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1988 (31)
1Author    ManfredL. Ziegler, Klaus Blechschmitt, Harald Bock, Ernst Guggolz, RichardP. KorswagenRequires cookie*
 Title    Über die Reaktivität von [(CH 3 ) 2 N] 6 W 2 (W=W) gegenüber CS 2 /S 8 und CS 2 /Se, Röntgenstrukturanalyse von [(CH 3 ) 2 NCS 2 ] 2 W(S)(S 2 ) Reactivity of [(CH 3 ) 2 N] 6 W 2 (W=W) Towards CS 2 /S 8 and CS 2 /Se 8 . X-Ray Structure Analysis of [(CH 3 ) 2 NCS 2 ] 2 W(S)(S 2 )  
 Abstract    In this paper we report two improved preparation methods for [(CH 3) 2 N] 6 W 2 (W=W) (1), one starting from WC1 4 (yield 51%), and a second one starting from W 2 C1 6 (THF) 4 (ca. 60% yield). We have studied the reactions of 1 with different nucleophiles, among them triphenylalkylidenphos-phoranes (like Ph 3 P=CH 2 and Ph 3 P=CHPh • LiCl; Ph = phenyl), sulfur and CS 2 . 1 reacts with S 8 and CS 2 in hexane to yield the two new compounds (Me 2 NCS 2) 2 WS(S 2) (4) and W(CS 2 H)(Me 2 NCS 2) 2 (5), both containing dithiocarbamato ligands formed by insertion of CS 2 into the W-N bond. The two mononuclear compounds were characterized spectroscopically, in the case of 4 an X-ray diffraction structure analysis was performed. The reaction of 1 with Se and CS 2 , leads to the compounds 4, (Me 2 NCS 2) 2 W 2 S 4 (6) and [(Me 2 N) 2 C]CS 2 (7), which were also characterized spectroscopically. No Se-containing compounds could be isolated. 4 crystallizes monoclinically, C 5 2h -P2Jn, with a = 648.6(3), b = 1346.7(6) and c = 1745.9(7) pm, ß = 91.85(3)°, V = 1524xl0 6 pm 3 , Z = 4. The structure of the seven-coordinate tungsten compound is discussed and compared to complexes with similar ligands and geometry. 
  Reference    Z. Naturforsch. 43b, 590—598 (1988); eingegangen am 28. Dezember 1987 
  Published    1988 
  Keywords    Reactivity, Synthesis, X-Ray 
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 Identifier    ZNB-1988-43b-0590 
 Volume    43 
2Author    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 
3Author    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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 TEI-XML for    default:Reihe_B/43/ZNB-1988-43b-1144.pdf 
 Identifier    ZNB-1988-43b-1144 
 Volume    43 
4Author    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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 TEI-XML for    default:Reihe_B/43/ZNB-1988-43b-1683_n.pdf 
 Identifier    ZNB-1988-43b-1683_n 
 Volume    43 
5Author    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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 Identifier    ZNB-1988-43b-0138 
 Volume    43 
6Author    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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 Identifier    ZNB-1988-43b-0153 
 Volume    43 
7Author    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 
8Author    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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 Identifier    ZNB-1988-43b-0521 
 Volume    43 
9Author    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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 Identifier    ZNB-1988-43b-0599 
 Volume    43 
10Author    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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 Identifier    ZNB-1988-43b-0813 
 Volume    43 
11Author    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 
12Author    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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 Identifier    ZNB-1988-43b-1279 
 Volume    43 
13Author    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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 Identifier    ZNB-1988-43b-1391 
 Volume    43 
14Author    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 
15Author    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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 Identifier    ZNB-1988-43b-1616 
 Volume    43 
16Author    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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 Identifier    ZNB-1988-43b-1621 
 Volume    43 
17Author    Susanne Maier, Wolfgang Hiller, Joachim Strähle, Christina Ergezinger, Kurt DehnickeRequires cookie*
 Title      
 Abstract    The copper(I)amidinato complex Cu 2 [Ph-C(NSiMe 3) 2 ] ; has been prepared by the reaction of CuCl with N.N,N'-tris(trimethylsilyl)benzamidine in boiling acetonitrile. forming white crystals. The compound was characterized by its IR spectrum as well as by an X-ray structure determina-tion. Crystal data: space group PI, Z = 2 (2851 observed independent reflexions, R = 0.047). Lattice dimensions at 20 °C: a = 1135.0(3); b = 1219.6(4); c = 1372.4(4) pm; a = 106.74(3)°; ß = 107.92(4)°; y = 91.40(4)°. The compound forms dimeric molecules with a short Cu--Cu contact of 242 pm and two chelating amidinato ligands with Cu-N bond lengths of (averaged) 189.0 pm and bond angles N —C—N of 124.1°. 
  Reference    Z. Naturforsch. 43b, 1628—1632 (1988); eingegangen am 11. August/30. September 1988 
  Published    1988 
  Keywords    Synthesis, X-Ray, Copper(I) Amidinato Complex 
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 Identifier    ZNB-1988-43b-1628 
 Volume    43 
18Author    Dieter Fenske, Eberhard Böhm, Kurt Dehnicke, Joachim SträhleRequires cookie*
 Title    N-TrimethylsilyMminotriphenylphosphoran-Kupfer(II)-chlorid, (Me 3 SiNPPh 3 * CuCl 2 ]2 Synthese und Kristallstruktur N-Trimethylsilyl-iminotriphenylphosphorane Copper(II) Chloride, [Me 3 SiNPPh 3 * CuCl : ] 2 Synthesis and Crystal Structure  
 Abstract    The title compound has been prepared by the reaction of N-trimethylsilyl-iminotriphenylphos-phorane with copper(II) chloride in boiling CCl 4 /C 2 H 5 OH, and forms moisture sensitive crystals, which are green in transmittance and black in reflexion. [Me 3 SiNPPh 3 • CuCl 2 ] 2 was characterized by its IR spectrum as well as by a crystal structure determination (4197 observed, independent reflexions, R = 0.049). The lattice dimensions are at 20 °C: a = 1102.7. b = 1407.3. c = 1560.2 pm; ß = 94.27°; space group P2,/« with two formula units in the unit cell. The complex consists of centrosymmetric, dimeric molecules with a planar Cu 2 Cl 2 ring (Cu —CI bond lengths 229 and 231 pm). A terminally bonded CI atom (Cu —CI = 221 pm) and the N atom of the Me,SiNPPh 3 ligand (Cu —N = 198.5 pm) complete the coordination number four of the nearly planar surroundings of the Cu atoms. 
  Reference    (Z. Naturforsch. 43b, 1 [1988]; eingegangen am 4. September 1987) 
  Published    1988 
  Keywords    N-Trimethylsilyl-iminotriphenylphosphorane Copper(II) Chloride, Synthesis, IR Spectra, Crystal Structure 
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 Identifier    ZNB-1988-43b-0001 
 Volume    43 
19Author    Andrea Maurer, Dieter Fenske, Johannes Beck, Wolfgang Hiller, Joachim Strähle, Eberhard Böhm, Kurt DehnickeRequires cookie*
 Title    Kupfer(I)-chlorid-Addukte von Phosphoraniminen Die Kristallstrukturen von Ph 3 PNPh * CuCl und von 2,3-Bis(triphenylphosphoranylidenamino)maIeinsäure-N-methylimid- Kupfer(I)-chlorid Copper(I) Chloride Adducts of Phosphoranimines The Crystal Structures of Ph 3 PNPh-CuCl and of 2,3-Bis(triphenylphosphoranylideneamino)maleic Acid N-Methylimide Copper(I) Chloride  
 Abstract    The title compounds Ph,PNPhCuCl (1) and (Ph,P) 2 N : C 4 0 2 (NMe) CuCl (2) have been prepared by the reactions of CuCl with the corresponding phosphoranimines Ph 3 PNPh and 2.3-bis(triphenylphosphoranylideneamino)maleic acid N-methylimide, respectively. Both com-plexes were characterized by their IR spectra as well as by crystal structure determinations. PhiPNPh • CuCl (1): space group PI, Z = 4, 3639 independent observed reflexions, R = 0.038. Lattice dimensions (18 °C): a = 1047.6; b = 1251.5; c = 1755 pm; a = 103.43°; ß = 97.24°; y = 101.30°. The compound forms monomeric molecules; the asymmetric unit contains two crystallo-graphically independent molecules. The CuCl molecule is bonded via the N atom of the phos-phoranimine. Bond lengths: Cu—N = 189 pm; Cu —CI = 209 pm; bond angle N —Cu —CI = 177°. (PhiP),NiC 4 Oi(NMe) CuCl (2): space group Pbca, Z = 8, 5611 independent, observed reflex-ions, R = 0.069. Lattice dimensions (25 °C): a = 1224.3; b = 1962.5: c = 2994.0 pm. The compound forms monomeric molecules with the CuCl molecule bonded via one of the N atoms of the phosphoranimine groups. Bond lengths: Cu—N = 194 pm; Cu—CI = 212 pm; bond angle N—Cu —CI -175°. 
  Reference    (Z. Naturforsch. 43b, 5—11 [1988]; eingegangen am 4. September 1987) 
  Published    1988 
  Keywords    Copper(I) Chloride Adducts of Phosphoranimines, Synthesis, IR Spectra Crystal Structure 
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 Identifier    ZNB-1988-43b-0005 
 Volume    43 
20Author    M. Veith, J. PöhlmannRequires cookie*
 Title    Nitrogen Compounds of Elements of the Third Main Group with Intra-and Intermolecular Donor Acceptor Bonds, V [1] Special Gallium and Indium Amides with Alkoxo Groups  
 Abstract    The lithium alkoxoamidosilane (Me2Si(O r Bu)(N r Bu)Li)2 (4) and its trimethyltin derivative Me2Si(0'Bu)(N'Bu)SnMe3 (7) have been used, to introduce the ligand Me2Si(0'Bu)(N'Bu) = L into molecular compounds of gallium and indium. The following molecules were synthesized: L—M(Me)Cl (M = Ga (5), In (6)), L-InMe2 (8), L-InX2 (X = Cl (9), Br (10)), L2InX (X = Cl (11), Br (12)) and L2Ga2Cl2 (22). The ligand L is assumed to chelate the metal atom on the basis of temperature dependent 'H NMR spectra. The chelating effect is more pronounced in the gallium derivatives than in the indium analogues. Equilibria between L2InX/InX, and LInX: have been observed in diethylether solutions. No metal(I) derivatives LGa or Lin could be isolated. L2Ga2Cl2 (22), formally containing gallium(ll), can be sublimed without decomposition at 110 °C in vacuo. 
  Reference    Z. Naturforsch. 43b, 505—512 (1988); eingegangen am 28. Dezember 1987 
  Published    1988 
  Keywords    Synthesis, Chelated Metal Atoms, Intramolecular Rearrangements, Equilibria Followed by 'H NMR 
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 Identifier    ZNB-1988-43b-0505 
 Volume    43 
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