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Öğe Bis[?2-2,2?-dimethyl-N,N?-bis(2-oxido-benzyl)propane-1,3-diamine]-1?4O,N,N?,O?:2?2O,O?;2?2O,O?:3?4O,N,N?,O?-bis(N,N?-dimethylformamide)-1?O,3?O-di-?2-formato-1:2?2O:O?;2:3?2O:O?-trinickel(II)(Int Union Crystallography, 2007) Yildirim, Leyla Tatar; Atakol, Orhan; Kavak, GueltenThe title crystal structure, [Ni-3(C19H24N2O2)(2)(CHO2)(2)( C3H7NO)(2)], consists of discrete centrosymmetric homotrinuclear nickel complex molecules. In each molecule, the central Ni-II ion is in a distorted octahedral coordination environment, formed by four O atoms from two chelating DML2- ligands [DMLH2 = N,N'-bis(salicylidene)-2,2'dimethyl- 1,3- propanediamine] in the equatorial plane and two O atoms of two symmetry- related formate ligands in the axial positions. The terminal Ni-II ions also have distorted octahedral coordination environments and these are formed by two O and N atoms from chelating DML2- ligands in the equatorial plane; the axial positions are occupied by O atoms from a dimethylformamide ligand and a formate ligand. The overall result is three edge-shared octahedra in which the closest Ni center dot center dot center dot Ni distance is 3.0857 (14) A. The crystal structure is stabilized by weak C-H center dot center dot center dot O hydrogen bonds ( agnostic interactions).Öğe Diiodido-2?2I-bis(4-methylpyridine-1?N)-?-{2,2?-[1,3-propanediylbis(nitrilomethylidyne)]diphenolato-1?4O,N,N?,O?:2?2O,O?}nickel(II)zinc(II)(Int Union Crystallography, 2007) Yildirim, Leyla Tatar; Atakol, Orhan; Kavak, Guelten[Abstract Not Available]Öğe Ruthenium complexes of aminophosphine ligands and their use as pre-catalysts in the transfer hydrogenation of aromatic ketones: X-ray crystal structure of thiophene-2-(N-diphenylthiophosphino)methylamine(Pergamon-Elsevier Science Ltd, 2011) Aydemir, Murat; Baysal, Akin; Ozkar, Saim; Yildirim, Leyla TatarReaction of thiophene-2-methylamine with one or two equivalents of PPh2Cl in the presence of NEt3, proceeds in thf to give thiophene-2-(N-diphenylphosphino)methylamine, la and thiophene-2-(N, N-bis(diphenylphosphino))methylamine, 2a respectively, under anaerobic conditions. Oxidations of la and 2a with aqueous hydrogen peroxide, elemental sulfur or gray selenium in thf gives the corresponding oxides, sulfides and selenides [Ph2P(E)NHCH2-C4H3S] (E: O 1b, S 1c, Se 1d) and [(Ph2P(E))(2)NCH2-C4H3S], (E: O 2b, S 2c, Se 2d) respectively, in high yield. Furthermore, two novel Ru(II) complexes with the P-N ligands la and 2a were synthesized starting with the complex [Ru(eta(6)-p-cymene)(mu-Cl)Cl](2). The complexes were fully characterized by analytical and spectroscopic methods. P-31-{H-1} NMR, DEPT, H-1-13C HETCOR or H-1-H-1 COSY correlation experiments were used to confirm the spectral assignments. The molecular structure of thiophene-2-(N-diphenylthiophosphino)methylamine was also elucidated by single-crystal X-ray crystallography. Following activation by NaOH, compounds 3 and 4 catalyze the transfer hydrogenation of acetophenone derivatives to 1-phenylethanol derivatives in the presence of iso-PrOH as the hydrogen source. [Ru(Ph2PNHCH2-C4H3S)(eta(6)-p-cymene)Cl-2], 3 and [Ru((PPh2)(2)NCH2-C4H3S)-(eta(6)-p-cymene)Cl]Cl, 4 complexes are suitable catalyst precursors for the transfer hydrogenation of acetophenone derivatives in 0.1 M iso-PrOH solution. Notably 4 acts as an excellent catalyst giving the corresponding alcohols in excellent conversions up to 99% (TOF <= 744 h(-1)). This transfer hydrogenation is characterized by low reversibility under the experimental conditions. (C) 2010 Elsevier Ltd. All rights reserved.Öğe A ruthenium(II) bipyridine complex containing a 4,5-diazafluorene moiety: Synthesis, characterization and its applications in transfer hydrogenation of ketones and dye sensitized solar cells(Pergamon-Elsevier Science Ltd, 2015) Baysal, Akin; Aydemir, Murat; Durap, Feyyaz; Ozkar, Saim; Yildirim, Leyla Tatar; Ocak, Yusuf SelimThe ruthenium(B) complex [Ru(bpy)(2)L](PF6)(2), where bpy is 2,2'-bipyridine and L is 1,5-dihydro-2-H-cyclopenta[1,2-b:5,4-b']dipyridine-2-one, was synthesized from the reaction of cis-Ru(bpy)(2)Cl-2 center dot 2H(2)O with L, and isolated as the hexafluorophosphate salt. The structure of L was unequivocally elucidated by single-crystal X-ray diffraction analysis. The new ruthenium(II) complex was thoroughly characterized by H-1 and C-13 NMR spectroscopy, along with FTIR, UV-Vis and LC MS/MS Triple Quadrupole Mass spectroscopy and elemental analysis. The catalytic activity of [Ru(bpy)(2)L](PF6)(2) was tested in the transfer hydrogenation of various ketones in 2-propanol as both the solvent and hydrogen donor. The usage of [Ru(bpy)(2)L](PF6)(2) for the formation of a dye sensitized solar cell is also presented. (C) 2015 Elsevier Ltd. All rights reserved.Öğe Synthesis and characterization of new bis(diphenylphosphino)aniline ligands and their complexes: X-ray crystal structure of palladium(II) and platinum(II) complexes, and application of palladium(II) complexes as pre-catalysts in Heck and Suzuki cross-coupling reactions(Pergamon-Elsevier Science Ltd, 2009) Aydemir, Murat; Durap, Feyyaz; Baysal, Akin; Akba, Osman; Gumgum, Bahattin; Ozkar, Saim; Yildirim, Leyla TatarTwo new bis(diphenylphosphino)isopropylphenylamines, (PPh2)(2)N-C6H4-CH(CH3)(2), having the isopropyl substituent at the carbon atom 2 (1) or 4 (2), were prepared by the aminolysis of chlorodiphenylphosphine with isopropyl substituted aniline at the ortho- or para-position, respectively, under anaerobic conditions. Oxidation of 1 and 2 with either aqueous hydrogen peroxide, elemental sulfur or grey selenium in thf gave the corresponding oxides, sulfides and selenides (Ph2P=E)(2)N-C6H4-CH(CH3)(2), where E = O, S or Se, respectively. The palladium and platinum complexes [M{(Ph2P)(2)N-C6H4-CH(CH3)(2))Cl-2] (M = Pd, Pt) and the copper complex [Cu((Ph2P)(2)N-C6H4-CH(CH3)(2))(2)]PF6 were isolated from the reaction of the bis(phosphino)anilines with MCl2(cod) or [Cu(CH3CN)(4)]PF6, respectively. The new compounds were characterized by NMR, IR spectroscopy and elemental analysis. Furthermore, the solid-state structures of two representative complexes were determined using single crystal X-ray diffraction analysis. The compounds of palladium (1d) and platinum (1e), both mononuclear complexes, crystallize in the monoclinic P2(1)/c space group. In both compounds the metal ion has a distorted square-planar coordination geometry. The structural properties of complexes Id and le in the solid state are very similar. The palladium complexes were also tested for their catalytic activities in C-C coupling reactions. (C) 2009 Elsevier Ltd. All rights reserved.Öğe Synthesis and characterizations of 3,3?-bis(diphenylphosphinoamine)-2,2?-bipyridine and 3,3?-bis(diphenylphosphinite)-2,2?-bipyridine and their chalcogenides(Pergamon-Elsevier Science Ltd, 2007) Baysal, Akin; Aydemir, Murat; Durap, Feyyaz; Guemguem, Bahattin; Oezkar, Saim; Yildirim, Leyla TatarNew bis(phosphinoamine) and bis(phosphinite) derivatives of 2,2'-bipyridine were prepared through a single step reaction of 3,3'-diamino-2,2'-bipyridine or 3,3'-dihydroxy-2,2'-bipyridine with diphenylehlorophosphine, respectively. Their P = E chalcogenides (E = 0, S, Se) were also prepared. All the new compounds were characterized by elemental analysis, IR and NMR spectroscopies. The molecular structure of 3.3'-bis(diphenylthiophosphinite)-2,2'-bipyridine was elucidated by single-crystal X-ray crystallography. (c) 2007 Elsevier Ltd. All rights reserved.Öğe Synthesis and structural characterization of a novel seven-coordinate cobalt(II) complex: 2,9-Bis(ethanolamine)-1,10-phenanthrolinechlorocobalt(II) chloride(Elsevier Science Sa, 2011) Baysal, Akin; Aydemir, Murat; Durap, Feyyaz; Ozkar, Saim; Yildirim, Leyla TatarCondensation reaction of 2,9-dicarboxaldehyde-1,10-phenanthroline with 2-aminoethanol followed by NaBH4 reduction yielded the polydentate Schiff base ligand 2,9-bis(ethanolamine)-1,10-phenanthroline in its reduced form. This ligand was characterized by elemental analysis, LC-MS, IR, UV-Vis and NMR spectroscopy. Reaction of the reduced Schiff base ligand with aqueous solution of cobalt(II) chloride affords 2,9-bis(ethanolamine)-1,10-phenanthrolinechlorocobalt(II) chloride in high yield. Single crystals of the cobalt(II) complex were obtained from the crystallization in ethanol and its structure was elucidated by X-ray structural analysis. The cobalt(II) complex ion was found to be seven-coordinated in a pentagonal bipyramidal geometry, whereby cobalt(II) ion is surrounded by the six donor atoms in the ligand molecule and a chloride ion. (C) 2011 Elsevier B. V. All rights reserved.Öğe Synthesis, Characterization and Crystal Packing-Geometry of 1,5-dihydro-2H-cyclopenta [1,2-b:5,4-b?]dipyridin-2-One(Int Union Crystallography, 2009) Yildirim, Leyla Tatar; Baysal, Akin; Durap, Feyyaz; Ozkar, Saim[Abstract Not Available]Öğe Synthesis, Characterization and Molecular Structure of a Novel Schiff Base, N3,N3?-di-2-hydroxybenzylidene-[2,2?]bipyridinyl-3,3?-diamine(Int Union Crystallography, 2007) Baysal, Akin; Buldag, Aysegul; Gumgum, Bahattin; Ozkar, Saim; Yildirim, Leyla Tatar[Abstract Not Available]Öğe Synthesis, characterization, crystal and molecular structure of diphenyloxophosphinoethylenediamines(Pergamon-Elsevier Science Ltd, 2006) Guemguem, Bahattin; Akba, Osman; Durap, Feyyaz; Yildirim, Leyla Tatar; Uelkue, Dincer; Oezkar, SaimBis-, tris- and tetrakis(diphenyloxophosphino)ethylenediamine compounds can be synthesized starting with ethylenediamine and chlorodiphenylphosphine. Bis(diphenylphosphino)ethylenediamine and tris(diphenylphosphino)ethylenediamine are formed as intermediates and can be oxidized to the respective phosphine oxides by oxygen dissolved in the reaction solution, while tetrakis(diphenylphosphino)ethylenediamine is less liable to oxidation and its oxidation requires a stronger oxidizing agent such as hydrogen peroxide. All the three phosphine oxides and tetrakis(diphenylphosphino)ethylenediamine can be isolated as analytically pure solid materials and are fully characterized by elemental analysis, MS and NMR spectroscopies. The crystal and molecular structure of tris(diphenylphosphino)ethylenediamine was elucidated by single crystal X-ray diffraction analysis. (C) 2006 Elsevier Ltd. All rights reserved.Öğe trans- and cis-Ru(II) aminophosphine complexes: Syntheses, X-ray structures and catalytic activity in transfer hydrogenation of acetophenone derivatives(Elsevier Science Sa, 2011) Aydemir, Murat; Baysal, Akin; Ozkar, Saim; Yildirim, Leyla TatarThe ability of transition metal catalysts to add or remove hydrogen from organic substrates by transfer hydrogenation process is a valuable synthetic tool. For this aim, a novel Ru(II) complex with the P-N ligand [(Ph2P)(2)NCH2-C4H3S] derived from thiophene-2-methylamine was synthesized starting with the complex [Ru(eta(6)-p-cymene)(mu-Cl)Cl](2) and isolated in two isomeric forms: trans- and cis[Ru((PPh2)(2)NCH2-C4H3S)(2)Cl-2], 2 and 3, respectively. The structures of both isomers were also determined by single crystal X-ray diffraction. The cis-isomer 3 can be isolated from the solution of major trans-isomer 2 as yellow crystals. However, upon dissolution 3 is rapidly converted to the trans-isomer 2. The new ruthenium(II) complex provides high catalytic activity in the transfer hydrogenation of acetophenone derivatives to 1-phenylethanol derivatives in the presence of 2-propanol as the hydrogen source. This transfer hydrogenation is characterized by low reversibility under the experimental conditions. (C) 2010 Elsevier B.V. All rights reserved.