594-27-4Relevant articles and documents
Hypercoordinate aryltrialkylsilanes and -stannanes and their use in the synthesis of homodinuclear organometallic complexes with a 1,4-phenylene bridge
Steenwinkel, Pablo,Jastrzebski, Johann T. B. H.,Deelman, Berth-Jan,Grove, David M.,Kooijman, Huub,Veldman, Nora,Smeets, Wilberth J. J.,Spek, Anthony L.,Van Koten, Gerard
, p. 5486 - 5498 (1997)
New mono- and dinuclear aryltrialkylsilanes and -stannanes [Me3M{C6H3(CH2NMe2) 2-2,6}] (M = Si (5), Sn (6)) and [(Me3M)2-1,4-{C6(CH2NMe 2)4-2,3,5,6}] (M = Si (9), Sn (10)) have been prepared from transmetalation reactions of dimeric [Li{C6H3(CH2NMe2)2-2,6}]2 and new polymeric [Li2-1,4-{C6(CH2NMe2) 4-2,3,5,6}]∞ with (trimethylsilyl)trifluoromethanesulfonate or trimethyltin chloride. The X-ray crystal structures of dinuclear 9 and 10 have been determined and in the molecular geometries found the central 1,4-phenylene dimetalated aryl ligand system provides bidentate C,N-coordination to silicon in 9 and terdentate pseudofacial N,C,N′-coordination to tin in 10. Reactions of the newly prepared silanes 5 and 9 and stannanes 6 and 10 with diverse palladium(II) and platinum(II) substrates afford organometallic products arising from both aryl and methyl group transfer. For example, the reaction of dinuclear stannane 10 (or dinuclear silane 9) with palladium(II) species gives the bimetallic complex [(PdCl)2-1,4-{C6(CH2NMe2) 4-2,3,5,6}] (15), whereas its reaction with [PtCl2(COD)] (COD = cycloocta-1,5-diene) or Me3SnCl gives the ionic tin(IV) species [(Me2-Sn)2-1,4-{C6(CH2NMe 2)4-2,3,5,6}]2+(X-)2 with X being Cl (18a) or Me3SnCl2 (18b). The X-ray crystal structure of 18b has been determined and the molecular geometry found shows that the central dimetalated aryl ligand system provides terdentate meridional N,C,N′-coordination to both tin centers.
Polysulfonylamine XXXV. Synthese, Roentgenstrukturanalysen und hochaufgeloeste Festkoerper-NMR-Spektren der ionischen Organozinn(IV)-dimesylamide und 2
Blaschette, Armand,Hippel, Ilona,Krahl, Juergen,Wieland, Elke,Jones, Peter G.,Sebald, Angelika
, p. 279 - 297 (1992)
(4) was prepared by treating Me3SnN(SO2Me)2 (1) with liquid ammonia; single crystals suitable for X-ray diffraction were grown from a solution in liquid ammonia by slow evaporation of the solvent at -42 deg C. 2 (5) was obtained from dimethyl sulfoxide and Me2Sn2 or 1 in refluxing CCl4, the co-product in the latter case being SnMe4.The crystallographic data at -95 deg C are for 4: monoclinic, space group P21/c, a 650.3(2), b 1464.7(3), c 1479.6(4) pm, β 94.63(2) deg, U 1.4046 nm3, Z=4; for 5: triclinic, space group P, a 818.3(2), b 986.6(2), c 1119.9(3) pm, α 79.10(2), β 77.51(2), γ 77.58(2) deg, U 0.8524 nm3, Z=1.The structure refinement of 4 was based on 3092 reflections with F>4?(F) to give R=0.018.For 5, refinement using 3579 reflections with F>4?(F) yielded R=0.021.The crystals of both compounds consist of discrete (MeSO2)2N- anions and Me3Sn(NH3)2+ or Me2Sn(DMSO)42+ cations, respectively.The structures of the anions are similar to those observed in other ionic dimesylamides.In the cation of 4, the tin atom has an axially distorted trigonal-bipyramidal environment with apical NH3 molecules (Sn-N 232.8 and 238.3, Sn-C 211.7-212.4 pm, N-Sn-N 179.2, C-Sn-C 118.1-122.1, N-Sn-C 88.0-91.3 deg).The tin atom in the centrosymmetric cation of 5 displays trans-octahedral geometry with four DMSO molecules bonded through their oxygen atoms (Sn-C 211.4, Sn-O 219.9 and 221.4 pm, (O-Sn-O)cis 88.9 and 91.1, O-Sn-C 86.8-93.2 deg).The oxygen centres of the sulfoxide ligands are sp2-hybridized with Sn-O-S 121.8 and 123.1 deg, S-O 154.4 and 155.4 pm. 5 is the first example of a structurally characterized tin(IV)-sulfoxide complex in which four sulfoxide ligands are coordinated to a single tin centre. 13C, 15N and 119Sn CP/MAS NMR spectra of solid 4 and 5 agree very well with the X-ray diffraction results.In both cases, the isotropic 119Sn chemical shifts and their tensorial properties support the nearest-neighbours-environment as shown by crystallography.The slight inequivalences of the NH3 and DMSO ligands, respectively, are mirrored in the 15N and 13C CP/MASS spectra of 4 and 5.The 119Sn CP/MAS spectrum of 4 is complicated by the simultaneous presence of scalar and quadrupolar coupling of two inequivalent 14N nuclei with 119Sn.
Vibrational Spectra and Normal Coordinate Calculations for Trimethylstannane
Imai, Yoshika,Aida, Koyo
, p. 999 - 1002 (1982)
The infrared and Raman spectra of trimethylstannane and its deuterated analogues were obtained.Assignments for all the fundamentals except internal torsions were made and normal coordinate calculations were carried out to confirm the proposed assignments.
Ultrasonic Effects on Electroorganic Processes. Part 9. Current Efficiency and Product Selectivity in the Electroreduction of Alkyl Halides to Alkyl Stannanes at a Reactive Tin Cathode
Atobe, Mahito,Nonaka, Tsutomu
, p. 397 - 402 (1998)
The ultrasonic effects on the electroreduction of methyl and allyl halides (RX) to the corresponding stannanes (R3SnSnR3 and R4Sn) at a reactive (consumable) tin cathode were examined. The current efficiency and product selectivity for the reduction were found to be greatly affected by ultrasonic irradiation. For instance, the selectivity for (CH3)3SnSn(CH3)3 to (CH3)4Sn from CH3I was significantly increased under irradiation. This fact is rationalized as being due to because the intermediate species [(CH3)3Sn·] formed by the primary one-electron reduction of CH3I are activated for their coupling by mobilization on/from the cathode surface under irradiation. On the other hand, the ultrasonic effects on the reduction of CH3Br and C3H5Br seemed to be slightly different from those in the reduction of CH3I.
The first 1,1′-Digallylferrocene and a rodlike, polymeric donor-acceptor complex: Synthesis, properties, and structure of [Fe(η5-C5H4GaMe2)2] n and [Fe(η5-C5H4GaMe2)2(C 12H8N2)]n
Althoff, Alexander,Jutzi, Peter,Lenze, Norman,Neumann, Beate,Stammler, Anja,Stammler, Hans-Georg
, p. 3018 - 3022 (2002)
The reaction of 1,1?-bis(trichlorostannyl)ferrocene with trimethylgallium results in the formation of Fe(C5H4GaMe2)2 (1), the first digallylferrocene. An X-ray crystal structure analysis of 1 reveals a polymeric structure. NMR data confirm a monomeric structure of [1-2 donor] in donor solvents. The reaction of 1 with phenazine results in the formation of the supramolecular polyferrocene [1·phenazine]n. Its rodlike structure is proven by X-ray crystallography.
Group 13 and 14 alkyl derivatives of the imido-nitrido metalloligand [{Ti(η5-C5Me5)(μ-NH)} 3(μ3-N)]
Garcia-Castro, Maria,Martin, Avelino,Mena, Miguel,Yelamos, Carlos
, p. 408 - 416 (2007)
The reactivity of the imido-nitrido trinuclear complex [{Ti- (η5-C5Me5)(μ-NH)}3(μ 3-N)] (1) toward alkyl derivatives of group 13 and 14 elements has been investigated. Treatment of 1 with trialkyl der
SYNTHESE VON SULFINSAEUREIMIDAMIDOSTANNANEN
Haenssgen, Dieter,Steffens, Reinhard
, p. 53 - 60 (1982)
N-Lithiomethanesulfinicacidimide amides of the general composition MeS(NR)NRLi (II) are prepared by addition of methyllithium to sulfur diimides RN=S=NR (I) (R=t-Bu or SiMe3).The corresponding reaction with Me3Sn-N=S=N-SnMe3 yields the N-lithio salt (Me3S
Cleavage reactions of group IVa metal-metal bonds
Shaw III, C. Frank,Allred
, p. 1340 - 1343 (1971)
The reactions of hexamethyldimetal compounds containing unsymmetrical metal-metal bonds with iodine monochloride, hydrogen chloride, and trifluoroiodomethane are reported. The hypothesis that products of similar reactions are determined by polarity of the
The reactivity of metal-metal bonds. II. The tin-manganese bond
Clark,Tsai
, p. 1407 - 1415 (1966)
The reactions of trimethyltinpentacarbonylmanganese with tetrafluoroethylene, trifluoroethylene, chlorotrifluoroethylene, and ethylene are described. Only with tetrafluoroethylene is an adduct, namely, (CH3)3SnCF2CF2Mn(CO)5, obtained, although trimethyltin fluoride and fluorocarbon-carbonylmanganese products are also formed. With trifluoroethylene and chlorotrifluoroethylene, trimethyltin halides and fluorovinylpentacarbonylmanganese compounds are produced, although in the latter case perfluoroacryloylpentacarbonylmanganese, CF2=CFCOMn(CO)5, is a major product. Ethylene does not cleave the Sn-Mn bond, but rather displaces carbon monoxide to form (CH3)3SnMn(CO)4(π-C2H 4). The spectroscopic properties of the new compounds are discussed.
Octahedral Bis(phenoxy-imine)tin(IV) alkyl complexes: Synthesis, characterization, and reactivity toward ionizing species and ethylene
Annunziata, Liana,Pappalardo, Daniela,Tedesco, Consiglia,Pellecchia, Claudio
, p. 1947 - 1952 (2005)
The synthesis of new organotin compounds of the general formula L 2SnR2 (L = N-(3-tert-butylsalicylidene)-2,3,4,5,6- pentafluoroaniline; R = CH3 (1), n-C4H9 (3)) and L′2SnR2 (L′ = Ar-(3-tert- butylsalicylidene)aniline; R = CH3 (2), n-C4H9 (4)) is described herein. The compounds were characterized by 1H, 13C, and 119Sn NMR in solution; in some cases a fluxional behavior was observed by variable-temperature experiments. Characterization by single-crystal X-ray diffraction analysis has been obtained for compounds 1, 2, and 4. The reactivity of the synthesized compounds toward ionizing agents was studied by an NMR-tube reaction. Compounds 2 and 4 underwent an alkyl abstraction reaction with the carbenium salt [C(C6H5) 3]+[B(C6F5)4] . The obtained cationic species exhibited some activity in the oligomerization of ethylene under mild conditions, producing short-chain oligomers, with saturated end groups and methyl branches.
