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1987 (16)
1Author    Gertrud Weiler, Gottfried Huttner, Laszlo Zsolnai, Heinz BerkeRequires cookie*
 Title    Phosphordonor-substituierte Formylmangan-Komplexe Phosphorous Donor Substituted Formyl Manganese Complexes  
 Abstract    Phosphonomanganese complexes (CH 3 0) 2 (0)PMn(C0)3[P(0CH 3)3] 2 (lb), (CH 3 0) 2 (0)PMn(C0) 2 [P(0CH 3) 3 ] 3 (lc) are obtained via demethylation of the corresponding cationic substituted carbonylmanganese compounds with KHB(secBu) 3 . The reaction of NaBH 4 in methanol with cationic phosphorus donor substituted carbonyl manganese compounds leads to formyl complexes (OC) 3 L 2 MnCHO (L = P(OCH 3) 3 (3a), L = P(OEt) 3 (3c), L -P(0*Pr) 3 (3d), L = PPh 3 (3e)) and (OC) 2 [P(OCH 3) 3 ] 3 MnCHO (3b). 3d decomposes thermally to give an (OC) 3 [P(OzPr) 3 ] 2 MnH and an (0C) 2 [P(0/Pr) 3 ] 3 MnH complex. The latter has been characterized by an X-ray structure determination. 
  Reference    Z. Naturforsch. 42b, 203—209 (1987); eingegangen am 22. August 1986 
  Published    1987 
  Keywords    Formyl, Hydride Complexes, X-Ray 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-0203.pdf 
 Identifier    ZNB-1987-42b-0203 
 Volume    42 
2Author    Richard Neidlein, Dagmar Knecht, Alfred Gieren, Catalina Ruiz-PérezRequires cookie*
 Title      
 Abstract    The synthesis of 1 by reaction of phenanthro[9,10-c]-l,2,5-selenadiazole with ethylmagnesium-bromide and TeCI 4 is described; the X-ray structure analysis is reported. 
  Reference    (Z. Naturforsch. 42b, 84—90 [1987]; eingegangen am 9. August 1986) 
  Published    1987 
  Keywords    Chalkogen-Diimides, 1, 2, 5-Telluradiazole, X-Ray 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-0084.pdf 
 Identifier    ZNB-1987-42b-0084 
 Volume    42 
3Author    W. S. Sheldrick, P. BellRequires cookie*
 Title    Interaction of Metal Ions with 7-Deaza-8-aza-and 8-Aza-purines Preparation and X-Ray Structural Analysis of Copper(II) Complexes  
 Abstract    The reaction of 8-aza-and 7-deaza-8-aza-purines with Cu :+ cations in acid solution has been studied. At a pH value of 2, the 8-azaadenine complex [Cu(H 2 0) 4 (AAdH) 2 ](N0 3) 2 (1), which displays Cu-N9 coordination, may be isolated from solution. The reaction of CuCl 2 with 8-aza-hypoxanthine in concentrated HCl solution leads to ring opening at C 2 of the azapurine with subsequent formation of dichlorobis[(5-amino-4-carboxamide)[l — 3]triazole] copper(II) dihydrate 2, in which the triazole ligands display a chelating function, coordinating the metal via N7 and 06. The results for 1 and 2 suggest that copper coordination of the azapurine base is not a prerequisite for opening of the pyrimidine ring. Respectively N9-and N8-coordinated complexes [CUC13(A11H3)]" 3 and [CuCl 2 (H 2 0)(MAllH)] n (4) of allopurinol (A11H 2) and 9-methylallopurinol (MA11H) may be prepared by the reaction of CuCl 2 with the respective bases in HCl solution. In contrast, with the analogous l-methyl-4-aminopyrazolo[3,4-d]pyrimidine MAPP, only the salt (MAPPH)4(CU2C18) (5) could be isolated under similar conditions, indicating that N8 is less attractive as a binding site in this 7-deaza-8-azaadenine derivative. The structures of 1—5 have been established by X-ray structural analysis. A distorted octahedral [4+2]geometry is found for the copper atoms in 1 and 2. Chlorine bridged polymeric chain structures are adopted by the complexes 3 and 4. An intermediate coordination geometry between trigonal bipyramidal and square-pyrami-dal is observed for the metal atoms in 3, a distorted square-pyramidal geometry in 4. 
  Reference    Z. Naturforsch. 42b, 195—202 (1987); received August 18/October 17 1986 
  Published    1987 
  Keywords    8-Azapurines, Allopurinol, Copper(II) Complexes, X-Ray 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-0195.pdf 
 Identifier    ZNB-1987-42b-0195 
 Volume    42 
4Author    Wolfgang Hönle, Bernhard Hettich, Arndt SimonRequires cookie*
 Title    Preparation and Crystal Structure of LiGaCLj and LiGaI 4  
 Abstract    The crystal structures of LiGaCl 4 and LiGaI 4 have been determined by single crystal X-ray methods. Both compounds are isotypic with LiAlCl 4 and characterized by LiX 6 octahedra and GaX 4 tetra-hedra. Mean bond lengths are: d(Ga-X) = 217.4 pm (Cl) and 255.9 pm (I); d(Li-X) = 263.9 pm (Cl) and 305.3 pm (I), respec-tively. Common features of the isotypic compounds LiGaX 4 (X -Cl, Br. I) are discussed. 
  Reference    Z. Naturforsch. 42b, 248—250 (1987); eingegangen am 17. Oktober 1986 
  Published    1987 
  Keywords    Crystal Structure, X-Ray, Lithium Compounds 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-0248_n.pdf 
 Identifier    ZNB-1987-42b-0248_n 
 Volume    42 
5Author    K. Wieghardt, S. Brodka, K. Peters, E. M. Peters, A. SimonRequires cookie*
 Title    Säure-Base-Eigenschaften des zyklischen Triamins N,N',N"-Trimethyl-l,4,7-triazacyclononan: Die Kristallstruktur seiner monoprotonierten Form [C9H22N3KCIO4) Acid-Base Properties of the Cyclic Triamine N,N\N"-Trimethyl-l,4,7-triazacyclononane and Crystal Structure of its Monoprotonated Form [C 9 H 2 2N 3 ](C10 4 )  
 Abstract    The crystal structure of the monohydroperchlorate of N,N',N"-trimethyl-l,4,7-triazacyclo-nonane, [C 9 H 2 2N3](C10 4), has been determined by single crystal X-ray diffraction. The acidic proton of the cation is bonded to one amine nitrogen and it forms hydrogen bonds to the other two N-atoms in agreement with a proposed model, which has been invoked to interpret successive protonation constants of cyclic triamines. The salt [Me 6 [9]aneN 3 ](BF 4)3 has also been prepared. 
  Reference    Z. Naturforsch. 42b, 279—281 (1987); eingegangen am 8. Oktober/24. November 1986 
  Published    1987 
  Keywords    Macrocyclic Triamine, X-Ray, Acid-Base Properties 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-0279.pdf 
 Identifier    ZNB-1987-42b-0279 
 Volume    42 
6Author    Norbert Kuhn, Hans Schumann, Gotthelf WolmershäuserRequires cookie*
 Title    {tert-C 4 H 9 ) 3 PTe — ein typisches Tellurophosphoran? [1] (ferr-C 4 H 9 ) 3 PTe -a Typical Tellurophosphorane? [1]  
 Abstract    The P-Te bond length in (r<?rr-C 4 H 9) 3 PTe of 2.368 Ä corresponds to a bond order near 1.5. The distance may be influenced by the tert-C 4 H 9 groups, but the 125 Te NMR shift is well within the common R,PTe range, while 7(125 Te-31 P) is about 140 Hz smaller than in other tellurophos-phoranes. 
  Reference    Z. Naturforsch. 42b, 674—678 (1987); eingegangen am 15. Januar 1987 
  Published    1987 
  Keywords    Tellurophosphoranes, X-Ray, 125 Te NMR Spectra 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-0674.pdf 
 Identifier    ZNB-1987-42b-0674 
 Volume    42 
7Author    Z. NaturforschRequires cookie*
 Title    Darstellung und Kristallstrukturen von C a^ ^ N und Sr4In2N  
 Abstract    The new compounds Ca4In2N and Sr4In2N crystallize in the tetragonal system (space group 14,/am d, No. 141). In and Ca together form a rocksalt structure. All octahedral holes, which are built by Ca only, are occupied by nitrogen. The In atom s form In —In zig-zag-chains; the In —In bond lengths are 316.4 pm (Ca com pound) and 332.0 
  Reference    Z. Naturforsch. 42b, 825—827 (1987); eingegangen am 1. April 1987 
  Published    1987 
  Keywords    Crystal Structure, X-Ray, Alkaline E arth Indium Nitrides 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-0825.pdf 
 Identifier    ZNB-1987-42b-0825 
 Volume    42 
8Author    Regine Herbst, KatteshV. Katti, HerbertW. Roesky, GeorgeM. SheldrickRequires cookie*
 Title    Synthese und Struktur des ersten Cyclophosphazens mit einer M etall—Metall-Bindung im Ringgerüst Synthesis and Structure o f the First Cyclophosphazene Containing a Metal —Metal Bond within the Ring Skeleton  
 Abstract    The reaction of [H2NPPh2NPPh2N H 2]Cl (1) with WClft (2) proceeds with formation of NPPh2NPPh2NWCl3 (3) and HCl,N6P4Ph8W 2 (4). 3 is the main product of this reaction. 4 was characterized by an X-ray structure determination. 4 contains a seven and a six-membered phos-phorus-nitrogen ring with a W —W bond of 269.2 pm. 
  Reference    Z. Naturforsch. 42b, 1387 (1987); eingegangen am 22. Juni/6. August 1987 
  Published    1987 
  Keywords    Tungsten, 6;r-Systems, X-Ray, Phosphorus-Nitrogen Compound 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-1387.pdf 
 Identifier    ZNB-1987-42b-1387 
 Volume    42 
9Author    Peter Schreiber, Karl Wieghardt, Ulrich Flörke, Hans-Jürgen HauptRequires cookie*
 Title    Synthese von Wolframkomplexen  
 Abstract    des Typs [ L W (C O) 3X ] + (X = H , F, Br; L = 1,4,7-Triazacyclononan). Die Kristallstrukturen von [L W (C O) 3B r]B F 4 und [L W (C O) 3H ] 2[W O C l5] • h 2o Synthesis o f Tungsten Complexes o f the Type [L W (C O)3X ] + (X = H, F, Br; L = 1.4,7-triazacyclononane). The Crystal Structures o f [L W (C O)3Br]BF4 and [L W (C O)3H ]2[W O C l5] • H 20 The reaction of LW (C O), (L = 1,4,7-triazacyclononane) with Br2 in CHCl, yields orange [L W (C O)3Br](Br3) which was converted to its BF4~ salt. [L W (C O)3Br]BF4 crystallizes in the triclinic space group P 1 (a = 8.273(3), b = 8.628(2), c = 13.034(3) Ä , a = 80.10(2), ß = 72.69(2). y = 61.14(2)°, Z = 2); it consists of cations [L W (C O)3Br] + , with seven-coordinate W atoms, and BF4 -anions. The corresponding salt [L W (C O)3F](PFft) was obtained from L W (C O)3 with 20% aqueous HF in the presence of air and addition of NaPF6. The analogous reaction with 37% aqueous HC1 affords green crystals of [L W (C O)3H ]2[W OCl5] • H 20 which crystallize in the mono­ clinic space group P2,/c (a = 12.234(4), b = 18.853(7), c = 14.609(5) Ä . ß = 105.65(3)°, Z — 4). The W atoms in the [L W (C O)3H ]+ cations are seven-coordinate; the six-coordinate [W OCl5]: anions are not disordered. The W = 0 distance is short (1.72(1) Ä), the mean equatorial W —Cl distance is 2.390 Ä whereas the W —Cl bond distance trans to the W = 0 group is 2.562(5) Ä. 
  Reference    Z. Naturforsch. 42b, 1391 (1987); eingegangen am 2. Juli 1987 
  Published    1987 
  Keywords    Tungsten Complexes, X-Ray, Crystal Structure 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-1391.pdf 
 Identifier    ZNB-1987-42b-1391 
 Volume    42 
10Author    D. Ieter, F. Enske, PaulM. Aue, K. Urt, M. Erzw EilerRequires cookie*
 Title    Zur  
 Abstract    Reaktion von (f/5-C5H 5)F e(C O)2Br mit Se(SiM e3)2 D ie Kristallstruktur von [S e{F e(C O)2(C5H 5)} 3]2[Fe4Se4Br4] R eaction of (^ -C s H ^ F e ^ O ^ B r with Se(SiM e3) 2 T he C rystal S tructure of [Se {F e (C O)2 (C 5 H 5) } 3 ]2 [Fe4Se4 B r4] 
  Reference    Z. Naturforsch. 42b, 928 (1987); eingegangen am 17. Februar 1987 
  Published    1987 
  Keywords    Synthesis, X -Ray, Crystal Structure of [Fe4Se4B r4]2~-Cluster 
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 Identifier    ZNB-1987-42b-0928_n 
 Volume    42 
11Author    Joachim FuchsRequires cookie*
 Title    Kristallstrukturen und Schwingungsspektren zweier  
 Abstract    isomerer Oktadekawolframatodiarsenate, (NH4)6As2W180 62 • #iH20 C rystal S tructures and V ibrational Spectra of Tw o Isom ers of O ctadecatungsto-diarsenate (N H 4)6A s2W 18 0 6 2 • mH20 H o lg er N eu b e rt Six possible structures of A s2W ,80 626~ are discussed, and an exact nom enclature is proposed. The structures of the isomeric title compounds (I and II) were determ ined by X-ray diffraction. I crystallizes in space group P I with lattice param eters a = 12.965(4), b = 14.803(5), c = 18.515(6) Ä; a = 96.280(23)°, ß = 91.420(25)°, y — 115.320(25)°. The anion has the configuration first observed in K6P2W ,80 62-14 H 20 (D awson-structure). II was not known until now. It crystal­ lizes in the trigonal space group R 3 with lattice param eters a — b — 37.857(32). c = 13.108(13) Ä; a — ß = 90°, y = 120°. The structure of this anion differs from the D awson-structure by the 60° rotation of both polar groups of three W 0 6-octahedra (/3-type), followed by the 60° rotation of one of the two new AsWyO,,-units. Both rotations are about the 3-fold axis. The anion is centrosym m etric. Vibrational spectra and preparation of the isomers are described. 
  Reference    Z. Naturforsch. 42b, 951—958 (1987); eingegangen am 4. März/11. Mai 1987 
  Published    1987 
  Keywords    T ungstoarsenates, Isomers, X-Ray, V ibrational Spectra, Preparation 
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 Identifier    ZNB-1987-42b-0951 
 Volume    42 
12Author    Harald Labischinski, Dieter Naumann, Gerhard Barnickel, Wolfgang Dreißig, Wojciech Gruszecki, Andreas Hofer, Hans BradaczekRequires cookie*
 Title    Comparison between the Molecular and Crystal Structures of a Benzylpenicillin Ester and its Corresponding Sulfoxide with Drastically Reduced Biological Activity  
 Abstract    A comparative X-ray structure determination was performed to elucidate possible conforma-tional differences between penicillins and penicillin sulfoxides. Penicillin-G-acetoxy-methylester and its Iß-oxide were used as model substances, because the only chemical difference between both compounds resides in the thiazolidine ring sulfur oxidation. On the basis of the X-ray data as well as of infrared measurements it is discussed that the drastically reduced biological activity of the penicillin-G-sulfoxide might be related to conformational differences in thiazolidine ring puckering or, even more simply, to the geometric position of the sulfoxide oxygen atom, both of which may hamper the proper reaction of the sulfoxide with its target enzyme(s). 
  Reference    Z. Naturforsch. 42b, 367—375 (1987); received June 30/0ctober 14 1986 
  Published    1987 
  Keywords    X-Ray, Penicillin G, Penicillin G Sulfoxide, Thiazolidine Ring Conformation, Structure Activity Relationships 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-0367.pdf 
 Identifier    ZNB-1987-42b-0367 
 Volume    42 
13Author    Henry Strasdeit, Bernt Krebs, G. HenkelRequires cookie*
 Title    [Fe 6 Se 9 (SR) 2 ] 4 ' Clusters (R = Me, CH 2 Ph): Synthesis and Characterization, and the X-Ray Structure of (PhCH 2 NEt3)4[Fe 6 Se 9 (SMe)2]  
 Abstract    The compounds (PhCH 2 NEt 3) 4 [Fe 6 Se 9 (SMe) 2 ] (1) and (Et 4 N) 4 [Fe 6 Se 9 (SCH 2 Ph) 2 ] (2) have been isolated in good yields from Fe(SR) 3 (R = Me, CH 2 Ph)/"Na 2 Se 2 " reaction mixtures in methanol/N,N-dimethylformamide after addition of the appropriate tetraalkylammonium chlorides. 1 is monoclinic, space group P2]/c, Z = 4, with a = 18.697(14), b -22.606(16), c = 15.989(11) Ä, and/3 = 94.15(6)° at 140 K. Its structure has been refined to R (R w) -0.092 (0.075). The [Fe 6 Se 9 (SMe) 2 ] 4_ anion contains six coplanar iron atoms which are present in distorted tetrahedral Se 4 and Se 3 (SMe) ligand surroundings. The Se atoms are n, and fi 4 bridging. The four central Fe atoms and the Se atoms constitute a Fe 4 Se 9 group that is structurally related to 4[Fe 2 Se 3 ] 2_ double tetrahedral chains and 2 [FeSe] layers. The Fe atoms in the [Fe 6 Se 9 (SMe) 2 ] 4 ~ cluster are antiferromagnetically coupled. 1 has a room-temperature magnetic moment of 1.22 ,M B /Fe. Cyclic voltammograms, and electronic, infrared, and proton resonance spectra of 1 and 2 have been measured. 
  Reference    Z. Naturforsch. 42b, 565—572 (1987); received December 1 1986 
  Published    1987 
  Keywords    Hexanuclear Fe/Se/SR Complexes, Synthesis, X-Ray, Magnetic and Electrochemical Properties 
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 Identifier    ZNB-1987-42b-0565 
 Volume    42 
14Author    Dieter Fenske, Karin Völp, Kurt DehnickeRequires cookie*
 Title    N-Chlor-Nitrenokomplexe des Molybdäns: M oF4(NC1) und [C H 3C N -M oF4(N C 1)] N-Chloro-Nitrene Complexes o f Molybdenum: M oF 4(NC1) and [C H 3C N -M o F 4(NC1)]  
 Abstract    MoF4(NC1) has been prepared as a yellow crystal powder by the reaction of diluted fluorine with MoCl3(N 3S2) at room temperature. The compound is associated via fluorine bridges, accord­ ing to the IR spectrum. With acetonitrile, the monomeric complex [CH3CN —MoF4(NC1)] is obtained, which was characterized by its IR and l9F N M R spectra as well as by an X-ray structure determination. Crystal data: space group Pm, Z — 2 (1068 observed, independent reflexions, R — 0.03). Lattice dimensions at —90 °C: a — 507.1. b = 704.8, c = 995.8 pm, ß — 102.02°. The unit cell contains two crystallographically independent molecules [CH3CN —MoF4(NC1)], the M o = N —Cl groups being linear (bond angles 176°, 178°) with bond lengths MoN = 172 and NCI = 159. 162 pm. In the trans position to the MoNCl group, the nitrogen atom of the acetonitrile molecule is coordinated. 
  Reference    Z. Naturforsch. 42b, 1398—1402 (1987); eingegangen am 2. Juli 1987 
  Published    1987 
  Keywords    IR Spectra, I9F N M R Spectra, X-Ray, N-Chloro-Nitrene-Molybdenum Tetrafluoride, Acetonitrile Adduct 
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 Identifier    ZNB-1987-42b-1398 
 Volume    42 
15Author    WolfPeter Fehlhammer, Dagobert Achatz, Ulrike Plaia, Alfons VölklRequires cookie*
 Title    Metallkomplexe funktioneller Isocyanide, XIV [1] [3+2]-Cycloadditionen zwischen Metallo-Nitrilyliden und CS 2 und Carbenübertragung: Thiazolin-2-yliden-Komplexe von Chrom, Wolfram und Palladium Metal Complexes of Functional Isocyanides, XIV [1] [3+2] Cycloadditions between Metallo Nitrile Ylids and CS 2 and Carbene Transfer: Thiazoline-2-ylidene Complexes of Chromium, Tungsten and Palladium  
  Reference    Z. Naturforsch. 42b, 720—727 (1987); eingegangen am 26. Januar 1987 
  Published    1987 
  Keywords    a-Metalated Isocyanides, Reactions at Coordinated Ligands, Metals in Organic Synthesis, Carbenoid Heterocycles, X-Ray 
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 Identifier    ZNB-1987-42b-0720 
 Volume    42 
16Author    M. =., Ti, HeinzDieter Lutz, Klaus Wussow, Peter KuskeRequires cookie*
 Title    Ionic Conductivity, Structural, IR and Raman Spectroscopic Data o f Olivine, Sr2P b 0 4, and N a2CuF4 Type Lithium and Sodium Chlorides L i2Z n C l4 and N a 2M C l4 (  
 Abstract    The ionic conductivities (complex impedance measurements) of the olivine type Li2ZnCl4, Na2ZnCl4 and Na2CoCl4, the Sr2P b 0 4 type Na2MgCl4, Na2MnCl4, and Na2CdCl4, and the novel Na2CrCl4 with monoclinically distorted Sr2P b 0 4 structure (Na2CuF4 type) are presented. The specific conductivities of Li2ZnCl4 and the Na2MCl4 are about three orders of magnitude lower than those of the fast ionic conducting lithium chloride spinels Li[LiM ]Cl4 (M = Mg, Mn. Fe. Cd. etc.) indicating that in the latter compounds the tetrahedrally coordinated lithium ions exhibit higher mobility than those on octahedral sites. The X-ray data including those of Sr2P b 0 4 type Na2TiCl4 and both the IR and Raman spectra (together with a group theoretical treatment) are also given. The spectra obtained confirm the different structure types of the ternary chlorides. 
  Reference    Z. Naturforsch. 42b, 1379—1386 (1987); received July 15 1987 
  Published    1987 
  Keywords    Cr, Mn, Co, Zn, C d) Lithium Zinc Chloride Sodium Chlorides Olivine and Sr2P b 0 4 Type Ionic Conductivity, X-Ray 
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 Identifier    ZNB-1987-42b-1379 
 Volume    42 
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