The reaction of [Os3(CO)10(MeCN)2], with heterocyclic thioamides. The crystal and molecular structure of [Os3(µ-H)(CO)10(µ-SCNCH2CH2S)]

Brodie, Andrew M.; Holden, H. D.; Lewis, Jack; Taylor, Michael J.

doi:10.1039/dt9860000633

Cited by 48 publications

(11 citation statements)

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“…The structural changes occurring in ligand upon deprotonation and coordination to the Sn atom should be reflected by the changes in the 13 C NMR spectra of our complexes If the initial thione form of ligand changes to the thiolate on complexation, C 2 and/or C 6 should be further low frequency in the spectra of all complexes compared with those in free ligands, the shielding effect of the C@N bond being greater than that of the C@S bond [14]. As shown in Table 2, C 6 atom of complex 2 shows two signals (d 170.7, 160.5), one is similar to that of free ligand (d 169.5) and the other is shifted by 9 ppm to low frequency compared with it, indicating that two tpu act as thiolate and thione forms, respectively.…”

Section: Nmr Spectramentioning

confidence: 98%

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Investigation on coordination modes of organotin(IV) complexes with 6-thiopurine and related ligands

Sun

Shi

et al. 2005

Journal of Organometallic Chemistry

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Section: Nmr Spectramentioning

confidence: 98%

“…Thus, the geometry at tin atoms become distorted trigonal bipyramidal with C(6), C(6A) and S(1) atoms for Sn(1), C(7), C(7A) and S(2) atoms for Sn (2) occupying the equatorial plane. And the axial angle Cl(1)-Sn(1)-N(1) and Cl(2)-Sn(2)-N(2) are 164.19 (12) and 152.57 (14), respectively.…”

Section: (Me 2 Sncl) 2 (Dtpu) Ae H 2 O (9)mentioning

confidence: 99%

Investigation on coordination modes of organotin(IV) complexes with 6-thiopurine and related ligands

Sun

Shi

et al. 2005

Journal of Organometallic Chemistry

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“…Durch die Einbeziehung des Stickstoffatoms N2 in die Koordination wird eine Hochfeldverschiebung dieses "N-Signals um 5-20ppm bedingt [6]. In den 13C-NMR-Spektren zeigen sich die fur eine dreizahnige Koordination der Chelatliganden iiber X, N und 0 charakteristische Hochfeldverschiebung von C2-S (Thiocarbonylgruppierung) urn 15-25 ppm [7] bzw. Tieffeldverschiebung von C2-0 (Carbonylgruppierung) um 10-18 ppm [8], sowie Tieffeldverschiebung von C3 um 10-20ppm [4] gegeniiber dem unkoordinierten Liganden.…”

Section: Nmr-spektroskopische Untersuchungen A) Konstitution Der Kompunclassified

Darstellung und NMR‐spektroskopische Charakterisierung von konfigurationsstabilen Diorganozinn(IV)‐Komplexen RPhSnL mit Zinn als chiralem Zentrum

Knoll

Borsdorf

Tschwatschal

et al. 1997

Zeitschrift anorg allge chemie

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Im Gegensatz zur hohen optischen Stabilität von Zinntetraalkylverbindungen erweisen sich die meisten heteroleptisch substituierten Organozinn(IV)‐Verbindungen als konfigurativ instabil. Uns gelang die Darstellung enantiomerer und diastereomerer Diorganozinn‐Komplexe, in denen das Zinnatom als konfigurativ stabiles chirales Zentrum fungiert. Die Stabilisierung des optisch aktiven Zinnzentrums wurde durch Bildung pentakoordinierter Chelatkomplexe mit dreizähnigen, zweifach deprotonierbaren Ligandensystemen H2L vom Esterhydrazontyp realisiert, die eine Inversion am Zinnatom verhindern. Durch multinukleare NMR‐Untersuchungen in Lösung wurde der Nachweis der Chiralität des Zinnatoms und der konfigurativen Stabilität im Temperaturbereich von −90°C bis +160°C erbracht. Mittels Röntgenkristallstrukturanalyse wurden die Strukturen von Neophyl‐phenyl‐zinn‐2[(2‐methylmercaptothiocarbonyl)‐hydrazono]propionat II b und (2‐Methyl‐butyl‐1‐yl)‐phenyl‐zinn‐[S‐methyl‐β‐N‐(2‐salicylmethyliden)thiocarbazat] III g bestimmt.

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“…A search of the Cambridge Structural Database 4 (CSD) (5) revealed that the following bonding modes occur for the tzt -ligand in structurally characterized examples: monodentate bonding through sulfur (found in only two examples, MeHg(tzt) (6) and (Ph 3 P)Au(tzt) (7)); a single example of monodentate bonding through N, reported since the completion of our work (8); N,S-chelation; and bridging, which usually involves both N and the exocyclic S, although a single example of bridging solely through the exocyclic S is known (9). Of these, the N,S-bridging mode predominates.…”

Section: Introductionmentioning

confidence: 96%

A synthetic, structural, and¹¹³Cd NMR study of cadmium complexes of 1,3-thiazolidine-2-thionate, including the structures of Cd(C₃H₄NS₂)₂, (Cd(C₃H₄NS₂)₂(C₅H₅N)₃·C₅H₅N, and (Ph₄P)₂[I₂Cd(µ-C₃H₄NS₂)₂CdI₂]

Craig¹,

Dance²,

Dean³

et al. 2005

Can. J. Chem.

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The crystallization of cadmium bis(1,3-thiazolidine-2-thionate), Cd(C 3 H 4 NS 2 ) 2 (1), is reported. Freshly prepared 1 reacts with Ph 4 P + X -in a 1:2 ratio to give (Ph 4 P) 2 [Cd 2 (C 3 H 4 NS 2 ) 2 X 4 ] (X = I (4) or Br (5)). Crystallization of 1 from pyridine produces a solvate 7, which loses pyridine readily. X-ray analyses show that 1 has a polymeric sheet structure in which the C 3 H 4 NS 2 -ligands act as bidentate bridges through N and the exocyclic S and the Cd has a CdN 2 S 2 kernel; 5 is isomorphous with 4, which contains a dimeric anion again with bridging through the N and exocyclic S of the heterocyclic ligands; and 7 is Cd(C 3 H 4 NS 2 ) 2 (C 5 H 5 N) 3 ·C 5 H 5 N, containing trigonal bipyramidal Cd(C 3 H 4 NS 2 ) 2 (C 5 H 5 N) 3 molecules, in which the C 3 H 4 NS 2 -ligands, both of which are monodentate and in equatorial positions, occur as a unique combination of S-and N-bound. Cadmium-113 NMR data for 1 in pyridine solution and solid-state CP-MAS 113 Cd data for 1, 7, bis(pyridinium-4-thiolate)cadmium, and tetrakis(pyridinium-2-thiolate)cadmium nitrate are reported and discussed. The compound 1 has chemical and NMR spectroscopic properties that make it a useful standard for solid-state CP-MAS 113 Cd NMR spectroscopy.Résumé : On a effectué la cristallisation du bis(1,3-thiazolidine-2-thionate) de cadmium, Cd(C 3 H 4 NS 2 ) 2 (1). Le composé 1 fraîchement préparé réagit avec le Ph 4 P + X -dans un rapport 1 : 2 pour conduire à la formation de (Ph 4 P) 2 [Cd 2 (C 3 H 4 NS 2 ) 2 X 4 ] (X = I (4) et Br (5)). La cristallisation du composé 1 dans la pyridine conduit à la formation du produit solvaté 7 qui perd facilement de la pyridine. Les données de la diffraction des rayons X montrent que le composé 1 existe dans une structure en feuillets polymériques dans laquelle les ligands C 3 H 4 NS 2 -agissent comme ponts bidentates entre l'azote et le soufre exocyclique et que le cadmium se trouve dans un noyau CdN 2 S 2 ; que le composé 5 est isomorphe de 4 qui contient un anion dimère qui se lie lui aussi par des ponts à l'azote et au soufre exocyclique des ligands hétérocycliques; que 7, Cd(C 3 H 4 NS 2 ) 2 (C 5 H 5 N) 3 ·C 5 H 5 N, comporte des molécules bipyramidales trigonales Cd(C 3 H 4 NS 2 ) 2 (C 5 H 5 N) 3 dans lesquelles les ligands C 3 H 4 NS 2 -, qui sont tous les deux monodentates et dans des positions équatoriales, se retrouvent comme une combinaison unique avec des liaisons au soufre et à l'azote. On a obtenu et on discute des données de RMN du 113 Cd pour le composé 1, en solution dans la pyridine, et des données de « CP-MAS » à l'état solide du 113 Cd pour les composés 1 et 7, le bis(pyridinium-4-thiolate)cadmium et le nitrate de tétrakis(pyridinium-2-thiolate)cadmium. Le composé 1 a des propriétés chimiques et spectroscopiques qui pourraient le rendre utile comme standard pour la spectroscopie RMN 113 Cd « CP-MAS » à l'état solide.Mots clés : cadmium, 1,3-thiazolidine-2-thionate, diffraction des rayons X, RMN du 113 Cd à l'état solide, composé standard pour la RMN du 113 Cd.[Traduit ...

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The reaction of [Os₃(CO)₁₀(MeCN)₂], with heterocyclic thioamides. The crystal and molecular structure of [Os₃(µ-H)(CO)₁₀(µ-SCNCH₂CH₂S)]

Cited by 48 publications

References 1 publication

Investigation on coordination modes of organotin(IV) complexes with 6-thiopurine and related ligands

Investigation on coordination modes of organotin(IV) complexes with 6-thiopurine and related ligands

Darstellung und NMR‐spektroskopische Charakterisierung von konfigurationsstabilen Diorganozinn(IV)‐Komplexen RPhSnL mit Zinn als chiralem Zentrum

A synthetic, structural, and¹¹³Cd NMR study of cadmium complexes of 1,3-thiazolidine-2-thionate, including the structures of Cd(C₃H₄NS₂)₂, (Cd(C₃H₄NS₂)₂(C₅H₅N)₃·C₅H₅N, and (Ph₄P)₂[I₂Cd(µ-C₃H₄NS₂)₂CdI₂]

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The reaction of [Os3(CO)10(MeCN)2], with heterocyclic thioamides. The crystal and molecular structure of [Os3(µ-H)(CO)10(µ-SCNCH2CH2S)]

Cited by 48 publications

References 1 publication

Investigation on coordination modes of organotin(IV) complexes with 6-thiopurine and related ligands

Investigation on coordination modes of organotin(IV) complexes with 6-thiopurine and related ligands

Darstellung und NMR‐spektroskopische Charakterisierung von konfigurationsstabilen Diorganozinn(IV)‐Komplexen RPhSnL mit Zinn als chiralem Zentrum

A synthetic, structural, and113Cd NMR study of cadmium complexes of 1,3-thiazolidine-2-thionate, including the structures of Cd(C3H4NS2)2, (Cd(C3H4NS2)2(C5H5N)3·C5H5N, and (Ph4P)2[I2Cd(µ-C3H4NS2)2CdI2]

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The reaction of [Os₃(CO)₁₀(MeCN)₂], with heterocyclic thioamides. The crystal and molecular structure of [Os₃(µ-H)(CO)₁₀(µ-SCNCH₂CH₂S)]

A synthetic, structural, and¹¹³Cd NMR study of cadmium complexes of 1,3-thiazolidine-2-thionate, including the structures of Cd(C₃H₄NS₂)₂, (Cd(C₃H₄NS₂)₂(C₅H₅N)₃·C₅H₅N, and (Ph₄P)₂[I₂Cd(µ-C₃H₄NS₂)₂CdI₂]