| | 1 | Author
| BemdW. Rackm, SergeiV. Ponomarevb | Requires 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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| default:Reihe_B/54/ZNB-1999-54b-0705.pdf | | | | Identifier
| ZNB-1999-54b-0705 | | | | Volume
| 54 | |
| 2 | Author
| Z. Naturforsch | Requires 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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| default:Reihe_B/54/ZNB-1999-54b-0018.pdf | | | | Identifier
| ZNB-1999-54b-0018 | | | | Volume
| 54 | |
| 3 | Author
| Z. Afar Iqbalc, H.E J | Requires 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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| default:Reihe_B/54/ZNB-1999-54b-0415.pdf | | | | Identifier
| ZNB-1999-54b-0415 | | | | Volume
| 54 | |
| 4 | Author
| Cornelia Borgmann, Christian Limberg, Läszlö Zsolnai, Katja Heinze | Requires 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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| default:Reihe_B/54/ZNB-1999-54b-0473.pdf | | | | Identifier
| ZNB-1999-54b-0473 | | | | Volume
| 54 | |
| 5 | Author
| Petra Prokop, Rainer Richter, Lothar Beyer | Requires 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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| default:Reihe_B/54/ZNB-1999-54b-0849.pdf | | | | Identifier
| ZNB-1999-54b-0849 | | | | Volume
| 54 | |
| 6 | Author
| BerndW. Rackmeyer1 ', Saqib Alib, Wolfgang Storch0, Martina Vosteenc | Requires 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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| default:Reihe_B/54/ZNB-1999-54b-1165.pdf | | | | Identifier
| ZNB-1999-54b-1165 | | | | Volume
| 54 | |
| 7 | Author
| KaterynaE. Gubina3, VladimirA. Ovchynnikova, VladimirM. Amirkhanov3, Tatyana Yu, ViktorV. Sliva3, Tadeusz Skopenko3, Henryk Glowiakb, Kozlowskib | Requires 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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| default:Reihe_B/54/ZNB-1999-54b-1357.pdf | | | | Identifier
| ZNB-1999-54b-1357 | | | | Volume
| 54 | |
| 8 | Author
| Dilip Kumar Dey, MrinalKanti Dasa, Heinrich Nöth | Requires 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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| default:Reihe_B/54/ZNB-1999-54b-0145.pdf | | | | Identifier
| ZNB-1999-54b-0145 | | | | Volume
| 54 | |
| 9 | Author
| Christoph Elschenbroich, Steffen Voß, Klaus Harms | Requires 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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| default:Reihe_B/54/ZNB-1999-54b-0209.pdf | | | | Identifier
| ZNB-1999-54b-0209 | | | | Volume
| 54 | |
| 10 | Author
| Karin Dölling, Kurt Merzweiler, Christoph Wagner, Horst Weichmann | Requires 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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| default:Reihe_B/54/ZNB-1999-54b-0293.pdf | | | | Identifier
| ZNB-1999-54b-0293 | | | | Volume
| 54 | |
| 12 | Author
| M. Ax Herberhold, U. Do Steffl, BerndW. Rackmeyer | Requires 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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| default:Reihe_B/54/ZNB-1999-54b-0057.pdf | | | | Identifier
| ZNB-1999-54b-0057 | | | | Volume
| 54 | |
| 13 | Author
| A. Rto, M. Aaninena, R. Ené, T. B. Oeré, Tristram Chivers0, M. Asood Parvezc | Requires cookie* | | | Title
| Preparation and X-Ray Structure of 4-N,N'-Bis(trimethylsilyl)- amino-3,5-diisopropylphenylselenium Trichloride | | | | Abstract
| The reaction of SeCU or SeCF with /V,/V'-bis(trimethylsilyl)-2,6-diisopropylaniline occurs not at the nitrogen atom but by electrophilic aromatic substitution at C-4 of the phenyl ring to give [(CH3)3Si]2NC6 H2('Pr:)SeCl3, which crystallizes as the chloro-bridged dimer in the triclinic system, space group P i, a -10.2598(17), b = 13.665(3), c = 9.7838(10) A, a = 90.056(13), ß = 102.439(11), 7 = 70.922(14)°, V = 1262.3(4) A \ Z = 1. The dimer contains an essentially planar CUSe^-Cl^SeCU unit, with trans apical (Me3SihNC6H2('Pr)2 groups, resulting in approximately square pyramidal geometry at Se. The bridging Se-Cl distances are unequal at 2.587(2) and 2.749(2) A. | | | |
Reference
| Z. Naturforsch. 54b, 1170—1174 (1999); received April 22 1999 | | | |
Published
| 1999 | | | |
Keywords
| Crystal Structure, 2, 6-Diisopropylaniline, Aryl Selenium Trichloride, Bridging Chloride, NMR Data | | | |
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| default:Reihe_B/54/ZNB-1999-54b-1170.pdf | | | | Identifier
| ZNB-1999-54b-1170 | | | | Volume
| 54 | |
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