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1.
Wolfgang Beck Wolf Peter Fehlhammer Klaus Feldl Thomas M. Klaptke Gernot Kramer Peter Mayer Holger Piotrowski Peter Pllmann Walter Ponikwar Thomas Schütt Erich Schuierer Martin Vogt 《无机化学与普通化学杂志》2001,627(8):1751-1758
The crystal structures of the monomeric palladium(II) azide complexes of the type L2Pd(N3)2 (L = PPh3 ( 1 ), AsPh3 ( 2 ), and 2‐chloropyridine ( 3 )), the dimeric [(AsPh4)2][Pd2(N3)4Cl2] ( 4 ), the homoleptic azido palladate [(PNP)2][Pd(N3)4] ( 5 ) and the homoleptic azido platinates [(AsPh4)2][Pt(N3)4] · 2 H2O ( 6 ) and [(AsPh4)2][Pt(N3)6] ( 7 ) were determined by X‐ray diffraction at single crystals. 1 and 2 are isotypic and crystallize in the triclinic space group P1. 1 , 2 and 3 show terminal azide ligands in trans position. In 4 the [Pd2(N3)4Cl2]2– anions show end‐on bridging azide groups as well as terminal chlorine atoms and azide ligands. The anions in 5 and 6 show azide ligands in equal positions with almost local C4h symmetry at the platinum and palladium atom respectively. The metal atoms show a planar surrounding. The [Pt(N3)6]2– anions in 7 are centrosymmetric (idealized S6 symmetry) with an octahedral surrounding of six nitrogen atoms at the platinum centers. 相似文献
2.
Zhong‐Lu You 《Acta Crystallographica. Section C, Structural Chemistry》2005,61(7):m339-m341
The title complex, [Cu(C11H14BrN2O)(N3)]n, is an interesting azide‐bridged polynuclear copper(II) compound. The CuII atom is five‐coordinated in a square‐pyramidal configuration, with one O and two N atoms of one Schiff base and one terminal N atom of a bridging azide ligand defining the basal plane, and another terminal N atom of another bridging azide ligand occupying the axial position. The {4‐bromo‐2‐[2‐(dimethylamino)ethyliminomethyl]phenolato}copper(II) moieties are linked by the bridging azide ligands, forming polymeric chains running along the b axis. Adjacent chains are further linked by weak Br⋯Br interactions into a sheet. 相似文献
3.
Tris(iso‐propyl)stibine complexes of palladium and platinum of the type [MX2(SbiPr3)2] [M, X = Pd, Cl (1a), Pd, Br (1b), Pd, I (1c), Pt, Cl (2)] have been prepared and characterized by elemental analysis, IR and 1H NMR spectral data. The structure of 1a, established by X‐ray structural analysis, revealed that the palladium atom is in a square planar environment with mutually trans SbiPr3 ligands. Copyright © 2001 John Wiley & Sons, Ltd. 相似文献
4.
A series of new chiral C2‐symmetric bis(phosphinite) ligands and their palladium(II) complexes have been synthesized and for the first time used as catalysts in the palladium‐catalysed asymmetric intermolecular Heck coupling reactions of 2,3‐dihydrofuran with iodobenzene or aryl triflate. Under optimized conditions, products were obtained with high conversions and moderate to good enantioselectivities. The new C2‐symmetric bis(phosphinite) ligands and their palladium(II) complexes were characterized using multinuclear NMR and Fourier transform infrared spectroscopies and elemental analysis. Copyright © 2015 John Wiley & Sons, Ltd. 相似文献
5.
Rafet Kılınçarslan M. Emin Günay Rukiye Fırıncı Serpil Denizaltı Bekir Çetinkaya 《应用有机金属化学》2016,30(5):268-272
A new series of sterically hindered ligands containing (1R,2S,4R)‐(+)‐menthoxymethyl group attached to benzimidazole‐based N‐heterocyclic carbene (NHC), palladium–bis‐NHC complexes and (κ2‐C,N)‐palladacyclic NHC complexes have been synthesized and characterized using appropriate spectroscopic techniques. Catalytic performance of the palladium complexes has been investigated for allylic alkylation, Suzuki and Heck carbon–carbon coupling reactions. These complexes smoothly catalyse the carbon–carbon bond formation reactions. Copyright © 2016 John Wiley & Sons, Ltd. 相似文献
6.
Two trans‐bis(saccharinato) (sac) complexes of cadmium(II ) with 2‐aminomethylpyridine (ampy) and 2‐aminoethylpyridine (aepy) were synthesized and characterized by means of elemental analysis, FT‐IR spectroscopy and thermal analysis. In addition, their solid‐state structures were determined by single crystal X‐ray diffraction studies. The [Cd(sac)2(ampy)2] ( 1 ) and [Cd(sac)2(aepy)] ( 2 ) complexes consist of neutral monomeric units and crystallize in the orthorhombic (Pbca) and monoclinic (P21/c) crystal systems, respectively. The cadmium(II ) ions in 1 and 2 sit on inversion centres andexhibit distorted octahedral coordination by two sac anions and two aminopyridine ligands. The sac ligands in both complexes are N‐coordinated and located in trans positions, while the ampy and aepy ligands act as a bidentate ligand forming two symmetrically chelate rings around cadmium(II ). IR spectra and thermal decompositions of the complexes are also discussed. 相似文献
7.
Sujittra Youngme Jaturong Phatchimkun Samran Prabpai Chaveng Pakawatchai Palangpon Kongsaeree 《Acta Crystallographica. Section C, Structural Chemistry》2007,63(2):m45-m47
The two new title complexes, [Cu(N3)(dpyam)2]PF6 (dpyam is di‐2‐pyridylamine, C10H11N3), (I), and [Cu(N3)(dpyam)2]Cl·4H2O, (II), respectively, have been characterized by single‐crystal X‐ray diffraction. Both complexes display a distorted square‐pyramidal geometry. Each Cu atom is coordinated in the basal plane by three dpyam N atoms and one azide N atom in equatorial positions, and by another N atom from the dpyam group in the apical position. In complex (I), the one‐dimensional supramolecular architecture is assembled via hydrogen‐bonding interactions between the amine N atom and terminal azide N atoms and the F atoms of the PF6− anion. For complex (II), hydrogen‐bonding interactions between the amine N atom, the Cl− anion and water O atoms result in a two‐dimensional lattice. 相似文献
8.
Naruyoshi Komiya Takeharu Kageyama Masaya Naito Takeshi Naota 《Acta Crystallographica. Section C, Structural Chemistry》2013,69(5):503-505
rac‐Bis{μ‐trans‐2,2′‐[pentane‐1,5‐diylbis(azanediyl)]ditroponato}dipalladium(II), [Pd2(C19H20N2O2)2], has been synthesized and fully characterized using single‐crystal X‐ray diffraction, 1H NMR, FT–IR and mass spectroscopy. The trans coordination, vaulted structure and anti conformation have been unequivocally established from the X‐ray diffraction studies. This is the first example of a bis(aminotroponato)palladium complex. In the crystalline state, the molecule has twofold symmetry and each molecular unit undergoes intermolecular offset π‐stacking of the tropone rings to afford heterochiral interpenetrating dimers that are aligned in a lamellar manner with a herringbone packing motif. 相似文献
9.
Novel (N‐heterocyclic carbene)Pd(pyridine)Br2 complexes for carbonylative Sonogashira coupling reactions: Catalytic efficiency and scope for arylalkynes,alkylalkynes and dialkynes
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Mansur Ibrahim Imran Malik Waseem Mansour Muhammad Sharif Mohammed Fettouhi Bassam El Ali 《应用有机金属化学》2018,32(4)
New N,N′‐substituted imidazolium salts and their corresponding dibromidopyridine–palladium(II) complexes were successfully synthesized and characterized. Reactions of palladium bromide with the newly synthesized N,N′‐substituted imidazolium bromides ( 2a and 2b ) in pyridine afforded the corresponding new N‐heterocyclic carbene pyridine palladium(II) complexes ( 3a and 3b ) in high yields. Their single‐crystal X‐ray structures show a distorted square planar geometry with the carbene and pyridine ligands in trans position. Both complexes show a high catalytic activity in carbonylative Sonogashira coupling reactions of aryl iodides and aryl diiodides with arylalkynes, alkylalkynes and dialkynes. 相似文献
10.
Douglas M. Ho Michael J. Zdilla 《Acta Crystallographica. Section C, Structural Chemistry》2011,67(4):m100-m104
trans‐Bis(3‐isopropyl‐7‐oxocyclohepta‐1,3,5‐trien‐1‐olato)copper(II) trans‐bis(3‐isopropyl‐7‐oxocyclohepta‐1,3,5‐trien‐1‐olato)palladium(II) as the (5/1) and (3/2) composites [Cu(C10H11O2)2]·0.2[Pd(C10H11O2)2] and [Cu(C10H11O2)2]·0.67[Pd(C10H11O2)2], respectively, where 3‐isopropyl‐7‐oxocyclohepta‐1,3,5‐trien‐1‐olate is the systematic name for the hinokitiolate anion (hino), are the first mixed‐metal cocrystalline products isolated from the Mx(hino)y family of complexes. These cocrystals contain square‐planar trans‐Cu(hino)2 and trans‐Pd(hino)2 molecules possessing crystallographic inversion symmetry. The bulk formulation for these cocrystalline compounds is Cu1−xPdx(hino)2, where x is 0.166 (4) for the (5/1) product and 0.399 (4) for the (3/2) product. This bulk formulation is simply a convenient average expression of the whole‐molecule substitutional disorder present in these compounds. The M—O bonds are in the range 1.9210 (11)–1.9453 (10) Å, the O—M—O bite angles are in the range 82.94 (4)–83.36 (4)°, and all of the hinokitiolate O atoms are involved in C—H...O hydrogen‐bonding interactions. 相似文献
11.
Jaime Vzquez Sylvain Berns Ruth Melndrez Roberto Portillo Ren Gutirrez 《Acta Crystallographica. Section C, Structural Chemistry》2005,61(9):m424-m427
The title compounds, trans‐dichlorobis[(1R,2R,3R,5S)‐(−)‐2,6,6‐trimethylbicyclo[3.1.1]heptan‐3‐amine]palladium(II), [PdCl2(C10H19N)2], and trans‐dichlorobis[(1S,2S,3S,5R)‐(+)‐2,6,6‐trimethylbicyclo[3.1.1]heptan‐3‐amine]palladium(II) hemihydrate, [PdCl2(C10H19N)2]·0.5H2O, present different arrangements of the amine ligands coordinated to PdII, viz. antiperiplanar in the former case and (−)anticlinal in the latter. The hemihydrate is an inclusion compound, with a Pd coordination complex and disordered water molecules residing on crystallographic twofold axes. The crystal structure for the hemihydrate includes a short Pd⋯Pd separation of 3.4133 (13) Å. 相似文献
12.
Reaction of RuCl2(PPh3)3 with N‐Phenyl‐pyridine‐2‐carbaldehyde thiosemicarbazone (C5H4N–C2(H)=N3‐N2H–C1(=S)N1HC6H5, Hpytsc‐NPh) in presence of Et3N base led to loss of ‐N2H‐proton and yielded the complex [Ru(pytsc‐NPh)2(Ph3P)2] ( 1 ). Similar reactions of precursor RuCl2[(p‐tolyl)3P]3 with a series of thiosemicarbazone ligands, viz. pyridine‐2‐carbaldehyde thiosemicarbazone (Hpytsc), salicylaldehyde thiosemicarbazone (H2stsc), and benzaldehyde thiosemicarbazone (Hbtsc), have yielded the complexes, [Ru(pytsc)2{(p‐tolyl)3P}2] ( 2 ), [Ru(Hstsc)2{(p‐tolyl)3P}]2 ( 3 ), and [Ru(btsc)2{(p‐tolyl)3P}2] ( 4 ), respectively. The reactions of precursor Ru2Cl4(dppb)3 {dppb = Ph2P–(CH2)4–PPh2} with H2stsc, Hbtsc, furan‐2‐carbaldehyde thiosemicarbazone (Hftsc) and thiophene‐2‐carbaldehyde thiosemicarbazone (Httsc) have formed complexes of the composition, [Ru(Hstsc)2(dppb)] ( 5 ), [Ru(btsc)2(dppb)] ( 6 ), [Ru(ftsc)2(dppb)] ( 7 ), and [Ru(ttsc)2(dppb)] ( 8 ). The complexes have been characterized by analytical data, IR, NMR (1H, 31P) spectroscopy and X‐ray crystallography ( 1 and 5 ). The proton NMR confirmed loss of –N2H– proton in all the compounds, and 31P NMR spectra reveal the presence of equivalent phosphorus atoms in the complexes. In all the compounds, thiosemicarbazone ligands coordinate to the RuII atom via hydrazinic nitrogen (N2) and sulfur atoms. The arrangement around each metal atom is distorted octahedral with cis:cis:trans P, P:N, N:S, S dispositions of donor atoms. 相似文献
13.
Nobuo Okabe Yasunori Muranishi Mamiko Odoko 《Acta Crystallographica. Section C, Structural Chemistry》2004,60(7):m345-m347
The crystal structures of the title complexes, namely trans‐bis(isoquinoline‐3‐carboxylato‐κ2N,O)bis(methanol‐κO)cobalt(II), [Co(C10H6NO2)2(CH3OH)2], and the corresponding nickel(II) and copper(II) complexes, [Ni(C10H6NO2)2(CH3OH)2] and [Cu(C10H6NO2)2(CH3OH)2], are isomorphous and contain metal ions at centres of inversion. The three compounds have the same distorted octahedral coordination geometry, and each metal ion is bonded by two quinoline N atoms, two carboxylate O atoms and two methanol O atoms. Two isoquinoline‐3‐carboxylate ligands lie in trans positions, forming the equatorial plane, and the two methanol ligands occupy the axial positions. The complex molecules are linked together by O—H⋯O hydrogen bonds between the methanol ligands and neighbouring carboxylate groups. 相似文献
14.
Jolanta Bucher Olivier Blacque Helmut W. Schmalle Heinz Berke 《Acta Crystallographica. Section C, Structural Chemistry》2008,64(2):m87-m90
The title compounds, [Mo(C2H4NO2)2(NO)2], (I), and [Mo(C2H6NS)2(NO)2]·CH3CN, (II), contain distorted octahedral complexes in which the monoanionic N,S‐ and N,O‐bidentate ligands coordinate the molybdenum centres in different modes. The anionic O atoms of the glycinate ligands in (I) are coordinated trans to the nitrosyl ligands and the amine N atoms are located trans to each other, whereas in (II) the anionic S atoms are coordinated trans to each other and the amine N atoms are located trans to the nitrosyl ligands. Each compound has a single complete complex in the asymmetric unit on a general position. Six N—H...O contacts with N...O distances of less than 3.2 Å are observed in (I) between the amine groups and the nitrosyl and carboxylate O atoms. In the 1:1 solvate (II), the acetonitrile molecule forms short N—H...N contacts (N...N < 3.2 Å) between the solvent N atoms and one of the amine H atoms. In addition, three weak intermolecular N—H...S interactions (N...S > 3.3 Å) contribute to the stabilization of the structure of (II). 相似文献
15.
Activation of Sulfur Dioxide by Bis[N,N′‐diisopropylbenzamidinato(−)]silicon(II): Synthesis of Neutral Six‐Coordinate Silicon(IV) Complexes with Chelating O,O′‐Sulfito or O,O′‐Dithionito Ligands
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Konstantin Junold Felix M. Mück Claudia Kupper Johannes A. Baus Dr. Christian Burschka Prof. Dr. Reinhold Tacke 《Chemistry (Weinheim an der Bergstrasse, Germany)》2014,20(40):12781-12785
The neutral six‐coordinate silicon(IV) complexes 2 and 3 (mixture of cis‐ 3 and trans‐ 3 ) were synthesized by reaction of the donor‐stabilized silylene bis[N,N′‐diisopropylbenzamidinato(?)]silicon(II) ( 1 ) with SO2. Compounds 2 and 3 are the first silicon(IV) complexes with chelating sulfito or dithionito ligands, and 3 is even the first molecular compound with a chelating dithionito ligand. Compounds 2 and 3 were structurally characterized by crystal structure analyses and multinuclear NMR spectroscopic studies in the solid state and in solution. 相似文献
16.
Cross‐coupling reactions in water using ionic liquid‐based palladium(II)–phosphinite complexes as outstanding catalysts
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Nermin Meriç Murat Aydemir Uğur Işik Yusuf Selim Ocak Khadichakhan Rafikova Salih Paşa Cezmi Kayan Feyyaz Durap Alexey Zazybin Hamdi Temel 《应用有机金属化学》2014,28(11):818-825
Two new phosphinite ligands based on ionic liquids [(Ph2PO)C7H14N2Cl]Cl ( 1 ) and [(Cy2PO)C7H14N2Cl]Cl ( 2 ) were synthesized by reaction of 1‐(3‐chloro‐2‐hydoxypropyl)‐3‐methylimidazolium chloride, [C7H15N2OCl]Cl, with one equivalent of chlorodiphenylphosphine or chlorodicyclohexylphosphine, respectively, in anhydrous CH2Cl2 and under argon atmosphere. The reactions of 1 and 2 with MCl2(cod) (M = Pd, Pt; cod = 1,5‐cyclooctadiene) yield complexes cis‐[M([(Ph2PO)C7H14N2Cl]Cl)2Cl2] and cis‐[M(Cy2PO)C7H14N2Cl]Cl)2Cl2], respectively. All complexes were isolated as analytically pure substances and characterized using multi‐nuclear NMR and infrared spectroscopies and elemental analysis. The catalytic activity of palladium complexes based on ionic liquid phosphinite ligands 1 and 2 was investigated in Suzuki cross‐coupling. They show outstanding catalytic activity in coupling of a series of aryl bromides or aryl iodides with phenylboronic acid under the optimized reaction conditions in water. The complexes provide turnover frequencies of 57 600 and 232 800 h?1 in Suzuki coupling reactions of phenylboronic acid with p‐bromoacetophenone or p‐iodoacetophenone, respectively, which are the highest values ever reported among similar complexes for Suzuki coupling reactions in water as sole solvent in homogeneous catalysis. Furthermore, the palladium complexes were also found to be highly active catalysts in the Heck reaction affording trans‐stilbenes. Copyright © 2014 John Wiley & Sons, Ltd. 相似文献
17.
《Journal of Coordination Chemistry》2012,65(21):3700-3710
Nickel(II) and palladium(II) form neutral 1?:?2 chelates with aromatic thiohydrazides, for example. thiobenzhydrazide, o-hydroxythiobenzhydrazide, furan-2-thiohydrazide, and thiophen-2-thiohydrazide. All the compounds are diamagnetic and have been characterized by elemental analysis and spectroscopic methods. o-Hydroxythiobenzhydrazido complexes of nickel(II) and palladium(II) were crystallized from DMSO and their structures were solved by X-ray diffraction. The complexes are isostructural with planar structures. Metal ion is linked to two identical deprotonated ligands through trans hydrazinic nitrogen and sulfur. Hydrogen of OH is involved in intramolecular hydrogen-bonding. 相似文献
18.
Jennifer A. Saltmarsh Bob A. Howell Philip J. Squattrito 《Acta Crystallographica. Section C, Structural Chemistry》2000,56(8):e335-e337
The title complexes, [Pt(C4H7NO)2I2], (I), and [Pt(C4H9NO)2I2], (II), possess similar square‐planar coordination geometries with modest distortions from ideality. For (I), the cis‐L—Pt—L angles are in the range 87.0 (4)–94.2 (3)°, while the trans angles are 174.4 (3) and 176.4 (3)°. For (II), cis‐L—Pt—L are 86.1 (8)–94.2 (6)° and trans‐L—Pt—L are 174.4 (6) and 177.4 (5)°. One 3,6‐dihydro‐2H‐1,2‐oxazine ligand in (I) is rotated so that the N—O bond is out of the square plane by approximately 70°, while the N—C bond is only ca 20° out of the plane. The other oxazine ligand is rotated so that the N—C bond is about 80° out of the plane, while the N—O bond is out of the plane by approximately 24°. In (II), the 3,4,5,6‐tetrahydro‐2H‐1,2‐oxazine ligands are also positioned with one having the N—O bond further out of the plane and the other having the N—C bond positioned in that fashion. Both ligands, however, are rotated approximately 90° compared with their positions in (I). In both complexes, this results in an unsymmetrical distortion of the I—Pt—N bond angles in which one is expanded and the other contracted. These features are compared to those of reported cis‐diaminediiodoplatinum(II) complexes. 相似文献
19.
Maria H. Johansson ke Oskarsson 《Acta Crystallographica. Section C, Structural Chemistry》2002,58(2):m102-m104
Tetrakis(dimethyl sulfide)palladium(II) bis(tetrafluoroborate), [Pd(C2H6S)4](BF4)2, (I), and tetrakis(1,4‐oxathiane‐κS)palladium(II) bis(tetrafluoroborate), [Pd(C4H8OS)4](BF4)2, (II), both crystallize as mononuclear square‐planar complexes with tetrafluoroborate as the counter‐ions. The Pd atom accepts four S‐donor atoms and is positioned at an inversion centre in both compounds. The two unique S atoms in the dimethyl sulfide complex, (I), are disordered. The Pd—S distances are in the range 2.3338 (12)–2.3375 (12) Å in (I), and the corresponding distances in the thioxane complex, (II), are 2.3293 (17) and 2.3406 (17) Å. The anions in both compounds interact weakly with the Pd atom. 相似文献
20.
William M. Motswainyana Martin O. Onani Jeroen Jacobs Luc Van Meervelt 《Acta Crystallographica. Section C, Structural Chemistry》2013,69(3):209-211
The title imino–phosphine compound, [PdCl2(C26H22NP)]·CH3CN, was prepared by reaction of N‐[2‐(diphenylphosphanyl)benzylidene]‐2‐methylaniline with dichlorido(cycloocta‐1,5‐diene)palladium(II) in dry CH2Cl2. The PdII cation is coordinated by the P and N atoms of the bidentate chelating ligand and by two chloride anions, generating a distorted square‐planar coordination geometry. There is a detectable trans influence for the chloride ligands. The methyl group present in this structure has an influence on the crystal packing. 相似文献