| 1 | Author
| Gertrud Weiler, Gottfried Huttner, Laszlo Zsolnai, Heinz Berke | Requires 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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| default:Reihe_B/42/ZNB-1987-42b-0203.pdf | | | Identifier
| ZNB-1987-42b-0203 | | | Volume
| 42 | |
2 | Author
| Richard Neidlein, Dagmar Knecht, Alfred Gieren, Catalina Ruiz-Pérez | Requires 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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| default:Reihe_B/42/ZNB-1987-42b-0084.pdf | | | Identifier
| ZNB-1987-42b-0084 | | | Volume
| 42 | |
3 | Author
| W. S. Sheldrick, P. Bell | Requires 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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| default:Reihe_B/42/ZNB-1987-42b-0195.pdf | | | Identifier
| ZNB-1987-42b-0195 | | | Volume
| 42 | |
4 | Author
| Wolfgang Hönle, Bernhard Hettich, Arndt Simon | Requires 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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| default:Reihe_B/42/ZNB-1987-42b-0248_n.pdf | | | Identifier
| ZNB-1987-42b-0248_n | | | Volume
| 42 | |
5 | Author
| K. Wieghardt, S. Brodka, K. Peters, E. M. Peters, A. Simon | Requires 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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| default:Reihe_B/42/ZNB-1987-42b-0279.pdf | | | Identifier
| ZNB-1987-42b-0279 | | | Volume
| 42 | |
9 | Author
| Peter Schreiber, Karl Wieghardt, Ulrich Flörke, Hans-Jürgen Haupt | Requires 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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| default:Reihe_B/42/ZNB-1987-42b-1391.pdf | | | Identifier
| ZNB-1987-42b-1391 | | | Volume
| 42 | |
10 | Author
| D. Ieter, F. Enske, PaulM. Aue, K. Urt, M. Erzw Eiler | Requires 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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| default:Reihe_B/42/ZNB-1987-42b-0928_n.pdf | | | Identifier
| ZNB-1987-42b-0928_n | | | Volume
| 42 | |
11 | Author
| Joachim Fuchs | Requires 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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| default:Reihe_B/42/ZNB-1987-42b-0951.pdf | | | Identifier
| ZNB-1987-42b-0951 | | | Volume
| 42 | |
12 | Author
| Harald Labischinski, Dieter Naumann, Gerhard Barnickel, Wolfgang Dreißig, Wojciech Gruszecki, Andreas Hofer, Hans Bradaczek | Requires 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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| default:Reihe_B/42/ZNB-1987-42b-0367.pdf | | | Identifier
| ZNB-1987-42b-0367 | | | Volume
| 42 | |
13 | Author
| Henry Strasdeit, Bernt Krebs, G. Henkel | Requires 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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| default:Reihe_B/42/ZNB-1987-42b-0565.pdf | | | Identifier
| ZNB-1987-42b-0565 | | | Volume
| 42 | |
14 | Author
| Dieter Fenske, Karin Völp, Kurt Dehnicke | Requires 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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| default:Reihe_B/42/ZNB-1987-42b-1398.pdf | | | Identifier
| ZNB-1987-42b-1398 | | | Volume
| 42 | |
15 | Author
| WolfPeter Fehlhammer, Dagobert Achatz, Ulrike Plaia, Alfons Völkl | Requires 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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| default:Reihe_B/42/ZNB-1987-42b-0720.pdf | | | Identifier
| ZNB-1987-42b-0720 | | | Volume
| 42 | |
16 | Author
| M. =., Ti, HeinzDieter Lutz, Klaus Wussow, Peter Kuske | Requires 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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| default:Reihe_B/42/ZNB-1987-42b-1379.pdf | | | Identifier
| ZNB-1987-42b-1379 | | | Volume
| 42 | |
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