
Hydroxystibonium complex [(2,6-(OMe)2C6H3)3SbOH]I (I) was obtained by recrystallization of the product of iodination of tris(2,6-dimethoxyphenyl)stibine from wet pyridine. The reaction of benzene solutions of tris(2,6-dimethoxyphenyl)antimony dibromide and silver perchlorate followed by recrystallization from ethanol afforded complex [(2,6-(OMe)2C6H3)3SbOH]ClO4 & centerdot;0.5EtOH (II) with a similar antimony organic cation. Comparative characterization of the compounds was carried out using IR spectroscopy and X-ray diffraction methods. According to X-ray diffraction data (CCDC nos. 2 556 559 (I), 2 556 560 (II)), the tetrahedral [(2,6-(OMe)2C6H3)3SbOH]+ cations of the compounds have a structural similarity. The OSbC bond angles are 101.8(1)degrees-112.1(1)degrees (I), 98.3(1)degrees-110.6(1)degrees, 97.1(1)degrees-110.3(1)degrees (II); the CSbC angles are 104.8(1)degrees-115.1(1)degrees (I), 108.2(1)degrees-114.7(1)degrees, 105.3(1)degrees-118.2(1)degrees (II). The Sb-O and Sb-C interatomic distances are 1.910(3) & Aring; (I), 1.914(3), 1.918(3) & Aring; (II); and 2.073(3)-2.080(3) & Aring; (I), 2.074(4)-2.089(3), 2.072(4)-2.083(4) & Aring; (II).
Coordination compound [Mg(HKoj-)2]n is synthesized by the reaction of kojic acid (H2Koj) with magnesium acetate in an aqueous solution. The empirical formula of the synthesized compound is determined from the elemental and thermogravimetric analyses data. The thermal oxidative stability of magnesium kojate is studied by simultaneous thermal analysis in air. The molecular structure of the complex is discussed using spectral methods (NMR and IR spectroscopy) and studied in detail using X-ray diffraction (XRD) analysis (CIF file CCDC no. 2513260). Magnesium kojate is a coordination polymer with the chelate environment of the metal cation. The compound crystallizes in the triclinic symmetry group .
Two heterometallic Ru(II)–Fe(II) complexes, bridged by either thiophene-2,5-dicarboxylate or 1,1′-ferrocenedicarboxylate, were synthesized via chloride substitution from the precursor [FcCH=CHRuCl(CO)(PPh3)2] using the corresponding sodium dicarboxylate. In each product, the ruthenium center is coordinated by two triphenylphosphine ligands, monocarboxyl ligand, a ferrocenyl ethylene moiety, and a carboxylate group from the bridging dicarboxylate. This carboxylate binds to ruthenium in a chelating η2-fashion, with the π-conjugated spacer (2,5-thiophenediyl or 1,1′-ferrocenediyl) linking the two carboxylate units. Both complexes were fully characterized by elemental microanalysis, 1H and 31P1H NMR spectroscopy, and ESI mass spectrometry. The solid-state structure of complex I (thiophene-bridged) was unambiguously determined by single-crystal X‑ray diffraction. Furthermore, the electrochemical and photophysical properties of the two complexes were systematically investigated, providing insight into the influence of the conjugated spacer on metal–metal electronic communication and potential applicability in molecular electronics or light-harvesting systems.
As part of a study of the influence of non-covalent interactions involving halogen atoms on the structure of coordination compounds of cadmium and zinc with 1,10-phenanthroline (phen) and anions of halogenated benzoic acids, a series of compounds with anions of 2,4-dichlorobenzoic (Cl2bz) [Cd3(phen)2(Cl2bz)6] (I), 4-bromobenzoic (4-Brbz) [Cd2(phen)2(4-Brbz)4] (II), [Zn(phen)(4-Brbz)2]·MeOH (III), 2,5-dibromobenzoic acid (2,5-Br2bz) [Cd4(phen)4(2,5-Br2bz)8] (IV), 2[Cd2(phen)2(2,5-Br2bz)4]·C6H6 (V), 3,5-dibromobenzoic (3,5-Br2bz) [Cd2(phen)2(3,5-Br2bz)4] (VI), 2,4,6-tribromo-3-hydroxybenzoic (OHBr3bz) [Cd2(MeOH)2(phen)2(OHBr3bz)2(OBr3bz)] (VII), [Zn(phen)3]·2(OHBr3bz)·2(H2O) (VIII), 2,3,4,5-tetrabromobenzoic (Br4bz) [Cd(phen)(Br4bz)2]n (IX), 2,3,5-triiodobenzoic (I3bz) [Cd2(phen)2(I3bz)4]·DMF (X), [Zn(H2O)(phen)2(I3bz)](I3bz)·2(H2O).MeCN (XI) and 4-bromo-2,3,5,6-tetrafluorobenzoic (BrF4bz) [Cd(phen)(BrF4bz)2]n (XII), [Zn(phen)(BrF4bz)2]n (XIII) acids. The synthesized compounds exhibit significant structural diversity: mononuclear, binuclear, trinuclear, as well as unique tetranuclear complex IV, which has no structural analogues, and zinc coordination polymer XIII were obtained. It has been shown that an increase in the number of halogen substituents and the transition from chlorine to bromine and iodine leads to an increase in the role of non-covalent interactions involving halogen atoms in the formation of molecular and crystalline structures.
Complexes of potassium and lithium with cucurbit[6]uril (CB[6]) of composition [K2(H2O)5(CB[6])](H2btc)2·2H2O (I) and [Li3(H2O)2(CB[6])](H2btc)2(NO3)·2H3btc·5.5H2O (II) obtained by heating (100°C) an aqueous solution of mixtures of potassium hydroxide or lithium nitrate, cucurbit[6]uril and trimesic acid (H3btc). According to X-ray diffraction data, the crystal contains cationic polymer chains [K2(H2O)5(CB[6])]2+ in the compound I and [Li3(H2O)2(CB[6])]3+ in compound II they are arranged in alternating layers. In the space between the layers there are guest water molecules, H3btc (in II) and H2btc– anions, participating in the formation of a branched network of hydrogen bonds involving coordinated and uncoordinated water molecules, carboxyl and carboxylate groups of H3btc molecules and H2btc− anions, as well as carbonyl groups of the portals of cucurbit[6]uril molecules. The obtained compounds were characterized by IR spectra and elemental analysis data.