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1Author    BemdW. Rackm, SergeiV. PonomarevbRequires cookie*
 Title    Decomposition of Ethoxyethynyl(trimethyl)tin -Studied by 119Sn and 13 C NMR Spectroscopy  
 Abstract    A The thermally induced decomposition o f ethoxyethynyl(trimethyl)tin (1) was studied by ll9Sn NM R which revealed the formation o f bis(trimethylstannyl) ketene (2) as the major product, bis(trimethylstannyl) acetic acid ethyl ester (3) as a minor product, and a small amount o f tetramethyltin (4). Full NM R data sets, including coupling constants and isotope induced chemical shifts 1 _ \ 12 13C(1 l9Sn) are provided for 1 -3 . The first example o f ultra-high resolution " 9Sn NM R is shown. 
  Reference    Z. Naturforsch. 54b, 705 (1999); received February 23 1999 
  Published    1999 
  Keywords    lkynes, Ketenes, Tin, NMR Data 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0705.pdf 
 Identifier    ZNB-1999-54b-0705 
 Volume    54 
2Author    0. Ch, Ch, Joseph Grobe, Nikolaos VoulgarakisRequires cookie*
 Title    Atran-analoge Verbindungen des Typs Me2Si-Y-M Me2(OCH2CH2)NMe m I I V 1 ) Atrane Analogous Compounds of Type Me2Si-Y-M'Me2(OCH2CH2)NMe ! I (I) 0 CH 2 CH 2  
 Abstract    Heterocyclic ring compounds of type I (compounds 9 and 10) have been prepared by condensation reactions of a,co-difunctional derivatives XMe2SiCH2M'Me2X (X = Cl, NMe2; M' — Si, Sn) with N-methyldiethanolamine using the "Dilution Principle". The starting compounds XMe2SiCH2M'Me2X are obtained by reacting XMe2SiCH2MgCl with ClM'Me2X (Scheme, Abb. 1). The existence of transanular N-*Si or N->M' interactions depends on the N-M distance and the acidity of the acceptor atoms. In order to clarify the weight of these factors acyclic analoga of compounds 9 and 10 have been prepared. In den letzten 20 Jahren wurden verschiedene anorganische Ester des Di-bzw. Triethanolamins sowie Derivate des Typs R"_3M(OCH2CH2)3N und R"_2M(OCH2CH2)2NR 
  Reference    Z. Naturforsch. 38b, 269—279 (1983); eingegangen am 23. August 1982 
  Published    1983 
  Keywords    Silatrane, Stannatrane, Transanular N-^M-Interaction, NMR Data 
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 TEI-XML for    default:Reihe_B/38/ZNB-1983-38b-0269.pdf 
 Identifier    ZNB-1983-38b-0269 
 Volume    38 
3Author    M. Arkus Wieber, Stefan Lang, StefanRalph Rohse, Christian Habersack, BurschkaRequires cookie*
 Title    Synthese und Kristallstruktur von Triphenyltelluroniumsulfid Synthesis and Crystal Structure of Triphenyltelluroniumsulfide  
 Abstract    The synthesis of triphenyltelluroniumsulfide (Ph3TeS)4 is described together with a NMR-spectroscopic characterization. The structure of the title compound was determined by single crystal X-ray diffraction. Crystals of triphenyltelluroniumsulfide are triclinic (space group P I) with the cell parameters a = 1178.0(3) pm. b = 1295.8(6) pm. c = 1298.7(4) pm, a = 77.67(3)°, ß = 82.18(2)°, y = 66.00(2)° (V = 1766(1) x 106 pm3) and Z = 2. The compound appears to form a step-like structure of two [Ph3TeS]2 units and crystallizes with two m ole­ cules of CH2C12 per unit cell. 
  Reference    Z. Naturforsch. 49b, 1654—1658 (1994); eingegangen am 5. Mai 1994 
  Published    1994 
  Keywords    Triphenyltelluroniumsulfide, Synthesis, NMR Data, Crystal Structure, Secondary Bonding 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-1654.pdf 
 Identifier    ZNB-1994-49b-1654 
 Volume    49 
4Author    Z. NaturforschRequires cookie*
 Title    R eaction o f 9-B orabicyclo[3.3.1]nonane with N-Trim ethylsilylam ines -C leavage o f the N-Si or N -H Bond  
 Abstract    The reaction of dimeric 9-borabicyclo[3.3.1]no-nane 1 with N-trimethylsilyl-aniline 2 affords 9-anilino-9-borabicyclo[3.3.1]nonane 5 by elimina­ tion of trimethylsilane. In contrast, 1 reacts with the N-trimethylsilyl-2-aminopyridines 3 and 4 se­ lectively by elimination of H 2 to give the corre­ sponding N-trimethylsilyl-aminoboranes 6 and 7. The latter reactions proceed via formation of bo-rane-pyridine adducts. 
  Reference    Z. Naturforsch. 53b, 393—395 (1998); received December 29 1997 
  Published    1998 
  Keywords    Aminoborane, Aminosilane, Boron, Pyridine, NMR Data 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0393_n.pdf 
 Identifier    ZNB-1998-53b-0393_n 
 Volume    53 
5Author    Max Herberhold, Silke Gerstmann, Bernd WrackmeyerRequires cookie*
 Title    Tetrakis(sulfurdiimido)silane, -germane and -stannane  
 Abstract    Two tetrakis(sulfurdiimido)silanes [Si(NSNR)4 (R = rBu la, SiMe3 lb)], two germanes [Ge(NSNR)4 (R = rBu 2a, SiMe3 2b)] and one stannane [Sn(NSN?Bu)4Sn 3a] were prepared and characterised by 'H, l3C, i5N, 29Si and ll9Sn NMR spectroscopy in solution, and 3a was also studied in the solid state by 1 l9Sn CP/MAS NMR. Whereas la,b and 2a,b are monomeric in solution, the 119Sn NMR data suggest that 3a is associated both in solution and in the solid state, and that the tin atoms are hexa-coordinated. The attempted stepwise synthesis of la by using one, two, three or four equivalents of K[(NSN)rBu] led to mixtures of la with Cl3Si(NSNrBu) 4a, Cl2Si(NSN/Bu)2 5a, and ClSi(NSNfBu)3 6a. Only one sulfurdiimido ligand of the silane la reacted with hexachlorodisilane by oxidative addition and cleavage of the Si-Si bond to give the new heterobicyclic derivative 7a which is held together by two different coordinative N-Si bonds. 
  Reference    Z. Naturforsch. 53b, 573—580 (1998); received March 30 1998 
  Published    1998 
  Keywords    Silicon, Germanium, Tin, Sulfur Diimides, Heterocycles, NMR Data 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0573.pdf 
 Identifier    ZNB-1998-53b-0573 
 Volume    53 
6Author    Michael Schmidt, Hubert SchmidbaurRequires cookie*
 Title    Ligand Redistribution Equilibria in Aqueous Fluoroberyllate Solutions  
 Abstract    The composition of aqueous fluoroberyllate solutions has been studied by 9Be and l9F NMR spectroscopy for various ratios of the beryllium and fluorine concentrations, and at different pH values. The equilibrium constants have been determined for the ligand exchange processes, which involve the species [Be(OH2)4]2+, [BeF(OH2)3]+, [BeF2(OH2)2], [BeF3(OH2)]_ , and [BeFzi]2 -. These equilibria are shifted towards [BeF4]2_ at high pH. No polynuclear fluo­ roberyllates have been detected. The fluoride exchange between the individual species is slow on the NMR time scale at room temperature, and separate sharp signals with the expected multiplicity are therefore recorded. Calculated 9Be chemical shifts are in good agreement with experimental data. 
  Reference    Z. Naturforsch. 53b, 1294—1300 (1998); received July 17 1998 
  Published    1998 
  Keywords    Fluoroberyllates, Beryllium Fluoride, Ligand Redistribution, NMR Data 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-1294.pdf 
 Identifier    ZNB-1998-53b-1294 
 Volume    53 
7Author    Z. NaturforschRequires cookie*
 Title    The Stereochemistry of Chloro-bis(N-morpholino)phenylsilane  
 Abstract    Treatment of phenyltrichlorosilane with an excess of morpholine and N-lithium-morpholide in pentane/toluene affords only the disubstitution product Cl(Ph)Si(M or)2 with Mor = 0 (C H 2C H :)2N-. The third halogen atom is not replaced owing to sterical hindrance. The title compound crystallizes with two independent molecules in the unit cell. These two molecules can be classified as enantiomers, because a disrotatory twist of the two morpholino ligands away from the potential mirror plane induces a chiral conformation. In benzene solution there is racemization owing to completely free rotation, chair/boat interconversion, and nitrogen inversion of the morpholino groups on the NMR time scale, but all CH 2 protons remain anisochronous (diastereotopic). 
  Reference    (Z. Naturforsch. 54b, 18—20 [1999]; received October 15 1998) 
  Published    1999 
  Keywords    Silylamines, Aminosilanes, Symmetry, NMR Data, Crystal Structure 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0018.pdf 
 Identifier    ZNB-1999-54b-0018 
 Volume    54 
8Author    Z. Afar Iqbalc, H.E JRequires cookie*
 Title    Isoperadione: A New Triterpenoid from Salvia bucharica  
 Abstract    V iqar U d d in A h m a d 3 *, M uham m ad Z ah id c, M uham m ad Shaiq A li3, Z ulfiqar A li3, N aseer A lam 3, R asool B akhsh T areenb, M uham m ad A new isomer of peradione (2) named as isoperadione (1) has been isolated along with peradione (2) and perovskone (3) from the hexane soluble part of Salvia bucharica. The structures of 1 -3 were elucidated with the aid of modern spectroscopic techniques. 
  Reference    Z. Naturforsch. 54b, 415—418 (1999); received September 8 1998 
  Published    1999 
  Keywords    Salvia bucharica, Lamiaceae, Triterpenoids, Isoperadione, NMR Data 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0415.pdf 
 Identifier    ZNB-1999-54b-0415 
 Volume    54 
9Author    Cornelia Borgmann, Christian Limberg, Läszlö Zsolnai, Katja HeinzeRequires cookie*
 Title    Syntheses, Structures, and Spectroscopic Properties of Alkoxide, Hydroxide, and Siloxide Complexes with (r73-Allyl)Mo Moieties  
 Abstract    Salts with binuclear anions of the general formula [(?73-C3H4R)(CO)2Mo(^-OR')2(/i-OR")-Mo(CO)2(f?3-C3H4R) r (R = h , R',R" = Me, 2 ; R = CH3, R' = CH(CH3)2, R" = OH, 3; R = CH3, R' = OH, R" = OSiMe3, 4) have been synthesised via reaction of [(r/3-C3H4R)-Mo(CO)2(CH3CN)2(thf)]+BF4_ , 1, with NaOMe, NaO'Pr, and KOSiMe3. All products were characterised spectroscopically and investigated by single crystal X-ray analysis. In the case of 3 low temperature 2D-NMR spectra revealed that the solid state structure is maintained in solution and that the compound shows a trigonal twist-rearrangement at room temperature. 
  Reference    Z. Naturforsch. 54b, 473—481 (1999); received October 28 1998 
  Published    1999 
  Keywords    Molybdenum Complexes, Allyl, Alkoxides, Hydroxides, NMR Data 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0473.pdf 
 Identifier    ZNB-1999-54b-0473 
 Volume    54 
10Author    Petra Prokop, Rainer Richter, Lothar BeyerRequires cookie*
 Title    Zur Reaktion von 2,4-Dioxo-4-ferrocenyl-butansäureethylester mit primären aromatischen Aminen On the Reaction of Ethyl 2,4-Dioxo-4-ferrocenyl-butanoate with Primary Aromatic Amines  
 Abstract    Starting from ethyl 2,4-dioxo-4-ferrocenyl-butanoate (1) a series of new ferrocene derivatives has been prepared. While the reaction with o-phenylene diamine leads to two ferrocene-con­ taining heterocyclic compounds, 4-ferrocenyl-3//-l,5-benzodiazepine-2-carbonic acid ethyl ester (3) and 3-(2-ferrocenyl-2-oxo-ethylidene)-3,4-dihydro-l//-quinoxalin-2-one • H20 (4), reactions with m-and /?-phenylene diamine give both the mono-and disubstituted products 5 -8, respectively. The conversion of 4 by Lawesson's reagent results in 2-ferrocenvl-thieno[2,3-b]quinoxaline (9). The new compounds have been characterized by their 'H , 1 C NMR, and mass spectra. The molecular structures of 4-ferrocenyl-4-oxo-2-phenylamino-but-2-enoic acid ethyl ester 2, and of 4 and 9 have been determined by X-ray crystal structure analysis. 
  Reference    Z. Naturforsch. 54b, 849—857 (1999); eingegangen am 12. März 1999 
  Published    1999 
  Keywords    Ferrocene, /3-Diketones, Enaminoketones, NMR Data, Crystal Structure 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0849.pdf 
 Identifier    ZNB-1999-54b-0849 
 Volume    54 
11Author    BerndW. Rackmeyer1 ', Saqib Alib, Wolfgang Storch0, Martina VosteencRequires cookie*
 Title    2-[N,N-Bis(trimethylstannyl)amino]pyridine and Bis[N-(N-trimethyIsiIyI- 2-aminopyridyI)]dimethyltin -Intramolecular N-Sn Co-ordination  
 Abstract    2-[N,N-Bis(trimethylstannyl)amino]pyridine (1), bis[N-(N-trimethylsilyl-2-aminopyridyl)]-dimethyltin (2) and bis[N-(N-trimethylsilyl-2-amino-3-methyl-pyridyl)]dimethyltin (3) were prepared and characterized by 'H, i3C, l5N, 29Si and ll9Sn NMR spectroscopy. In the case of 1, intramolecular pyridine-N-Sn co-ordination was established by the low temperature ll9Sn NMR spectra which show two resonance signals, one for a penta-co-ordinate and one for a tetra-co-ordinate tin site. In the cases of 2 and 3, intramolecular pyridine-N-Sn co-ordination follows conclusively from l3C, l5N and ll9Sn NMR parameters. In contrast with the known behaviour of the corresponding trimethyltin derivative, the methyl group in 3-position of the pyridine ring does not prevent this type of co-ordination in 3. 
  Reference    Z. Naturforsch. 54b, 1165—1169 (1999); received June 17 1999 
  Published    1999 
  Keywords    Tin, Amines, Pyridine, Co-ordination, NMR Data 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-1165.pdf 
 Identifier    ZNB-1999-54b-1165 
 Volume    54 
12Author    KaterynaE. Gubina3, VladimirA. Ovchynnikova, VladimirM. Amirkhanov3, Tatyana Yu, ViktorV. Sliva3, Tadeusz Skopenko3, Henryk Glowiakb, KozlowskibRequires cookie*
 Title    Carbacylamidophosphates: Structure and Properties of Bis(N,N,-morpholido)-[(N"-morpholido)-carboxamido] phosphate  
 Abstract    The bis(N,N'-morpholido)-[(N"-morpholido)-carboxamido] phosphate: 0 (CH2 CH2)NC(0)-N(H)P(0)[N (CH 2 CH 2)0 ] 2 [HL], has been prepared and characterized by means of IR, 31P and 'H NM R spectroscopy and X-ray diffraction (triclinic, a = 9.282(2), b = 9.308(2), c = 21.341(4) Ä, a = 80.79(3)°, ß = 80.92(3)° 7 = 66.92(3)°, V = 1665.1(6) Ä 3, space group P i, Z = 4 and R = 0.0423, wR2 = 0.1303 for 6774 unique reflections used). The unit cell consists of two independent molecules connected by hydrogen bonds N-H...O=P into non-symmetric dimers. The compound behaves as a HL molecule with a protonation constant corresponding to the -C (0)N (H)P (0)-group of pK = 8.65 as determined by potentiometric studies. 
  Reference    Z. Naturforsch. 54b, 1357—1359 (1999); received March 29 1999 
  Published    1999 
  Keywords    Carbacylamidophosphates, X-Ray Data, NMR Data 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-1357.pdf 
 Identifier    ZNB-1999-54b-1357 
 Volume    54 
13Author    Frank Leßmann3, Lothar Beyer3, Rainer Richter3, Reinhard MeusingerbRequires cookie*
 Title    N-Benzoylthiocarbamoyl Amino Acid Ethyl Esters as Chelate Ligands for Transition Metal Ions  
 Abstract    The reactions of benzoyl isothiocyanate with amino acid ethyl esters (N-butyl glycine ethyl ester, (S)-(-)-proline ethyl ester) give N-benzoylthiocarbamoyl amino acid ethyl esters. Apart from the expected N-benzoylthiocarbamoyl (S)-(-)-proline ethyl ester the racemic N-benzoyl­ thiocarbamoyl (/?)/(S)-proline ethyl ester is formed because of base catalyzed racemization of the educt (5')-(-)-proline ethyl ester during the reaction of (S)-(-)-proline ethyl ester hy­ drochloride with triethylamine. The structures of both compounds were established by X-ray crystal structure analysis and specific optical rotation measurements. The ligands yield neutral 2:1 chelates with Ni , Cu11, Pd11 and Pt11. The carboxylic oxygen atoms are not involved in the chelation. The ligands and the resultant complexes show configurational E/Z isomerism. In the case of the chelates of the racemic N-benzoylthiocarbamoyl (/?)/(5)-proline ethyl ester, additional R/S isomerism is observed as shown by 
  Reference    Z. Naturforsch. 53b, 981—990 (1998); received November 11 1997 
  Published    1998 
  Keywords    Thioureas, Amino Acid Ethyl Esters, Chelates, NMR Data, Crystal Structure 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-0981.pdf 
 Identifier    ZNB-1998-53b-0981 
 Volume    53 
14Author    ViktorP. Balema, Steffen Blaurock, Evamarie Hey-HawkinsRequires cookie*
 Title    Synthesis and Molecular Structure of a Superbulky Tertiary Phosphine: Bis[2-phenyl-l,2-dicarba-c/oso-dodecaboran-l-yl(12)]phenylphosphine  
 Abstract    Bis[2-phenyl-l,2-dicarba-c/oso-dodecaboran-l-yl(12)]phenylphosphine (2) was obtained in 91% yield from phenyldichlorophosphine and two equivalents of l-lithium-2-phenyl-l ,2-dicarba-c/o5o-dodecaborane(12) in ether and characterized by spectroscopy (3IP, 1 B, 'H, l3C NMR; IR) and by X-ray structure determination. 
  Reference    Z. Naturforsch. 53b, 1273—1276 (1998); received May 20 1998 
  Published    1998 
  Keywords    Synthesis, Molecular Structure, X-Ray Data, NMR Data, Phosphine 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-1273.pdf 
 Identifier    ZNB-1998-53b-1273 
 Volume    53 
15Author    Dilip Kumar Dey, MrinalKanti Dasa, Heinrich NöthRequires cookie*
 Title    Synthesis, Spectroscopy and Structure of Diorganotin(IV) Schiff Base Complexes  
 Abstract    Three diorganotin(IV) chelates with a tetradentate Schiff base, H2Vanophen, [FLVanophen = N,N'-l,2-phenylen-bis(3-methoxysalicylideneimine)] of the type R2Sn(Vanophen) (R = Ph: 1; R = rt-Bu: 2; R = Me: 3) have been synthesized by the reaction of R2SnCl2 (R = Ph, n-Bu, Me) and FLVanophen in the presence of triethylamine in benzene. The complexes have been characterised by IR and NMR spectroscopy and by elemental analysis. The <$(' l9Sn) values for the complexes 1 -3 are -543.0, -414.2 and -398.2 ppm respectively, indicating hexacoordinated Sn centers. These have been ascertained by X-ray crystal structure determinations of 1 and 3. The distances between tin and the two axial carbon atoms in each complex differ not significantly [2.17(1) Ä in 1, and 2.100(3) and 2.115(3) A in 3). The C-Sn-C angles for 1 and 3 are 165.9(4)° and 159.96(9)°, respectively. The solution NMR spectra ('H , l3C, 1|ySn) show clearly that the solid state structures are retained in solution. 
  Reference    Z. Naturforsch. 54b, 145—154 (1999); received September 16 1998 
  Published    1999 
  Keywords    Diorganotin(IV) Complexes, FLVanophen, X-Ray Data, Infrared Data, NMR Data 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0145.pdf 
 Identifier    ZNB-1999-54b-0145 
 Volume    54 
16Author    Christoph Elschenbroich, Steffen Voß, Klaus HarmsRequires cookie*
 Title    Metal Complexes of Heteroarenes, X [1]. 7 7 1 -Coordination of Phosphinine: Synthesis and Structure of cis-Dichloro-bis(2,6-dimethyl-4-phenyI-phosphinine)platinum  
 Abstract    C/5-Dichloro-bis(2 ,6 -dimethyl-4 -phenyl-77'-phosphinine)platinum (3) has been prepared by ligand substitution from cis -dichloro(2,5-cyclooctadiene)platinum and characterized by spec­ troscopy ('H , 13C, 31P NMR, IR, UV-Vis), CV and X-ray diffraction (space group P2|/c, a = 14.998, b = 16.540, c -11.506 Ä, a = 7 = 90°, ß = 92.46°, Z = 4). In line with findings for simi­ lar P hybridization states, the Pt-P bond length (221 pm) in 3 equals that in 771 -phosphaalkene Pt complexes and falls short of the respective parameters in Pt phosphane species. The stretching frequencies u^c\ and the bond length Pt-Cl indicate that phosphinines and phosphaalkenes, relative to phosphanes, adopt a lower position on the rram'-influence scale. This gradation is also suggested by the coupling constants 1 J (195Pt,31P). 
  Reference    Z. Naturforsch. 54b, 209—213 (1999); received September 9 1998 
  Published    1999 
  Keywords    Phosphinine Complex, Platinum, X-Ray Data, NMR Data, frans-Influence 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0209.pdf 
 Identifier    ZNB-1999-54b-0209 
 Volume    54 
17Author    Karin Dölling, Kurt Merzweiler, Christoph Wagner, Horst WeichmannRequires cookie*
 Title    3-Triorganostannyl-N-diphenylmethylen-alaninestern Synthesis, Structure and Reactivity o f 3-Triorganostannyl-N-diphenylmethylene- alanine Esters  
 Abstract    The deprotonation of N-diphenylmethylene-glycine esters, obtained from glycine ester hy­ drochlorides and benzophenone imine, and reaction of the resulting carbanions with iodo-methyl triorganostannanes gives the 3-triorganostannyl-N-diphenylmethylene-alanine esters Me2RSnCH2CH(N=CPh2)COOR' (la -e\ R = Me, 'Bu; R' = Me, Et, 'Bu, Bz). These title compounds are transformed into their tin monochlorides MeR(Cl)SnCH2CH(N=CPh2)COOR' (2a -e) by a redistribution reaction with Me2SnCl2. IR and NMR data and the crystal structure of Me2(Cl)SnCH2CH(N=CPh2)COOEt (2b) reveal for 2a -e an intramolecular coordination of the ester C = 0 group at the tin atom. Mild two-phase hydrolysis of la -e with IN HC1 gives the 3-triorganostannyl-alanine ester hydrochlorides Me2RSnCH2CH(NH 2)COOR' • HC1 (3a -e). The transformation of 3a -e into the corresponding alanine esters Me2RSnCH2CH (N H 2)COOR' (4a -e) could be realized with NH3 in chloroform. 4a -e are of limited thermal stability. 
  Reference    Z. Naturforsch. 54b, 293—299 (1999); eingegangen am 10. November 1998 
  Published    1999 
  Keywords    Stannyl Alanine Ester Derivatives, Intramolecular Pentakoordination, NMR Data, Crystal Structure 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0293.pdf 
 Identifier    ZNB-1999-54b-0293 
 Volume    54 
18Author    ThomasP. Brauna, PaulA. Gutsch, Hans ZimmerRequires cookie*
 Title    Complexes of N-Aryltriphenylphosphinimines with Mercury(II) Halides  
 Abstract    The synthesis, IR and '' P NMR spectra of the complexes of various N-aryltriphenylphosphin-imines with some mercury dihalides as well as the corresponding phosphonium salts are reported. It is shown by an X-ray crystal structure analysis of the complex of the unsubstituted phosphinimine with HgCb that in the solid state these complexes form dimers via two Hg --/W 2-Cl--Hg bridges. 
  Reference    Z. Naturforsch. 54b, 858—862 (1999); received December 30 1998 
  Published    1999 
  Keywords    Phosphinimines, Mercury Halide Complexes, Crystal Structure, NMR Data, X-Ray Data 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0858.pdf 
 Identifier    ZNB-1999-54b-0858 
 Volume    54 
19Author    Nils Wiberg, Angelika Wörner, Hans-Wolfram Lerner, Konstantin Karaghiosoff1, Heinrich Nöth1Requires cookie*
 Title    Darstellung  
 Abstract    , Struktur und Reaktivität des Pentaphosphids (/Bu3Si)3P5Na2 und des Pentaphosphans (fBu3Si)3P5 [2] Supersilyl Compounds of Phosphorus, V [1]. Preparation, Structure, and Reactivity of the Pentaphosphide (?Bu3Si)3P5Na2 and the Pentaphosphane (?Bu3Si)3P5 [2] The orange THF adduct (fBu3Si)3 P5Na2(THF)4 of the pentaphosphide (rBu3Si)3P5Na2 (3) has been prepared, (i) by protolysis of the tetraphosphide (?Bu3Si)2P4Na2(THFj;! (2) with CF3C 0 2H in THF (molar ratio 2 : 1) , (ii) by dissolving crystalline 2 in toluene, and (iii) by the reaction of P4 with /Bu3 SiNa(THF)2 in benzene (molar ratio 1 : 4). According to an X-ray structural analysis, the THF adduct of 3 contains a P3 ring with two PNa(Si?Bu3) substituents in cis position and one SifBu3 substituent in trans position to the former groups. The protolysis of 3 with CF3C 0 2H leads to the pentaphosphane P5 H2(SifBu3) 3 (9), the silylation of 3 with Me2SiCl2 to the pentaphosphane P5(SiMe2)(Si?Bu3) 3 (10), and the oxidation of 3 with C2(CN)4 to the pentaphosphane P5 (Si/Bu3) 3 (5). The structures of 3,5,9, and 10 have been assigned from 1|P and ~4Si NMR data. The pentaphosphane 5 contains a hitherto unknown Ps backbone of a P3 ring anellated with a P4 ring. Supersilylverbindungen des Phosphors, V [1]. 
  Reference    Z. Naturforsch. 53b, 1004—1014 (1998); eingegangen am 17. April 1998 
  Published    1998 
  Keywords    Silicon, Phosphorus, Supersilyl, Oligophosphides and -phosphanes, NMR Data, X-Ray Data 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-1004.pdf 
 Identifier    ZNB-1998-53b-1004 
 Volume    53 
20Author    M. Ax Herberhold, U. Do Steffl, BerndW. RackmeyerRequires cookie*
 Title    l,3-Distanna-2-phospha-[3]ferrocenophanes -Synthesis, Reactivity and NMR Spectroscopic Properties  
 Abstract    -organo(R)-l,3-distanna-2-phospha-[3]ferrocenophanes [R = Me (2a), rBu (2b), CöH i i (2c), Ph (2d)] and one arsa-analogue 2d(As) were obtained from the reaction of l,l'-bis(chlorodim ethylstannyl)ferrocene 1 with either bis(trimethylsilyl)methylphosphane or the dilithio derivatives, Li2PR and Li^AsPh, respectively. All compounds 2 react with chalco-gens (oxygen, sulfur, selenium) by cleavage of the Sn-P bonds and formation of the known l,3-distanna-2-chalcogena-[3]ferrocenophanes. In contrast, 2d traps pentacarbonylmetal frag­ ments [M(CO)5] to give the stable phosphane complexes [M = Cr (4d), Mo (5d), W (6d)]. The l,l'-bis(diorganophosphanostannyl)ferrocenes [R = fBu (3b), Ph (3d)] were prepared for comparison of NMR data. The ferrocenophanes 2 are fluxional with respect to fast movement of the cyclopentadienyl rings which induces inversion at the pyramidal phosphorus atom. This dynamic process is slow in the cases of 2d(As) and of the pentacarbonyl complexes 4d -6d. All new compounds were characterised by 'H , i3C, 31P and 1 l9Sn NMR spectroscopy. Various 2D heteronuclear shift correlations {e.g. 11P /1H and ll9Sn/'H) were carried out for the com ­ pounds 2 and also for non-cyclic derivatives such as bis(trimethylstannyl)phenvlphosphane and -arsane in order to determine absolute signs of coupling constants [e.g. 7(n S n,''P) > 0 and 2J(] l9Sn,' l7Sn) < 0]. The NM R data suggest that the molecular frameworks of the ferroceno­ phanes 2 are not particularly strained. 
  Reference    (Z. Naturforsch. 54b, 57—62 [1999]; received July 28 1998) 
  Published    1999 
  Keywords    Ferrocene, Tin, Phosphorus, NMR Data, Coupling Signs l, l, 3, 3-Tetramethyl-2 
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 Identifier    ZNB-1999-54b-0057 
 Volume    54 
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