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1986[X]
1Author    R. Ajib, Lai De, Heinrich VahrenkampRequires cookie*
 Title    Synthesen neuer Fe—P-Käfigverbindungen Syntheses of New Fe —P Cage Compounds  
 Abstract    Four reaction types were used with the aim of obtaining new cage com pounds o f com position F e v(C O)v(P R). with R = M e, Ph. Tol; oxidation of the com pounds Fe2(C O)A(P H R)2. photolysis thereof, reaction betw een RPC12 and Fe2(C O)x:_ , and reaction betw een P —Cl containing iron com plexes and F e(C O)42" . Besides several known products, e.g. F e,(C O)y(P R)2 or F e4(C O)M(P R)2, and derivatives of the Fe2(C O)ft(P R X)2 butterfly type com plexes, the new octabisvalene shaped com pounds Fe4(C O)I2(P R)4 with R = M e. Ph. Tol were obtained and confirm ed by a crystal structure analysis for R = Me. Side products of the oxidative conversions were Fe4(C O),2(P 2M e2) (M e P -C 2H 4-P M e) and Fe4(C O)12(P2T ol2)(P H T ol)2 which can be derived from the octabisvalene type. Side products o f the irradiative conversions were F e,(C O)s(P P h)(P H P h)2 and (C O),F e(a-P H P h)2F e(C O)(Q ,H 8), the structure o f the latter being proved crystallographically. 
  Reference    Z. Naturforsch. 41b, 273 (1986); eingegangen am 23. O ktober 1985 
  Published    1986 
  Keywords    Iron Phosphorus Cage Com pounds, Synthesis, Structure 
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 Identifier    ZNB-1986-41b-0273 
 Volume    41 
2Author    Rajib Lai, DorisW. Olters, Heinrich VahrenkampRequires cookie*
 Title    Preparation and Reactions of the T etrahedrane Molecule Fe2(CO )6(P-/m -C 4Hg)2  
 Abstract    The F e2P2 tetrahedrane com pound Fe2(CO)f,(P—fBu)2 has been obtained by oxidation of Fe2(C O)A («-PH rB u)2. D ue to its short (206 pm) P —P bond it can be called a diphosphene com ­ plex. In contrast to this the P —P bond is its principal centre o f reactivity: CO , C2H 4, and C2H 2 (with concom itant hydrogenation) are inserted, H 2 and HC1 are added with P —P cleavage, and reductive cleavage occurs with L iB H E t,. The crystal structures of the title com pound and of its CO and C2H 4 insertion products have been determ ined. 
  Reference    Z. Naturforsch. 41b, 283—291 (1986); eingegangen am 23. Oktober 1985 
  Published    1986 
  Keywords    Tetrahedrane M olecule F e2P2, Synthesis, Reactivity 
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 Identifier    ZNB-1986-41b-0283 
 Volume    41 
3Author    HeribertW. Adle, Elke Conradi, Ulrich Müller, Kurt DehnickeRequires cookie*
 Title    Synthese und Kristallstruktur von [W Cl3(N 3S2)(Pyridin)] Synthesis and Crystal Structure of [WCl3(N 3S2)(Pyridine)]  
 Abstract    1,1.1 -T richloro-1 -pyridine-cyclo-1 Ä6-tungsta-3.5-dithia-2,4, 
  Reference    Z. Naturforsch. 41b, 796—798 (1986); eingegangen am 14. Februar 1986 
  Published    1986 
  Keywords    6-triazine, Synthesis, IR Spectra, Crystal Structure 
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 Identifier    ZNB-1986-41b-0796_n 
 Volume    41 
4Author    Gerhard Bremer3, Roland Boeseb, Mustafa Keddoa, Thomas Kruck3Requires cookie*
 Title    Dialkylchalkogenidverbrückte Carbonylzweikernkomplexe des Typs  
 Abstract    [M]2ER2 mit M = {CpMn(CO)2} und {Cr(CO)5}; E = S, Se, Te; R = Me oder R2 = (CH2)3 bzw. (CH2)4; Röntgenstrukturanalyse von [CpMn(CO)2]2S(CH2)3 Dialkylchalcogenide-Bridged Dinuclear Carbonyl Complexes of the Type [M]2ER2 with M = {CpMn(CO)2} and {Cr(CO)5}; E = S, Se, Te; R = Me or R2 = (CH2)3, (CH2)4; X-Ray-Structure Analysis of [CpMn(CO)2]2S(CH2)3 The reaction o f C pM n(C O)2T H F or C r(C O)sT H F with alkylchalcogenides E R 2 (E = S, Se, Te; R = M e or R 2 = (C H 2)3, (C H 2)4) in the molar ratio of 2:1 gives alkylchalcogenide-bridged dinuclear com plexes [C pM n(C O)2]2E R 2 and [C r(C O)5]2E R 2. The heteronuclear com plex C p (C O)2Mn — (u-SM e2) -C r (C O) 5 can be synthesized by reacting C pM n(C O)2SM e2 with C r(C O)5TH F. X-ray structure analysis o f the com pound [CpM n(CO)2]2S(C H 2) 3 dem onstrates the bridging character o f the alkylchalcogenides. 
  Reference    Z. Naturforsch. 41b, 981—986 (1986); eingegangen am 24. Februar/25. April 1986 
  Published    1986 
  Keywords    Synthesis, C halcogenide-Bridged Carbonyl C om plexes, X-Ray 
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 TEI-XML for    default:Reihe_B/41/ZNB-1986-41b-0981.pdf 
 Identifier    ZNB-1986-41b-0981 
 Volume    41 
5Author    Reinhold Tacke3, M. Atthias Linka, H. Artm Ut Joppienb, LudgerE. Rnstc, G. Esellschaft Für, B. Iotechnologische, Forschung, G. B., M. Ascheroder, W. EgRequires cookie*
 Title    Sila-Pharmaka, 35. Mitt  
 Abstract    [1] Sila-Substitution des Akarizids Fenbutatinoxid und einiger seiner Derivate: Synthese und Eigenschaften von Hexakis[(dimethylphenylsilyl)methyl]distannoxan und Tris[(dimethylphenylsilyl)methyl](l,2,4-triazoI-l-yl)stannan Sila-Pharmaca, 35th Communication [1] Sila-Substitution of the Acaricide Fenbutatinoxide and Some of its Derivatives: Synthesis and Properties of Hexakis[(dimethylphenylsilyl)methyl]distannoxane and Tris[(dim ethylphenylsilyl)m ethyl](l,2,4-triazol-l-yl)stannane Starting from SnCl4. hexasila-fenbutatinoxide (2b) [a silicon analogue o f the acaricide fen­ butatinoxide (2b)] and its derivatives lb and 3b were prepared (SnCl4 —> lb —» 2b —> 3b). The distannoxanes 2a and 2b were found to react very easily with H20 to give the corresponding stan n ols4a and 4b, respectively. In solution (Q ,D ,,or CDC13) the equilibria 2 a/2b + H20 ^ 2 4a/4b were observed ('H N M R). With regard to the system 2a/4a/H20 , this observation is at variance with an earlier report in which the sterically bulky neophyl substituents [C6H 5 (C H 3)2C C H 2] are said to prevent the condensation o f 4a to give 2a. — l b —3b were found to be potent acaricides showing activities similar to those o f their carbon analogues l a —3a (test organisms: adult fem ales o f Tetranychus urticae Koch). 
  Reference    Z. Naturforsch. 41b, 1123—1128 (1986); eingegangen am 2. Mai 1986 
  Published    1986 
  Keywords    Sila-Substitution Fenbutatinoxide H exasila-Fenbutatinoxide, A caricides, Syntheses 
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 Identifier    ZNB-1986-41b-1123 
 Volume    41 
6Author    Wolfgang Willing, Ruth Christophersen, Ulrich Müller, K. Urt DehnickeRequires cookie*
 Title    Synthese und Kristallstruktur von VBr2(N3S2)(Pyridin) 2 Synthesis and Crystal Structure of VBr2(N3S2)(pyridine)2  
 Abstract    VBr2(N 3S2)(pyridine)2 is obtained in form o f brown-black, moisture sensitive crystals by the 
  Reference    Z. Naturforsch. 41b, 831 (1986); eingegangen am 22. April 1986 
  Published    1986 
  Keywords    Cyclo-thiazeno Vanadium Dibrom ide D ipyridine, Synthesis, IR Spectra, Crystal Structure 
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 TEI-XML for    default:Reihe_B/41/ZNB-1986-41b-0831.pdf 
 Identifier    ZNB-1986-41b-0831 
 Volume    41 
7Author    Borylated Carbodiimides, Wolfgang Einholz, Wolfgang HauboldRequires cookie*
 Title    Borylierte Carbodiimide  
 Abstract    The borylated carbodiim ides 3 a, 3b and 4 can be synthesized by reaction o f the 2-ch loro-l,3,2-diazaborolidines 2 a, 2b with M e3Si —N = C —N —SiM e3 (1) or M e3Si —N = C = N —'Bu respectively. In the reaction of the non cyclic haloboranes R 2BH al (R = Ph, M e, M e2N) 2 c —e with 1 R3B is formed and for R = M e, M e2N polym eric (R BN C N)" is obtained, whilst the spectroscopically identified intermediate products only in the case o f R = Ph can be isolated. The chloroborolane 2 f leads to the polymeric diborylated carbodiim ide 3f, probably due to intermolecular B —N-coordi-nation. H2N —CN forms with 9-BBN the m onoborylated cyanam ide 8 . 
  Reference    Z. Naturforsch. 41b, 1367—1372 (1986); eingegangen am 3. A p ril/14. August 1986 
  Published    1986 
  Keywords    Boron-Nitrogen C om pounds, Carbodiim ides, Synthesis, Structure, Spectral Data 
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 TEI-XML for    default:Reihe_B/41/ZNB-1986-41b-1367.pdf 
 Identifier    ZNB-1986-41b-1367 
 Volume    41 
8Author    Wolfgang Willing, Ulrich Müller, Udo Dem, Kurt DehnickeRequires cookie*
 Title    Synthesen und Kristallstrukturen von PPh4[RuCl4(NO)(NSCl)] und (PPh4)2[RuCl4(NS)]2-4C H 2CI2 Syntheses and Crystal Structures of PPh4[RuCl4(NO)(NSCl)] and (PPh4)2[RuCl4(NS)]2-4 CH 2C12  
 Abstract    By reaction o f trithiazylchloride, (NSC1)3, with PPh4[RuCl4(N O)]2 in dichlorom ethane the thiazylchloridenitrosyl com plex PPh4[RuCl4(N O)(N SC l)] is obtained; its vacuum pyrolysis at 2 0 0 -2 2 0 °C yields the thionitrosyl com plex (PPh4)2[RuCl4(N S)]2 which crystallizes from C H 2C12 solution with four m olecules o f CH 2C12. Both com pounds were charaterized by their IR spectra and by X-ray crystal structure determ inations. Crystal data: PPh4[RuCl4(N O)(N S C l)], m on o­ clinic, space group P 2 xln, Z = 4, a = 982.6, b = 1700.0, c = 1772.3 pm , ß = 104.79° (2548 observed reflexions, R = 0.046); (PPh4)2[RuCl4(N S)]2-4 C H 2C12, triclinic, P I , Z = 1, a = 952.9, b = 1380.0, c — 1458.5 pm , a — 112.91, ß = 106.67, y = 92.61° (3760 observed reflexions, R = 0.053). In the [RuCl4(N O)(N S C l)]e ion the nitrosyl and thiazyl chloride ligands occupy e x ­ positions; bond lengths indicate double bonds in the linear Ru = N -0 group, while the NSC1 m olecule is attached by a donor-acceptor interaction R u -N = S -C l , although with a rather short Ru —N bond o f 198 pm (N = S 144 pm, S —Cl 213 pm). The centrosymm etric [RuC14(N S)]220 ions have chloro bridges and NS ligands in axial positions; the nearly linear R u = N = S group has bond lengths R u = N 175 pm and N = S 147 pm. 
  Reference    Z. Naturforsch. 41b, 560 (1986); eingegangen am 29. Januar 1986 
  Published    1986 
  Keywords    Thionitrosyl and Thiazylchloride C om plexes o f Ruthenium, Syntheses, IR Spectra, Crystal Structure 
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 Identifier    ZNB-1986-41b-0560 
 Volume    41 
9Author    WolfgangH. Eininger, R. Olf Stucka, Günter NagorsenRequires cookie*
 Title    Ein neues Silicat-Anion: [Si(NCS)6]2 A N ew Silicate Anion: [Si(N C S)6]2  
  Reference    Z. Naturforsch. 41b, 702—707 (1986); eingegangen am 7. Februar 1986 
  Published    1986 
  Keywords    New H exacoordinated Anionic Silicon Complex, H exaisothiocyanatosilicate, Synthesis, IR Spectra, X-Ray Spectra 
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 TEI-XML for    default:Reihe_B/41/ZNB-1986-41b-0702.pdf 
 Identifier    ZNB-1986-41b-0702 
 Volume    41 
10Author    Hans-Günter Hauck, W. Olfgang, Willing, Ulrich Müller, Kurt DehnickeRequires cookie*
 Title    Brom-und Chlorthionitrenkomplexe des Rheniums Die Kristallstruktur von (PPh4)2[ReBr4(N S)(N SBr)] *CH2Br2 Bromo-and Chlorothionitrene Complexes of Rhenium The Crystal Structure of (PPh4)2[ReBr4(NS)(NSBr)] ■ C H 2B r2  
 Abstract    The thionitrosyl-halothionitrene com pounds (PPh4)2[R eX 4(N S)(N S X)]-2 C H 2X 2, X = Cl or Br, are obtained by nucleophilic ring cleavage o f the R e(N 2S2) rings o f com plexes [R eX 4(N 2S2)]e with PPh4X in C H 2X 2. (A sP h4)2[R eC l4(N S)(N SC l)] • C H 2C12 can also be obtained by the reaction 
  Reference    Z. Naturforsch. 41b, 825 (1986); eingegangen am 7. März 1986 
  Published    1986 
  Keywords    Bromo- and Chlorothionitrene Complexes of Rhenium, Synthesis, IR Spectra, Crystal Structure 
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 Identifier    ZNB-1986-41b-0825 
 Volume    41 
11Author    M. Veith, R. RosierRequires cookie*
 Title    Alkoxistannate, II [1] Tri(te/*-butoxi)alkalistannate(II): Darstellung und Strukturen Alkoxistannate, II [1] Tri(rerr-butoxi)alkalistannates(II): Synthesis and Structures  
 Abstract    Tri(terf-butoxi)alkalistannates (M (O rBu)3Sn, M = Li, Na, K, Rb, Cs) are obtained by reaction of alkali-fert-butanolates with tindi-terf-butoxide. If M equals Li or Na (1, 2) molecular com ­ 
  Reference    Z. Naturforsch. 41b, 1071 (1986); eingegangen am 12. F eb ru ar/17. März 1986 
  Published    1986 
  Keywords    Synthesis, Polycyclic C om pounds, Crystal Structure, M olecular Structure, X -R ay 
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 Identifier    ZNB-1986-41b-1071 
 Volume    41 
12Author    Z. NaturforschRequires cookie*
 Title    Über Erdalkalimetallverbindungen des l,l-Dicyanoethylen-2,2-dithiolats, III+ Die Kristallstruktur von SrS2C4N2 * 5 H20  
 Abstract    By reaction of CS2 with m aleonitrile in presence of sodium ethanolate in ethanol, N a2S2C4N 2 is obtained. SrS2C4N2-5 H 20 was synthesized by reaction of Sr(NCS) 2 with N a2S2C4N2 in ethanol. It crystallizes monoclinically, space group P2!/c, with a = 9.201(2), b — 9.990(6), c = 14.605(5) Ä,/3 = 122.3(3)°, Z = 4. The com pound is isotypical with CaS2C4N2-5 H 20 . A structural model based on equivalent metal positions was refined to R -0.057. The crystal structure contains layers of nearly planar [S2C = C (C N)2]2' anions held together by interspersed Sr2+ cations in a tricapped trigonal prismatic surrounding of 6 0 and 3N atoms. The S atom s of the ligand are not included in the coordination sphere of Sr2+ but are involved in several O — H -S hydrogen bonds. 
  Reference    Z. Naturforsch. 41b, 1206—1210 (1986); eingegangen am 1. April/26. Juni 1986 
  Published    1986 
  Keywords    Strontium -l, l-dicyanoethylene-2, 2-dithiolate P entahydrate, Synthesis, Crystal Structure 
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 Identifier    ZNB-1986-41b-1206 
 Volume    41 
13Author    CarlH. Abben, A. Nton Meller, M. Atthias, N. Oltem Eyer, GeorgeM. SheldrickRequires cookie*
 Title    Synthese, Molekül-und Kristallstruktur von 3,5-Dimethyl-2,6-bistrimethylsilyl- l-thia-2,4,6-triaza-3,5-diborinan-wolframpentacarbonyl Synthesis, M olecular and Crystal Structure of 3,5-Dimethyl-2,6-bistrimethylsilyl- l-thia-2,4,6-triaza-3,5-diborinane-tungstenpentacarbonyl  
 Abstract    The am m onolysis o f 3,5-dim ethyl-2,6-bistrim ethylsilyl-l,4-dithia-2,6-diaza-3,5-diborinane leads to 3,5-dim ethyl-2,6-bistrim ethylsilyl-l-thia-2,4,6-triaza-3,5-diborinane, which reacts with tungstenpentacarbonyl • TH F to give the title-com pound. 'H , " B , 13C, 14N , 29Si N M R spectra, IR and MS data, and the results o f an X-ray analysis are reported. 
  Reference    Z. Naturforsch. 41b, 799—802 (1986); eingegangen am 19. Februar 1986 
  Published    1986 
  Keywords    l-Thia-2, 4, 6-triaza-3, 5-diborinanes, Tungstenhexacarbonyl, Synthesis, M olecular Structure, Crystal Structure 
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 Identifier    ZNB-1986-41b-0799 
 Volume    41 
14Author    Ryszard Stolarski3, Zygmunt Kazimierczuk3, Piotr Lassotab, David Shugara-Requires cookie*
 Title    Acyclo Nucleosides and Nucleotides: Synthesis, Conformation and Other Properties, and Behaviour in Some Enzyme Systems, of 2',3'-Seco Purine Nucleosides, Nucleotides and 3 ':5'-Cyclic Phosphates, Analogues of cAMP and cGMP  
 Abstract    The 3':5'-cyclic phosphates of 2',3'-secoadenosine and guanosine, structural analogues of cAMP and cGMP, were synthesized by cyclization of the 5'-phosphates of 2',3'-secoadenosine and guanosine, respectively. The 2',3'-seco-3':5'-cAMP was converted to the IM P analogue by nitrous acid deamination, and to the 8-bromo analogue by bromination. Chemical phosphorylation of 2',3'-secoadenosine gave four products, the major one of which, in 50% yield, was 2',3'-seco-3':5'-cAMP, identical to that obtained by the cyclization reaction above. The three other products have been tentatively identified. The conformations in solution of the seco nucleosides, their 5'-monophosphates, and their 3':5'-cyclic phosphates, were determined with the aid of 'H , 13C and 31P N M R spectroscopy, particular attention being devoted to orientations about the C —O bonds and the glycosidic bond, and the results compared with crystallographic data available for the 2',3'-seco congener of ribofuranosyl benzimidazole. The findings are briefly discussed in relation to substrate and inhibitor properties in some enzyme systems. Some of the foregoing compounds have been examined as potential enzyme substrates and inhibitors. In particular, the seco 3':5'-cyclic phosphates are resistant to cAM P cyclic phos­ phodiesterase of mammalian origin, but are slowly hydrolyzed by purified higher plant cyclic nucleotide phosphodiesterase to the corresponding monophosphates. 
  Reference    Z. Naturforsch. 41c, 758—770 (1986); received March 17 1986 
  Published    1986 
  Keywords    2', 3'-Seco Cyclic Nucleotides, cAMP and cGMP Analogues, Synthesis, Phosphorylation, N M R and Conformation, Enzymology 
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 Identifier    ZNC-1986-41c-0758 
 Volume    41