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141Author    Alfred-Dirk Bacher, Ulrich MüllerRequires cookie*
 Title    Synthese und Kristallstruktur von INa(15-Krone-5)]2S6 Synthesis and Crystal Structure of [Na(15-crown-5)]2S6  
 Abstract    [Na(15-crown-5)]2S6 was obtained from N a 2S4 und 15-crown-5 in acetonitrile. Its crystal structure was determined by X-ray diffraction with 2968 observed reflexions, R = 0.119. Crys­ tal data: a = 861.4(9), 6 = 1006(1), c = 2097(1) pm, a = 89.7(1), ß = 100.20(8), y = 114.6(1)°, Z = 2, space group P 1. The chain-like S62-ion has transoid conform ations, each o f its terminal atom s is in contact with one N a + ion which in turn is coordinated with one crown ether m ole­ cule. 
  Reference    Z. Naturforsch. 47b, 1063—1066 (1992); eingegangen am 6. Februar 1992 
  Published    1992 
  Keywords    Sodium -Crown Hexasulfide, Synthesis, Crystal Structure 
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 Identifier    ZNB-1992-47b-1063 
 Volume    47 
142Author    Dieter Sellmann, W. Olfgang, Soglowek, M. Atthias, MollRequires cookie*
 Title    Übergangsmetallkomplexe mit Schwefelliganden, XCI+ Fen-Komplexe des fünfzähnigen Thioether-Thiolat-Aminliganden 'buN HS4'-H2: Synthese, Charakterisierung, Reaktivität und Stereochemie ('buNHS4'-H2 = 2 ,2 -Bis(2-mercapto-3,5-di-tertiärbutyl-phenylthio)diethylamin)  
 Abstract    Transition M etal Complexes with Sulfur Ligands, X C I+ Fe11 Complexes o f the Pentadentate Thioether-Thiolate-Amine Ligand 'buN HS4'-H 2: Synthesis, Characterization, Reactivity and Stereochemistry (,buN HS4'-H 2 = 2,2'-Bis(2-mercapto-3,5-di-tertiarybutyl-phenylthio)diethylamine) In search o f m odel com pounds for the active centers o f nitrogenases, [Fe(L)('buN HS4')] complexes o f the pentadentate thioether-thiolate-amine ligand 'buN HS4'2-('buN HS4'-H2 = 2,2'-bis(2-mercapto-3,5-di-tertiarybutyl-phenylthio)diethylamine) were obtained. A lkylation o f 'buS2'-H2 with (BrC2H4),N H yielded the new ligand 'buN HS4'-H2 as a mixture o f positional isomers. Isolation o f single isomers was achieved by reacting the mixture with FeCl2-4 H 20 and CO in order to give the corresponding [Fe(CO)] complexes which were se­ parated and hydrolyzed to yield the free ligands. R eaction o f 'buN HS4'-H2 with FeCl2 -4 H 20 led to the high-spin complex [Fe('buN HS4')] which is extremely air-sensitive in solution. It rapidly reacts with L = CO, NO, PM e3, and N 2H4, and is the m ost suitable starting material for syntheses o f [Fe(L)('buN HS4')l complexes which were characterized for L = CO, N O +, N O , PM e3 and N 2H4. All complexes are considerably better soluble in organic solvents than the corresponding parent compounds [Fe(L)('NHS4')], ('N hS4'-H 2 = 2,2'-bis(2-mercaptophenylthio)diethylamine), but have similar properties in most other respects. In the oxidation o f [F e(N 2H 4)('buN HS4')] at low temperatures, there is evidence for the form ation o f the diazene com plex [u-N 2H2{Fe('buN HS4')}2]. 
  Reference    Z. Naturforsch. 47b, 1105 (1992); eingegangen am 10. April 1992 
  Published    1992 
  Keywords    Iron Complexes, Thioether-Thiolate Ligand, Synthesis 
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 Identifier    ZNB-1992-47b-1105 
 Volume    47 
143Author    Rene Wollert, SigridW. Ocadlo, K. Urt Dehnicke, Helmut Goesmann, Dieter FenskeRequires cookie*
 Title    Die Kristallstrukturen von (PPh4)2 [TiCl3 (NSiMe3) ] 2 * CH3CN und (PPh4)2 [TiCl4(OSPCl2) ] 2 The Crystal Structures of (PPh4)2[TiCl3(NSiM e3)]2 -C H 3CN and (PPh4)2[TiCl4(OSPCl2)]2  
 Abstract    (PPh4)2[TiCl3(N SiM e3)]2 C H 3CN has been prepared from [TiCl^NSiM ej)]^ with PPh4Cl in acetonitrile solution as yellow crystals. The com pound crystallizes in the triclinic space group P 1 with one formula unit per unit cell, 3447 observed unique reflections, R = 0.053. Lattice dimensions at 200 K: a = 1030(1), b = 1253(1), c = 1374(1) pm, a = 77.46(8)°, ß = 73.93(8)°, y = 69.99(9)°. The structure consists o f PPh4+ ions and centrosymmetric dimeric anions [TiCl3(N SiM e3)]2~, in which pentacoordinate titanium atom s are associated via the nitrogen atoms o f the silylimido groups. (PPh4)2[TiCl4(OSPCl2)]2 has been prepared by the reaction o f PPh^fOSPClJ with titanium tetrachloride in C H 2C12 solution as orange crystals. (Space group P I , Z = 1, 3242 observed unique reflections, R = 0.033). Lattice dim ensions at 193 K: a = 1114.8(2), b = 1190.6(2), c = 1218.7(2) pm, a = 72.18(1)°, ß = 85.45(1)°, y = 69.19(1)°. The structure consists o f PPh4+ ions and centrosymmetric dimeric anions [TiCl4(O SPCl2)]^~, in which hexacoordinate titanium atom s are associated via two chlorine atoms. The OSPCl2_ group is coordinated via the oxygen atom. 
  Reference    Z. Naturforsch. 47b, 1386—1392 (1992); eingegangen am 9. März 1992 
  Published    1992 
  Keywords    Dimeric Titanium Complexes, Synthesis, IR Spectra, Crystal Structure 
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 TEI-XML for    default:Reihe_B/47/ZNB-1992-47b-1386.pdf 
 Identifier    ZNB-1992-47b-1386 
 Volume    47 
144Author    Wolfgang Tremel, Bernt Krebs, Klaus Greiwe, Wolfgang Simon, Hans-Oscar Stephan, Gerald HenkelRequires cookie*
 Title    [Mn(SPh)3Cl]2-, [Mn(SPh)3Br)2_, [Mn(SePh)4]2-, [Mn(TePh)4]2-, and ICo4(SPh)6Cl4l2-: New Mixed Halide/Thiolate and Chalcogenolate Complexes of Manganese and Cobalt  
 Abstract    The reactions of 1:1:1 m olar ratio mixtures of N aSPh/M nC l2/E t4NBr and N aSPh/CoCl2/ Et4NCl in methanol afford the com pounds [Et4N]4[Mn(SPh)3Br][Mn(SPh)3Cl] (1) and 
  Reference    Z. Naturforsch. 47b, 1580—1592 (1992); received February 7 1992 
  Published    1992 
  Keywords    Transition Metal Chalcogen Complexes, Synthesis, X-Ray Structure 
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 Identifier    ZNB-1992-47b-1580 
 Volume    47 
145Author    Adalbert Lossin, Gerd MeyerRequires cookie*
 Title    Dimere und Ketten in Praseodym(III)acetat-sesquihydrat, Pr(CH3COO)3 * 1,5 H20 Dimers and Chains in Praseodymium(III)acetate-sesquihydrate, Pr(C H 3C OO)3-1.5 H20  
 Abstract    Pr(C H 3COO)3-1.5H-,0 crystallizes with the triclinic system. P i (no. 2), Z = 4, a = 844.2(4), b = 1009.8(5), c = 1340.1(7) pm, a = 87.10(5), ß = 76.25(6), y = 75.65(2)°, Vm = 161.9(1) cm3/ mol, R = 0.049, Rw = 0.035. The crystal structure contains centrosymmetric dimers {[Pr(CH3C 0 0) 4(H 20)]~}2 and one-dimensional chains i,[Pr(CH3C 0 0) 2(H 20)]+ along the [100] direction. Both units are built up by bridging acetate groups. The chains are linked by the dimers to layers parallel (101) sharing oxygen atoms. Crystal water molecules between these planes form hydrogen bonds to neighbouring layers. 
  Reference    Z. Naturforsch. 47b, 1602—1608 (1992); eingegangen am 14. April 1992 
  Published    1992 
  Keywords    Praseodymium Acetate, Sesquihydrate, Synthesis, Crystal Structure, Thermal Behaviour 
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 Identifier    ZNB-1992-47b-1602 
 Volume    47 
146Author    Alfred-Dirk Bacher, Ulrich Müller, K. Arin Ruhlandt-SengeRequires cookie*
 Title    Synthese und Kristallstruktur von [K(18-Krone-6)]2S6 * 2 CH3CN Synthesis and Crystal Structure of [K( 18-Crown-6)]2S6 * 2 C H 3CN  
 Abstract    [K(18-crown-6)]2S6-2 C H 3CN was obtained from K2S5 and 18-crown-6 in acetonitrile. The crystalline com pound easily loses the incorporated acetonitrile. Its crystal structure was deter­ 
  Reference    Z. Naturforsch. 47b, 1673—1676 (1992); eingegangen am 11. August 1992 
  Published    1992 
  Keywords    Potassium-Crown Hexasulfide, Synthesis, Crystal Structure 
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 Identifier    ZNB-1992-47b-1673 
 Volume    47 
147Author    Sabine Kühnei, Klaus-Jürgen RangeRequires cookie*
 Title    Darstellung und Kristallstruktur von Rubidiumdicyanoargentat(I), Rb|Ag(CN)2] * 0,4 H 20 Synthesis and Crystal Structure o f Rubidium Dicyanoargentate(I), Rb[Ag(CN)2] * 0,4 H 20  
 Abstract    Rb[A g(C N)2] 0 ,4 H 20 was synthesized by reaction o f silver cyanide with RbOH and liquid 
  Reference    Z. Naturforsch. 48b, 133—139 (1993); eingegangen am 3. September 1992 
  Published    1993 
  Keywords    Rubidium Dicyanoargentate(I), Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/48/ZNB-1993-48b-0133.pdf 
 Identifier    ZNB-1993-48b-0133 
 Volume    48 
148Author    Adalbert Lossin, Gerd MeyerRequires cookie*
 Title    CsPr2(CH3COO)7, ein caesiumarmes wasserfreies ternäres Caesium-Praseodym-Acetat CsPr2(C H 3COO)7, a Cesium Poor Anhydrous Ternary Cesium Praseodymium (III) Acetate  
 Abstract    Single crystals of CsPr2(CH 3CO O)7 were obtained from an acetic acid solution of Pr(CH 3COO)3-H-,0 and C s ^ O j in a m olar ratio of 4:1 at 120 °C. It crystallizes in the triclinic system', PT (no. 2), Z = 2, a = 1028.1(5), b = 1034.6(5), c = 1199.4(6) pm, a = 84.82(2), ß = 67.07(3), y = 76.01(2)°, Vm = 343.3(3) cm3/mol, R = 0.031, R w = 0.027. The crystal structure contains infinite chains, i[P r2(CH 3COO)6], running along the [1 1 0] direction. The chains are built up by bridging acetate ions coordinated to two crystallographically different P r3+ ions which are both surrounded by 9 oxygen ligands. These chains are linked by "intercalated" Cs(CH3COO) to layers parallel (100). C s+ has contacts to oxygen atoms of neighbouring layers, such that a three-dimensional network is formed. 
  Reference    Z. Naturforsch. 48b, 886—892 (1993); eingegangen am 8. M ärz 1993 
  Published    1993 
  Keywords    Cesium Praseodym Acetate, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/48/ZNB-1993-48b-0886.pdf 
 Identifier    ZNB-1993-48b-0886 
 Volume    48 
149Author    Blaschette Arm, Karl-Heinz Nagel, PeterG. JonesRequires cookie*
 Title    Polysulfonylamine, XLIV [1] Synthese von |Na(15-Krone-5)][N(S02CH3)2l und Kristallstruktur bei -9 5 °C Polysulfonylamines, XLIV [1] Synthesis of [Na(15-Crown-5)][N(S02C H 3)2] and Crystal Structure at -9 5 °C  
 Abstract    The complex [Na(15-crown-5)][N(S02C H 3)2] crystallizes at -2 5 °C from a methanol solu­ tion containing equimolar am ounts of N aN (S 0 2C H 3)2 and 15-crown-5. Its crystallographic data at -9 5 °C are: monoclinic, space group P2,/c, a = 852.1(5), b = 2731.9(12), c = 909.2(4) pm, ß = 115.53(4)°, V = 1.910 nm3, Z = 4, D v = 1.445 M gm 3. The structure in the solid state consists of ion pairs. The sodium cation is coordinated to the five oxygen atoms of the crown ether, one oxygen atom o f the anion, and to the nitrogen atom of the anion. The bond distances are N a-O (crow n) 238.7-247.2, Na sodium ion lies 78 pm out of the plane o f the crown the coronand is described. 
  Reference    Z. Naturforsch. 48b, 893—897 (1993); eingegangen am 5. Februar 1993 
  Published    1993 
  Keywords    Polysulfonylamines, (15-Crown-5)sodium Dimesylamide, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/48/ZNB-1993-48b-0893.pdf 
 Identifier    ZNB-1993-48b-0893 
 Volume    48 
150Author    Michael Plate, Peter Hofacker, WernerM. Assa, Birgit Schwarz, Bernhard Neumüller, Kurt DehnickeRequires cookie*
 Title    Synthese und Kristallstrukturen der Wolfram(VI)-Alkinkomplexe |WCl4(P h -C = C -I)(T H F )l und [WCl4( P h -C = C -T e -C 4H9)(THF)| Synthesis and Crystal Structures o f the Tungsten(VI) Alkyne Complexes [WCl4(P h -C = C -I)(T H F )] and [WCl4( P h -C = C -T e -C 4H 9)(THF)]  
 Abstract    [WCl4(P h -C = C -I)(T H F)] has been prepared by the reaction o f mrns-[WCl4(SEt2)2] with P h -C = C -I in TH F solution, whereas [WCl4(P h -C = C -T e -n C 4H 9)(THF)] has been syn­ thesized by the reaction o f P h -C = C -T e -« C 4H 9 with tungsten hexacloride in the presence o f C2C14 and THF. Both complexes were characterized by IR spectroscopy and by crystal struc­ ture determinations. [WCl4(P h -C = C -I)(T H F)]: Space group P 2,/c, Z = 4, 2617 observed unique reflections, R = 0.064. Lattice dimensions at -7 0 °C: a = 1518.2(3), b = 714.5(1), c = 1540.0(3) pm, ß = 90.09(3)°. [WCl4(P h -C = C -T e -« C 4H9)(TH F)]. Space group P 1, Z = 2, 3911 observed unique reflec­ tions, R = 0.067. Lattice dimensions at 20 °C: a = 844.0(3), b = 974.6(4), c = 1002.4(3) pm, a = 76.00(4),/? = 105.14(1), y = 82.03(3)°. Both complexes have molecular structures, in which the tungsten atom s are seven-coordi­ nate by four chlorine ligands, by the two alkyne carbon atom s, and in trans position to the latter by the oxygen atom o f the T H F molecule. The WC bond lengths are 198 and 200(1) in the telluro complex and 206 and 196(1) pm in the iodine derivative. 
  Reference    Z. Naturforsch. 48b, 1105—1111 (1993); eingegangen am 21. April 1993 
  Published    1993 
  Keywords    Tungsten Alkyne Complexes, Synthesis, IR Spectra, Crystal Structure 
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 Identifier    ZNB-1993-48b-1105 
 Volume    48 
151Author    Herrn Prof, DrRequires cookie*
 Title    Zur Struktur des Pentaazadienidions [tol-N =N -N -N =N -tol]  
 Abstract    _. Synthese und Kristallstruktur von Cs2(18-Krone-6)(tolN5tol)2 und (NH4)[Cr(NH3)6(H20) 4](tolN5tol)4 T h e S tru c tu re o f th e P e n ta a z a d ie n id e A n io n [ to l-N = N -N -N = N -to l] _. S yn th esis a n d C ry sta l S tru c tu re o f C s2(1 8 -C ro w n -6)(to lN 5to l)2 an d (N H 4)[C r(N H 3)6(H 20) 4] (to lN 5to l)4 S u san n e D ie te ric h , Jo a c h im S träh le* A concentrated solution of CsCl, 18-crown-6, and to l-N = N -N (H)-N = N -to l in aqueous am m onia affords Cs2(18-crown-6)(tolN5tol)2, which crystallizes in the triclinic space group P 1 with a = 852.6(2), b = 1139.4(3), c -1373.9(4) pm, a = 104.17(3),ß = 95.94(2), y = 110.74(2)°, Z = 1. In the structure centrosym m etrical [Cs2(18-crown-6)]2+ moieties are packed with pairs of l,5-bis(tolyl)pentaazadienide anions to built up columns along [100]. The N -N distances N 1 -N 2 = 128 pm and N 4 -N 5 = 129 pm in the pentaazadienide anions indicate localized double bonds, while the distances N 2 -N 3 and N 3 -N 4 of 134 pm can be assigned to single bonds. A m ixture of C r(N H 3)^+ and tolN N N (H)N N tol in concentrated aqueous am monia yields triclinic (N H 4)[C r(N H 3)6(H 20) 4](tolN 5tol)4 crystallizing in the space group P 1 with the lattice param eters a = 1561.1(1), b = 1619.3(3), c = 1703.3(2) pm, a = 107.03(1), ß = 116.81(1), y = 101.75(1)°, Z = 2. The structure contains tolN5toh anions, NH^ cations and [C r(N H 3)6(H 2Ö)4]3+ complexes in which four triangular faces of the Cr(N H 3)6 octahedron are capped by w ater molecules which are linked via hydrogen bonds. Within the pentaazadienide anions which are connected with the [Cr(N H 3)6(H 20) 4]3+ complexes also via hydrogen bonds an indication for localized double bonds N 1=N2 and N 4=N 5 has been obtained. 
  Reference    Z. Naturforsch. 48b, 1574—1580 (1993); eingegangen am 26. Juli 1993 
  Published    1993 
  Keywords    Pentaazadienide A nion, Synthesis, Crystal Structure 
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 Identifier    ZNB-1993-48b-1574 
 Volume    48 
152Author    Z. NaturforschRequires cookie*
 Title    Die isoelektronischen Molekülkomplexe TiCl3(NPPh3) und TiCl3(OSiPh3)  
 Abstract    The Isoelectronic M olecular C om plexes TiC l3(N P P h 3) and T iC l3(O SiPh3) Thilo R übenstahl, D o ro th ea W olff von G udenberg, F ra n k W eller, K u rt D ehnicke* TiCl3(NPPh3) and TiCl3(OSiPh3) have been prepared from titanium tetrachloride and Me3SiNPPh3 and HOSiPh3, respectively. Both complexes were characterized by IR spectrosco­ py and by crystal structure determmations. TiCl3(N PPhj): Space group R3, Z = 6, structure analysis with 959 observed unique reflec­ tions, R = 0.039. Lattice dimensions at -6 8 °C: a = b = 1370.5(7), c = 1845.9(9) pm. TiCl}(OSiPh3): Space group P2,/c, Z = 8, structure analysis with 4549 observed unique re­ flections, R = 0.049. Lattice dimensions at 19 °C: a = 2127.7(2), b = 947.2(1), c = 2136.8(1) pm, ß = 105.081(5)°. Both complexes form monomeric molecules in which the titanium atom is tetrahedrally coordinated by three chlorine atoms, the nitrogen atom of the phosphorone iminato ligand and the oxygen atom of the silyloxy group, respectively. The bond lengths TiN of 171.9(4) pm and TiO of 171.0(3) (in average) correspond to double bonds. 
  Reference    (Z. Naturforsch. 49b, 15—20 [1994]; eingegangen am 7. September 1993) 
  Published    1994 
  Keywords    Monomerie Titanium Complexes, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-0015.pdf 
 Identifier    ZNB-1994-49b-0015 
 Volume    49 
153Author    Dieter Sellmann+, Helge Friedrich, Falk Knoch, Matthias MollRequires cookie*
 Title    Übergangsmetallkomplexe mit Schwefelliganden, C*. Unerwartet einfache Bildung von Diazen-Komplexen und ein neuer Typ von Diastereomerie: [/#-N2H2{Fe(PPr3)('S4')}2] und analoge Komplexe mit [FeS]-Zentren. ( 'S /2-= l,2-Bis(2-mercaptophenylthio)ethan(2-)) Transition Metal Complexes with Sulfur Ligands, C*. Unexpectedly Facile Formation of Diazene Complexes and a New Type of Diastereomerism: [a-N2H2{Fe(PPr3)('S4')}2] and Analogous Complexes with [FeS]-Centers. ('S4'2~ = l,2-Bis(2-mercaptophenylthio)ethane(2-))  
 Abstract    Single pot reactions of FeCl2-4H20 with the tetradentate thioether-thiol 'S4-H 2' = 1,2-bis(2-mercaptophenylthio)ethane, phosphines such as PEt3, PPr3 or PBu3, and a ca. 40-fold excess of N2H4-H20 yield, in the presence of air, diazene complexes of the general formula [M-N2H2{Fe(PR3)('S4')}2]. In contrast to previous syntheses of diazene complexes, the yields can excel 80%, and the syntheses can be carried out on a 10 g scale. [M-N2H2{Fe(PPr3)('S4')}2], 1 and [M-N2H2{Fe(PEt3)('buS4')}2], 2 were characterized by X-ray structure analysis. 2 contains 'buS4'2-= l,2-bis(3,5-ditertiarybutyl-2-mercaptophenylthio)-ethane(2-), which is the tertiary-butyl derivative of 'S4'2-. 1 and 2 contain fram-HN=NH which bridges enantiomeric [Fe(PPr3)('S4')] or [Fe(PEt3)('buS4')] fragments. HN=NH is stabilized by 4c -6 e~-jr bonds, strong tricentric N -H — (S)2 bridges, and steric shielding. NMR studies show that centrosymmetric 1 isomerizes in solution at temperatures around 0 °C in order to give a diastereomerie diazene complex which is also centrosymmetric. The diastereomerism is traced back to bridging the chiral [Fe(PPr3)('S4')] fragments by frara-HN=NH in a differ­ ent way. The two different bridging modes are verified by X-ray structure analyses of analo­ gous ruthenium complexes. Because this new type of diastereomerism is basically caused by a different position only of the N -H — (S)2 bridges, it is termed hydrogen bridge diastereo­ merism. A mechanism for the isomerization is suggested. 1 exhibits three anodic waves in the cyclovoltammogram. The second wave indicates formation of the dication [1]2+, which is a redox isomer of the diprotonated (and as yet hypothetical) dinitrogen complex [a-N2{Fe(PPr3)('S4')}2]. The significance of [1]2+ and of its Lewis basic thiolate donors with respect to electrochemical reduction of molecular dinitrogen under mild conditions is dis­ cussed. 
  Reference    (Z. Naturforsch. 49b, 76—88 [1994]; eingegangen am 9. Juli 1993) 
  Published    1994 
  Keywords    Diazene, Iron Sulfur Complexes, Synthesis, X-Ray 
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 Identifier    ZNB-1994-49b-0076 
 Volume    49 
154Author    Thom As Schleid, Falk LissnerRequires cookie*
 Title    Oxidsulfidchloride der Lanthanide vom Typ M 4OS4Cl2 (M = L a-N d ) M 4OS4Cl2-Type Oxysulfide Chlorides of the Lanthanides (M = L a -N d )  
 Abstract    Oxysulfide chlorides, M4OS4Cl2, o f the lanthanides (M = L a -N d) are obtained upon the oxi­ dation o f the metals with sulfur in the presence o f MOC1 (or M 20 3) and MC13 in appropriate molar ratios. Additional NaCl or an excess o f MC13 serving as a flux provide even single crys­ talline material after reactions at 850 °C for seven days in sealed tantalum capsules. The crys­ tal structure o f M4OS4Cl2 (hexagonal, P 6 3mc, no. 186, Z = 2; M = La: a = 933.19(3), c = 701.22(4) pm, c/a = 0.7514, R = RH = 0.020; M = Ce: a = 925.49(3), c = 694.13(3) pm, c/a = 0.7500; M = Pr: a = 919.72(4), c = 688.53(4) pm, c/a = 0.7486; M = Nd: a = 914.25(4), c = 683.12(4) pm, c/a = 0.7472, R = 0.022, Rw = 0.019) contains isolated 0 2--centered (M 3+)4 te-trahedra which are surrounded by twelve S2-and six Cl-, capping vertices, edges, and faces o f each tetrahedron and linking to other [OM4] units. Basically, the structure is identical to that o f Ba4OCl6 if Ba2+ is substituted by M 3+ and 2/3 o f the CL anions are replaced by S2-to secure charge neutrality in M4OS4Cl2. Different models for the C L /S 2-replacement are presented on the basis o f comparisons o f the Madelung part o f the lattice energy (M A PLE) with the M APLE sum o f the binaries (M 20 3, M 2S3, and MC13). 
  Reference    Z. Naturforsch. 49b, 340 (1994); eingegangen am 27. September 1993 
  Published    1994 
  Keywords    Lanthanides, Oxysulfide Chlorides, Synthesis, Crystal Structure 
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 Identifier    ZNB-1994-49b-0340 
 Volume    49 
155Author    Frank Weller, Fritjof Schmock, Kurt Dehnicke, Kurt Findeisen Bayer-WerkRequires cookie*
 Title    Synthese, IR-Spektrum und Kristallstruktur von 1.3.5-Trichlortriazinium-hexachloroantimonat, [HC3N3C13]SbCl6 Synthesis, IR Spectrum and Crystal Structure of 1.3.5-Trichlortriazinium Hexachloroantim onate, [HC3N3Cl3]SbCl6  
 Abstract    ,3,5-Trichlortriazinium hexachloroantimonate has been prepared by the reaction of CCl2 = N-COCl with antimony pentachloride in boiling dichloromethane. The compound was characterized by IR spectroscopy and by a crystal structure determination. [HC3N3Cl3]SbCl6 crystallizes in the monoclinic space group P 2 Jn with four formula units per unit cell. 2503 observed unique reflections, R = 0.029. Lattice dimensions at 19 °C: a = 1314.1(1), b = 958.2(1), c = 1329.1(1) pm, ß = 117.113(5)°). The compound forms ion pairs via a linear N -H • • • Cl bridge, thus distorting the SbCl6~ ion from octahedral geometry. The C3N3 skeleton of the [HC3N3C13]+ ion is nearly planar, but the hydrogen atom lies about 30 pm out of this plane. 
  Reference    Z. Naturforsch. 49b, 360—364 (1994); eingegangen am 3. November 1993 1.3. 
  Published    1994 
  Keywords    5-Trichlortriazinium Salt, Synthesis, IR Spectra, Crystal Structure 1 
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 Identifier    ZNB-1994-49b-0360 
 Volume    49 
156Author    Andreas Ahle, K. Urt Dehnicke, CäciliaM. Aichle-Mössmer, Joachim SträhleRequires cookie*
 Title    Synthesis and Crystal Structure of [Na( 12-Crown-4)2]2[Fe4Se4Cl4]  
 Abstract    [N a(12-crow n-4)2]2[Fe4Se4Cl4] has been pre­ pared by the reaction o f FeCl2 with N a2Se4 in di-methylform amide solution in the presence o f 12-crown-4 as dark red crystals, which were char­ acterized by a_ crystal structure determination. Space group P 1, Z = 2, 6295 observed unique re­ flections, R = 0.085. Lattice dim ensions at 20 °C: a = 1397.3(3), b = 1501.8(4), c = 1570.1(4) pm, a = 85.86(2)°, ß = 64.06(2)°, y = 65.01(2)°. The structure consists o f [Na(12-crown-4)2]+ cations and cuban-like anions [Fe4Se4Cl4]2" with Fe — Fe contacts o f 282.8(3) pm. 
  Reference    Z. Naturforsch. 49b, 434 (1994); eingegangen am 30. September 1993 
  Published    1994 
  Keywords    Tetranuclear Iron Selenium Cluster Dianion, Synthesis, Crystal Structure 
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 Identifier    ZNB-1994-49b-0434_n 
 Volume    49 
157Author    Dieter Sellm, Helge Friedrich, Falk KnochRequires cookie*
 Title    Synthese und Struktur von *1,33N2H4 Transition Metal Com plexes with Sulfur Ligands, Cl*. Synthesis and Structure of N 2H 5[Fe(N 2H4)(S2C6H4)2] * 1,33 N 2H 4  
 Abstract    A ttem pts to coordinate N2H4 to [Fe(S2C6H 4)2] fragments lead to N2H 5[Fe(N2H 4)(S2C6H4)2], which crystallizes from M eOH/N2H 4 solutions as the solvate [(N2H 5){Fe(N2H4)(S2C6H4)2} T.33 N2H 4], 1, and has been characterized by X-ray structure analysis. 1 contains three discrete N2H 5+ cations, four N2H4 solvate molecules and three independent [Fe(N2H4)(S2C6H4)2] anions which are connected via an extended network of N -H —N and N -H —S bridges. N2H 5[Fe(N2H 4)(S2C6H4)2] and 1 contain high-spin Fe(III) centers and labile N2H4 ligands. Ubergangsmetallkomplexe mit Schwefelliganden, CI*. 
  Reference    Z. Naturforsch. 49b, 660—664 (1994); eingegangen am 22. Dezember 1993 
  Published    1994 
  Keywords    Iron Sulfur Hydrazine Complexes, Synthesis, X-Ray 
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 Identifier    ZNB-1994-49b-0660 
 Volume    49 
158Author    S. Möhr, Hk Müller-BuschbaumRequires cookie*
 Title    Uber ein gemischtvalentes Oxoniobat mit planaren Polygonen um Niob und Barium: BaNb2+Nb2+0 6 On a Mixed Valent Oxoniobate Containing Planar Polygons A round Niobium and Barium: BaNb2 +N b^+0 6  
 Abstract    Single crystals of B aN b30 6 were prepared by C 0 2-LA SER high temperature technique. The compound crystallizes with trigonal symmetry C fv-R 3 m , a = 11.4333, c -3.4949Ä , Z = 3. The new structure type is characterized by planar N b 0 4 and planar B a 0 6 polygons. The results are discussed with respect to related compounds like Ca0.75 Nb3O6 or N aNb30 6. 
  Reference    Z. Naturforsch. 49b, 915 (1994); eingegangen am 17. Februar 1994 
  Published    1994 
  Keywords    Barium, Niobium, Oxide, Synthesis, Crystal Structure 
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 Identifier    ZNB-1994-49b-0915 
 Volume    49 
159Author    YueQing Zheng, Arnold AdamRequires cookie*
 Title    Ein neues Carbonat mit Baylissit-Struktur: Rb2[M g(C 03)2(H 20 )4] A New Carbonate with Baylissite Structure: Rb2 [Mg(C0 3 )2(H 2 0 )4]  
 Abstract    The new complex carbonate Rb2[M g (C 0 3)2(HoC))4] crystallizes in the Baylissite-tvpe structure with a = 1130,4(3), b = 641,9(1), c = 703,3(2) pm, ß = 99,62(1)°, V EZ = 503,2(2), space group P2l/n (No. 14) and Z = 2. In comparison with the isostructural potassium compound the cell dimensions increase in b-and c-and decrease in ö-direction. This effect depends on the greater coordination number of Rb+ and the rigidity of strong hydrogen bonds. The carbonate anion exhibits significant deviations from D 3h-symmetry (C -O : 127,1(5)-130,2(5) pm, Z_ O -C -O : 117.9(4)-121,1(3)°). 
  Reference    Z. Naturforsch. 49b, 1368—1372 (1994); eingegangen am 25. April 1994 
  Published    1994 
  Keywords    M etal-Carbonato-Complex, Baylissite Type, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-1368.pdf 
 Identifier    ZNB-1994-49b-1368 
 Volume    49 
160Author    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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 Identifier    ZNB-1994-49b-1654 
 Volume    49 
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