general positions. The asymmetric unit of 2 consists of two cobalt cations, four iso­seleno­canate anions and eight 2-methyl­pyridine N-oxide coligands in general positions, because two crystallographically independent complexes are present. In compound 1, the Co^II cations are fivefold coordinated to two terminally N-bonded anionic ligands and three 2-methyl­pyridine N-oxide coligands within a slightly distorted trigonal–bipyramidal coordination, forming discrete complexes with the O atoms occupying the equatorial sites. In compound 2, each of the two complexes is coordinated to two terminally N-bonded iso­seleno­cyanate anions and four 2-methyl­pyridine N-oxide coligands within a slightly distorted cis-CoN₂O₄ octa­hedral coordination geometry. In the crystal structures of 1 and 2, the complexes are linked by weak C—H⋯Se and C—H⋯O contacts. Powder X-ray diffraction reveals that neither of the two compounds were obtained as a pure crystalline phase.

Despite the facile inter­conversion of its conformers in solution, 4-benzyl-1H-pyrazole adopts a chiral crystal structure (space group P2₁). Its 3,5-di­amino derivative, however, crystallizes in the centrosymmetric space group P2₁/c. In both crystal structures, the aromatic moieties are organized in alternating bilayers in which they stack in parallel columns in two orthogonal directions, and the pyrazole units form catemer motifs by N—H⋯N and N—H⋯π hydrogen bonding, respectively.

The crystal structures of 4-benzyl-1H-pyrazole (C₁₀H₁₀N₂, 1) and 3,5-di­amino-4-benzyl-1H-pyrazole (C₁₀H₁₂N₄, 2) were measured at 150 K. Although its different conformers and atropenanti­omers easily inter­convert in solution by annular tautomerism and/or rotation of the benzyl substituent around the C(pyrazole)—C(CH₂) single bond (as revealed by ¹H NMR spectroscopy), 1 crystallizes in the non-centrosymmetric space group P2₁. Within its crystal structure, the pyrazole and phenyl aromatic moieties are organized into alternating bilayers. Both pyrazole and phenyl layers consist of aromatic rings stacked into columns in two orthogonal directions. Within the pyrazole layer, the pyrazole rings form parallel catemers by N—H⋯N hydrogen bonding. Compound 2 adopts a similar bilayer structure, albeit in the centrosymmetric space group P2₁/c, with pyrazole N—H protons as donors in N—H⋯π hydrogen bonds with neighboring pyrazole rings, and NH₂ protons as donors in N—H⋯N hydrogen bonds with adjacent pyrazoles and other NH₂ moieties. The crystal structures and supra­molecular features of 1 and 2 are contrasted with the two known structures of their analogs, 3,5-dimethyl-4-benzyl-1H-pyrazole and 3,5-diphenyl-4-benzyl-1H-pyrazole.

The crystal structure of the mol­ecular complex between 2-(allyl­thio)­pyridine and 1,2,4,5-tetra­fluoro-3,6-di­iodo­benzene, which exhibits an N⋯I halogen bond, has been determined at 100 K.

The crystal structure of the title 2:1 mol­ecular complex between 2-(allyl­thio)­pyridine and 1,2,4,5-tetra­fluoro-3,6-di­iodo­benzene, C₆F₄I₂·2C₈H₉NS, at 100 K has been determined in the monoclinic space group P2₁/c. The most noteworthy characteristic of the complex is the halogen bond between iodine and the pyridine ring with a short N⋯I contact [2.8628 (12) Å]. The Hirshfeld surface analysis shows that the hydrogen⋯hydrogen contacts dominate the crystal packing with a contribution of 32.1%.

The title salt features N—H⋯Cl and C—H⋯Cl cation-to-anion hydrogen bonds and complementary anion-to-cation Cl⋯π inter­actions.

In the title mol­ecular salt, (C₁₂H₁₄N₂)[CoCl₄], the dihedral angle between the pyridine rings of the cation is 52.46 (9)° and the N—C—C—N torsion angle is −128.78 (14)°, indicating that the ring nitro­gen atoms are in anti-clinal conformation. The Cl—Co—Cl bond angles in the anion span the range 105.46 (3)–117.91 (2)°. In the extended structure, the cations and anions are linked by cation-to-anion N—H⋯Cl and C—H⋯Cl inter­actions, facilitating the formation of R⁴₄(18) and R⁴₄(20) ring motifs. Furthermore, the crystal structure features weak anion-to-cation Cl⋯π inter­actions [Cl⋯π = 3.4891 (12) and 3.5465 (12) Å]. Hirshfeld two-dimensional fingerprint plots revealed that the most significant inter­actions are Cl⋯H/H⋯Cl (45.5%), H⋯H (29.0%), Cl⋯C/C⋯Cl (7.8%), Cl⋯N/N⋯Cl (3.5%), Cl⋯Cl (1.4) and Co⋯H (1%) contacts.

The crystal structures of two chromium(II) acetate complexes with N-heterocyclic carbene coligands were determined.

Tetra­kis(μ-acetato-κ²O:O′)bis­{[1,3-bis­(2,6-diiso­propyl­phen­yl)imidazol-2-yl­idene-κC²]chromium(II)} tetra­hydro­furan disolvate, [Cr₂(C₂H₃O₂)₄(C₂₇H₃₆N₄)₂]·2C₄H₈O or [Cr₂(OAc)₄(IDipp)₂]·2C₄H₈O (1), and tetra­kis­(μ-acetato-κ²O:O′)bis­{[1,3-bis­(2,4,6-tri­methyl­phen­yl)imidazol-2-yl­idene-κC²]chromium(II)},{Cr₂(C₂H₃O₂)₄(C₂₁H₂₄N₂)₂] or [Cr₂(OAc)₄(IMes)₂] (2), were synthesized from anhydrous chromium(II) acetate [Cr₂(OAc)₄] and the corresponding NHC (NHC = N-heterocyclic carbene) in toluene as solvent. Both complexes crystallize in the triclinic system, space group P

The crystal structure of tricarbon­yl[η⁴-6-exo-(tri­phenyl­phosphino)cyclo­hepta-2,4-dien-1-one]iron(0) tetra­fluoro­borate is described. The two independent tricarbon­yl[η⁴-6-exo-(tri­phenyl­phosphino)cyclo­hepta-2,4-dien-1-one] iron(0) cations and their corresponding anions form dimers, which constitute the asymmetric unit of the structure within the (100) plane.

The mol­ecular structure of tricarbon­yl[η⁴-6-exo-(tri­phenyl­phosphino)cyclo­hepta-2,4-dien-1-one]iron(0) tetra­fluoro­borate di­chloro­methane hemisolvate, [Fe(C₂₈H₂₂O₄)(CO)₃]BF₄·0.5CH₂Cl₂, as determined by single-crystal X-ray diffraction is reported. The two independent tricarbon­yl[η⁴-6-exo-(tri­phenyl­phosphino)cyclo­hepta-2,4-dien-1-one] iron(0) cations and their corresponding anions form dimers, which constitute the asymmetric unit of the structure parallel to the (100) plane. Solid-state stability within that asymmetric unit as well as between neighboring dimeric units is afforded by C—H⋯O and C—H⋯F hydrogen bonds and C—H⋯π and Y—X⋯π (Y = B, C; X = F, O) inter­actions, which yield diperiodic sheets and a three-dimensional extended network.

The crystal structures of 2-[1′-(carb­oxy­meth­yl)-4,4′-bi­pyridine-1,1′-diium-1-yl]acetate tetra­fluoro­borate, C₁₄H₁₃N₂O₄⁺·BF₄⁻ or (Hbcbpy)(BF₄), and neutral 1,1′-bis­(carboxyl­atometh­yl)-4,4′-bi­pyridine-1,1′-diium (bcbpy), C₁₄H₂₀N₂O₈, are reported.

The crystal structures of 2-[1′-(carb­oxy­meth­yl)-4,4′-bi­pyridine-1,1′-diium-1-yl]acetate tetra­fluoro­borate, C₁₄H₁₃N₂O₄⁺·BF₄⁻ or (Hbcbpy)(BF₄), and neutral 1,1′-bis­(carboxyl­atometh­yl)-4,4′-bi­pyridine-1,1′-diium (bcbpy), C₁₄H₂₀N₂O₈, are reported. The asymmetric unit of the (Hbcbpy)(BF₄) consists of a Hbcbpy⁺ monocation, a BF₄⁻ anion, and one-half of a water mol­ecule. The BF₄⁻ anion is disordered. Two pyridinium rings of the Hbcbpy⁺ monocation are twisted at a torsion angle of 30.3 (2)° with respect to each other. The Hbcbpy monocation contains a carb­oxy­lic acid group and a deprotonated carboxyl­ate group. Both groups exhibit both a long and a short C—O bond. The cations are linked by inter­molecular hydrogen-bonding inter­actions between the carb­oxy­lic acid and the deprotonated carboxyl­ate group to give one-dimensional zigzag chains. The asymmetric unit of the neutral bcbpy consists of one-half of the bcbpy and two water mol­ecules. In contrast to the Hbcbpy⁺ monocation, the neutral bcbpy mol­ecule contains two pyridinium rings that are coplanar with each other and a carboxyl­ate group with similar C—O bond lengths. The mol­ecules are connected by inter­molecular hydrogen-bonding inter­actions between water mol­ecules and carboxyl­ate groups, forming a three-dimensional hydrogen-bonding network.