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1997 (258)
101Author    Abdel-Fattah Shihada, Frank WellerbRequires cookie*
 Title    The Crystal Structures of Et2S n (0 2PMe2)2 and Ph2Sn(02PMe2)2; Synthesis and Spectral Studies of Ph2Sn(02PMe2)2  
 Abstract    Crystal Structure, Vibrational Spectra, Diethyltin Bis(dimethylphosphinate), Diphenyltin Bis(dimethylphosphinate) Ph2Sn(02PMe2)2 has been synthesized by the reaction of H02PMe2 with Ph^SnO in toluene or by treating H02PMe2 with Ph2SnCl2 in methanol. X-ray diffraction studies of Et2Sn(02PMe2)2 and Ph2Sn(0 2 PMe2)2 show that the 0 2 PMe2 ligands function as bidentate bridges between the tin atoms. The ethyl and the phenyl groups are in trans-position in the resulting octahedral environment around tin. Et2Sn(0->PMe2)2 crystallizes in the monoclinic space group P2i/n (a = 817.11(9), b = 974.1(1), c = 970.1(1) pm, ß = 113.749(6)°, Z = 2 and R = 0.032) and con­ sists of a polymeric layer structure with centrosymmetric (SnOPO)4 sixteen-membered rings. Ph2Sn(02PMe2)2 also crystallizes monoclinically in the space group P2|/n (a= 1060.9(1), b = 999.4 (1), c = 1768.9(2) pm, ß = 90.93(1)°, Z = 4 and R = 0.057) and has a polymeric ring-chain structure with centrosymmetric (SnOPO)2 eight-membered rings. The IR and Raman spectra of Ph2Sn(0 2 PMe2)2 have been assigned and discussed in the light of structural information. The Sn(02PMe2)+ ion represents the base peak in the mass spectrum of Ph2Sn(02PMe2)2. 
  Reference    Z. Naturforsch. 52b, 587—592 (1997); received December 17 1996 
  Published    1997 
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 Identifier    ZNB-1997-52b-0587 
 Volume    52 
102Author    Jan Geicke, Ingo-Peter Lorenz, Petra Mürschel, Kurt PolbomRequires cookie*
 Title    Dppa als Komplexligand: Metall-Koordination und P-N-Spaltung in Komplexen des Typs [CpM(L)dppa]X (M = Fe, Mn; L = CO, NO) Dppa as a Ligand: Metal Coordination and P-N Cleavage in Complexes of the Type [CpM(L)dppa]X (M = Fe, Mn; L = CO, NO)  
 Abstract    Dppa Ligand, Mono and Bidentate, Nucleophilic Attack, Cleavage Reaction of P-N The reactions of [CpMn(CO)2(NO)]BF4 or CpFe(CO)2Cl with PPh2NHR (R = Ph, PPh2) lead to the salts [CpML(CO)PPh2NHR]X with monodentate aminophosphine ligands. In the case of R = PPh2 (= dppa) the complexes [CpML(dppa)]X with bidentate dppa are also formed. The salt [CpFe(CO)(dppa)]Cl can be deprotonated to give the neutral complex CpFe(CO){(PPh2)2N)} with the diphosphinoamide ligand, which can be N-alkylated by Mel to afford [CpFe(CO){(PPh2)2NMe}]I. The complex [CpMn(NO)(dppa)]BF4 undergoes a P-N cleavage reaction by the solvent methanol to form [CpMn(NO)(PPh2NH2)(PPh2OMe)]BF4. The non-chelated complexes [CpFe(CO)2PPh2NHR]Cl are deprotonated by DBU to give the neutral ferrioiminophosphoranes CpFe(CO)2PPh2 = NR. For R = PPh2 photolysis leads to CO-elimination and to CpFe(CO)(PPh2NPPh2). CpFe(CO)2PPh2NPPh2 can be alkylated by Mel or metallated by CpFe(CO)2Cl to form [CpFe(CO)2PPh2NPPh2Me]I or [CpFe(CO)2PPh2NPPh2(CO)2FeCp]Cl, respectively. Oxidation of CpFe(CO)2PPh2NPPh2 is possible by (SiMe3)20 2, sulfur, or selenium to lead to the neutral complexes CpFe(CO)2PPh2=NPPh2 = E (E = O, S, Se) with a heterodiene system. The IR and NMR spectra of all species as well as the X-ray structures of the complexes [CpFe(CO)dppa]Cl, [CpMn(NO)dppa]BF4 and [CpMn(NO)(PPh2NH2)(PPh2OMe)]BF4 are reported and discussed. 
  Reference    Z. Naturforsch. 52b, 593—603 (1997); eingegangen am 30. Dezember 1996 
  Published    1997 
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 Identifier    ZNB-1997-52b-0593 
 Volume    52 
103Author    J. Beck, M. ReitzRequires cookie*
 Title    Synthese und Kristallstruktur von 7-Azaindolato-Silber, einem dimeren Ag(I)-Komplex mit kurzem Ag-Ag-Abstand  
 Abstract    Synthesis and Crystal Structure o f 7-A zaindolate-silver, a D im eric A g(I) C om plex w ith a Short A g-A g D istance 7-Azaindole, d l(,-dl0-Interactions, Crystal Structure, Silver(I) Complex [Ag(C7H5N2)]2 is obtained by the slow addition of a tetrahydrofuran (thf) solution of AgC104 to a solution of Na(C7H5N2) in thf. The slightly yellow compound crystallizes in the monoclinic space group P 2\ln with the lattice constants a = 554.5(1) pm, b = 954.6(2) pm, c = 1196.5(3) pm, ß = 99.67(2)°. The structure consists of centrosymmetric, planar, dimeric complexes with ligand disorder in the crystal. The N atoms coordinate the Ag+ ions nearly linearly (N-Ag-N = 168°, Ag-N = 213 pm). The Ag+ ions in the dimeric unit have a short distance of 284 pm. The complexes are linked by weak intermolecular i f -Ag-C interactions to chains. 
  Reference    Z. Naturforsch. 52b, 604 (1997); eingegangen am 17. Januar 1997 
  Published    1997 
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 Identifier    ZNB-1997-52b-0604 
 Volume    52 
104Author    N. Orbert Kuhn, Riad Faw, M. Anfred, Steim Ann, JörgW. Iethoff, HerrnRequires cookie*
 Title    Zur Reaktion von Derivaten des l,3-Dimethyl-2-iminoimidazolins mit CS2 [1]  
 Abstract    1,3-Dimethyl-2-iminoimidazoline (4, ImNH) reacts with CS2 to give the imidazolium salt [ImNH2][(ImNCS2)2H] (7) in which two dithioformimide fragments are linked by a hydrogen bridge. From the trimethylsilyl derivative ImNSiMe3 (11) and CS2 the adduct ImNSiMe3 • CS2 (12) is obtained which reacts with oxygen to give the disulfide (ImNCS2) (14). The X-ray structures of 7 and 14 were determined. 
  Reference    Z. Naturforsch. 52b, 609—614 (1997); eingegangen am 19. Februar 1997 
  Published    1997 
  Keywords    Imidazoles, Carbon Disulfide, X-Ray 
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 Identifier    ZNB-1997-52b-0609 
 Volume    52 
105Author    Antje Albert, D. Ietrich, M. OotzRequires cookie*
 Title    Formation and Crystal Structures of the Hydrates of 18-Crown-6 [1]  
 Abstract    The melting diagram of the system 18-crown-6/water has been set up and the existence of four binary hydrates confirmed. Crystal structures have been determined for three of these, in addition to that for the hexahydrate already published. The hydrates are monoclinic, a tetrahydrate (previously reported as a 4.5-hydrate) with space group P2|/c and Z = 2 formula units per unit cell, an octahydrate with I2/a and Z = 4, and a dodecahydrate with P2i/n and Z= 2. In each structure the crown ether molecule has the (pseudo) D.^ conformation common for many of its complexes, and is immediately hydrogen-bonded by a group of four water molecules in a similar, characteristic pattern. In the tetrahydrate, with one of the waters disordered, the total connectivity is that of a 1D chain, while the overall structures of the octa-and dodecahydrate are 3D networks. Four of the six independent water molecules in the dodecahydrate are linked with each other into a rare 2D ice-like layer. 
  Reference    Z. Naturforsch. 52b, 615—619 (1997); received January 15 1997 
  Published    1997 
  Keywords    Crown Ether, Crystal Structure, Hydrate, Hydrogen Bonding, Melting Diagram 
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 Identifier    ZNB-1997-52b-0615 
 Volume    52 
106Author    Lothar BeyerRequires cookie*
 Title    Substituierte l,2,4-Thiadiazolium-dichloroaurate(I) und -tetra- chloroaurate(III) als Reaktionsprodukte von N-Thiocarbamoyl- benzamidinen mit TetrachIorogold(III)-Verbindungen  
 Abstract    Substituted 1,2,4-T hiadiazolium dichloroaurates(I) and -tetrachloroaurates(III) as Products o f the R eaction o f N -T hiocarbam oyl-benzam idines w ith Tetrachlorogold(III) Com pounds U w e Schröder3, R ainer R ichter3, Jürgen H artung3, U lrich A bram b, 
  Reference    Z. Naturforsch. 52b, 620—628 (1997); eingegangen am 12. März 1997 
  Published    1997 
  Keywords    1, 2, 4-Thiadiazoliumchloroaurates(I/III), Synthesis, X-Ray, EM Spectra, N-Thiocarbamoylbenzamidines 
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 Identifier    ZNB-1997-52b-0620 
 Volume    52 
107Author    Z. NaturforschRequires cookie*
 Title    Neue Synthesen mit Magnesiumhydrid Teil 2: Wege zu neuen komplexen Hydriden und zum Aluminiumwasserstoff  
 Abstract    The reaction between autocatalytically prepared magnesium hydride (Tego® Magnan) and aluminium halides in ethers generates a new class of reducing agents, i.e. magnesium alumi­ nium hydridohalides. By choosing dioxane-1,4 as solvent a route to an aluminium hydride dioxane complex is opened. The new reducing agents show outstanding selectivity especially in the field o f organosilico-nes, combined with a maximum of safety in their application. 
  Reference    Z. Naturforsch. 52b, 629 (1997); eingegangen am 21. Januar 1997 
  Published    1997 
  Keywords    Magnesium Aluminium Hydridohalides, Reducing Agents, Aluminium Hydride, Magnesium Hydride 
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 Identifier    ZNB-1997-52b-0629 
 Volume    52 
108Author    Requires cookie*
 Title    Synthese und Kristallstrukturen der neuen Zinn-Chalkogen-Vierringe [{Cp(Ph3P)Ni}2Cl2Sn2E2] (E = Se, S)  
  Reference    Z. Naturforsch. 52b, 635 (1997) 
  Published    1997 
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 Identifier    ZNB-1997-52b-0635 
 Volume    52 
109Author    Requires cookie*
 Title    Die zu BaMg2Cu8V60 26 isotypen Cadmium-Kupferoxovanadate KCdo,67CU49 33V 3 0 i3, RbCdo^Cu^X^O^ sowie TlCdo^Cu^^^O^  
 Abstract    The BaM g2Cu8V 60 26-Isotypic C adm ium C opperoxovanadates K C d0.67Cu4.33V3O13, RbCdo,5C u4,5V 3O i3 and TlCdo,5C u4 5V 3O i3 B. M ertens, Hk. M üller-B uschbaum * Institut für A n organ isch e C h em ie der C hristian-A lb rechts-U niversität, O lshausenstraße 40, D -24098 K iel (D eu tsch lan d) Z. Naturforsch. 52b, 6 3 9 -6 4 2 (1997); e in gegan gen am 7. Februar 1997 A lkaline. Thallium , C adm ium , C opper, V anadium O xide Single crystals o f K Cdo67Cu4 33V 3 0 13 (I), R b C d o5C u4 5V 3O i3 (II) and TlC d()5C u4 5V 30 13 (III) have been prepared by crystallization from m elts. X-ray analysis led to m onoclin ic sym m etry, space group C 2h-P 2i/m (Nr. 11) and the lattice constants (I) — (III): a = 10.728(1), 10.746(3), 10.746(3), b = 6.155(1), 6 .163(2), 6.175(2), c = 8.363(2), 8.350(2), 8.337(3) A , ß = 97.69(2), 97.73(2), 97.61(5)°, Z = 2. The crystal structures are isotypic to the B aM g2C U 8V 60 26 type. C u2+ occurs in square pyram idal and unusual trigonal bipyram idal coord in ation by oxygen . The M g 0 6 octahedra o f the aristo type B aM g2C u8V 60 26 are statisti­ cally occupied by cadm ium and copper. The distortion o f the (C d /C u)0 6 octahedra is discus­ sed with respect to the polyhedra netw ork. 
  Reference    Z. Naturforsch. 52b, 639 (1997) 
  Published    1997 
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 Identifier    ZNB-1997-52b-0639 
 Volume    52 
110Author    Requires cookie*
 Title    Dicobaltoarsenat -(C oA s07) -Baugruppen im Cobaltoxid-Tellurat Co60 2[T e04(C oA s05)2]  
  Reference    Z. Naturforsch. 52b, 643 (1997) 
  Published    1997 
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 Identifier    ZNB-1997-52b-0643 
 Volume    52 
111Author    Requires cookie*
 Title    Kondensationsreaktionen von Trifluornitrosomethan CF3NO mit Sulfanilamid H2NC6H4S 0 2NH2 -Darstellung von CF3NNC6H4S 0 2NH2, CF3NNC6H4S 0 2NNCF3, CH3C (0)N (H )C 6H4S 0 2NNCF3 und CF3C (0)N (H )C 6H4S 0 2NH2  
  Reference    Z. Naturforsch. 52b, 647 (1997) 
  Published    1997 
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 Identifier    ZNB-1997-52b-0647 
 Volume    52 
112Author    Requires cookie*
 Title    Übergangsmetall-substituierte Acylphosphane und Phosphaalkene  
 Abstract    , XXXIY [1] Methylendiyl(thioxo)-und MethyIendiyl(selenoxo)-A5,<r3-phosphorane als //-Liganden in [(j/5-C5H5)2Fe2(CO)3]-Komplexen. Synthese und Struktur von (i/5-C5H5)(CO)Fe0/-CO)[^-C(PHrBu)(SMe)]Fe(i75-C5H5) 
  Reference    Z. Naturforsch. 52b, 655 (1997) 
  Published    1997 
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 Identifier    ZNB-1997-52b-0655 
 Volume    52 
113Author    Requires cookie*
 Title    Zum Mineral Johillerit verwandte Oxovanadate RbCd4Y3Oi2 und TlCd4V3Oi2  
 Abstract    O xovan ad ates R bC d4V 30 12 and TlCd4V 30 12 R elated to the M ineral Johillerite B. M ertens, Hk. M üller-Buschbaum * Institut für A norganische C h em ie der C hristian-A lb rechts-U niversität, O lshausenstr. 4 0 -6 0 , D -24098 K iel (D eutsch lan d) 
  Reference    Z. Naturforsch. 52b, 663 (1997) 
  Published    1997 
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 Identifier    ZNB-1997-52b-0663 
 Volume    52 
114Author    Requires cookie*
 Title    Introduction of Functional Silyl Groups into Tris(dialkylamino)phosphonium Methylides  
  Reference    Z. Naturforsch. 52b, 669 (1997) 
  Published    1997 
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 Identifier    ZNB-1997-52b-0669 
 Volume    52 
115Author    K. Arl-H, Andreas Einz Dreihäupl, Hubert Bauer, SchmidbaurRequires cookie*
 Title    Bis(silylation) of Tris(dimethylamino)phosphonium Methylide  
 Abstract    Treatment of (MezNX^PCHSiMe.^ with Me.^SiOTf (OTf = triflate) affords the phospho-nium salt [(Me2N)3PCH(SiMe?)2]OTf (2a), which can be converted into the correspond­ ing ylide (Me2NbPC(SiM e3)2 (3a) in high yield using NaN(SiMe3>2. The compounds with SiMe2Ph substituents (2, 3b) are obtained following an analogous procedure. The ylide (Me2N)3PC[Si(OMe)3]2 (3c) is available in 50% yield by direct transylidation of (M eObSiOTf with (Me2N)3PCH2 in the molar ratio 2:3, with [(Me2N)3PMe]OTf as the by-product. Com­ pound 3c is a distillable liquid, but 3a,b are crystalline solids the structure of which has been determined by single crystal X-ray diffraction. Both compounds feature a trigonal planar ylidic carbon atom and short ylidic P-C and Si-C bonds. The nitrogen atoms are also in a planar configuration with non-standard orientations of the NMe2 groups at the phosphorus atoms. These data are in agreement with the results of recent quantum chemical calculations of simple prototypes which show very flat energy profiles for internal motions (rotation, inversion) of dimethylamino groups at the phosphorus atoms in phosphines and phosphoranes. 
  Reference    Z. Naturforsch. 52b, 674—678 (1997); received April 21. 1997 
  Published    1997 
  Keywords    Silylation Ylides, Phosphorus Ylides, Aminophosphines 
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 Identifier    ZNB-1997-52b-0674 
 Volume    52 
116Author    Thom As Häusler, W. Illiam, S. SheldrickRequires cookie*
 Title    Metal-Mediated Assembly of Hexameric Ethylcycloarsoxane (C2H5AsO)6 in Mono-and Dinuclear Complexes with Tetrahedral and Octahedral Coordination Spheres  
 Abstract    A metal-assisted ring expansion from the preferred solution species (EtAsO),,, n = 3,4, to the hexameric ligand (EtAsO)6 is observed for the reactions of [ReBr(CO)5], [RuCLCPh^P)?], RhCfv3 H2 0 and [C^CCF.^SO.OaCCftHft)] with ethylcycloarsoxane. Whereas two metal frag­ ments are facially coordinated by the upper and lower three As atoms of a flattened AsftOö cuboctahedron in both [{ReBr(CO)2} 2 {M-[cyc/o-(EtAsO)6]}] (1) and [Cu2{n-[cyclo-(EtAs0)6]}(Me2PhP)2](CF3S03)2 (4), potential ring strain restricts the reaction with the other compounds to the formation of mononuclear complexes [RuCl2{cvc/o-(EtAsO)6}(Ph3P)] (2) 
  Reference    Z. Naturforsch. 52b, 679—686 (1997); received March 6 1997 
  Published    1997 
  Keywords    Ethylcycloarsoxane, Transition Metal Complexes, Metal-Mediation, Ring Expansion 
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 Identifier    ZNB-1997-52b-0679 
 Volume    52 
117Author    AnjaL. Oose, W. Illiam, S. SheldrickRequires cookie*
 Title    Quaternary Selenidogermanates(IV) A3[AgGe4Se10]*2H2O and A2[MnGe4Se10]*3H2O (A = Rb, Cs) with Open Framework Structures  
 Abstract    Hydrothermal reaction of Ge and Se with Ag(CH3COO) in the presence of alkali metal carbonates affords the open framework selenidogermanates(IV) A^fAgGejSeiol ^H^O (A = Rb, Cs), 1 and 2, which contain corner linked adamantane-like Ge4Seio cages and AgSe4 tetrahedra. The analogous reaction with Mn(CHiCOO)2 yields the isostructural tetragonal compounds A2[MnGe4Seio]-3 H2 0 (A = Rb, Cs), 3 and 4. The cations are sited at a general position in the channels of the silver bridged anionic framework of 1 and 2 and exhibit a disordered pattern of occupation (s.o.f. = 0.75) with one of the two crystallographically independent water oxygen atoms 0 (2) (s.o.f. = 0.25). In contrast, the Rb+ cations in 3 are disordered over all three cation/oxygen sites, and the cation/water occupation pattern is fully reversed for the larger Cs+ cations in 4 in comparison to 1 and 2. 
  Reference    Z. Naturforsch. 52b, 687—692 (1997); received March 13 1997 
  Published    1997 
  Keywords    Selenidogermanates(IV), Silver, Manganese, Hydrothermal Synthesis, Framework Structure 
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 Identifier    ZNB-1997-52b-0687 
 Volume    52 
118Author    Requires cookie*
 Title    Vanadiumkomplexe mit dreizähnigen diaciden Liganden. Bis[2-(2'-hydroxyphenyl)-chinolin-8-olato]dimethoxo-dioxo-divanadium(V) -ein neuer Strukturtyp  
  Reference    Z. Naturforsch. 52b, 693 (1997) 
  Published    1997 
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 Identifier    ZNB-1997-52b-0693 
 Volume    52 
119Author    A. M. Orgenstern, H. OppermannRequires cookie*
 Title    Untersuchungen zur thermischen Zersetzung von Ammoniumlanthanhalogeniden Investigation on the Thermal D ecom p osition o f A m m onium H alides  
 Abstract    The decomposition equilibria of Ammonium Lanthanum Halides (NH4)2LaX5 were determined by total pressure measurements in a membrane zero manometer. The phases (NH4j2LaX5 decompose in one step to give solid LaX3 and gaseous NH3 and HX. From the decomposition functions the enthalpies of formation and the standard entropies of the phases are derived. ^H £(N H 4)2LaCl5,f,298) = -4 1 1 ,7 ± 2,2 kcal/mol; S°((NH4)2LaCl5,f,298) = 86,7 ± 2,3cal/Kmol; ^H^(NH4)2LaBr5,f,298) = -351,6 ± 3,8 kcal/mol; S°((NH4)2LaBr5,f,298) = 101,1 ± 1,8 cal/Kmol; _}H£(NH4)2LaI"f,298) = -2 6 8 ,9 ± 3,9 kcal/mol; S°((NH4)2LaI5,f,298) = 115,5 ± 4,3 cal/Kmol. 
  Reference    Z. Naturforsch. 52b, 696—706 (1997); eingegangen am 17. Februar 1997 
  Published    1997 
  Keywords    Synthesis, Ammonium Lanthanum Halides, Thermal Decomposition, Thermochemical Data 
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 Identifier    ZNB-1997-52b-0696 
 Volume    52 
120Author    M. Jansen, S. B. ZikRequires cookie*
 Title    Darstellung und Charakterisierung der Carbosilazane Bis  
 Abstract    [tris(methylamino)silyl]methan und Bis[tris(phenylamino)silyl]methan Preparation and Characterization o f the C arbosilazanes B is[tris(m ethylam ino)silyl]m ethane and B is[tris(phenylam ino)silyl]m ethane Crystal Structure, Carbosilazane Bis[tris(methylamino)silyl]methane (1) and bis[tris(phenylamino)silyl]methane (2) have been synthesized as potential precursors of porous oxygen-free solids by the reaction of bis(trichlorsilyl)methane with methylamine and with lithiated aniline, respectively. Compound 2 was characterized by a crystal structure analysis. It crystallizes in the monoclinic space group P 2 ,/c with the unit cell parametersa= 10.963(2),6= 17.801(2), c= 17.557(2) Ä, ß = 97.96(2)° and Z = 4 (/?, = 4,4 %, wR2 = 9,8 %, 5950 independent reflections). 
  Reference    Z. Naturforsch. 52b, 707—710 (1997); eingegangen am 10. Februar 1997 
  Published    1997 
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 Identifier    ZNB-1997-52b-0707 
 Volume    52 
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