Metallkomplexe mit funktionalisierten Schwefelliganden, XV [1]. Reaktionen von Platin(0)-Komplexen mit 1,2,4-Trithiolanen, 1,2,4,5-Tetrathianen, 1,2,3,5,6-Pentathiepanen sowie Thioketonen. Kristallstrukturanalyse von (Ph3P)2Pt(η2-Ph2C=S) / Metal Complexes of Functionalized Sulfur Containing Ligands, XV [1]. Reactions of Platinum(O) Complexes with 1,2,4-Trithiolanes, 1,2,4,5-Tetrathianes, 1,2,3,5,6-Pentathiepanes as well as Thioketones. X-Ray Structure Analysis of (Ph3P)2Pt(η2-Ph2C=S)

2000 ◽  
Vol 55 (6) ◽  
pp. 453-458 ◽  
Author(s):  
Wolfgang Weigand ◽  
Ralf Wünsch ◽  
Christian Robl ◽  
Grzegorz Mloston ◽  
Heinrich Nöth ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Metal Complexes ◽  
Single Crystal ◽  
Structure Analysis ◽  
X Ray ◽  
Sulfur Containing ◽  
Twofold Excess ◽  
Fourfold Excess

3,3,5,5-Tetraphenyl-1,2,4-trithiolane (1) reacts with twofold excess of (Ph3P)2Pt(η2-C2H4) (4) to give a 1:1 mixture of the complexes (Ph3P)2 (6a) and (Ph3P)2Pt(η2-Ph2C=S) (7a). Treatment of 3,3,6,6-tetraphenyl-1,2,4,5-tetrathiane (2) with a fourfold excess of 4 yields [Pt2(PPh3)4(μ-S)2] (8) and the platinum(O) compound 7a. The reaction of the 1,2,3,5,6- pentathiepane 3 with a fourfold excess of 4 affords a 1:1:1 mixture of 8, the platinum(O) complex 7b and the bis-thiolato platinum(II) complex 6b. The thioketone complexes 7a-c were formed in smooth reactions of 4 with the thioketones 5a-c. The molecular structure of (Ph3P)2Pt(η2-Ph2C=S) (7a) has been established by single-crystal X-ray analysis.

scholarly journals Arene Ruthenium Metalla-Assemblies with Anthracene Moieties for PDT Applications

Inorganics ◽  
2018 ◽  
Vol 6 (3) ◽  
pp. 97 ◽  
Author(s):  
Marie Gaschard ◽  
Farzaneh Nehzat ◽  
Thomas Cheminel ◽  
Bruno Therrien
Keyword(s):  
Molecular Structure ◽  
Single Crystal ◽  
General Formula ◽  
Structure Analysis ◽  
White Light ◽  
Light Irradiation ◽  
Synthesis And Characterization ◽  
X Ray

The synthesis and characterization of three metalla-rectangles of the general formula [Ru4(η6-p-cymene)4(μ4-clip)2(μ2-Lanthr)2][CF3SO3]4 (Lanthr: 9,10-bis(3,3’-ethynylpyridyl) anthracene; clip = oxa: oxalato; dobq: 2,5-dioxido-1,4-benzoquinonato; donq: 5,8-dioxido-1,4-naphthoquinonato) are presented. The molecular structure of the metalla-rectangle [Ru4(η6-p-cymene)4(μ4-oxa)2(μ2-Lanthr)2]4+ has been confirmed by the single-crystal X-ray structure analysis of [Ru4(η6-p-cymene)4(μ4-oxa)2(μ2-Lanthr)2][CF3SO3]4 · 4 acetone (A2 · 4 acetone), thus showing the anthracene moieties to be available for reaction with oxygen. While the formation of the endoperoxide form of Lanthr was observed in solution upon white light irradiation, the same reaction does not occur when Lanthr is part of the metalla-assemblies.

scholarly journals New Spiro-Tin Compounds: Reaction of N,N′-Dialkyl Sulfur Diimides with Cyclic Bis(amino)stannylenes - Unexpected Formation of a N-N Bond

1995 ◽  
Vol 50 (12) ◽  
pp. 1811-1817 ◽  
Author(s):  
Max Herberhold ◽  
Christian Köhler ◽  
Wolfgang Milius ◽  
Bernd Wrackmeyer
Keyword(s):  
Molecular Structure ◽  
Magnetic Resonance ◽  
Single Crystal ◽  
Structure Analysis ◽  
Membered Ring ◽  
Monoclinic Space Group ◽  
Unexpected Formation ◽  
Tin Compounds ◽  
X Ray ◽  
Tert Butyl

N,N′-Dialkyl sulfur diimides (1), R(NSN)R [R = Me (a), Et (b), nPr (c), nBu (d)] react with cyclic bis(amino)stannylenes such as 1,3-di-tert-butyl-4,4-dimethyl-1,3,4,2λ2-diazasilastannetedine (2) or 1,3-di-tert-butyl-4,4,5,5-tetramethyl-1,3,4,5,2λ2-diazadisilastannolidine (3) in a 2:1 ratio to give the new spiro-tin(IV) compounds 5a-d, 6b and 6c, built from the respective cyclic bis(amino)stannylene and a seven-membered ring in which the two sulfur diimide groups are coupled via a N-N bond and across the tin atom. A 1:1 adduct 4 is proposed as an intermediate which is the final product 4e in the case of R = tBu (1e). The products were characterized by multinuclear magnetic resonance (1H, 13C, 15N, 29Si, 119Sn NMR), and in the case of 5c the molecular structure was determined by single crystal X-ray structure analysis [monoclinic, space group C2/c ; a = 1504.1(3), b = 1393.3(3), c = 1688.6(3) pm; β = 115.71(3)°].

Metallkomplexe mit funktionalisierten Schwefelliganden, X [1] Ruthenium(II)-und Platin(II)-1-alkin-1-thiolato-Komplexe. Kristallstrukturanalyse von trans-(Ph3P)2Pt[S-C≡C-C(CH3)3]2 / Metal Complexes of Functionalized Sulfur Containing Ligands, X [1] Synthesis of Ruthenium (II) and Platinum(II) 1-Alkyne-1-thiolato Complexes. X-Ray Structure Analysis of trans-( Ph3P)2Pt[C-C≡C-C(CH3)3]2

1996 ◽  
Vol 51 (4) ◽  
pp. 501-505 ◽  
Author(s):  
Wolfgang Weigand ◽  
Michael Weishäupl ◽  
Christian Robl
Keyword(s):  
Crystal Structure ◽  
Metal Complexes ◽  
Structure Analysis ◽  
X Ray Diffraction ◽  
X Ray ◽  
Sulfur Containing

Abstract The 1-alkyne-1-thiolates R-C ≡C-SLi [1a: R = C(CH3)3, 1b: R = C6H11 ] react with L2PtCl2 (L = PPh3, 1/2 dppe) and CpRu(PPh3)2Cl, respectively to give the complexes trans-(Ph3P)2Pt[S-C ≡C-C(CH3)3]2 (2a), cis-dppePt[S-C≡C-C(CH3)3]2 (2b), and CpRu(PPh3)2-(S-C ≡ C-R) [3a: R = C(CH3)3, 3b: R = C6H11]. 2a has been characterized by 31P CP/MAS NM R spectroscopy and its crystal structure determined by X-ray diffraction.

Übergangsmetallkomplexe mit Schwefelliganden, LXX. / Transition Metal Complexes with Sulfur Ligands, LXX.

1991 ◽  
Vol 46 (11) ◽  
pp. 1449-1458 ◽  
Author(s):  
Dieter Sellmann ◽  
Bernd Seubert ◽  
Falk Knoch ◽  
Matthias Moll
Keyword(s):  
Molecular Structure ◽  
Nmr Spectroscopy ◽  
Transition Metal ◽  
Metal Complexes ◽  
Structure Analysis ◽  
Transition Metal Complexes ◽  
Pentagonal Bipyramid ◽  
X Ray ◽  
Hydrogen Bonded

In order to study specific properties of transition metal sulfur complexes, reactions of [Mo(NO)2(′S4′)] (1) with nucleophiles were investigated. With sodiumborohydride or hydrazine, 1 yields the hydroxylaminyl complex [Mo(η2-NH2O)(NO)(′S4′)] (2). 2 crystallizes from DMF as 2 · DMF whose molecular structure was determined by X-ray structure analysis (P21/c, Z = 4, a = 1204.4(3), b = 1579.7(4), c = 1253.0(4) pm, β = 117.44(2)°, R = 0,056, Rw = 0,040). The Mo centre is coordinated by two trans thiolato S, two cis thioether S atoms, the co-ligand NO and side-on NH2O in a distorted pentagonal bipyramid; the DMF molecule is hydrogen bonded to the NH2O-ligand. NMR spectroscopy shows that in solution 2 exists in two configurational isomers differing in the orientation of the side-on NH2O with respect to the [Mo(NO)(′S4′)] core. The mechanism of the reduction of 1 is discussed in terms of a 2e--2H+-transfer.

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.

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.

Übergangsmetallkomplexe mit Schwefelliganden, XCII. Oxidation von Thiolat-Amin- zu Schiffbase-Eisen(II)-Komplexen. Röntgenstrukturanalyse und Reaktivität von [Fe('N2S2')]2 (′N2S2′2- = Glyoxal-bis(2-mercaptoanil)(2 – )) / Transition Metal Complexes with Sulfur Ligands, XCII. Oxidation of Thiolate Amine to Schiff Base Iron(II) Complexes. X-Ray Structure Analysis and Reactivity of [Fe(′N2S2')]2 (′N2S2′2- = Glyoxal-bis(2-mercaptoanil)(2–))

1992 ◽  
Vol 47 (11) ◽  
pp. 1545-1550 ◽  
Author(s):  
Dieter Sellmann ◽  
Marcus Hannakam ◽  
Falk Knoch ◽  
Matthias Moll
Keyword(s):  
Schiff Base ◽  
Transition Metal ◽  
Metal Complexes ◽  
Single Crystal ◽  
Structure Analysis ◽  
Transition Metal Complexes ◽  
X Ray

Oxidation of [Fe(CO)2(′N2H2S2′')] (1) (′N2H2S2'2- = 1,2-ethanediamine-N,N′-bis(2-benzenethiolate)(2—)) gave insoluble [Fe(′N2S2')]2 (2) ('N2S2'2- = glyoxal-bis(2-mercaptoanil)(2—)). Dinuclear, thiolato-bridged 2 was characterized by single crystal X-ray structure analysis. It does not react with CO or H2, but yields bis or mono adducts with PR3 (R = Me, n-Bu, Cy).

Übergangsmetall-substituierte Diphosphene, XIV. Zur Reaktivität des Diphosphenylkomplexes (μ5-C5Me5)(CO)2Fe—P=P—Ar (Ar = 2,4,6-t-Bu3C6H2) gegenüber Schwefel, Selen und Tellur. Synthese und Struktur des ersten Thioxo-λ5-diphosphenyl-Komplexes (μ5-C5Me5)(CO)2Fe-P(=S)(=P-Ar) / Transition Metal Substituted Diphosphenes. On the Reactivity of the Diphosphenyl Complex (μ5-C5Me5)(CO)2Fe-P=P-Ar (Ar = 2,4,6-t-Bu3C6H2) towards Sulfur, Selenium, and Tellurium. Synthesis and X-Ray Structure Analysis of the First Thioxo-λ5-diphosphenyl Complex (μ5-C5Me5) (CO)2Fe - P(=S)(=P - Ar)

1988 ◽  
Vol 43 (6) ◽  
pp. 715-721 ◽  
Author(s):  
Lothar Weber ◽  
Georg Meine ◽  
Roland Boese ◽  
Norbert Niederprüm
Keyword(s):  
Molecular Structure ◽  
Transition Metal ◽  
Single Crystal ◽  
Structure Analysis ◽  
Elemental Analysis ◽  
Spectroscopic Data ◽  
Equimolar Amount ◽  
X Ray

AbstractThe diphosphenyl complex (μ5-C5Me5)(CO)2Fe-P=P-Ar (1a) (Ar = 2,4,6-tert-Bu3C6H2) reacts with an equimolar amount of sulfur to yield the first thioxo- λ5 -diphosphenyl complex (μ5-C5Me5)(CO)2Fe-P(=S)=P-Ar (2). Heating of 2 in boiling benzene affords the metal functionalized thiadiphosphirane 3. Similarily the selenoxo-λ5 -diphosphenyl complex (μ5-C5Me5)(CO)2Fe-P(=Se)=P-Ar (5) and selena-diphosphirane 6 are synthesized. The products have been characterized by elemental analysis as well as by spectroscopic data (IR, 1H, 13C, 31P NMR, MS). The molecular structure of 2 has been elucidated by single crystal X-ray analysis.

scholarly journals Synthesis of Bis(Carboranyl)amides 1,1′-μ-(CH2NH(O)C(CH2)n-1,2-C2B10H11)2 (n = 0, 1) and Attempt of Synthesis of Gadolinium Bis(Dicarbollide)

Molecules ◽  
2021 ◽  
Vol 26 (5) ◽  
pp. 1321
Author(s):  
Yasunobu Asawa ◽  
Aleksandra V. Arsent’eva ◽  
Sergey A. Anufriev ◽  
Alexei A. Anisimov ◽  
Kyrill Yu. Suponitsky ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Single Crystal ◽  
Quantum Chemical Calculations ◽  
Quantum Chemical ◽  
X Ray Diffraction ◽  
Stable Conformation ◽  
Acyl Chlorides ◽  
X Ray ◽  
Cesium Fluoride ◽  
The Stability

Bis(carboranyl)amides 1,1′-μ-(CH2NH(O)C(CH2)n-1,2-C2B10H11)2 (n = 0, 1) were prepared by the reactions of the corresponding carboranyl acyl chlorides with ethylenediamine. Crystal molecular structure of 1,1′-μ-(CH2NH(O)C-1,2-C2B10H11)2 was determined by single crystal X-ray diffraction. Treatment of bis(carboranyl)amides 1,1′-μ-(CH2NH(O)C(CH2)n-1,2-C2B10H11)2 with ammonium or cesium fluoride results in partial deboronation of the ortho-carborane cages to the nido-carborane ones with formation of [7,7′(8′)-μ-(CH2NH(O)C(CH2)n-7,8-C2B9H11)2]2−. The attempted reaction of [7,7′(8′)-μ-(CH2NH(O)CCH2-7,8-C2B9H11)2]2− with GdCl3 in 1,2-dimethoxy- ethane did not give the expected metallacarborane. The stability of different conformations of Gd-containing metallacarboranes has been estimated by quantum-chemical calculations using [3,3-μ-DME-3,3′-Gd(1,2-C2B9H11)2]− as a model. It was found that in the most stable conformation the CH groups of the dicarbollide ligands are in anti,anti-orientation with respect to the DME ligand, while any rotation of the dicarbollide ligand reduces the stability of the system. This makes it possible to rationalize the design of carborane ligands for the synthesis of gadolinium metallacarboranes on their base.

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