- Gdańsk, Pomeranian Voivodeship, Poland
Jaroslaw Chojnacki
Gdansk University of Technology, Inorganic Chemistry Department, Department Member
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Abstract The reactivity of phosphanylphosphinidene Pt(0) complexes [DppePt(η2-P-PtBu2)] (1) and [(p-Tol3P)2Pt(η2-P-PtBu2)] (2) toward sulfur was studied. Reactions of 1 and 2 with an excess of sulfur led to the formation of the first... more
Abstract The reactivity of phosphanylphosphinidene Pt(0) complexes [DppePt(η2-P-PtBu2)] (1) and [(p-Tol3P)2Pt(η2-P-PtBu2)] (2) toward sulfur was studied. Reactions of 1 and 2 with an excess of sulfur led to the formation of the first transition metal complexes 3 and 4 with phosphinothioyltrithiophosphonato ligands with the formula [tBu2P(=S)-P(=S)S2]2-. In contrast to previous reports on the phosphanylphosphinidene moiety sulfurization, the P-P bond was not cleaved during these reactions. The structures of sulfurization products 3 and 4 were elucidated using NMR spectroscopy, X-ray diffraction, and DFT calculations.
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Herein, we present the synthesis of the first fully characterized monomeric triphosphinoboranes. The simple reaction of boron tribromide with 3 equiv of bulky lithium phosphide tBu2PLi yielded triphosphinoborane (tBu2P)3B.... more
Herein, we present the synthesis of the first fully characterized monomeric triphosphinoboranes. The simple reaction of boron tribromide with 3 equiv of bulky lithium phosphide tBu2PLi yielded triphosphinoborane (tBu2P)3B. Triphosphinoboranes with diversified phosphanyl substituents were obtained via a two-step reaction, in which isolable bromodiphosphinoborane (tBu2P)2BBr is first formed and then reacts with 1 equiv of less bulky phosphide R2PLi (R2P = Cy2P, iPr2P, tBuPhP, or Ph2P). By utilizing this method, we obtained a series of triphosphinoboranes with the general formula (tBu2P)2BPR2. On the basis of structural and theoretical studies, two main types of triphosphinoborane structures can be distinguished. In the first type, all three electron lone pairs interact with the formally empty p orbital of the central boron atom, resulting in delocalized π bonding, whereas in the second type, one localized P=B bond and two P–B bonds are observed. The Lewis acidic–basic properties of triphosphinoboranes during the reaction of (tBu2P)2BPiPr2 with H3B·SMe2 were analyzed. The P–B bond-containing compound mentioned above not only formed an adduct with BH3 but also activated the B–H bond of the borane molecule, resulting in the incorporation of the BH2 unit into two phosphorus atoms and migration of a hydride to the boron atom of the parent triphosphinoborane. The structures of the triphosphinoboranes were confirmed by single-crystal X-ray analysis, multinuclear nuclear magnetic resonance spectroscopy, and elemental analysis.
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The title compound, (C8H20N)[Cd(C5H10NS2)2I], containing a heteroleptic five-coordinate mononuclear anionic cadmium complex, crystallizes in orthorhombic form in the space group Pnma. Both anion and cation lie about mirror planes. Unlike... more
The title compound, (C8H20N)[Cd(C5H10NS2)2I], containing a heteroleptic five-coordinate mononuclear anionic cadmium complex, crystallizes in orthorhombic form in the space group Pnma. Both anion and cation lie about mirror planes. Unlike other known [Cd(dtc)2X]-type complexes (where dtc is dithiocarbamate and X is a halogen or pseudohalogen), the central CdS4I core shows a square-pyramidal configuration, with a basal plane defined by four S atoms from two chelating dithiocarbamate ligands related by a symmetry plane. The central Cd atom is displaced from the basal S4 plane towards the apical I atom of the square pyramid.
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[(η5-C5H5)ZrCl3] reacts with [C5H4CH2CH2NMe2]Li yielding the coordination polymer [(C5H5)(C5H4CH2CH2NMe2)ZrCl2]n (1) as a brown solid which is very sensitive to moisture. The reaction of 1 with 1.35 equivalent of HCl (methanolic solution)... more
[(η5-C5H5)ZrCl3] reacts with [C5H4CH2CH2NMe2]Li yielding the coordination polymer [(C5H5)(C5H4CH2CH2NMe2)ZrCl2]n (1) as a brown solid which is very sensitive to moisture. The reaction of 1 with 1.35 equivalent of HCl (methanolic solution) yields pale yellow green crystals of [(η5-C5H5)(η5-C5H4CH2CH2NHMe2)ZrCl2]2[ZrCl6] (2). Compound 2 was fully characterized on the basis of NMR data and X-ray crystal structure analysis. The formation of this product
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A family of cyclic medium-sized disulfanes and related sulfanes was synthesized and characterized, followed by desulfurization and disulfane ammonolysis.
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Research Interests: Chemistry, Organic Chemistry, Medicine, Humans, Stereochemistry, and 10 moreQuantitative Structure Activity Relationship, Hydrogen Bonding, Molecules, HeLa cells, HeLa, Molecular Conformation, Antineoplastic Agents, Minimum inhibitory concentration, Sulfonamides, and Minimum Inhibitory Concentration
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First manganese(II) trialkoxysilanethiolates have been prepared using tri-tert-butoxysilanethiol as the ligand source and their structure determined by X-ray diffraction. Acetonitrile or methanol used as reaction solvents was found to... more
First manganese(II) trialkoxysilanethiolates have been prepared using tri-tert-butoxysilanethiol as the ligand source and their structure determined by X-ray diffraction. Acetonitrile or methanol used as reaction solvents was found to enter Mn coordination sphere. Obtained heteroleptic silanethiolate complexes represent two distinct structural types. Either O,S-chelation by tri-tert-butoxysilanethiolate ligand and simultaneous electronic assistance provided by acetonitrile in [Mn{SSi(OBut)3}2(MeCN)] or formation of four intramolecular, interligand O–H ⋯ O hydrogen bonds in the case of [Mn{SSi(OBut)3}2(MeOH)4] serve to stabilize the complexes.
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Research Interests: Computer Science, Chemistry, Medicine, EDTA Chelation, CHEMICAL SCIENCES, and 4 moreTris, Tetra, Iodide, and Pyrrolidine
ABSTRACT The title compound, (C16H36N)2[CdBr4]·2C7H8, consists of a [CdBr4]2− anion possessing crystallographic symmetry and two tetra-n-butylammonium cations of twofold symmetry accompanied by two toluene molecules disordered around a... more
ABSTRACT The title compound, (C16H36N)2[CdBr4]·2C7H8, consists of a [CdBr4]2− anion possessing crystallographic symmetry and two tetra-n-butylammonium cations of twofold symmetry accompanied by two toluene molecules disordered around a twofold axis. The anion is enclosed within a cage formed of four cations and four solvent molecules.
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Reactions of triphosphinoboranes with borane dimethylsulfide provided access to boraphosphacycloalkanes with diverse structures.
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Herein, we present a simple synthesis of mixed-valent phosphinophosphoranes bearing three- and five-coordinate phosphorus centers. Compounds with phosphorus–phosphorus bonds were synthesized via a reaction of lithium phosphides RR′PLi... more
Herein, we present a simple synthesis of mixed-valent phosphinophosphoranes bearing three- and five-coordinate phosphorus centers. Compounds with phosphorus–phosphorus bonds were synthesized via a reaction of lithium phosphides RR′PLi with cat2PCl (cat = catecholate), whereas derivatives with methylene-linked phosphorus centers were obtained via a reaction of phosphanylmethanides RR′CH2Li with cat2PCl. The presence of accessible lone-pair electrons on the P-phosphanyl atom of phosphinophosphoranes during the reaction of the title compounds with H3B·SMe2, where phosphinophosphorane-borane adducts were formed quantitatively, was confirmed. Furthermore, the Lewis basic and Lewis acidic properties of the phosphinophosphoranes in reactions with phenyl isothiocyanate were tested. Depending on the structure of the starting phosphinophosphorane, phosphinophosphorylation of PhNCS or formation of a five-membered zwitterionic adduct was observed. The structures of the isolated compounds were unambiguously determined by heteronuclear nuclear magnetic resonance spectroscopy and single-crystal X-ray diffraction. Moreover, by applying density functional theory calculations, we compared the Lewis basicity and nucleophilicity of diversified trivalent P-centers.
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A simple method for the generation of phosphinoborinium cations utilizing synthetically accessible bromophosphinoboranes.
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Research Interests: Chemistry, Inorganic Chemistry, Medicinal Chemistry, Catalysis, Medicine, and 15 moreManganese, Liver, Alcohol, Methanol, Nitrogen, Hydrogen Bond, Hydrogen Bonding, Imidazole, Molecular Conformation, Inorganic Biochemistry, Imidazoles, Organometallic Compounds, Ligands, Alcohol Dehydrogenase, and binding sites
Metathesis reactions between diimido complexes of tungsten(VI) [(ArN)2WCl2] (Ar = 2,6‐iPr2C6H3) and lithium derivatives of diphosphanes R2P–P(SiMe3)Li (R = tBu and iPr) yield two anionic diimido complexes of tungsten with side‐on bonded... more
Metathesis reactions between diimido complexes of tungsten(VI) [(ArN)2WCl2] (Ar = 2,6‐iPr2C6H3) and lithium derivatives of diphosphanes R2P–P(SiMe3)Li (R = tBu and iPr) yield two anionic diimido complexes of tungsten with side‐on bonded phosphanylphosphinidene ligands, [(ArN)2WCl(η2‐R2P–P)]–. Both complexes are structurally characterized. A possible reaction mechanism and the role of donor solvents are discussed on the basis of NMR spectroscopic results.
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An entry from the Cambridge Structural Database, the world's repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely... more
An entry from the Cambridge Structural Database, the world's repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.
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The title compound, C42H42O7Si2, was obtained as a by-product from the reaction of (p-Tol-O)3SiCl with [PhC(S)S]2Mg·2THF (p-Tol is p-tolyl and THF is tetrahydrofuran). The molecule has \overline{3} symmetry and is an example of a... more
The title compound, C42H42O7Si2, was obtained as a by-product from the reaction of (p-Tol-O)3SiCl with [PhC(S)S]2Mg·2THF (p-Tol is p-tolyl and THF is tetrahydrofuran). The molecule has \overline{3} symmetry and is an example of a compound with an Si–O–Si valence angle of 180°. The distribution of this angle within disiloxanes is briefly described and discussed.
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By the reaction of benzoyl chloride, potassium isothiocyanate and the appropriate halogenoaniline, i.e. 2/3/4-(bromo/iodo)aniline, we have obtained five new 1-benzoyl-3-(halogenophenyl)thioureas, namely,... more
By the reaction of benzoyl chloride, potassium isothiocyanate and the appropriate halogenoaniline, i.e. 2/3/4-(bromo/iodo)aniline, we have obtained five new 1-benzoyl-3-(halogenophenyl)thioureas, namely, 1-benzoyl-3-(2-bromophenyl)thiourea and 1-benzoyl-3-(3-bromophenyl)thiourea, C14H11BrN2OS, and 1-benzoyl-3-(2-iodophenyl)thiourea, 1-benzoyl-3-(3-iodophenyl)thiourea and 1-benzoyl-3-(4-iodophenyl)thiourea, C14H11IN2OS. Structural and conformational features of the compounds have been analyzed using X-ray diffraction and theoretical calculations. The novel compounds were characterized by solid-state IR and 1H/13C NMR spectroscopy. The conformations and intermolecular interactions, such as hydrogen bonds, π–π and S(6)...π stacking, and X...O (X = I or Br), I...S and I...π, have been examined and rationalized, together with four analogous compounds described previously in the literature. The set of nine compounds was chosen to examine how a change of the halogen atom and its position on the phenyl ring affects the molecular and crystal structures.
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The first compound with an unusual type of anion, [Li(S<i>R</i>)<sub>2</sub>]<sup>–</sup>: bis(μ<sub>2</sub>-aqua-<i>d</i><sub>2</sub>)tetrakis(aqua-<i>d</i><sub
The title complex, [Li2(D2O)6][Li(C9H27SSiO3)2]2.2D2O, is the first compound with an S-M bond (M = alkali metal) within an unusual type of lithate anion, [Li(SR)2]- {where R is Si[OC(CH3)3]3}. There is a centre of symmetry located in the... more
The title complex, [Li2(D2O)6][Li(C9H27SSiO3)2]2.2D2O, is the first compound with an S-M bond (M = alkali metal) within an unusual type of lithate anion, [Li(SR)2]- {where R is Si[OC(CH3)3]3}. There is a centre of symmetry located in the middle of the Li2O2 ring of the cation. All Li atoms are four-coordinate, with LiO4 (cations) and LiO2S2 (anions) cores. The singly charged [Li(SR)2]- anions are well separated from the doubly charged [Li2(D2O)6]2+ cations; the distance between Li atoms from differently charged ions is greater than 5 A. Both ion types are held within an extended network of O-D...O and O-D...S hydrogen bonds.
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Cubane-like structure of a silanethiol ? primary amine assembly ? a novel, unusual hydrogen bond patternElectronic supplementary information (ESI) available: experimental details, table with data of hydrogen bonds, Ortep plots in colour of 1, 2 and 3. See http://www.rsc.org/suppdata/cc/b3/b313576d/more
A reaction of silanethiol and primary amine leads to a product whose crystals are built of well-defined supermolecules--assemblies of four ammonium silanethiolate units... more
A reaction of silanethiol and primary amine leads to a product whose crystals are built of well-defined supermolecules--assemblies of four ammonium silanethiolate units (RS(-)H(3)N(+)R&amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;#39;)(4) with a novel, unusual 3D hydrogen bond pattern.