Acta Crystallographica Section E: Crystallographic Communications最新文献

In the crystal structure of the title compound, Ni(NCS)₂(C₆H₇N)₂ (C₆H₇N = 4-methyl­pyridine), the Ni^II cations are in an octa­hedral coordination and are linked by pairs of anionic ligands into corrugated chains in which the cations show alternating all-trans and cis–cis–trans coordination geometries. Upon heating, the title compound transforms into Ni(NCS)₂(C₆H₇N), which is isotypic to its Cd analog as proven by a Rietveld refinement.

The title compound, [Ni(NCS)₂(C₆H₇N)₂]_n, was prepared by the reaction of Ni(NCS)₂ with 4-methyl­pyridine in water. Its asymmetric unit consists of two crystallographically independent Ni^II cations, of which one is located on a twofold rotational axis whereas the second occupies a center of inversion, two independent thio­cyanate anions and two independent 4-methyl­pyridine co­ligands in general positions. Each Ni^II cation is octa­hedrally coordinated by two 4-methyl­pyridine coligands as well as two N- and two S-bonded thio­cyanate anions. One of the cations shows an all-trans, the other a cis–cis–trans configuration. The metal centers are linked by pairs of μ-1,3-bridging thio­cyanate anions into [101] chains. X-ray powder diffraction shows that a pure crystalline phase has been obtained and thermogravimetry coupled to differential thermoanalysis reveals that the title compound loses half of the 4-methyl­pyridine coligands and transforms into Ni(NCS)₂(C₆H₇N). Nearly pure samples of this compound can be obtained by thermal annealing and a Rietveld refinement demonstrated that it is isotypic to its recently reported Cd analog [Neumann et al., (2020#). CrystEngComm.22, 184–194] In its crystal structure, the metal cations are linked by one μ-1,3(N,S)- and one μ-1,3,3(N,S,S)-bridging thio­cyanate anion into single chains that condense via the μ-1,3,3(N,S,S)-bridging anionic ligands into double chains.

The cystallization and capture of hexa­chloro­thallium within the phospho­tunsgate and caesium chloride matrix is described.

Crystal formation of caesium thallium chloride phospho­tungstates, Cs₉(TlCl₆)(PW₁₂O₄₀)₂·9CsCl showcases the ability to capture and crystallize octa­hedral complexes via the use of polyoxometalates (POMs). The large number of caesium chlorides allows for the POM [α-PW₁₂O₄₀]³⁻ to arrange itself in a cubic close-packing lattice extended framework, in which the voids created enable the capture of the [TlCl₆]³⁻ complex.

This study describes the synthesis, characterization, and Hirshfeld surface analysis of a small organic ammonium bromide salt. The analysis reveals a torsion angle of −64.8 (2)° between the ammonium group and the bromine substituent.

This study presents the synthesis, characterization and Hirshfeld surface analysis of a small organic ammonium salt, C₂H₇BrN⁺·Br⁻. Small cations like the one in the title compound are considered promising components of hybrid perovskites, crucial for optoelectronic and photovoltaic applications. While the incorporation of this organic cation into various hybrid perovskite structures has been explored, its halide salt counterpart remains largely uninvestigated. The obtained structural results are valuable for the synthesis and phase analysis of hybrid perovskites. The title compound crystallizes in the solvent-free form in the centrosymmetric monoclinic space group P2₁/c, featuring one organic cation and one bromide anion in its asymmetric unit, with a torsion angle of −64.8 (2)° between the ammonium group and the bromine substituent, positioned in a gauche conformation. The crystal packing is predominantly governed by Br⋯H inter­actions, which constitute 62.6% of the overall close atom contacts.

The title complex possesses pseudo-octa­hedral geometry where one face of the octa­hedron is occupied by three carbonyl ligands and the other face is occupied by one sp² nitro­gen atom of the sulfonamide group and two sp³ nitro­gen atoms of the dien backbone.

The title compound, [Re(C₁₇H₂₂N₃O₂S)(CO)₃] is a net neutral fac-Re(I)(CO)₃ complex of the 4-methyl­biphenyl sulfonamide derivatized di­ethyl­enetri­amine ligand. The NNN-donor monoanionic ligand coordinates with the Re core in tridentate fashion, establishing an inner coordination sphere resulting in a net neutral complex. The complex possesses pseudo-octa­hedral geometry where one face of the octa­hedron is occupied by three carbonyl ligands and the other faces are occupied by one sp² nitro­gen atom of the sulfonamide group and two sp³ nitro­gen atoms of the dien backbone. The Re—Nsp² bond distance, 2.173 (4) Å, is shorter than the Re—Nsp³ bond distances, 2.217 (5) and 2.228 (6) Å, and is similar to the range reported for typical Re—Nsp² bond lengths (2.14 to 2.18 Å).

In the crystal, mol­ecules are linked by inter­molecular N—H⋯O, C—H⋯O, C—H⋯F and C—H⋯Br hydrogen bonds, forming a three-dimensional network. In addition, C—H⋯π inter­actions connect mol­ecules into ribbons along the b-axis direction, consolidating the mol­ecular packing.

In the title compound, C₁₉H₁₈BrFN₂O, the pyrrolidine ring adopts an envelope conformation. In the crystal, mol­ecules are linked by inter­molecular N—H⋯O, C—H⋯O, C—H⋯F and C—H⋯Br hydrogen bonds, forming a three-dimensional network. In addition, C—H⋯π inter­actions connect mol­ecules into ribbons along the b-axis direction, consolidating the mol­ecular packing. The inter­molecular inter­actions in the crystal structure were qu­anti­fied and analysed using Hirshfeld surface analysis.

The title compound contains infinite linear zigzag vanadate (V₂O₆)²⁻chains, constructed from corner-sharing VO₄ tetra­hedra, running parallel to the a axis.

The structure of polymeric catena-poly[2-amino­benzimidazolium [[dioxidovanadium(V)]-μ-oxido]], {(C₇H₈N₃)₂[V₂O₆]}_n, has monoclinic symmetry. The title compound is of inter­est with respect to anti­cancer activity. In the crystal structure, infinite linear zigzag vanadate (V₂O₆)²⁻ chains, constructed from corner-sharing VO₄ tetra­hedra and that run parallel to the a axis, are present. Two different protonated 2-amino­benzimidazole mol­ecules are located between the (V₂O₆)^2– chains and form classical N—H⋯O hydrogen bonds with the vanadate oxygen atoms, which contribute to the cohesion of the structure.

A reaction between cucurbit[6]uril (CB6) with an excess of Pr(NO₃)₃·6H₂O lead to the isolation of new mononuclear complex [Pr(CB6)(NO₃)(H₂O)₅](NO₃)₂·9.56H₂O (1), which crystallizes in the P2₁/n space group. The asymmetric unit of 1 contains two crystallographically independent [Pr(CB6)(NO₃)(H₂O)₅]²⁺ complex cations, four nitrate counter-anions for charge balance and 19.12 inter­stitial water mol­ecules. The coordination environments of the Pr^III ions in 1 are formed by two carbonyl O atoms from bidentate cucurbit[6]uril units, two oxygen atoms from the bidentate nitrate anion and five water mol­ecules.

A new mononuclear complex, penta­aqua­(cucurbit[6]uril-κ²O,O′)(nitrato-κ²O,O′)praseodymium(III) dinitrate 9.56-hydrate, [Pr(NO₃)(CB6)(H₂O)₅](NO₃)₂·9.56H₂O (1), was obtained as outcome of the hydro­thermal reaction between the macrocyclic ligand cucurbit[6]uril (CB6, C₃₆H₃₆N₂₄O₁₂) with a tenfold excess of Pr(NO₃)₃·6H₂O. Complex 1 crystallizes in the P2₁/n space group with two crystallographically independent but chemically identical [Pr(CB6)(NO₃)(H₂O)₅]²⁺ complex cations, four nitrate counter-anions and 19.12 inter­stitial water mol­ecules per asymmetric unit. The nona­coordinated Pr^III in 1 are located in the PrO₉ coordination environment formed by two carbonyl O atoms from bidentate cucurbit[6]uril units, two oxygen atoms from the bidentate nitrate anion and five water mol­ecules. Considering the differences in Pr—O bond distances and O—Pr—O angles in the coordination spheres, the coordination polyhedrons of the two Pr^III atoms can be described as distorted spherical capped square anti­prismatic and muffin polyhedral.

The two Mn^II atoms in the complex display a different coordination number, viz. five with a distorted trigonal–bipyramidal Cl₃N₂ and six with a distorted octa­hedral Cl₃N₂O coordination set.

A new quinoline derivative, namely, 6-(di­ethyl­amino)-4-phenyl-2-(pyridin-2-yl)quinoline, C₂₄H₂₃N₃ (QP), and its Mn^II complex aqua-1κO-di-μ-chlorido-1:2κ⁴Cl:Cl-di­chlorido-1κCl,2κCl-bis­[6-(di­ethyl­amino)-4-phenyl-2-(pyridin-2-yl)quinoline]-1κ²N¹,N²;2κ²N¹,N²-dimanganese(II), [Mn₂Cl₄(C₂₄H₂₃N₃)₂(H₂O)] (MnQP), were synthesized. Their compositions have been determined with ESI-MS, IR, and ¹H NMR spectroscopy. The crystal-structure determination of MnQP revealed a dinuclear complex with a central four-membered Mn₂Cl₂ ring. Both Mn^II atoms bind to an additional Cl atom and to two N atoms of the QP ligand. One Mn^II atom expands its coordination sphere with an extra water mol­ecule, resulting in a distorted octa­hedral shape. The second Mn^II atom shows a distorted trigonal–bipyramidal shape. The UV–vis absorption and emission spectra of the examined compounds were studied. Furthermore, when investigating the aggregation-induced emission (AIE) properties, it was found that the fluorescent color changes from blue to green and eventually becomes yellow as the fraction of water in the THF/water mixture increases from 0% to 99%. In particular, these color and intensity changes are most pronounced at a water fraction of 60%. The crystal structure contains disordered solvent mol­ecules, which could not be modeled. The SQUEEZE procedure [Spek (2015#). Acta Cryst. C71, 9–18] was used to obtain information on the type and qu­antity of solvent mol­ecules, which resulted in 44 electrons in a void volume of 274 ų, corresponding to approximately 1.7 mol­ecules of ethanol in the unit cell. These ethanol mol­ecules are not considered in the given chemical formula and other crystal data.

The zwitterionic, isomeric, title compounds, Gly-Met and Met-Gly are me­thio­nine-containing dipeptides, which show very different conformations in the solid state.

The oxidation of me­thionyl peptides can contribute to increased biological (oxidative) stress and development of various inflammatory diseases. The conformation of peptides has an important role in the mechanism of oxidation and the inter­mediates formed in the reaction. Herein, the crystal structures of the isomeric dipeptides Gly-Met (Gly = glycine and Met = me­thio­nine) and Met-Gly, both C₇H₁₄N₂O₃S, are reported. Both mol­ecules exist in the solid state as zwitterions with nominal proton transfer from the carb­oxy­lic acid to the primary amine group. The Gly-Met mol­ecule has an extended backbone structure, while Met-Gly has two nearly planar regions kinked at the C atom bearing the NH₃ group. In the crystals, both structures form extensive three-dimensional hydrogen-bonding networks via N—H⋯O and bifurcated N—H⋯(O,O) hydrogen bonds having N⋯O distances in the range 2.6619 (13)–2.8513 (13) Å for Gly-Met and 2.6273 (8)–3.1465 (8) Å for Met-Gly.

The synthesis, crystal structure and a Hirshfeld surface analysis of tris­{N,N-diethyl-N′-[(4-nitro­phen­yl)(oxo)meth­yl]carbamimido­thio­ato}cobalt(III) are described.

The synthesis, crystal structure, and a Hirshfeld surface analysis of tris­{N,N-diethyl-N′-[(4-nitro­phen­yl)(oxo)meth­yl]carbamimido­thio­ato}cobalt(III) conducted at 180 K are presented. The complex consists of three N,N-diethyl-N′-[(4-nitro­benzene)(oxo)meth­yl]carbamimido­thio­ato ligands, threefold sym­metric­ally bonded about the Co^III ion, in approximately octa­hedral coordination, which generates a triple of individually near planar metallacyclic (Co—S—C—N—C—O) rings. The overall geometry of the complex is determined by the mutual orientation of each metallacycle about the crystallographically imposed threefold axis [dihedral angles = 81.70 (2)°] and by the dihedral angles between the various planar groups within each asymmetric unit [metallacycle to benzene ring = 13.83 (7)°; benzene ring to nitro group = 17.494 (8)°]. The complexes stack in anti-parallel columns about the