Synthesis and crystal structures of bis[1-oxopyridin-2-olato(1−)]bis(pentafluorophenyl)silicon(IV)–tetrahydrofuran–pentane (2/1/1), bis[1-oxopyridin-2-olato(1−)]bis(p-tolyl)silicon(IV), and dimesitylbis[1-oxopyridin-2-olato(1−)]silicon(IV)
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SUBMITTER: Kraft B
PROVIDER: S-EPMC10915655 | biostudies-literature | 2024 Feb
REPOSITORIES: biostudies-literature
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Project description:Two aryl-substituted thiourea compounds, N,N′-bis[2-(dimethylamino)phenyl]thiourea (1) and N,N′-bis[2-(diethylamino)phenyl]thiourea (2), both exhibit intramolecular hydrogen bonds, corresponding to the N—H resonance acquired from 1H NMR spectroscopy. The other N—H bonds form close contacts with the sulfur atom in an adjacent molecule. Different basicity of the NR2 substituents accounts for the red shift of the N—H stretch in 1 compared to that of 2 acquired from IR spectroscopy. N,N′-Bis[2-(dimethylamino)phenyl]thiourea, C17H22N4S (1), and N,N′-bis[2-(diethylamino)phenyl]thiourea, C21H30N4S (2), were prepared by the treatment of 1,1′-thiocarbonyldiimidazole and 2 equivalents of 2-amino-N,N′-dialkylaniline. Both compounds exhibit intramolecular hydrogen bonds between the N—H(thiourea) and NR2 (R = Me, Et) groups. The other N—H bonds face the sulfur atoms of S=C bonds in an adjacent molecule, which forms an intermolecular interaction in the packed structure. The structural details match the spectroscopic data acquired from NMR and IR spectroscopy.
| S-EPMC9912467 | biostudies-literature
Project description:The cations in the title salts, [Si(OPO)3]Cl·2CDCl3, (I), [Si(OPO)3]Cl·xCH3CN, (II), and fac-[Si(OPTO)3]Cl·2CDCl3, (III) (OPO = 1-oxo-2-pyridin-one, C5H4NO2, and OPTO = 1-oxo-2-pyridine-thione, C5H4NOS), have distorted octa-hedral coordination spheres. The first two structures contain the same cation and anion, but different solvents of crystallization led to different solvates and packing arrangements. In structures (I) and (III), the silicon complex cations and chloride anions are well separated, while in (II), there are two C-H⋯Cl distances that fall just within the sum of the van der Waals radii of the C and Cl atoms. The pyridine portions of the OPO ligands in (I) and (II) are modeled as disordered with the planar flips of themselves [(I): 0.574 (15):0.426 (15), 0.696 (15):0.304 (15), and 0.621 (15):0.379 (15); (II): 0.555 (13):0.445 (13), 0.604 (14):0.396 (14) and 0.611 (13):0.389 (13)], demonstrating that both fac and mer isomers are co-crystallized. In (II), highly disordered solvent, located in two independent channels along [100], was unable to be modeled. Reflection contributions from this solvent were fixed and added to the calculated structure factors using the SQUEEZE [Spek (2015 ▸). Acta Cryst. C71, 9-18] function of program PLATON, which determined there to be 54 electrons in 225 Å(3) accounted for per unit cell (25 electrons in 109 Å(3) in one channel, and 29 electrons in 115 Å(3) in the other). In (I) and (II), all species lie on general positions. In (III), all species are located along crystallographic threefold axes.
| S-EPMC4719831 | biostudies-literature
Project description: Not available
| S-EPMC10561225 | biostudies-literature
Project description: Not available
| S-EPMC11223691 | biostudies-literature
Project description:The crystal structure of the title compound consists of discrete octahedral complexes, which are linked by intermolecular C—H⋯S and C—H⋯N hydrogen bonds into chains. Single crystals of the title compound, [Co(NCS)2(C5H4BrN)2(C2H3N)2], were obtained by the reaction of Co(NCS)2 with 3-bromopyridine in acetonitrile. The CoII cations lie on crystallographic inversion centers and are coordinated by two N-bonded thiocyanate anions, two 3-bromopyridine and two acetonitrile ligands thereby forming slightly distorted CoN6 octahedra. In the crystal, these complexes are linked by C—H⋯S and C—H⋯N hydrogen bonds into a three-dimensional network. In the direction of the crystallographic b-axis, the complexes are arranged into columns with neighboring 3-bromopyridine ligands stacked onto each other, indicating π–π interactions. The CN stretching vibration of the thiocyanate anions is observed at 2066 cm−1, in agreement with the presence of only N-bonded anionic ligands. TG-DTA measurements reveal that in the first mass loss the acetonitrile ligands are removed and that in the second step, half of a 3-bromopyridine ligand is lost, leading to the formation of a polymeric compound with the composition [(Co(NCS)2)2(C5H4BrN)3]n already reported in the literature.
| S-EPMC9815133 | biostudies-literature
Project description:The crystal structures of the disulfide derivative of (Z)-ethene-1,2-bis(diphenylphosphine) as well as its complex with PtII are described here. The structure of the phosphine sulfide features intramolecular π–π interactions and C—H⋯S hydrogen bonds, as well as intermolecular π–π and C—H⋯π interactions. The structure of the platinum(II) complex features intermolecular C—H⋯Cl and C—H⋯S hydrogen bonds. The crystal structures of (Z)-(ethene-1,2-diyl)bis(diphenylphosphine sulfide), C26H22P2S2 (I), along with its complex with PtII dichloride, dichlorido[(Z)-(ethene-1,2-diyl)bis(diphenylphosphine sulfide)-κ2S,S′]platinum(II), [PtCl2(C26H22P2S2)] (II), are described here. Compound I features P=S bond lengths of 1.9571 (15) and 1.9529 (15) Å, with a torsion angle of 166.24 (7)° between the two phosphine sulfide groups. The crystal of compound I features both intramolecular C—H⋯S hydrogen bonds and π–π interactions. Molecules of compound I are held together with intermolecular π–π and C—H⋯π interactions to form chains that run parallel to the z-axis. The intermolecular C—H⋯π interaction has a H⋯Cg distance of 2.63 Å, a D⋯Cg distance of 3.573 (5) Å and a D—H⋯Cg angle of 171° (where Cg refers to the centroid of one of the phenyl rings). These chains are linked by relatively long C—H⋯S hydrogen bonds with D⋯A distances of 3.367 (4) and 3.394 (4) Å with D—H⋯A angles of 113 and 115°. Compound II features Pt—Cl and Pt—S bond lengths of 2.3226 (19) and 2.2712 (19) Å, with a P=S bond length of 2.012 (3) Å. The PtII center adopts a square-planar geometry, with Cl—Pt—Cl and S—Pt—S bond angles of 90.34 (10) and 97.19 (10)°, respectively. Molecules of compound II are linked in the crystal by intermolecular C—H⋯Cl and C—H⋯S hydrogen bonds.
| S-EPMC9815131 | biostudies-literature
Project description:In the crystal structure of the title compound, discrete centrosymmetric complexes are observed, in which the Ni cations are octahedrally coordinated by two terminal N-bonded selenocyanate anions and four pyridine coligands. The reaction of nickel chloride hexahydrate with potassium selenocyanate and pyridine in water leads to the formation of crystals of the title complex, [Ni(NCSe)2(C5H5N)4], which were characterized by single-crystal X-ray diffraction. Its crystal structure consists of discrete complexes, located on centers of inversion, in which the Ni cations are sixfold coordinated by two terminal N-bonded selenocyanate anions and four pyridine ligands within a slightly distorted octahedral coordination. In the crystal, the complexes are connected by weak C—H⋯Se interactions. PXRD investigations revealed that a pure crystalline phase has formed. In the IR and Raman spectra, the C—N stretching vibrations are observed at 2083 and 2079 cm−1, respectively, in agreement with the presence of only terminally bonded anionic ligands. Upon heating, one well-resolved mass loss is observed, in which two of the four pyridine ligands are removed, leading to a compound with the composition Ni(NCSe)2(C5H5N)2. In this compound, the C—N stretching vibration is shifted to 2108 cm−1 (Raman) and 2115 cm−1 (IR), indicating the presence of μ-1,3-bridging anionic ligands. In its PXRD pattern, very broad reflections are observed, indicating for poor crystallinity and/or very small particle size. This crystalline phase is not isotypic to its Co and Fe analogs.
| S-EPMC9912460 | biostudies-literature
Project description:A 1,3,5-trisubstituted 2,4,6-trialkylbenzene derivative with bis(hydroxyethyl)amino and 2,4-dimethylpyridinylamino substituents was synthesized and its structure determined by single-crystal X-ray diffraction. The crystal packing is stabilized by intra- and intermolecular hydrogen bonds and weak C—H⋯π contacts. In the crystal structure of the title compound, C30H50N4O4, the two bis(hydroxyethyl)amino moieties and the 2,4-dimethylpyridinylamino unit of the molecule are located on one side of the central benzene ring, while the ethyl substituents are oriented in the opposite direction. The dihedral angle between the planes of the aromatic rings is 73.6 (1)°. The conformation of the molecule is stabilized by intramolecular O—H⋯O (1.86–2.12 Å) and C—H⋯N (2.40, 2.54 Å) hydrogen bonds. Dimers of inversion-related molecules represent the basic supramolecular entities of the crystal structure. They are further connected via O—H⋯O hydrogen bonding into undulating layers extending parallel to the crystallographic bc plane. Interlayer interaction is accomplished by weak C—H⋯π contacts.
| S-EPMC9361370 | biostudies-literature
Project description:In the title compound, [Sn(C(7)H(7))(C(9)H(6)NO)(2)Cl], the Sn(IV) ion is in a distorted octa-hedral coordination environment formed by the O and N atoms of two bis-chelating quinolin-8-olate ligands, a Cl atom and a C atom from a benzyl ligand. The axial sites are occupied by an N atom of a quinolinate ligand and the C atom of the benzyl ligand. The axial Sn-N bond is slightly shorter than the equatorial Sn-N bond.
| S-EPMC2977110 | biostudies-literature
Project description:A series of Pt(IV) prodrugs has been obtained by oxidative halogenation of either cisplatin or carboplatin. Iodobenzene dichloride is a general reagent that cleanly provides prodrugs bearing axial chlorides without the need to prepare intervening Pt(IV) intermediates or handle chlorine gas. Elemental bromine and iodine afford Pt(IV) compounds as well, although in the case of the iodine-mediated oxidation of carboplatin, an amido-bridged Pt(IV) side product also formed. A detailed analysis of the changes in spectroscopic and structural parameters induced by varying the axial halide is presented. A number of recurring motifs are observed in the solid state structures of these compounds.
| S-EPMC4252584 | biostudies-literature