Coinage metal complexes supported by a “PN3P” scaffold

2015 ◽  
Vol 44 (44) ◽  
pp. 19153-19162 ◽  
Author(s):  
Gyandshwar Kumar Rao ◽  
Serge I. Gorelsky ◽  
Ilia Korobkov ◽  
Darrin Richeson
Keyword(s):  
Metal Complexes ◽  
Single Crystal ◽  
X Ray Diffraction ◽  
Coinage Metal ◽  
X Ray ◽  
Multinuclear Nmr

Monovalent group 11 complexes, [2,6-{Ph2PNMe}2(NC5H3)]CuBr 1, [2,6-{Ph2PNMe}2(NC5H3)]CuOTf 2, [2,6-{Ph2PNMe}2(NC5H3)]AgOTf 3, and [2,6-{Ph2PNMe}2(NC5H3)](AuCl)24, supported by a neutral PN3P ligand have been synthesized and characterized by multinuclear NMR and single crystal X-ray diffraction studies.

Diphenyl(1-pyridyl)phosphine Sulfide as a Ligand in Mono-and Binuclear Coinage Metal Complexes

1997 ◽  
Vol 52 (3) ◽  
pp. 385-390 ◽  
Author(s):  
M. Elena Olmos ◽  
Annette Schier ◽  
Hubert Schmidbaur
Keyword(s):  
Metal Complexes ◽  
Silver Atom ◽  
Gold Atom ◽  
X Ray Diffraction ◽  
Coinage Metal ◽  
X Ray ◽  
Metal Atoms ◽  
Tetrahedral Environment ◽  
Mixed Metal Complexes ◽  
Phosphine Sulfide

Abstract Diphenyl(1-pyridyl)phosphine sulfide, Ph2pyPS, 1, gives a 1:1 complex (2) with AuCl upon treatment with (C4H8S)AuCl. According to an X -ray diffraction analysis, this compound is isomorphous with the Ph3PS complex. [Ph3PAu]BF4 and 1 give the cationic complex [Ph3PAuSPpyPh2]BF4 (3 ) . With two equivalents of the same reagent the binuclear complex 4 is generated, in which the metal atoms are S- and N-bonded. The reaction of 2 equivalents of 1 with [(tetrahydrothiophene)2Au]ClO4 affords the 2:1 complex 5 with the gold atom exclusively S-bonded. The analogous reaction with AgBF4 gives the 2:1 complex 6, the structure of which has also been determined by X-ray diffraction. The silver atom is engaged in coordinative bonding with both sulfur and both nitrogen atoms in a quasi-tetrahedral environment. Addition of AgClO4 to com pound 5, and of [(MeCN)4Cu]B F4 to 6, gives mixed-metal complexes (7, 8) with head-to-head structures, the silver atoms being exclusively S-bonded.

Study on the Acid-Induced Ring-Expansion of an Oxaphosphirane Complex with an Electron-Withdrawing C-Substituent

2017 ◽  
Vol 70 (4) ◽  
pp. 442 ◽  
Author(s):  
Cristina Murcia García ◽  
Gregor Schnakenburg ◽  
Rainer Streubel
Keyword(s):  
Mass Spectrometry ◽  
Single Crystal ◽  
Elemental Analysis ◽  
Ring Expansion ◽  
X Ray Diffraction ◽  
X Ray ◽  
Multinuclear Nmr ◽  
Fluorinated Ligands ◽  
Ring Expansion Reaction

A study on the acid-induced ring-expansion reaction of the first oxaphosphirane complexes bearing an electron-withdrawing C-substituent is described. The stereoselectively obtained 1,3,4-dioxaphospholane complexes 4a–c, representing the first examples of such fluorinated ligands, were unambiguously characterized by multinuclear NMR, elemental analysis, mass spectrometry, and single-crystal X-ray diffraction studies.

scholarly journals Ring opening polymerisation of L and rac lactide using group 4 permethylpentalene aryloxides and alkoxides

2021 ◽  
Author(s):  
Zoe Turner ◽  
Jessica Lamb ◽  
Thomas Robinson ◽  
Dipa Mandal ◽  
Jean-Charles Buffet ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Ring Opening ◽  
X Ray Diffraction ◽  
X Ray ◽  
Multinuclear Nmr ◽  
New Family ◽  
Group 4 ◽  
Multinuclear Nmr Spectroscopy

A new family of group 4 permethylpentalene (C8Me62–; Pn*) aryloxide and alkoxide complexes have been synthesised and fully characterised by multinuclear NMR spectroscopy and single-crystal X-ray diffraction; (η8-C8Me6)Zr(OR)2 (R =...

Cyclophan-Metall-Komplexe: Synthese und Kristallstruktur von ([2](l,4)Naphthalino[2]paracyclophan)gallium(I)-tetrabromogallat(III)/Cyclophane Metal Complexes: Synthesis and Crystal Structure of ([2]( 1,4)Naphthalino[2]paracyclophane)gallium(I) Tetrabromogallate(III)

1987 ◽  
Vol 42 (2) ◽  
pp. 147-150 ◽  
Author(s):  
H. Schmidbaur ◽  
W. Bublak ◽  
G. Müller
Keyword(s):  
Crystal Structure ◽  
Metal Complexes ◽  
Single Crystal ◽  
Benzene Ring ◽  
Title Complex ◽  
Outer Side ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Secondary Reactions

AbstractThe title complex has been prepared from Ga[GaBr4] and [2](1,4)naphthalino[2]paracyclophane in toluene as a solvent, and the crystal structure of this adduct determined by single crystal X-ray diffraction. The structure is composed of dimeric units Ga2[GaBr4]2 , which are crosslinked into sheets through Ga(I)-arene coordination. Both the benzene ring and the substituted ring of the naphthalene system are η6-bonded from the outer side of the cyclophane cage, each to an univalent metal. The benzene and the naphthalene form an interplane angle of 49.3°. The distance to the benzene ring (2.67 Å) is much shorter than the distance to the naphthalene (2.85 Å), suggesting a stronger complexation with the unperturbed π-system of the former. [2.2](l,4)Naphthalinophane forms no adduct with Ga[GaBr4], and with [2](l,5)naphthalino[2]paracyclophane secondary reactions are observed.

scholarly journals Darstellung neuer Monofluorphosphine und einiger ihrer Übergangsmetallkomplexe; Einkristall-Röntgenstrukturanalyse eines Platin(II)-Komplexes / Preparation of New Monofluorophosphines and Some of their Transition Metal Complexes; Single Crystal X-Ray Diffraction Study of a Platinum(II) Complex

1993 ◽  
Vol 48 (7) ◽  
pp. 875-885 ◽  
Author(s):  
Thomas G. Meyer ◽  
Peter G. Jones ◽  
Reinhard Schmutzler
Keyword(s):  
Transition Metal ◽  
Metal Complexes ◽  
Single Crystal ◽  
Diffraction Study ◽  
Structure Analysis ◽  
Transition Metal Complexes ◽  
Classical Method ◽  
X Ray Diffraction ◽  
X Ray

The reaction of lithiated precursors with PCl2F led to a number of monofluorophosphines, including the known di-tert-butylmonofluorophosphine, 1. Bis(phenylethinyl)monofluorophosphine (2) was accessible only via this route (the classical method of synthesizing 2 by chlorine/fluorine exchange is impossible, because the corresponding chlorophosphine is unknown). Bis(2-methoxyphenyl)fluorophosphine (5) was prepared via the organolithium/PCl2F route. The NMR results for 5 thus prepared were inconsistent with previous reports, implying that the previously reported synthesis of 5 is in error. From 5 a cis-dichloroplatinum(II) complex (6) was synthesized and subjected to a single crystal X-ray structure analysis, confirming the expected planar coordination. From bis(2,3-dimethoxynaphthyl)monofluorophosphine (7) a rhodium(I) (8) and an iron(0)tetracarbonyl complex (9) were prepared. An iron(0)tetracarbonyl complex (11) was synthesized from bis(9-anthryl)monofluorophosphine (10) which was found to be stable to redox disproportionation.

Coordination of N-Heterocyclic Carbene to H2SiX2 (X = Cl, OTf) and H3SiOTf (OTf = OSO2CF3): Synthesis of Donor-stabilized Parent Silylium Salts with Four- and Five-coordinate Silicon Atoms

2013 ◽  
Vol 68 (5-6) ◽  
pp. 445-452 ◽  
Author(s):  
Yun Xiong ◽  
Shenglai Yao ◽  
Matthias Driess
Keyword(s):  
Single Crystal ◽  
Spectroscopic Data ◽  
Ion Pairs ◽  
X Ray Diffraction ◽  
X Ray ◽  
Multinuclear Nmr ◽  
Neutral Compounds ◽  
New Compounds ◽  
Ir Spectroscopic

The reactivity of the N-heterocyclic carbene (NHC) 1,3-bis(2,6-diisopropylphenyl)imidazol-2- ylidene towards dichlorosilane H2SiCl2, bis(trifluoromethanesulfonato)silane H2Si(OTf)2 (OTf = OSO2CF3), and silyl trifluoromethanesulfonate H3SiOTf has been investigated. It turned out that the coordination of the NHC ligand can occur stepwise to form the three neutral compounds (NHC)SiH2Cl2 (1), (NHC)2SiH2Cl2 (2), (NHC)SiH2(OTf)2 (3), as well as the two ion pairs [(NHC)SiH3]+(OTf-) (4) and [(NHC)2SiH3]+(OTf-) (5); the latter represent the first NHC adducts of the parent silylium cation (H3Si+). The multinuclear NMR and IR spectroscopic data of the products reflect the characteristics of four-, five-, and six-coordinate silane complexes. All new compounds were structurally characterized by single-crystal X-ray diffraction analyses

Heavy transition metal complexes of biologically important molecules. I. The crystal and molecular structure of trans-dichloro(bis(isopropyl)-sulfoxide-S)(1-methylcytosine-N)platinum(II)

1976 ◽  
Vol 54 (1) ◽  
pp. 53-58 ◽  
Author(s):  
Colin James Lyne Lock ◽  
Robert Anthony Speranzini ◽  
John Powell
Keyword(s):  
Molecular Structure ◽  
Transition Metal ◽  
Metal Complexes ◽  
Single Crystal ◽  
Least Squares ◽  
Transition Metal Complexes ◽  
Crystal And Molecular Structure ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray

The crystal and molecular structure of trans-dichloro(bis(isopropyl)sulfoxide-S)(1-methylcytosine-N)platinum(II) has been determined by single crystal X-ray diffraction. The crystals are triclinic with a = 16.205(5), b = 8.078(2), c = 6.776(2) Å, α = 106.53(2), β = 96.35(2), γ = 98.54(2)°. The space group is [Formula: see text] and there are two molecules per unit cell. A total of 2294 independent reflections, of which 2023 were observed, were examined on a Syntex [Formula: see text] diffractometer. The structure was refined by full matrix least squares analysis to an R2 value of 0.0427. The ligands form a rough square around the platinum atom with Pt—Cl(1), 2.304(3), Pt—Cl(2), 2.287(4), Pt—S, 2.232(2), Pt—N, 2.058(7). Distances within the ligands are normal. The plane of the cytosine ring is at 84.4° to the plane formed by the ligands around platinum.

scholarly journals Half-Sandwich Arene-Osmium(II) Complexes with Phosphinite Ligands

Molbank ◽  
10.3390/m1110 ◽  
2020 ◽  
Vol 2020 (1) ◽  
pp. M1110 ◽  
Author(s):  
Rebeca González-Fernández ◽  
Javier Borge ◽  
Pascale Crochet ◽  
Victorio Cadierno
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Diffraction Study ◽  
Elemental Analysis ◽  
X Ray Diffraction ◽  
X Ray ◽  
Multinuclear Nmr ◽  
Intramolecular Exchange ◽  
Multinuclear Nmr Spectroscopy ◽  
Half Sandwich

The synthesis of a series of arene-osmium(II) complexes containing phosphinite-type ligands, namely, [OsCl2(η6-p-cymene){R2PO(CH2)nPh}] (R = Ph, n = 1 (4a), 2 (4b), 3 (4c); R = iPr, n = 1 (5a), 2 (5b), 3 (5c)) and [OsCl2(η6-benzene){iPr2PO(CH2)2Ph}] (7), is presented. All these compounds were characterized by elemental analysis and multinuclear NMR spectroscopy (31P{1H}, 1H and 13C{1H}), and the structure of [OsCl2(η6-p-cymene){Ph2PO(CH2)3Ph}] (4c) unequivocally confirmed through a single-crystal X-ray diffraction study. Attempts to generate the tethered species [OsCl2{η6:κ1(P)-C6H5(CH2)nOPR2}] by intramolecular exchange of the coordinated arene in 4-5a-c or 7, upon thermal or MW heating, failed.

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