Bis(2-methylpyridinium) tetrachloridocuprate(II): synthesis, structure and Hirshfeld surface analysis

The title compound, (C6H8N)2[CuCl4], crystallizes in the monoclinic space group I2/c. The coordination around the copper atom is a distorted tetrahedron. The 2-methylpyridinium ion (C6H8N+) interacts with the tetrachlorocuprate anion through N—H...Cl and C—H(phenyl)...Cl contacts, forming a hydrogen-bonded layer-like structure. The supramolecular structure is further stabilized by C—H(methyl)...Cl interactions between the layers.

Structure and vibrational spectroscopy of lithium and potassium methanesulfonates

In this work, we have determined the structures of lithium methanesulfonate, Li(CH 3 SO 3 ), and potassium methanesulfonate, K(CH 3 SO 3 ), and analysed their vibrational spectra. The lithium salt crystallizes in the monoclinic space group C 2/ m with two formula units in the primitive cell. The potassium salt is more complex, crystallizing in I 4/ m with 12 formula units in the primitive cell. The lithium ion is fourfold coordinated in a distorted tetrahedron, while the potassium salt exhibits three types of coordination: six-, seven- and ninefold. Vibrational spectroscopy of the compounds (including the 6 Li and 7 Li isotopomers) confirms that the correlation previously found, that in the infrared spectra there is a clear distinction between coordinated and not coordinated forms of the methanesulfonate ion, is also valid here. The lithium salt shows a clear splitting of the asymmetric S–O stretch mode, indicating a bonding interaction, while there is no splitting in the spectrum of the potassium salt, consistent with a purely ionic material.

N-Ethyl-N′-(3-methylbenzoyl)-S,S-diphenylsulfodiimide

The asymmetric unit of the title sulfodiimide, C22H22N2OS, consists of two crystallographically independent molecules with similar conformations The environment around each sulfur atom is a slightly distorted tetrahedron with two S=N bonds and two S—C bonds. The S= N(m-methylbenzoyl) and S=N(NEt) bond lengths are 1.584 (3) and 1.528 (2) Å, respectively, for one molecule, and 1.575 (2) and 1.529 (3) Å, respectively, for the other. The dihedral angles between the two phenyl rings in the molecules are 86.76 (8) and 82.49 (8)°. The N—S—N—C(m-methylbenzoyl) and N—S—N—C(ethyl) torsion angles are −60.5 (2) and −50.28 (19)°, respectively, for one molecule, and 62.9 (2) and 44.2 (3)°, respectively, for the other. In the crystal, each independent molecule is linked to its inversion-related molecule via a pair of C—H...O hydrogen bonds, forming a dimer.

S,S-Diphenyl-N-tosyl sulfone diimine

In the title compound [systematic name: N-(iminodiphenyl-λ6-sulfanylidene)-4-methylbenzene-1-sulfonamide], C19H18N2O2S2, the configuration around the sulfur atom of the sulfonediimine group is a slightly distorted tetrahedron structure with two S=N bonds and two S—C bonds. The bond lengths of S=N (p-toluenesulfonyl) and S=N (NH) are 1.5785 (15) and 1.5158 (18) Å, respectively. The S—N=S plane makes a dihedral angle of 74.24 (14)° with the p-toluene ring, while it makes dihedral angles of 73.43 (13) and 41.98 (14)° with the phenyl rings. The two torsion angles of S—N=S—C (phenyl) and the S—N=S=N angle are 105.86 (12), −144.54 (11) and −25.67 (17)°, respectively. In the crystal, molecules are connected by pairs of N—H...O hydrogen bonds, forming inversion dimers with an R 2 2(12) ring motif. The dimers are linked by C—H...O interactions, forming a tape structure along the a-axis direction.

Redetermination of the crystal structure of K2Hg(SCN)4

Single crystals of K2Hg(SCN)4[dipotassium tetrathiocyanatomercurate(II)] were grown from aqueous solutions of potassium thiocyanate and mercury(II) thiocyanate and studied by single-crystal X-ray diffraction. In comparison with the previously reported structure model [Zvonkova (1952).Zh. Fiz. Khim.26, 1798–1803], all atoms in the crystal structure were located, with lattice parameters and fractional coordinates determined to a much higher precision. In the (crystal) structure, the HgIIatom is located on a twofold rotation axis and is coordinated in the form of a distorted tetrahedron by four S atoms of the thiocyanate anions. The K+cation shows a coordination number of eight.

μ3-Chlorido-μ2-chlorido-(μ3-pyrrolidine-1-carbodithioato-κ4S:S,S′:S′)tris[(triethylphosphane-κP)copper(I)]: crystal structure and Hirshfeld surface analysis

The title trinuclear compound, [Cu3(C5H8NS2)Cl2(C6H15P)3], has the dithiocarbamate ligand symmetrically chelating one CuIatom and each of the S atoms bridging to another CuIatom. Both chloride ligands are bridging, one being μ3- and the other μ2-bridging. Each Et3P ligand occupies a terminal position. Two of the CuIatoms exist within Cl2PS donor sets and the third is based on a ClPS2donor set, with each coordination geometry based on a distorted tetrahedron. The constituents defining the core of the molecule,i.e.Cu3Cl2S2, occupy seven corners of a distorted cube. In the crystal, linear supramolecular chains along thecaxis are formedviaphosphane–methylene-C—H...Cl and pyrrolidine–methylene-C—H...π(chelate) interactions, and these chains pack without directional interactions between them. An analysis of the Hirshfeld surface points to the predominance of H atoms at the surface,i.e.contributing 86.6% to the surface, and also highlights the presence of C—H...π(chelate) interactions.

Ba2VO4Br

Single crystals of dibarium vanadate(V) bromide, Ba2VO4Br, were grown from a melt of Ba3(VO4)2and BaBr2. Ba2VO4Br crystallizes in the space groupPbcmand is isotypic with the structure of chlorspodiosite, Ca2PO4Cl. Although the ionic radii in chlorspodiosite are different from those in dibarium vanadate bromide, the structures are very similar to one another. The V atom is coordinated by four O atoms, forming a slightly distorted tetrahedron. The Ba atoms occupy two different sites and are coordinated by six O atoms and three or four Br atoms, depending on the site occupied.

Two new ternary chalcogenides Ba2ZnQ3 (Q = Se, Te) with chains of ZnQ4 tetrahedra: syntheses, crystal structure, and optical and electronic properties

Single crystals of Ba2ZnQ3 (Q = Se, Te) were obtained by solid-state reactions at 1173 K. These isostructural compounds crystallize in the K2AgI3 structure type. The Zn atoms in this structure are coordinated to four Q atoms (2 Q1, 1 Q2, 1 Q3) and these form a distorted tetrahedron around each Zn atom. Each ZnQ4 tetrahedron shares two corners with neighboring ZnQ4 tetrahedra resulting in the formation of infinite chains of [ZnQ44−] units. The absorption spectrum of a single crystal of Ba2ZnTe3 shows an absorption edge at 2.10(2) eV, consistent with the dark-red color of the crystals. From DFT calculations Ba2ZnSe3 and Ba2ZnTe3 are found to be semiconductors with electronic band gaps of 2.6 and 1.9 eV, respectively.

Crystal structure of [Co(NH3)6][Co(CO)4]2

Hexaamminecobalt(II) bis[tetracarbonylcobaltate(-I)], [Co(NH3)6][Co(CO)4]2, was synthesized by reaction of liquid ammonia with Co2(CO)8. The CoIIatom is coordinated by six ammine ligands. The resulting polyhedron, the hexaamminecobalt(II) cation, exhibits point group symmetry -3. The Co-Iatom is coordinated by four carbonyl ligands, leading to a tetracarbonylcobaltate(−I) anion in the shape of a slightly distorted tetrahedron, with point group symmetry 3. The crystal structure is related to that of high-pressure BaC2(space groupR-3m), with the [Co(NH3)6]2+cations replacing the Ba sites and the [Co(CO)4]−anions replacing the C sites. N—H...O hydrogen bonds between cations and anions stabilize the structural set-up in the title compound.