Synthesis and characterization of self-assembled inorganic–organic hybrid arsenotungstates

A series of 12 inorganic–organic hybrid 4f-substituted arsenotungstates decorated with 3d-based complexes along with organic ligands (acetate and 1,10-phenanthroline) have been synthesized under open-air conditions and characterized by SC-XRD, PXRD, FT–IR, UV–Vis and thermogravimetric analysis.

Observation of an infrequent enanti­omer/conformer substitutional disorder in ethyl 13-ethyl-4-oxo-8,13-di­hydro-4H-benzo[5,6]azepino[3,2,1-ij]quinoline-5-carboxyl­ate heptane hemisolvate

The crystal structure of a racemic benzazepine derivative shows an infrequent kind of substitutional disorder where a conformer of one enanti­omer replaces the equivalent conformer of the other enanti­omer.

A new two-dimensional Cd^II coordination polymer based on 1,3-bis­(2-methyl-1H-imidazol-1-yl)benzene and 1,3-phenyl­enedi­acetic acid: synthesis, crystal structure and physical properties

A cadmium(II) compound prepared by reaction of Cd(NO₃)₂·6H₂O with 1,3-phenyl­enedi­acetic acid and 1,3-bis­(2-methyl-1H-imidazol-1-yl)benzene in H₂O, possesses a new (4,4) two-dimensional Cd^II coordination polymeric structure parallel to the bc plane. The compound exhibits strong fluorescence emissions and a highly photocatalytic degradation activity for the degradation of methyl­ene blue in the solid state at room temperature.

Synthesis, structure and photoluminescence properties of a three-dimensional cadmium(II) (4,5)-connected coordination network

Hydro­thermal reaction between Cd(NO₃)₂·4H₂O, 4,4′-oxydi­benzoic acid and trans-1,2-bis­(pyridin-3-yl)ethyl­ene gave rise to colourless block-shaped crystals of a three-dimensional (4,5)-connected coordination network with the rare TCS (ThCr₂Si₂ prototype) topology. The title compound exhibits good thermal stability and photoluminescence properties.

Solvomorphs of tyraminium 5,5-di­ethyl­barbiturate: a rare example of the barbiturate R₃³(12) hydrogen-bond motif and a crystal structure with Z′ = 4

A tyraminium barbitalate solvomorph (pseudopolymorph) contains disordered chloro­form mol­ecules and its Z′ value is 4. A second solvomorph, a rare example of a crystal structure with a hydrogen-bonded (12) ring motif, exhibits a layered structure, with cavities containing disordered water and ethanol mol­ecules.

Structure and properties of Na₅FeSi₄O₁₂ crystallized from 5Na₂O–Fe₂O₃–8SiO₂ glass

The crystal structure of Na₅FeSi₄O₁₂, crystallized from a stoichiometric glass, was solved by single-crystal X-ray diffraction. Fe is present in its trivalent state and occupies a single unique octa­hedral site, while Na occurs in several disordered independent positions.

New triple molybdate Rb₂AgIn(MoO₄)₃: synthesis, framework crystal structure and ion-transport behaviour

The new material Rb₂Ag_1+3xIn_1–x(MoO₄)₃ (0 ≤ x ≤ 0.02) extends the series of rhombohedral framework molybdates with a ∼ 10 Å and long c axes. The compound undergoes a `blurred' first-order phase transition at 535 K with increasing electrical conductivity up to 1.1 × 10⁻² S cm⁻¹ at 720 K.

A combined X-ray crystallography and theoretical study of N—H⋯OX (X is =P and —C) hydrogen bonds in two new structures with a (C—O)₂(N)P(=Y) (Y is O and S) skeleton

The N—H⋯O hydrogen bonds were studied, both theoretically and experimentally, in two new phospho­rus(V)-based structures. A comparison was made with regard to the O atoms of the P=O or C—O—P groups.

Two new cobalt(II) rhodamine 6G hydrazone complexes: structure, fluorescence and magnetism

Rhodamine 6G-labelled hydra­zone Co^II complexes with an N₄O₂ donor set show inter­molecular π–π stacking inter­actions between xanthene moieties to form a supra­molecular one-dimensional chain structure. The ring-opened rhodamine 6G ligands are responsible for a green fluorescence and the temperature-dependent magnetic susceptibilities of the complexes are dominated by the structural distortion and spin-orbit coupling of Co^II.

New polysubstituted monoterpenic thia­zolidinones: synthesis, spectroscopic and crystal structure studies

Three new polysubstituted monoterpenic thia­zolidin-4-ones were synthesized starting from the corresponding thio­semicarbazones obtained from naturally occurring (R)-camphor. All the newly obtained thia­zolidin-4-ones have been fully characterized by HRMS and ¹H and ¹³C (1D and 2D) NMR spectroscopy, and two of them were identified by single-crystal X-ray crystallography, confirming the synthetic pathway and the spectroscopic analyses.

Proton disorder in a short intra­molecular hydrogen bond investigated by single-crystal neutron diffraction at 2.5 and 170 K

Single-crystal neutron diffraction at 2.5 K and a subset of neutron data collected at 170 K, combined with information from X-ray diffraction at the same temperature, suggest static disorder for the proton in the short intra­molecular hydrogen bond of 3-[2-(pyridin-4-yl)eth­yl]pentane-2,4-dione.

Iron(II) complexes of di­methyl­tri­aza­cyclo­phane

Iron(II) complexes of the ortho-tri­aza­cyclo­phane 1,4-di­methyl­tribenzo[b,e,h][1,4,7]tri­aza­cyclo­nona-2,5,8-triene (L1) have been prepared from Fe[N(SiMe₃)₂]₂. Diiron(II) complex Fe₂(L1)₄ and monoiron complex (L1)₂Fe(THF)₂ reversibly convert into each other by addition or removal of tetra­hydro­furan (THF). The ligand is present as the asymmetric saddle rather than the expected bowl-shaped crown conformer, preventing chelating κ³-coordination to the metal. Diiron complex Fe₂(L1)₄ was also studied computationally to reveal bonding and charges.

Copper(I) iodide ribbons coordinated with thio­urea derivatives

Double and quadruple ribbons of copper(I) iodide coordinated with thio­urea-derived organic ligands have been synthesized and characterized. (CuI)_n kernels show similarity to phase V of the high-pressure structure of copper(I) iodide.

Polymorphism in some new bis-hydrazone compounds

The polymorphism of four bis-hydrazone compounds is discussed. A small conformational adjustment of the mol­ecules in the crystal structure of two of the compounds leads to simple polymorphism. Conformational polymorphism has been observed in the other two compounds due to conformational changes of the mol­ecules in the crystal structures.

Chloro–formyl steroids as precursors for hybrid heterosteroids: synthesis, spectroscopic characterization, and mol­ecular and supra­molecular structures

Two new steroids containing chloro and formyl substituents in ring A have been synthesized from ketosteroid precursors using the Vilsmeier reaction and characterized spectroscopically, and the crystal structures of three such compounds have been determined. When the fusion between rings A and B is trans, 3-chloro-2-formyl products are formed, but when this ring fusion is cis, a 3-chloro-4-formyl product is formed.

Peculiarities of supra­molecular organization of cyclic ketones with vinyl­acetyl­ene fragments

Supra­molecular bonding in a series of symmetrical and unsymmetrical vinyl­acetyl­ene-substituted cyclo­alkyl ketones was investigated. Motifs typical for acentric crystals are revealed.

The structures of benzimidazole derivatives and their potential as tuberculostatics

Searches for new tuberculostatics are important considering the occurrence of drug-resistant strains of Mycobacterium tuberculosis. The structures of two benzimidazoles – potentially tuberculostatic compounds – were determined by X-ray diffraction.

Comparison of computationally cheap methods for providing insight into the crystal packing of highly bromo­methyl­ated azo­benzenes

Various computationally cheap tools are applied to five bromo­methyl­ated azo­benzene derivatives in order to provide insight into their crystal packing arrangements. The procedures and caveats for the various tools are discussed in detail. We find a surprising lack of halogen–halogen inter­actions in the structures.

Crystal structure, spectroscopic studies and theoretical studies of thio­barbituric acid derivatives: understanding the hydrogen-bonding patterns

The absolute configurations for six thio­barbituric acid (TBA) derivatives were confirmed by single-crystal X-ray crystallography, which indicates the formation of intra­molecular hydrogen bonding in all cases and inter­molecular hydrogen bonding in one case.

Crystal structure of the layered arsenide Rb₃Cu₃As₂

The new ternary arsenide Rb₃Cu₃As₂ is isotypic with K₃Cu₃P₂. The structure features layers of inter­linked CuAs₂ linear moieties.

Two- and three-dimensional coordination polymers based on zinc(II) and furan-2,5-di­carb­oxy­lic acid: structure variation due to metal-to-linker ratio

Two Zn^II-based coordination polymers were synthesized by the hydro­thermal method, using Zn(NO₃)₂·6H₂O and furan-2,5-di­carb­oxy­lic acid, one polymer exhibiting two-dimensional networks consisted of 2₁ double-stranded helices and the other a three-dimensional network, with the pores filled with cations and solvent mol­ecules.

Charge-assisted hydrogen bonding in three di­amino­benzene salts

The crystal structures of three protonated benzenedi­amine salts with sulfate, perchlorate, and tetra­choridozincate(II) counter-ions are reported. The sulfate salt is a second crystalline modification of a previously reported compound. Hydrogen-bonding inter­actions are explored using Hirshfeld surface analysis and DFT calculations.

Mixed natural aryl­olefin–quinoline platinum(II) complexes: synthesis, structural characterization and in vitro cytotoxicity studies

The syntheses and structures of five new platinum(II) complexes bearing (iso)propyl eugenoxyacetate and quinolines are presented, as well as their in vitro cytotoxicity on four human cancer cell lines.

Low-dimensional bis­muth(III) iodide hybrid material with high activity for the fast removal of rhodamine B

The lead-free perovskite-type compound tetra­kis­(1,2,3-tri­methyl­imidazolium) di-μ₃-iodido-tetra-μ₂-iodido-deca­iodido­tetra­bis­muth(III), (C₆H₁₁N₂)₄[Bi₄I₁₆], has been successfully synthesized by a simple solvothermal method. It exhibits a zero-dimensional tetra­meric structure, including edge-sharing [Bi₄I₁₆]⁴⁻ distorted octa­hedra. The band gap of 2.0 eV is close to that of (NH₄)₃[Bi₂I₉].

Structures and phase transition of three isomers of 1-phenyl­indolin-2-one derivatives: 6-chloro-1-phenyl­indolin-2-one, 4-chloro-1-phenyl­indolin-2-one and 1-(3-chloro­phen­yl)indolin-2-one

Among the structures of three isomers, the 6-chloro-1-phenyl­indolin-2-one crystal exhibits a phase transition from the monoclinic space group P2₁/c at 295 K to triclinic P at 90 K, which may be associated with the oscillation-frozen state of the phenyl group of the mol­ecule.

Polymorphic modifications of a 1H-pyrrolo­[3,2,1-ij]quinoline-5-carboxamide possessing strong diuretic properties

Two polymorphic modifications of 6-hy­droxy-N-(4-meth­oxy­phen­yl)-4-oxo-2,4-di­hydro-1H-pyrrolo­[3,2,1-ij]quinoline-5-carboxamide possessing strong diuretic properties have been studied comprehensively. Differences in the crystal packing have been analyzed using a method based on a comparison of pairwise inter­action energies in the crystal phase.

Four inter­penetrating hydrogen-bonded three-dimensional networks in divanillin

The crystal structure of divanillin was solved and refined from laboratory powder X-ray diffraction data. The crystal structure is composed of an intricate diamond-type arrangement of four interpenetrating hydrogen-bonded networks that explains the different solubilities of the freshly synthesized material and the product aged for 15 min in the mother liquor.

One-dimensional networks formed via the self-assembly of anthracenedi­benzoic acid with zinc(II)

This work focuses on the self-assembly of 4,4′-(anthracene-9,10-di­yl)di­benzoic acid with Zn^II, and the different outcomes based on metal loading and choice of solvent.

Computational Chemistry