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21Author    JuanB. Rodriguez, EduardoG. Gros, AngelM. StokaRequires cookie*
 Title    Synthesis and Activity of Juvenile Hormone Analogues (JHA)  
 Abstract    From geranylacetone and by the use of a variety of reagents, twelve analogues of the juvenile hormone III were synthesized. The compounds (5—16) have an isoprenic structure bearing at the extreme of the chain functional groups as carbonate, carbamate, thiolcarbonate, thiolcarbamate, carbonyloxyimino and thiol carbonyloxyimino. Compounds 5—9 present the normal unsaturated isoprenic chain while compounds 10—16 have a monoepoxide function. All the compounds were tested for their respective juvenile hormone activity for Triatoma infestans and Rhodniusprolixus. The most active compounds were those having a thiol carbonate group independently of the oxidation state of the molecule. The synthetic procedures and the biological results are discussed. 
  Reference    Z. Naturforsch. 43b, 1038—1042 (1988); received March 8. 1988 
  Published    1988 
  Keywords    Juvenile Hormone Analogues, Activity, Synthesis 
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 TEI-XML for    default:Reihe_B/43/ZNB-1988-43b-1038.pdf 
 Identifier    ZNB-1988-43b-1038 
 Volume    43 
22Author    Siegfried Pohl, Rainer Lötz, Detlev Haase, Wolfgang SaakRequires cookie*
 Title    Iodoantimonate der Zusammensetzung A + Sb 2 I 7 : Diskrete Anionen in (Me 4 N) 4 Sb 8 I 2 8 und (Me 3 S) 4 Sb 8 I 28 , polymere Ketten in (Me 3 NCH 2 Ph)Sb 2 I 7 (Me = CH 3 , Ph = C 6 H 5 ) Iodoantimonates of Composition A~Sb 2 I 7 ~: Discrete Anions in (Me 4 N) 4 Sb 8 I 28 and (Me 3 S) 4 Sb s I 28 , Polymerie Chains in (Me 3 NCH 2 Ph)Sb 2 I 7 (Me = CH 3 , Ph -C 6 H 5 )  
 Abstract    The reaction of Sbl 3 with Me 4 NI, Me ? SI, and Me^NCH^Phl in acetonitrile (molar ratios 2:1) yields (Me 4 N) 4 Sb 8 I 28 (1). (Me,S) 4 Sb K I 28 (2). and (Me,NCH 2 Ph)Sb : I 7 (3), respectively. The struc-tures of 1—3 were determined from single crystal X-ray diffraction data. 1—3 crystallize in the monoclinic space group P2,/«. 2: a -1434.2(3). b -1484.1(4). c = 2102.6(4) pm. ß = 105.4(1)°, Z = 2. 1: a = 1441.7(1), b = 1545.1(1). c = 2117.3(1) pm. ß = 106.4(1)°, Z = 2. 3: a = 1004.4(1). b = 1378.8(1). c = 1899.3(2) pm. ß = 94.2(1)°. Z = 4. The structures of 1 and 2 are very similar and consist of isolated cations and anions. The Sb s I 28 
  Reference    Z. Naturforsch. 43b, 1144—1150 (1988); eingegangen am 24. Mai 1988 
  Published    1988 
  Keywords    Iodoantimonates, Synthesis, Crystal Structure 
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 Identifier    ZNB-1988-43b-1144 
 Volume    43 
23Author    CarlD. Habben, Mathias NoltemeyerRequires cookie*
 Title    Molekül-und Kristallstruktur  
 Abstract    des l,l-Diethyl-3,5-dimethyl-lA 6 ,4,2,6,3,5-dithiadiazadiborins Molecular and Crystal Structure of l,l-Diethyl-3,5-dimethyl-H 6 ,4,2,6,3,5-dithiadiazadiborine The title compound, isolated from the reaction of SS-diethyl-N,N'-bistrimethylsilylsulfodiimide and 3.5-dimethyl-l,2,4-trithiadiborolane, crystallizes in space group Pbca with cell constants a — 1218.7(6), b = 1295.8(6), c = 1455.7(9) pm, V = 2.2987 nm 3 , Z = 8, Q — 1.167 MgirT 3 . The X-ray structure was refined to R = 0.053. 
  Reference    Z. Naturforsch. 43b, 1683—1684 (1988); eingegangen am 11. August 1988 
  Published    1988 
  Keywords    Crystal Structure, Synthesis, Dithiadiazadiborines 
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 Identifier    ZNB-1988-43b-1683_n 
 Volume    43 
24Author    Petra Krieger-Beck, A. Ndreas Brodbeck, Joachim SträhleRequires cookie*
 Title    Synthesis and Structure of K2A u3, a New Phase in the System Potassium —Gold  
 Abstract    K2A u 3 is obtained from the elem ents in a sealed Ta am poule as air-sensitive needles with a golden lustre. It crystallizes in the orthorhom bic space 
  Reference    Z. Naturforsch. 44b, 237—239 (1989); eingegangen am 18. O ktober 1988 
  Published    1989 
  Keywords    Dipotassium Triauride, Synthesis, Crystal Structure 
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 Identifier    ZNB-1989-44b-0237_n 
 Volume    44 
25Author    HansG. Eorg Stammler, Johannes WeissRequires cookie*
 Title    Synthese  
 Abstract    und Kristallstruktur von (S4N3)2Se2Cl10, (S4N3)2Se2CI6 und [(S4N3)SeCl5]n Synthesis and Crystal Structure of (S4N3)2Se2C l10, (S4N3)2Se2Cl6, and [(S4N 3)SeCl5]" (S4N 3)2S e2C l10, (S4N 3)2Se2Clft and [(S4N 3)SeC l5]" are formed by the reaction o f S4N 4, Se2Cl2, and SO C l2. The structures o f the three com pounds where determ ined by X-ray diffraction. The yellow crystals o f (S4N 3)2Se2C l10 are monoclinic, space group P 2,/a, a = 817.5(2) pm , b = 1790.4(5) pm, c = 843.1(6) pm, ß = 104.31(4)°, Z = 2. The Se2C l102~ anion consists o f 2 Cl-bridged distorted octahedra. (S4N 3)2Se2Cl6 forms red m onoclinic crystals, space group P2,/c, a = 1036.5(3) pm , b = 1376.5(5) pm , c = 1400.4(4) pm ,/3 = 100.65(2)°, Z = 4. In the Se2Cl62" anion the Se atoms have a square planar environm ent. The yellow crystals o f (S4N 3)SeC l5 are orthorhom bic, space group P 2 12 12 1, a = 734.2(3) pm , b — 989.4(4) pm , c = 1627.4(6) pm , Z = 4. In the SeC l5_ anion the Se atom has an octahedral environm ent o f chlorine atom s, thus forming a polym eric structure. 
  Reference    Z. Naturforsch. 44b, 1483 (1989); eingegangen am 5. Mai 1989 
  Published    1989 
  Keywords    Thiotrithiazyl-chloroselenates, Synthesis, Crystal Structure 
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 Identifier    ZNB-1989-44b-1483 
 Volume    44 
26Author    Georg Ingram, Peter Jaitner, KarlEberhard SchwarzhansRequires cookie*
 Title    Synthese und Charakterisierung ruthenocen-und osmocenhaltiger Hetero-Oligometallocene Synthesis and Characterization of Hetero-Oligometallocenes Containing Ruthenocene and Osmocene  
 Abstract    Improved syntheses o f ruthenocene (Rue) and osm ocene (Osc) are described. These lithiated metallocenes (R ucLi,_3 and OscLi,_3) react with cobaltocenium-hexafluorophosphate (C oc+PF6~) to give the corresponding oligom etallocenes C oc+-R u c P F 6~ (1), l,l'-(C o c +)2-Ruc(PF6)2 (2), C oc+-O sc P F 6" (4), and l,l'-(C o c +)2-O sc (P F 6)2 (5). The products were charac­ terized by IR, MS, N M R and elemental analysis. 
  Reference    Z. Naturforsch. 45b, 781 (1990); eingegangen am 15. Dezember 1989 
  Published    1990 
  Keywords    Hetero-Oligometallocenes, Ruthenocene, Osmocene, Synthesis 
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 TEI-XML for    default:Reihe_B/45/ZNB-1990-45b-0781.pdf 
 Identifier    ZNB-1990-45b-0781 
 Volume    45 
27Author    SylviaM. Agull, Bernhard Neumüller, K. Urt DehnickeRequires cookie*
 Title    Synthese und Kristallstrukturen der Polyselenido-Mercurate (PPh4)2|H g(Se4)2| und |Cs(18-Krone-6)|2|H g2(Se4)3l Syntheses and Crystal Structures of the Polyselenido M ercurates (PPh4)2[Hg(Se4)2] and [Cs(18-Crown-6)]2[Hg2(Se4)3]  
 Abstract    (PPh4)2[Hg(Se4)J has been prepared by the reaction o f (PPh4)2[Sn(Se4)3] with H g(C H 3COO)2 in dimethylformamide (D M F) solution. [Cs(18-crown-6)]2[Hg2(Se4)3] has been prepared by the reaction o f a lithium polyselenide solution in D M F with H g(C H 3COO)2 in the presence o f CsBr and 18-crown-6. Both com pounds are obtained as dark red crystals and characterized by X-ray structure determinations. (PPh4) 2[H g(Se4) 2]: Space group P 2,/c, Z = 4, 3021 observed unique reflexions, R = 0.082. Lattice dim ensions at 20 °C: a = 1046.0(3), b = 2129.4(2), c = 2213.1(3) pm,/? = 97.62(2)°. The com pound consists o f PPh4+ ions and anions [Hg(Se4)2]2", in which the mercury atom is a spi-rocenter o f puckered HgSe4 rings. [ Cs(18-crown-6) J2[H g2(Se4)3J: Space group la, Z = 4, 2859 observed unique reflexions, R = 0.074. Lattice dimensions at 20 °C: a = 2018(1), b = 1097.0(2), c = 2317.1(5) pm, ß = 99.40(3)°. The compound forms an ion triple which originates from Cs-Se contacts o f 382 to 390 pm with the [Hg2(Se4)3]2~ ion. The latter can be described as a [FlgtSe^JJ2-ion, which has contacts with a HgSe4 fragment. 
  Reference    Z. Naturforsch. 46b, 985—9 (1991); eingegangen am 12. Dezember 1990 
  Published    1991 
  Keywords    Polyselenido Mercurates, Synthesis, Crystal Structure 
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 Identifier    ZNB-1991-46b-0985 
 Volume    46 
28Author    Bernhard NeumüllerRequires cookie*
 Title    Darstellung und Kristallstruktur von [(Me3Si)2CH(7-Pr)InCll2 Synthesis and Crystal Structure o f [(Me3Si)2CH(/-Pr)InCl]2  
 Abstract    The title com pound 1 has been prepared by the reaction o f z-PrlnCl, with LiC H (SiM e3)2 in diethylether at -3 0 °C. The colorless substance 1 was characterized by N M R , IR, and RE spectroscopy, as well as by mass spectrometry. 1 is dimer in solution and the solid state and crystallizes in the space group P 2 ,/c with the cell parameters a = 1206.4(3) pm, b = 905.7(2) pm, c = 1591.2(5) pm, and ß = 101.18(2)°. The unit cell contains two centrosymmetri-cal dimeric molecules. 
  Reference    Z. Naturforsch. 46b, 1539—1543 (1991); eingegangen am 12. April 1991 
  Published    1991 
  Keywords    Diorganoindiumchloride, Synthesis, Crystal Structure 
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 Identifier    ZNB-1991-46b-1539 
 Volume    46 
29Author    K. Arin Ruhlandt-Senge, AlfredDirk Bacher, G. Ertraude Koellner, Birgit Siewert, Ulrich MüllerRequires cookie*
 Title    Tetraphenylphosphonium-nonachlorodivanadat(III), (PPh4)3[V2Cl9l * 7 CH2C12 Tetraphenylphosphonium Nonachlorodivanadate(III), (PPh4)3[V2Cl9] * 7 C H 2C12  
  Reference    Z. Naturforsch. 47b, 814—818 (1992); eingegangen am 14. O ktober 1991 
  Published    1992 
  Keywords    N onachlorodivanadate, Synthesis, Crystal Structure 
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 Identifier    ZNB-1992-47b-0814 
 Volume    47 
30Author    Gudrun Stieglitz, Bernhard Neumüller, K. Urt DehnickeRequires cookie*
 Title    Synthesen und Kristallstrukturen der Lithiumphosphide { Li(DME)[P(f-Bu)2]} 2 und [Li(DM E)PPh2l00 Syntheses and Crystal Structures of the Lithium Phosphides {Li(DME)[P(/-Bu)2]}2 and [Li(DM E)PPh2]0 0  
 Abstract    The title com pounds have been prepared by the reaction o f rc-butyllithium with the corre­ sponding diorganophosphanes H PR 2 (R = r-Bu, Ph) in D M E solutions. Both compounds were characterized by crystal structure determinations. {Li(DM E)[P(f-Bu)2]}2: Space group P 1, Z = 1, 2027 observed unique reflections, R = 0.055. Lattice dimensions at —80 °C: a = 879.9(3), b = 986.3(1), c = 1064.0(2) pm, a = 70.69(1)°, ß = 70.63(2)°, y -69.89(2)°. The com pound forms centrosymmetric dimers o f symmetry Q with L i-P bond lengths o f 260.0 and 257.3 pm for the Li2P2 four-membered ring. [Li(DM E)PPh2]0C : Space group P 2 ,/«, Z = 4. 3437 observed unique reflections, R = 0.055. Lattice dimensions at -8 0 °C: a = 1034.8(2), b = 812.48(9), c = 1978.4(3) pm, ß = 103.30(2)°. The com pound forms polymeric chains via LiP bridges with L i-P bond lengths o f 256.3 and 254.1 pm. 
  Reference    Z. Naturforsch. 48b, 156 (1993); eingegangen am 8. Oktober 1992 
  Published    1993 
  Keywords    Lithium Phosphides, Synthesis, Crystal Structure 
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 Identifier    ZNB-1993-48b-0156 
 Volume    48 
31Author    Jorge Blanco, Eduardo Gayoso, JoseManuel Vila, Miguel Gayoso, CäciliaM. Aichle, -. M. Össmer, Joachim SträhleRequires cookie*
 Title    Synthesis and Structure of Di-I/i-acetato(0,0')-ferrocenylmethyliden- 2,4,6-trimethylaniline(N,C)-palladium(II)l  
 Abstract    Di-[//-acetato(0,0')-ferrocenylmethylidene-2,4,6-trimethylaniline(N,C)-palladium(II)], 
  Reference    Z. Naturforsch. 48b, 906—910 (1993); received M arch 8 1993 
  Published    1993 
  Keywords    Cyclometallation, Synthesis, Crystal Structure 
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 Identifier    ZNB-1993-48b-0906 
 Volume    48 
32Author    Jörn Müller, PetraEscarpa Gaede, Ke QiaoRequires cookie*
 Title    ^-Olefin-Iridium-Komplexe, XXII [1] C -H -Aktivierung von aromatischen und aliphatischen Solvensmolekülen RH bei der Reaktion von [Cp*IrCI2 ] 2 mit Butadienmagnesium unter Bildung von [Cp*Ir(773-C4H 7)R] sowie Kristallstruktur von [Cp*Ir(i/3-C4H 7)C6H 5] jr-Olefin Iridium Complexes, XXII [1] C -H Activation of Aromatic and Aliphatic Solvent Molecules RH in the Reaction of [Cp*IrCl2 ] 2 with Butadienemagnesium with Formation of [Cp*Ir(?;3 -C4 H 7 )R], and Crystal Structure of [Cp*Ir(773 -C4 H 7 )C6 H 5] Activation of C -H , (l-Methylallyl)(pentamethylcyclopentadienyl)iridium-a-organyl Com­ plexes  
 Abstract    Reactions of [Cp*IrCl2]2 (Cp* = ^3-C5M e5) with [MgC4H6 -2 THF]" at low temperature give [Cp*Ir(^4-C4H6)] together with [Cp*Ir(/73-C4H 7)R] compounds, the latter being formed via C -H activation of solvent molecules RH (RH = benzene, toluene, anisole, thiophene, furane, N-methylpyrrole, pentane, cyclohexane. THF). In the case of pyrrole, C -N -activation occurs. The ratio of syn and anti isomers of the 1-methylallyl com plexes as well as the sites o f C -H activation of RH were investigated by NM R spectrometry. An enantiomorphous crystal of [Cp*Ir(773-C4H7)C6Hs] was characterized by X-ray diffraction analysis which reveals trigonal planar coordination at the Ir atom and an exo, syn conformation o f the 1-methylallyl ligand. A mechanism of the reaction which involves 16-electron intermediates is discussed. The corresponding system [Cp*RhCl2]2/butadienemagnesium/RH gives only [Cp*Rh(>/4-C4H6)], and no C -H activation is observed. 
  Reference    Z. Naturforsch. 49b, 1645—1653 (1994) 
  Published    1994 
  Keywords    Synthesis, NMR Spectra, Crystal Structure 
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 Identifier    ZNB-1994-49b-1645 
 Volume    49 
33Author    Z. NaturforschRequires cookie*
 Title    A -P r 2S3, D -H o2S3 und E -Y b 2S3: Synthese und Einkristallstrukturuntersuchungen  
 Abstract    The oxidation of reduced chlorides (MC12) or chloride-hydrides (MC1HV) of the lanthani­ des with sulfur (700-850 °C, 7 d, sealed tantalum capsules or evacuated silica vessels) usually results in the formation of the sesquisulfides M2S3 as the main products. In the presence of appropriate fluxes (e.g., alkali halides), the products often are obtained as single crystals, and the flux decides which modification is favoured. Ternary halides of the trivalent lanthanides with the corresponding alkali metal can mostly be found as the second components. Crystal growth and structural investigations of thus produced single crystals of Pr2S3 (from PrClH() 67 + S + NaCl, 5:5:1, A type: orthorhombic, Pnma (No. 62), Z = 4, a = 748.22(5), b = 405.51(3), c = 1560.74(9) pm, R = 0.024, Rw = 0.020), Ho^S, (from U -H o^S , + KI, 1:1, D type: mono­ clinic, P 2xim (No. 12), Z = 6, a = 1746.15(9), b = 400.23(3), c = 1012.43(6) pm, ß = 98.529(4)°, R = 0.041, Rw = 0.035), and YbiS3 (from T-Yb^S^ + KI, 1:1, E type: trigonal, R 3c (No. 167), Z = 6, a = 674.97(2), c = 1820.11(9) pm'. R = 0.019, Rw = 0.018) are reported here. In accordance with the lanthanide contraction, the trivalent cations (M3+) exhibit sulfur coordination numbers of 7 and 8 in A -P r 2S3, 6 and 7 in D -H o 2S3, and 6 in E -Y b 2S3 (corundum-type structure). 
  Reference    Z. Naturforsch. 51b, 733—738 (1996); eingegangen am 4. Oktober 1994 
  Published    1996 
  Keywords    Lanthanides, Sesquisulfides, Synthesis, Crystal Structure 
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 Identifier    ZNB-1996-51b-0733 
 Volume    51 
34Author    H. V., A. Fischerb, P. G. JonesbRequires cookie*
 Title    Eine unerwartete Synthese des Triphenyphosphazenium-chlorids, [(C6H5)3PNH2]+CI_ und eine Neubestimmung seiner Kristallstruktur  
 Abstract    Triphenylphosphazenium chloride has been prepared by the reaction of triphenylphos-phine with trimethylsilylazide in impure, wet dichloromethane. Yields are improved as stoi­ chiometric quantities of w ater are added. Colourless crystals are obtained by recrystallization from the same solvent. The crystals are triclinic, space group P I, Z=2, a = 894,6(3), b -979,8(3), c = 1142,9(4) pm, a = 107,27(3), ß = 93,70(3), y = 92,97(3)°. In the solid state the compound exists as [(C6H 5)3PNH2]+ cations, and Cl-anions. Dimeric units are formed by H-bonding. The crystal structure contains one molecule CH 2C12 per one molecule (C6H 5)3PNH2C1. The cation has a slightly irregular tetrahedral geometry around the P-atom with a relatively short P-N bond. 
  Reference    Z. Naturforsch. 51b, 865—868 (1996); eingegangen am 21. O ktober 1995 
  Published    1996 
  Keywords    Triphenylphosphazenium Chloride, Synthesis, Crystal Structure 
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 Identifier    ZNB-1996-51b-0865 
 Volume    51 
35Author    G. Eorge Sosnovsky, Jan Lukszo, C. Ert, BraschRequires cookie*
 Title    Preparation of an Aminoxyl Analog of the Anticancer Agent Miltefosine  
 Abstract    The synthesis and a few properties of hexadecyl 2-[N,N-dimethyl-N-(2,2,6.6-tetramethyl-l-oxyl-piperidin-4-yl)ammonio] ethyl phosphate are described. This compound is a spin la­ beled analog of the antineoplastic drug hexadecylphosphocholine (Miltefosine). 
  Reference    Z. Naturforsch. 51b, 888—890 (1996); received Decem ber 11 1995 
  Published    1996 
  Keywords    Anticancer Agents, Aminoxyl, Nitroxyl, Synthesis 
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 Identifier    ZNB-1996-51b-0888 
 Volume    51 
36Author    N. Stock, W. SchnickRequires cookie*
 Title    Synthese, Kristallstruktur und Eigenschaften von l,l>3 ?3 ?3 -Pentaam*n° -l  
 Abstract    oxo-lA 5 ,3A 5 -diphosphaz-2-en, (NH2)2 (0)P-N=P(NH2)3 Synthesis, Crystal Structure, and Properties of 1,1,3,3,3-Pentaam ino-l-oxo-l A 5 , 3 A 5 -diphosphaz-2-ene, (NH2)2(0)P-N =P(N H i)3 Coarse crystalline (NH2)2(0)P-N=P(NH2)3 is obtained from a NH;* saturated CH2C12 suspen­ sion of (NH2)2(0)P-N=P(NH2)3 NH4C1 at room temperature. (NH2)2(0)P-N=P(NH2)3 NH4C1 is synthesized" by slow addition of C12(0)P-N=PC13 to a solution of NH3 in CH2C12 at -78 °C. Excess NH4C1 is removed by treatment with HNEt2 followed by extraction with CH2C12. The crystal structure of (NH2)2(0)P-N=P(NH2)3 has been determined by single crystal X-ray methods (P2(/c; a = 1462.8(3), b = 944.8(2), c = 1026.9(2) pm, /3 = 110.69(3)°; Z = 8). In the unit cell there are two crystallographically unique molecules. They form a three dimensional network by intermolecular hydrogen bonding interactions (N-H- • N > 313 pm. N-H • 0 > 293 pm). The investigation of the thermal properties shows decomposition with evolution of NH3 above 80 °C. 
  Reference    Z. Naturforsch. 51b, 1079—1083 (1996); eingegangen am 7. Dezember 1995 
  Published    1996 
  Keywords    Aminophosphazene, Synthesis, Crystal Structure Precursor 
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 Identifier    ZNB-1996-51b-1079 
 Volume    51 
37Author    Wolfgang Czado, Ulrich MüllerRequires cookie*
 Title    (PPh4)4Sb8Br28 Tetraphenylphosphonium Ikosioctabromooctaantimonate(III), (PPh4)4Sb8Br28  
 Abstract    The title compound was obtained by the reaction of PPh4Br, Sb2Se3, and bromine in dichloro-methane. Its crystal structure was determined by X-ray diffraction. Crystal data: a = 1249.1(2), b = 1307.8(2), c = 2152.3(4) pm, a = 102.93(2), ß = 100.83(2), 7 = 100.42(2)°, Z = 2, triclinic, space group P I . (PPh4)4Sb8Br28 is isotypic with (PPh4)4Sb8I28. The Sb8Br284~ ion can be taken as the association product of eight SbBr3 molecules with four B r-ions. Each Sb atom has a distorted octahedral coordination with three shorter (252 to 274 pm) and three longer (300 to 353 pm) Sb-Br bonds. The octahedra share common edges in two parallel rows of four octahedra each. The arrangement of the 28 bromine atoms corresponds to a section of a closest packing of spheres. Tetraphenylphosphonium-ikosioctabromooctaantimonat(III), 
  Reference    Z. Naturforsch. 51b, 1245—1247 (1996); eingegangen am 22. März 1996 
  Published    1996 
  Keywords    Ocataikosabromooctaantimonate, Synthesis, Crystal Structure 
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 Identifier    ZNB-1996-51b-1245 
 Volume    51 
38Author    StefanH. Orstm, AnnW. Olfgang SchnickRequires cookie*
 Title    Synthese  
 Abstract    , K rista llstru k tu r und Eigenschaften von 1 ,1 , 1 > 3 * 3 , 3 -H e x a a m i n o -lA 5,3A5-diphosphazenium ehlorid[(N H 2)3PNP(NH2)3]Cl Synthesis, C rystal Structure, and Properties of 1,1,1,3,3,3-Hexaam ino-1 A5,3A5-diphosphazenium Chloride [(N H 2)3PN P(N H 2)3]C1 [(NH2)3PNP(NH2)3 ]C1 has been prepared by a three step synthesis. The last step is the ammo-nolysis of [C13PNPC13]C1. Single crystals of 1,1,1,3,3,3-hexaamino-1 A \ 3As-diphosphazenium chloride were obtained from an acetonitrile solution in a temperature gradient between 60 °C and room temperature. Between room temperature and -1 0 0 °C [(NH2)3PNP(NH2)3]C1 is sub­ ject to a phase transition. Therefore, the crystal structure was determined by single crystal X-ray methods at room temperature (P i, a = 584.7(1) pm, b = 732.1(1) pm, c = 1092.0(2) pm. q = 71.05(3)°, ß = 76.36(3)°, 7 = 89.83(3)°, Z = 2, R = 4.75 %, wR = 2.47 %). The cation [(NH2)3PNP(NH2)3]+ is built up by two corner sharing PN4 tetrahedra. Remarkably short P-N bonding distances have been observed and both PN4 tetrahedra exhibit a significant distortion resulting in two large and four small N-P-N bond angles. 
  Reference    Z. Naturforsch. 51b, 1732—1738 (1996); eingegangen am 26. Juni 1996 
  Published    1996 
  Keywords    Aminophosphazenes, Synthesis, Crystal Structure 
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 Identifier    ZNB-1996-51b-1732 
 Volume    51 
39Author    G. Rebe, Frank Weller, Kurt Dehnicke, ProfRequires cookie*
 Title    Jutta  
 Abstract    N-Iodo-triphenylphosphaneimine, Ph3PNI, has been prepared by thermolysis of the donor acceptor complex [Me3SiNPPh3-ICl] in boiling acetonitrile in the presence of potassium fluo­ ride. Both compounds have been characterized by IR spectroscopy and by crystal structure determinations. [Me3SiNPPh3 ICl]: Space group P I, Z = 2, a = 888.3(1), b = 1070.7(1), c = 1310.2(1) pm, a = 9 5 .15(1)°, ß = 108.67(1)°, 7 = 97.78(1)° at 20°C. The complex has a molecular structure in which the N atom of the phosphaneimine is connected with the iodine atom of the IC1 molecule in a linear arrangement N-I-Cl with bond lengths N-I = 232.7 pm, I-Cl = 255.37 pm. Ph3PNI: Space group P2,/n, Z = 4, a = 952.8(1), b = 1800.8(2), c = 1003.6(1) pm, ß = 110.25(1)° at -50°C. The compound forms monomeric molecules with bond lengths PN = 159.1 pm, I-N = 205.6 pm and an INP bond angle of 113.3°. N-Iod-triphenylphosphanimin. Synthese und Kristallstrukturen von [Me3SiNPPh3 ICl] und Ph3PNI 
  Reference    Z. Naturforsch. 51b, 1739—1743 (1996); eingegangen am 12. April 1996 
  Published    1996 
  Keywords    Phosphaneimine Complexes, Synthesis, Crystal Structure 
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 Identifier    ZNB-1996-51b-1739 
 Volume    51 
40Author    Olaf Reckeweg, H.-Jürgen MeyerRequires cookie*
 Title    Unsymmetrische BN23'-Ionen in den Strukturen von Ca2ClBN2 und Sr2ClBN2. Unsymmetric BN23~-Ions in the Structures of Ca2ClBN2 and Sr2ClBN2  
 Abstract    The new compounds Ca2ClBN2 (1) and Sr2ClBN2 (2) were prepared from the respective metal, its dihalide and h-BN in sealed tantalum ampoules at 1200 °C. The crystals obtained were transparent yellow (1) and blue (2), respectively. The crystal structures were determined from single crystal X-ray data. Ca2ClBN2 and Sr2ClBN2 are isotypic and crystallize in the orthorhombic space group Pnma (No. 62), Z = 4 (Ca2ClBN 2: a = 1166.7(2), b = 390.26(4), c = 899.8(1) pm, R 1 = 0.043, wR2 = 0.115 for 554 independent reflections; Sr-,C1BNT: a = 1242.8(1), b = 416.75(4), c = 920.8(1) pm, R\ = 0.031, wR2 = 0.054 for 6 6 2 'independent reflections). The structures contain two different layers of M 2+, C P and BN23~ alternating along the [010] direction. The bond angles N-B-N are 177.2(4)° for (1) and 176,6(5)° for (2), the bond distances of the BN23_ ions are dB_ N] = 134.6(5) pm for (1), 136,3(7) pm for (2) and dg_N2 = 132.4(5) pm for (1) and 131,3(7) pm for (2). The unsymmetric structure of the BN23~ ion, as is manifested particularly in the Sr compound (2), is caused by the coordination of N 1 to four cations while N2 is coordinated only to three. 
  Reference    Z. Naturforsch. 52b, 340—344 (1997); eingegangen am 12. November 1996 
  Published    1997 
  Keywords    Boronitrides, Synthesis, Crystal Structure 
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 Identifier    ZNB-1997-52b-0340 
 Volume    52 
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