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101Author    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 
102Author    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 
103Author    M. Veith, A. BeloRequires cookie*
 Title    Stickstoffverbindungen von Elementen der dritten Hauptgruppe mit intra-und intermolekularen Donor-Akzeptor-Bindungen, III [1]. Dynamische Phänomene und Lewis-Säure-Stärke Nitrogen Compounds of Elements of the Third Main Group with Intra-and Intermolecular Donor Acceptor Bonds, III [1]. Dynamic Phenomena and Lewis Acidity  
 Abstract    Compounds of the general formula f BuN(H)-SiMe 2 -N(r Bu)ElX 2 (El = B, X = Me (lm), F (If), Cl (lc); El = AI, X = Me (2m), Cl (2c), Br (2b); El -Ga, X -Me (3m), Cl (3c), Br (3b); El -In, X -Me (4m), Cl (4c), Br (4b); El -Tl, X -Me (5m)) and r BuN(D)-SiMe 2 -N(r Bu)ElMe 2 (El = Al (2d), Ga (3d), In (4d)) have been characterized by IR and temperature dependent ! H NMR techniques with respect to their structural changes in solution. A reversible, dynamic, intramolecular equilibrium between two enantiomeric four-membered rings has been established to be responsible for the changes in the spectra. The cyclic form Bl, which arises from Lewis acid base interaction of the rerr-butyl-amino with the E1X 2 group, transforms to the mirror-image B2 via an acyclic intermediate, in which reorien-tation of the groups by rotation or inversion can take place. In the boron derivatives (lm, lc, and If) no comparable N—B interaction can be detected. The Lewis acidity of the E1X 2 group deduced from NH wave numbers increases within the following series: TlMe 2 <GaMe 2 ~InMe 2 <AlMe 2 <GaBr 2 =InBr 2 <GaCl 2 ~AlBr 2 ~InCl 2 <AlCl 2 . Intramolecular hydrogen transfer from one nitrogen atom to the other can be excluded by comparison of the rate constant k H vs. k D . The free enthalpy of activation A G* depends on the acidity of E1X 2 , the steric requirements and the relative masses of X. The syntheses and characterisation of If, 2b, 3b, 4b, 2d, 3d, and 4d are described. 
  Reference    Z. Naturforsch. 42b, 525—535 (1987); eingegangen am 6. November 1986 
  Published    1987 
  Keywords    Temperature Dependent NMR, Synthesis, Intramolecular Rearrangements, Donor Acceptor Bonds 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-0525.pdf 
 Identifier    ZNB-1987-42b-0525 
 Volume    42 
104Author    Reinhard Nesper, Jan CurdaRequires cookie*
 Title    das erste Chalcogenid mit zweiwertigem Aluminium Al 7 Te 10 — the First Chalcogenide of Divalent Aluminum  
 Abstract    Al 7 Te 10 is prepared from a melt of the elements in stoichiometric amounts in a corundum crucible contained in a sealed quartz ampoule. The ruby red cube shaped crystals are stable below 840 K. The structure of Al 7 Te, 0 (R32-D^; a = 1439.5 pm, c = 1793.2 pm, Z = 6, R = 0.03) is a distorted defect variant of a tetrahedral arrangement of the 4H-polytype. The central unit, a double barrelane [Te 4 Al 4 —Al 4 Te 4 ], contains an Al —Al bond of 260 pm, which is somewhat longer (n = 0.83) than an expected single bond (250 pm, n = 1). This homopolar bond disturbs the electrostatically favorable (Al—Te—)" sequence in the structure which is compensated by the occurrence of four-membered Al 2 Te 2 rings. Al 7 Te 10 is a Zintl phase according to l/2{[Al 2+ -Al 2+ ][Al 3+ ] !2 [Te 2 ~] 20 } and exhibits semiconducting and diamagnetic behaviour. 
  Reference    Z. Naturforsch. 42b, 557 (1987); eingegangen am 9. Dezember 1986 
  Published    1987 
  Keywords    Synthesis, Crystal Structure, Divalent Aluminum, Aluminum-Aluminum Bonds 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-0557.pdf 
 Identifier    ZNB-1987-42b-0557 
 Volume    42 
105Author    K. Brodersen, H. Procher, Hans-U HummelRequires cookie*
 Title    Synthesis and Crystal Structure of PbZn(NCS) 4  
 Abstract    PbZn(NCS) 4 is obtained from the binary compounds Pb(SCN) 2 and Zn(NCS) 2 with traces of water in an ultra-sound bath. The space group of the complex is Pn2[a (standard: Pna2,) with Z = 4. The structure consists of as-connected octahedra ^.[PbS 2 S 4/2 ] forming two-dimensional layers. All SCN-groups are bound to Zn 2+ via their N atoms. The resulting ZnN 4 tetrahedra are arranged in the cavities formed by the PbS 6 octahedra. 
  Reference    Z. Naturforsch. 42b, 679—681 (1987); eingegangen am 6. November 1986/27. Januar 1987 
  Published    1987 
  Keywords    Lead(II) Tetraisothiocyanatozincate, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-0679.pdf 
 Identifier    ZNB-1987-42b-0679 
 Volume    42 
106Author    Kay Jansen, Kurt DehnickeRequires cookie*
 Title    Synthese und Kristallstruktur von (PPh4)2[Mo2(02C—Ph)4Cl4] * 2 CH2C12, einem Komplex mit Mo=Mo-Bindung Synthesis and Crystal Structure of (PPh4 )2 [Mo2 (0 2 C —Ph)4 Cl4] -2 CH 2 C12, a Complex with M o=M o Bonding  
 Abstract    The title com pound has been prepared from (PPh4)2[M o2(0 2C —Ph)4Cl2] and CC14 in C H 2C12 solution as moisture sensitive crystals, which are black in reflexion and yellow in transmission. (PPh4)2[M o2(0 2C —Ph)4Cl4] • 2 C H 2C12 was characterized by a X-ray crystal structure determ ination (7873 observed independent reflexions, R = 0.048). It crystallizes in the space group P 1 with one formula unit in the unit cell; the lattice constants are a = 1186.4; b = 1404.0; c = 1451.0 pm; a = 61.98°; ß = 78.91°; y = 78.26°. The structure consists o f PPh4® ions, C H 2C12 m olecules and centrosym m etric anions [M o2(0 2C —Ph)4Cl4]20 containing a molybdenum d3d3 unit with a relatively long M o = M o bond o f 249.6 pm. The M o= M o group is spanned in a chelate manner by four O atoms of two benzoate groups and by two further single O atoms o f two further benzoate groups. Two terminal Cl atom s on each Mo atom com plete the pentagonal bipyramidal coordination spheres about the Mo atoms. 
  Reference    Z. Naturforsch. 42b, 1097—1101 (1987); eingegangen am 2. März 1987 
  Published    1987 
  Keywords    Tetrabenzoato-tetrachloro-dim olybdate, Synthesis, IR Spectra, Crystal Structure 
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 Identifier    ZNB-1987-42b-1097 
 Volume    42 
107Author    H. Lermer, K. K. UngerRequires cookie*
 Title    .6-Diaminohexan als Schablonenverbindung in der Synthese von Zeolith ZSM-5 1.6-Diaminohexane as Tem plate in the Synthesis of Zeolite ZSM-5  
 Abstract    A mixture characterized by the molar ratios of H20 /S i 0 2 = 20, S i0 2/A l20 3 = 120. Na20 / S i 0 2 = 0.3 and 1.6 diaminohexane (D A H) as template was reacted at 182 °C. Dependent on the reaction time, the ratio of 0 H ~ /S i0 2 and DAH/SiO: ZSM-5 was crystallised with a-quartz as by-product. The materials were characterized by X-ray diffraction, scanning electron microscopy, infrared spectroscopy, thermogravimetry and differential thermal gravimetry. 
  Reference    Z. Naturforsch. 42b, 1256—1262 (1987); eingegangen am 9. Juni 1987 
  Published    1987 
  Keywords    High-Silica Zeolite, Synthesis, 16-Diaminohexane 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-1256.pdf 
 Identifier    ZNB-1987-42b-1256 
 Volume    42 
108Author    MatthiasC. Hund, Arno Tißler, Peter Polanek, Martin Dräger, KlausK. UngerRequires cookie*
 Title    Zur Bildungskinetik des Zeolithen ZSM-11 On the Kinetics of Formation of the Zeolite ZSM-11  
 Abstract    The synthesis of pentasil ZSM-11 with Bu4N H S 0 4 as template was first optimized in a teflon-coated autoclave of 200 ml volume (163 °C, 3 days) and then transferred to a stirring autoclave of 1000 ml volume. The latter allowed sampling over the period of crystallization. Pure ZSM-11 crystallized at temperatures between 150 and 180 °C. In this range the induction period decreased from 15 to 2 hours while the rate of crystallization was enhanced from 2.5 to 5.6% per minute. From these values energies of activation for nucleation and crystallization were determined (99.8 and 43.4 kJ mol-1). 
  Reference    Z. Naturforsch. 42b, 1510—1514 (1987); eingegangen am 3. August 1987 
  Published    1987 
  Keywords    Zeolites ZSM-11, Synthesis, Kinetics of Formation 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-1510.pdf 
 Identifier    ZNB-1987-42b-1510 
 Volume    42 
109Author    Eberhard Böhm, Kurt Dehnicke, Johannes Beck, Wolfgang Hiller, Joachim Strähle, Andreas Maurer, Dieter FenskeRequires cookie*
 Title    Die Kristallstrukturen von Ph 3 PNPh, [Ph 3 PN(H)Ph][AuI 2 ] und von 2,3-Bis(triphenylphosphoranimino)maIeinsäure-N-methyIimid The Crystal Structures of Ph 3 PNPh, [Ph 3 PN(H)Ph][AuI 2 ] and of 2,3-Bis(triphenylphosphoranimino)maleic Acid-N-methylimide  
 Abstract    [Ph 3 PN(H)Ph][AuI 2 ] (2) is formed by the reaction of Aul with N-Phenyl-iminotriphenylphos-phorane, Ph 3 PNPh in a toluene suspension. 2,3-Bis(triphenylphosphinimino)maleic acid-N-methylimide (3) has been prepared by the Staudinger reaction of 2,3-bis(azido)maleic acid-N-methylimide with PPh, in THF solution in the form of red crystals. Crystal structure determina-tions of three iminophosphoranes were carried out by X-ray methods. Ph 3 PNPh (1): space group P2]/c, Z = 4, 2176 independent observed reflexions, R = 0.057. Lattice dimensions (-30 °C): a = 1126.4, b = 1148.6, c = 1476.0 pm; ß = 97.21°. The compound forms monomeric molecules with P=N = 160.2 pm and an PNC angle of 130.4°. [Ph 3 PN(H)Ph][AuP] (2): space group PI, Z = 2, 1780 independent observed reflexions, R = 0.057. Lattice dimensions (18 °C); a = 824.9, b = 1022, c = 1476.2 pm; a = 89.23°, ß = 87.41°, y = 85.65°. The compound consists of ions [Ph 3 PN(H)Ph]® with P=N = 162.4 pm and PNC = 129.3°, and anions [Aul 2 ] e with Au-I = 261.9 and 259.3 pm, IAuI = 176.8°. (PhiP) 2 N-,C 4 0 2 (NMe) (3): space group PI, Z = 2, 4972 independent observed reflexions, R = 0.050. Lattice dimensions (-90 °C): a = 904.7, b = 993.8, c = 2017.4 pm; a = 101.55°, ß = 96.39°, y — 105.81°. The compound forms monomeric molecules with ^«-conformation of the two NPPh 3 groups. Bond lengths: P=N = 157.1; 155.3 pm, bond angles: PNC = 133°; 136°. 
  Reference    Z. Naturforsch. 43b, 138—144 (1988); eingegangen am 2. September/6. November 1987 
  Published    1988 
  Keywords    Iminophosphoranes, Synthesis, IR Spectra, Crystal Structure 
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 TEI-XML for    default:Reihe_B/43/ZNB-1988-43b-0138.pdf 
 Identifier    ZNB-1988-43b-0138 
 Volume    43 
110Author    M. '., Y., M. =. Zn, Cd, =. Al, Ga, In, X. =. Se, Te, Y. =. Cl, Klaus-Jürgen Range, Karin HandrickRequires cookie*
 Title    Synthese und Hochdruckverhalten quaternärer Chalkogenidhalogenide M 2 M X 3 Y (M = Zn, Cd; M = AI, Ga, In; X = Se, Te; Y = CI, Br, I) Synthesis and High-Pressure Behaviour of Quaternary Chalcogenide Halides M  
 Abstract    Quaternary chalcogenide halides M 2 M'X 3 Y (M = Zn, Cd; M' = Al, Ga. In; X = Se. Te; Y = Cl. Br, I) can be synthesized by heating stoichiometric amounts of the binary components MX. MY 2 , and M 2 X 3 in evacuated sealed quartz ampoules. In the case of aluminium and gallium compounds, a mixture of the M' and X elements rather than the binary compounds has been used. The products are typical tetrahedral compounds, crystallizing with either the defect wurtzite-type or the defect zinc-blende-type structure. At 25 kbar. and 1400 °C, Cd 2 InSe 3 Cl. Cd 2 InSe 3 Br, and Cd 2 InSe 3 I transform from the defect wurtzite-type structure to quenchable high-pressure phases with defect NaCl-type structure. The retransformation to the ambient-pressure phases proceeds via intermediates having the defect zinc-blende-type structure. Some aspects of the apparent non-stoichiometry in the high-pressure phases are discussed. 
  Reference    Z. Naturforsch. 43b, 153—158 (1988); eingegangen am 2. November 1987 
  Published    1988 
  Keywords    Quaternary Chalcogenide Halides, Synthesis, Crystal Structure High-Pressure Reactions 
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 TEI-XML for    default:Reihe_B/43/ZNB-1988-43b-0153.pdf 
 Identifier    ZNB-1988-43b-0153 
 Volume    43 
111Author    Peter Stolz, Siegfried PohlRequires cookie*
 Title    Iodomanganate(II): Darstellung und Kristallstrukturen von (Ph 4 P)MnI 3 L, MnI 2 L 3 , [MnIL 5 ]I 3 und [MnL 6 ](I 3 ) 2 (L = Tetrahydrofuran) Iodomanganates(II): Synthesis and Crystal Structures of (Ph 4 P)MnI 3 L, MnI 2 L 3 , [MnIL 5 ]I 3 and [MnL 6 ](I 3 ) 2  
 Abstract    The compounds (Ph 4 P)MnI 3 L (1), MnI 2 L 3 (2), [MnIL 5 ]I 3 (3), and [MnL A ](I 3) 2 (4) (L = C 4 H H O, thf) were prepared in thf solution and their structures determined from single crystal X-ray diffraction data. 1 crystallizes in the monoclinic space group C2/c with a = 1743.6(1), b — 1985.8(1), c = 1806.7(1) pm, ß = 98.74(1)°, Z = 8. The structure of 1 exhibits tetrahedral anions. The Mn—I distance was found to be 268.0 pm (mean). 2: monoclinic, C2/c with a = 1252.3(2), b = 1255.0(3), c = 1271.8(3) pm ß = 113.88(2)°, Z = 4. The characteristic feature of the structure of 2 is the existence of neutral MnI 2 L 3 molecules with a distorted trigonal bipyramidal geometry and the iodine atoms in equatorial positions (Mn —I: 271.1 pm). The compound crystallizes from a solution of Mnl 2 in tetrahydrofuran. 3: monoclinic, C2/c with a = 1695.3(1), b = 1123.1(1), c = 1646.2(1) pm, ß = 96.91(1)°, Z = 4. The preparation of 3 from 2 and iodine yields octahedral MnIL, + cations (Mn —I: 278.8 pm) and triiodide anions. 4: monoclinic, P2,//z with a = 1005.5(1). b = 1056.8(1), c -1835.6(2) pm, ß = 91.16(1)°, Z -2. 4 is prepared from 3 and iodine in thf solution, and shows octahedral MnL 6 2+ cations and triiodide anions. 
  Reference    Z. Naturforsch. 43b, 175—181 (1988); eingegangen am 19. August/20. Oktober 1987 
  Published    1988 
  Keywords    Iodo-Complexes of Manganese(II), Synthesis, Crystal Structure 
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 Identifier    ZNB-1988-43b-0175 
 Volume    43 
112Author    Rupert MarxRequires cookie*
 Title    Darstellung und Kristallstruktur von Cäsiumhydroxid mit Methanol CsOH * CH 3 OH Properties and Crystal Structure of Cesium Hydroxide with Methanol CsOH * CH 3 OH  
 Abstract    Cesium hydroxide methanol, CsOHCH3OH, was obtained by recrystallising Cs0H H:0 in a mixture of liquid ammonia and methanol in sealed quartz ampoules. The colourless, air sensitive crystals are hexagonal (space group P63/m) with a = 1362 pm, c = 430 pm, Z = 6. A structural model derived by Patterson methods was refined to R = 0.033. The structure comprises of trigonal prismatic columns of Cs + and hydrogen bonded chains of OH^ and CH,OH along the c-axis. This leads to the tricapped prisms filled with Cs + and hydrophobic channels formed by the CH, groups. 
  Reference    Z. Naturforsch. 43b, 521—524 (1988); eingegangen am 14. Oktober/7. Dezember 1987 
  Published    1988 
  Keywords    Cesium Hydroxide Methanol, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/43/ZNB-1988-43b-0521.pdf 
 Identifier    ZNB-1988-43b-0521 
 Volume    43 
113Author    Günter KlarRequires cookie*
 Title    Elementorganische Verbindungen mit o-Phenylenresten, XV [1] Hexamethoxy-tetrachalcogena-tetrahydropentacene Organometallic Compounds with o-Phenylene Substituents, Part XV [1] Hexamethoxy-tetrachaleogena-tetrahydropentaeenes Peer Berges  
  Reference    Z. Naturforsch. 43b, 599—604 (1988); eingegangen am 21. Januar 1988 
  Published    1988 
  Keywords    tetrahydropentacene, Synthesis, 'H NMR Spectra, X-Ray 
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 TEI-XML for    default:Reihe_B/43/ZNB-1988-43b-0599.pdf 
 Identifier    ZNB-1988-43b-0599 
 Volume    43 
114Author    Wolfgang Saak, Siegfried PohlRequires cookie*
 Title      
 Abstract    Fe 4 S 4 I 2 (SPPh 3) 2 (1) was prepared by the reaction of Fe(THF) 6 Fe 4 S 4 I 4 (THF = C 4 H 8 0). SPPh,. and sulfur in toluene and CH 2 C1 2 . 1 has a lower stability than Fe 4 S 4 I 4 2_ and decomposes in solvents like THF and CH,CN. The crystal structure of 1 was determined from single crystal X-ray diffraction data. The compound crystallizes in the triclinic space group PI with a = 1025.5(1). b = 1082.4(1), c = 2135.5(3) pm. a = 89.82(1).ß -77.37(1), y = 73.56(1)°. V = 2214.1x10" pm'and Z = 2. The [Fe 4 S 4 ] 2+ core of 1 exhibits a slight tetragonal distortion. The mean Fe —S and Fe —Fe distances were found to be 227.6 (225.8-228.7) pm and 273.3 (272.9-274.4) pm, respectively. The Fe-SPPh, distances (231.6 and 232.1 pm) are longer than the terminal Fe — S bonds in RS coordinated [Fe 4 S 4 ] clusters. The Fe —I bonds are found at 251.6 and 251.8 pm. respectively. 
  Reference    Z. Naturforsch. 43b, 813—817 (1988); eingegangen am 15. Februar 1988 
  Published    1988 
  Keywords    Neutral, Mixed Terminal Ligand Iron-Sulfur Cluster, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/43/ZNB-1988-43b-0813.pdf 
 Identifier    ZNB-1988-43b-0813 
 Volume    43 
115Author    Fritjof Schmock, Aida El-Kholi, Ulrich Müller, Kurt DehnickeRequires cookie*
 Title    Synthesis and Crystal Structure of PPh 3 Me[HS0 4 ]  
 Abstract    PPh 3 Me[HS0 4 ] was prepared by the reaction of (PPh,Me)I with silver sulfate in aqueous solution. OPPh : Me and benzene being the by-products. The title compound was characterized by its IR spectrum as well as by an X-ray structure determination (1730 observed independent reflexions, R = 0.043). Crys-tal data: a = 910.4(3). b = 1587.8(4), c = 1294.2(6) pm, ß = 105.52(3)°. space group P2,/c t Z = 4. The structure consists of PPh,Me® cations and of HOSO, 0 ions that are associated via strong hydrogen bonds to dimeric centrosymmetric units. 
  Reference    Z. Naturforsch. 43b, 1069—1071 (1988); eingegangen am 13. April 1988 
  Published    1988 
  Keywords    Triphenylmethylphosphonium Hydrogensulfate, Synthesis, IR Spectra, Crystal Structure 
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 Identifier    ZNB-1988-43b-1069_n 
 Volume    43 
116Author    MervatEl Essawi, H. Gosmann, D. Fenske, F. Schmock, K. DehnickeRequires cookie*
 Title    Synthesen und Kristallstrukturen von [PPh 3 Me]N0 2 und [PPh 3 Me]HC0 2 H 2 0 Syntheses and Crystal Structures of [PPh 3 Me]N0 2 and [PPh 3 Me]HC0 2 H 2 0  
 Abstract    Triphenylmethylphosphonium nitrite and formate have been prepared by the reaction of [PPh,Me]I with silver nitrite, and lead formate, respectively, in aqueous solutions. [PPh 3 Me]N0 2 (1) forms pale yellow crystals, and [PPh 3 Me]HC0 2 H 2 0 (2) forms white crystals. Both com-pounds are soluble in water, ethanol, and dichloromethane. In moist air 2 is hydrated to yield [PPh 3 Me]HC0 2 -2H 2 0 (3). The compounds were characterized by their IR spectra. 1 and 2 also by X-ray crystal structure determinations. [PPh 3 Me]NO-> (1): space group P2,/«, Z = 4, 2088 independent observed reflexions, R = 0.062. Lattice dimensions (20 °C): a = 914.7(3), b = 1887.5(9), c = 1080.0(4) pm, ß = 110.29(3)°. The compound consists of PPh,Me + ions and NO-," anions with bond lengths of 114.2(6) pm and a bond angle of 124.1(7)°. [PPh 3 Me]HCOi • H^O (2): space group P2,/n, Z = 4, 2973 independent observed reflexions, R = 0.069. Lattice dimensions (-20 °C): a = 931(2), b = 1558(3), c = 1281(2) pm, ß = 105.9(1)°. The compound consists of PPh 3 Me + ions and formate anions which form centrosymmetric dimeric units [HCOvftO]?" through hydrogen bridges of the water molecules. Bond lengths CO 122.4(4) and" 120.9(4) pm. bond angle OCO 129.9(4)°. 
  Reference    Z. Naturforsch. 43b, 1279—1284 (1988); eingegangen am 27. Mai 1988 
  Published    1988 
  Keywords    Triphenylmethylphosphonium Nitrite and Formate, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/43/ZNB-1988-43b-1279.pdf 
 Identifier    ZNB-1988-43b-1279 
 Volume    43 
117Author    WolfgangA. Herrmann, RolandA. Fischer, JosefK. Felixberger, RoccoA. Paciello, Pavlo Kiprof, Eberhardt HerdtweckRequires cookie*
 Title    Organorheniumhalogenide: Synthesen, Strukturen und Reaktivität gegenüber Alkinen Organorhenium Halogenides: Synthesis, Structure and Reactivity upon Treatment with Alkynes  
 Abstract    [dichloro(/<-chloro)(^-pentamethylcyclopentadienyI)rhenium(IV)] 
  Reference    Z. Naturforsch. 43b, 1391—1404 (1988); eingegangen am 29. April 1988 
  Published    1988 
  Keywords    Organorhenium Halides, Synthesis, Crystal Structure, Reactivity Bis 
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 TEI-XML for    default:Reihe_B/43/ZNB-1988-43b-1391.pdf 
 Identifier    ZNB-1988-43b-1391 
 Volume    43 
118Author    Hans-Friedrich Klein, Michael Helwig, Udo Koch, Goetz Lull, Marko Tadic, Carl Kriiger, Peter HofmannRequires cookie*
 Title    Diolefinbis(trimethyIphosphine)cobalt(0) Compounds: Stable Organometallic Radicals with Distorted Ground State Structures  
 Abstract    Diolefincobalt(O) complexes Co(L,)(PMe 3), {L, -[CH, = CHSi(0Me),],0 (1), [CH 2 =CHSi(0Et) 2 ] 2 0 (2), (CH 2 =CHCH 2) 2 SiMe 2 (3), [(CH 2 =CHCH 2) 2 N] 2 CH 2 (4)} have been synthesized from Co(C 5 H 8)(PMe 3) 3 and diolefins at ambient temperatures. Reactions with allyl ethers or with allyltin or allylphosphorus compounds involve transfer of allyl groups to the cobalt, while allylamine simply replaces cyclopentene (C S H S) to give Co(CH 2 =CHCH 2 NH 2)(PMe 3) 3 (5). Cationic cobalt(I) complexes containing olefin ligands as in 1—4 could not be obtained under conditions where norbornadiene readily gave [Co(C 7 H 8)(PMe 3) 3 ]BF 4 (6). Paramagnetic 4 shows a magnetic moment /^ eff = 2.0 /u B (between 3.6 and 293 K), corresponding to one unpaired electron per cobalt atom. Compound 4 crystallizes in the space group P2,/c with Z = 4, a = 14.986(4), b = 17.223(5), c = 15.436(3) k,ß = 117.98(2)°, V = 3518.4 Ä 3 . Each cobalt atom is ^-coordinated to a diolefin involving the smaller of two possible chelating rings. The Co—C distances range only from 2.029(6) to 2.058(6) A for the olefin ligands, whereas Co—P bond lengths at each cobalt differ significantly: Col-Pl 2.188(2), Col-P2 2.248(2); Co2-P3 2.185(2), Co2-P4 2.258(2) A. This feature of two significantly different Co-L bond lengths is hitherto seen in all structurally characterized (bisolefin)CoL 2 complexes (L = PMe,, CH 3 CN) and can be rationalized by molecular orbital calculations (Extended Hückel) on the 17 electron model system (PH 3) 2 Co(C 2 H 4) 2 . 
  Reference    Z. Naturforsch. 43b, 1427—1438 (1988); received July 1 1988 
  Published    1988 
  Keywords    Cobalt Diolefin Complexes, Synthesis, Structure, Theory 
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 Identifier    ZNB-1988-43b-1427 
 Volume    43 
119Author    Abderraouf Khabou, Kurt Dehnicke, Kurt Findeisen, Farbenfabriken Bayer, Bayer-WerkD. Leverkusen, -5090 Leverkusen, Dieter FenskeRequires cookie*
 Title    Molybdännitridtrichlorid-2,3,3-trichloracrylnitril, [M0NCI3 * NC-C 2 C1 3 ] 2 Synthese, IR-Spektrum und Kristallstruktur Molybdenumnitridetrichloride-2,3,3-trichloroacrylnitrile, [MONC1 3 * NC—C 2 C1 3 ] 2 Synthesis, IR Spectrum, and Crystal Structure  
 Abstract    [MONC1 3 -NC —C 2 C1 3 ] 2 has been prepared by the reaction of MONC1 3 with trichloromethyl isocyanidedichloride, CC1 3 NCC1 2 , in CH 2 C1 2 suspension. The compound forms redbrown. mois-ture sensitive crystals, which were characterized by their IR spectrum as well as by a crystal structure determination (2482 independent observed reflexions, R = 0.048). Crystal data (-70 °C): Space group P2,/c, Z = 2, a = 674.2(2); b = 2128.2(11); c = 786.0(4) pm: ß = 102.81(3)°. [MONC1 3 • NC-C 2 C1 3 ] 2 forms centrosymmetric dimeric molecules via chloro bridges with Mo-Cl bond lengths of 240.7 and 276.0 pm. The longer MoCl bond of the MOC1 2 MO ring is caused by the trans influence of the nitride ligand; the MoN bond length of 167 pm corresponds with a triple bond. The 2,3,3-trichloroacrylnitrile ligand is bonded by its nitrogen atom with a bond length of Mo —N — 216 pm; the Mo-N=C—C sequence is almost linear with a remarkable short C—C bond of 143.0 pm. 
  Reference    Z. Naturforsch. 43b, 1616—1620 (1988); eingegangen am 19. Juli 1988 
  Published    1988 
  Keywords    Molybdenumnitridetrichloride-233-trichloroacrylnitrile, Synthesis, IR Spectra, Crystal Structure 
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 TEI-XML for    default:Reihe_B/43/ZNB-1988-43b-1616.pdf 
 Identifier    ZNB-1988-43b-1616 
 Volume    43 
120Author    Christina Ergezinger, Frank Weller, Kurt DehnickeRequires cookie*
 Title    Amidinatokomplexe von Bor, Aluminium, Gallium, Indium und Zinn Die Kristallstrukturen von Ph-C(NSiMe 3 ) 2 AICI 2 und Ph-C(NSiMe 3 ) 2 SnCl 3 Amidinato Complexes of Boron, Aluminium, Gallium, Indium, and Tin The Crystal Structures of Ph-C(NSiMe 3 ) 2 AlCl 2 and Ph-C(NSiMe 3 ) 2 SnCl 3  
 Abstract    The trichlorides of aluminium, gallium, and indium, as well as boron tribromide and tin tetra-chloride react with N,N,N'-tris(trimethylsilyl)benzamidine to form the monomeric N.N'-bis-(trimethylsilyl)benzamidinato complexes Ph-C(NSiMe,) 2 MX 2 (M = B, Al. Ga, In; X = Cl, Br) and Ph —C(NSiMe 3) 2 SnCl 3 , respectively. All compounds have been characterized by their IR spectra, two of them by X-ray diffraction studies. Ph — C(NSiMei) 2 AlCl 2 : Space group C2/c, Z = 4, 1152 independent observed reflexions, R = 0.052. Lattice dimensions (19 °C): a = 1558.6(1), b = 1116.6(1), c = 1307.0(1) pm, ß = 115.17(1)°. The compound forms monomeric molecules, in which the aluminium atom is tetra-hedrally coordinated by two chlorine atoms and by the two nitrogen atoms of the benzamidinato chelate. Bond length A1N = 188.2 pm. Ph — C(NSiMe^) 2 SnCU: Space group PI, Z = 2, 3293 independent observed reflexions, R = 0.034. Lattice dimensions (19 °C): a = 980.1(1), b = 1025.9(1), c = 1230.5(2) pm. a = 68.40(1)°, ß = 87.71(1)°, y — 68.92(1)°. The compound forms monomeric molecules, in which the tin atom is five-coordinated by three chlorine atoms and by the two nitrogen atoms of the benzamidinato chelate. Bond lengths SnN = 213.5 and 215.2 pm. 
  Reference    Z. Naturforsch. 43b, 1621—1627 (1988); eingegangen am 18. August 1988 
  Published    1988 
  Keywords    N, N'Bis-(trimethylsilyl)amidinato Complexes, Synthesis, IR Spectra Crystal Structure 
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 TEI-XML for    default:Reihe_B/43/ZNB-1988-43b-1621.pdf 
 Identifier    ZNB-1988-43b-1621 
 Volume    43 
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