| 23 | Author
| Z. Naturforsch | Requires cookie* | | Title
| U ntersuchungen an Polyhalogeniden, X X X IX  | | | Abstract
| [1] [(H 30)(1 8 -K r o n e -6)]I7, eine Struktur-Neubestim m ung Studies on Polyhalides, X X X IX [1] S tructure R efinem ent of [(H 30)(1 8 -cro w n -6)]I7 Sawsan A bd El K halika, M ervat El Essaw ia, Ingo D om brow skih, K arl-Friedrich T ebbeb * The structure analysis of the compound [(H30)(18-Krone-6)]I7 has been repeated. The al ready known structure could now be described with improved precision. The unique polyiodide chain i [ (I _'2I2) I2] may be derived from the regu lar three dimensional iodide-iodine lattice c»[U 3I2] by separation. | | |
Reference
| Z. Naturforsch. 54b, 136—139 (1999); eingegangen am 6. Oktober 1998 | | |
Published
| 1999 | | |
Keywords
| Polyhalogenide, Heptaiodide, Crown Ether, Oxonium Compound, Crystal Structure | | |
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| default:Reihe_B/54/ZNB-1999-54b-0136_n.pdf | | | Identifier
| ZNB-1999-54b-0136_n | | | Volume
| 54 | |
24 | Author
| Ju Tta, G. Rebe, G. Ertrau, G. Eiseier, KlausH. Arm, KurtD. Ehnicke | Requires cookie* | | Title
| Synthese und Kristallstruktur von P P h 4[P hIC l3] Synthesis and Crystal Structure of P Ph4[PhIC l3]  | | | Abstract
| Phenyl-trichloro-iodate(III), Synthesis, Crystal Structure Phenyl-iodo-dichloride reacts with tetraphenyl-phosphonium chloride in dichloromethane solu tion to give the phenyltrichloroiodate(III) com plex PPh4[PhICl3]. The compound forms pale yel low crystals, which have been characterized by a crystal structure determination. Space group P i, Z = 2, lattice dimensions at -50 °C: a = 1018.7(2), b = 1232.9(2), c = 1287.3(2) pm, a = 81.94(1)°, ß = 66.61(1)°, y = 71.62(1)°, /?, = 0.0425 for 3976 observed independent reflections. The structure consists of PPh4+ ions and anions [Ph-IC l3]~ with a planar coordination environment of the iodine atom. The I-C l bond length of the chlorine atom trans to the phenyl group is much longer (301.9(1) pm) than the cis chlorine atoms with 250,4(1) pm in average. | | |
Reference
| Z. Naturforsch. 54b, 140—143 (1999); eingegangen am 2. Oktober 1998 | | |
Published
| 1999 | | |
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| default:Reihe_B/54/ZNB-1999-54b-0140_n.pdf | | | Identifier
| ZNB-1999-54b-0140_n | | | Volume
| 54 | |
25 | Author
| Dilip Kumar Dey, MrinalKanti Dasa, Heinrich Nöth | Requires cookie* | | Title
| Synthesis, Spectroscopy and Structure of Diorganotin(IV) Schiff Base Complexes  | | | Abstract
| Three diorganotin(IV) chelates with a tetradentate Schiff base, H2Vanophen, [FLVanophen = N,N'-l,2-phenylen-bis(3-methoxysalicylideneimine)] of the type R2Sn(Vanophen) (R = Ph: 1; R = rt-Bu: 2; R = Me: 3) have been synthesized by the reaction of R2SnCl2 (R = Ph, n-Bu, Me) and FLVanophen in the presence of triethylamine in benzene. The complexes have been characterised by IR and NMR spectroscopy and by elemental analysis. The <$(' l9Sn) values for the complexes 1 -3 are -543.0, -414.2 and -398.2 ppm respectively, indicating hexacoordinated Sn centers. These have been ascertained by X-ray crystal structure determinations of 1 and 3. The distances between tin and the two axial carbon atoms in each complex differ not significantly [2.17(1) Ä in 1, and 2.100(3) and 2.115(3) A in 3). The C-Sn-C angles for 1 and 3 are 165.9(4)° and 159.96(9)°, respectively. The solution NMR spectra ('H , l3C, 1|ySn) show clearly that the solid state structures are retained in solution. | | |
Reference
| Z. Naturforsch. 54b, 145—154 (1999); received September 16 1998 | | |
Published
| 1999 | | |
Keywords
| Diorganotin(IV) Complexes, FLVanophen, X-Ray Data, Infrared Data, NMR Data | | |
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| default:Reihe_B/54/ZNB-1999-54b-0145.pdf | | | Identifier
| ZNB-1999-54b-0145 | | | Volume
| 54 | |
26 | Author
| Marcus Branda, Albert Fringsd, Peter Jenkner0, Robert Lehnerta, HansJürgen Mettemicha, Jaroslaw Monkiewiczd, Jürgen Schramc, HülsStructura Gmbh, Friedrich Von, Heyden Platz | Requires cookie* | | Title
| NMR-spektroskopische Untersuchungen zur Hydrolyse von funktionellen Trialkoxysilanen NMR-Spectroscopic Investigations on the Hydrolysis of Functional Trialkoxysilanes  | | | Abstract
| The hydrolysis of functional trialkoxysilanes was studied under various conditions by 'H NMR spectroscopy. The silane concentration was 1 -2% by weight in a water/acetone-system. Under these conditions, the reaction was found to be first order. In detail, influence of pH, grade of stirring, and size and structure of functional groups of the alkyltrialkoxysilanes were investigated in order to compare the relative reaction rates of the different compounds. | | |
Reference
| Z. Naturforsch. 54b, 155—164 (1999); eingegangen am 9. September 1998 | | |
Published
| 1999 | | |
Keywords
| Organofunctional Silanes, Trialkoxysilanes, Tetraalkoxysilanes, Hydrolysis, Siloxanes | | |
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| default:Reihe_B/54/ZNB-1999-54b-0155.pdf | | | Identifier
| ZNB-1999-54b-0155 | | | Volume
| 54 | |
27 | Author
| Barbara Wenzel, Peter Strauch | Requires cookie* | | Title
| Synthesis, Structural and EPR Investigations on Bis(tetraphenylphosphonium)- bis(l,2-dithiosquarato)oxovanadate(IV), (Ph4P)2[VO(dtsq)2]  | | | Abstract
| The molecular structure and EPR studies of bis(tetraphenylphosphonium)bis(1,2-dithiosquarato)oxovanadate(IV) are reported. (Ph4P)2[VO(dtsq)2] crystallizes in the mono clinic spaceogroup P2,/n with the unit cell parameters a = 10,9820(2), b = 15,4620(3), c = 14,5050(3) Ä, ß = 95,700(8)°, Z = 2. The g and hyperfine coupling tensors Av obtained from the EPR spectra in liquid and frozen solution are used to characterize the properties of the molecular orbital containing the unpaired electron and are compared to those obtained from EHT-MO calculations. | | |
Reference
| Z. Naturforsch. 54b, 165—170 (1999); eingegangen am 18. September 1998 | | |
Published
| 1999 | | |
Keywords
| Sulfur, Oxovanadate(IV), Synthesis, EPR Data, Crystal Structure | | |
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| default:Reihe_B/54/ZNB-1999-54b-0165.pdf | | | Identifier
| ZNB-1999-54b-0165 | | | Volume
| 54 | |
29 | Author
| Saalfrank, JochenN. Achtrab, Stephan Reck, Frank Hampel | Requires cookie* | | Title
| Synthese und Aggregatbildung eines 5-Hydroxy-2,5-dihydropyrrols. Enantiomerenreine, eindimensionale Stränge durch Wasserstoff- brückenbindungen und chiroselektive Selbstorganisation [1]  | | | Abstract
| Synthesis and A ggregation o f a 5-H ydroxy-2,5-dihydropyrrole. E nantiom erically Pure, O ne-dim ensional Strands via Hydrogen Bonds and Chiroselective S eif O rganization [ 1 ] R olf W. Reaction of dimethyl 1,3-acetonedicarboxylate 8 with oxalylchloride 2 and magnesium chlo ride as catalyst yielded 2,3-dioxo-2,3-dihydrofuran 9, which is in equilibrium with tautomer 10 (9:10 = 1:2). Addition of thionyl chloride to a mixture of 9/10 afforded 3-chloro-2(5H)-furanone 11. The structure of 11 was unequivocally established by X-ray diffraction, which indirectly pro ved the structure of 10 as well. Ring opening of 11 by nucleophilic attack with benzylamine 14 in C2-position and subsequent recyclization led to racemic 3-chloro-5-hydroxy-2-oxo-2,5-di-hydropyrrole 15. According to a single crystal X-ray analysis, 15 aggregates via stereospecific self selection through hydrogen bonds to give chiroselectively the one-dimensional strands 1 1(S)-15] and I [(R)-1SI | | |
Reference
| Z. Naturforsch. 54b, 179—186 (1999); eingegangen am 28. September 1998 | | |
Published
| 1999 | | |
Keywords
| 2(5H)-Furanones, Hydrogen-Bonding, Chiral Recognition, One-Dimensional Strand, Crystal Structure | | |
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| default:Reihe_B/54/ZNB-1999-54b-0179.pdf | | | Identifier
| ZNB-1999-54b-0179 | | | Volume
| 54 | |
30 | Author
| Kurt Polbom, Alfred Schmidpeterb, Gottfried Märklc, AngelaW. Illhalmb | Requires cookie* | | Title
| .2.4-Diazaphosphole und 1,2,4-DiazaarsoIe: Ringstruktur und Struktur wasserstoffbrücken-gebundener Paare und Helices 1.2.4-Diazaphospholes and 1,2,4-Diazaarsoles: Ring Structure and Structure of Hydrogen-Bonded Pairs and Helices  | | | Abstract
| Phosphaarenes, Arsaarenes, Hydrogen Bonds, Pyrazoles Among the large family of azaphospholes 1,2,4-diazaphospholes feature a particularly stable ring system. 3,5-Unsubstituted and 3,5-equally substituted 1,2,4-diazaphospholes and -diaza-arsoles are best made from 1,3-bis(dimethylamino)-2-phospha/arsaallyl chlorides and hydra zines. This way four examples for single crystal X-ray structure investigations were prepared: The unsubstituted 1,2,4-diazaphosphole 2 and -diazaarsole 4, the /V-substituted 1 -(2-pyridyl) 1.2.4-diazaphosphole 1, and the C-substituted 3,5-di-terf-butyl 1,2,4-diazaphosphole 3. They all possess planar rings with small angles at P (86°) and As (81°). The /V-unsubstituted mole cules are connected to each other by NH • N hydrogen bonds forming in case of the isotypic compounds 2 and 4 a helix along a crystallographic axis and in case of compound 3 for steric reasons a dimer. The structures of the aggregates found are compared to those of pyrazoles. | | |
Reference
| Z. Naturforsch. 54b, 187—192 (1999); eingegangen am 12. August 1998 | | |
Published
| 1999 | | |
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| default:Reihe_B/54/ZNB-1999-54b-0187.pdf | | | Identifier
| ZNB-1999-54b-0187 | | | Volume
| 54 | |
31 | Author
| Y. Inada3, Y. Tsutsuib, H. Wasadac, S. Funahashib | Requires cookie* | | Title
| Solvation Structure of Solvated Cu(I) Ions in Non-Aqueous Solvents as Studied by EXAFS and ab initio Molecular Orbital Methods  | | | Abstract
| Solvation Structure, EXAFS, ab initio Molecular Orbital Method, Copper(I) Ion The structure parameters around the Cu(I) ion in pyridine (PY), 4-methylpyridine (4MPY), 2-methylpyridine (2MPY), 2,6-dimethylpyridine (26DMPY), and acetonitrile (AN) were de termined by the extended X-ray absorption fine structure (EXAFS) method. The solvation structures of the Cu(I) ion in PY, 4MPY, and AN are 4-coordinate tetrahedral with Cu-N bond lengths of 205, 205, and 200 pm, respectively. In the case of 2MPY and 26DMPY, the Cu(I) ion has a 3-coordinate triangular structure with a Cu-N bond length of 201 pm. Such a decrease in the coordination number was interpreted in terms of the bulkiness of the solvent molecules. In order to clarify the most stable solvation structure of the Cu(I) ion, we carried out ab initio molecular orbital calculations for the solvation system of [Cu(NCH)"]+ (n = 1 -6) where the steric effect is negligible. The Gibbs free energy of solvation was the smallest in the case of n -4 and the 4-coordinate tetrahedral solvation of the Cu(I) ion was theoretically evaluated as most stable. The enthalpy of solvation monotonously decreases with increasing n, while the entropy of solvation proportionally increases. Although a larger gain of enthalpy is observed for the octahedral structure rather than the tetrahedral one, the entropic loss for the former overcomes the enthalpic gain. | | |
Reference
| Z. Naturforsch. 54b, 193—199 (1999); received September 23 1998 | | |
Published
| 1999 | | |
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| default:Reihe_B/54/ZNB-1999-54b-0193.pdf | | | Identifier
| ZNB-1999-54b-0193 | | | Volume
| 54 | |
32 | Author
| Karl Hensena>, Markus Kettner3, T., Peter Pickel3, Michael Bolteb | Requires cookie* | | Title
| Neue dikationische Silicium-Komplexe mit N-Methylimidazol New Dicationic Silicon Complexes with N-M ethylimidazole  | | | Abstract
| The reactions of the dibromosilanes Et2SiBr2, Ph2SiBr2, EtHSiBr2, PhHSiBr2 and MeHSiBr2 with N-methylimidazole (NMI) led to white powders stable at room temperature (with Et2SiBr2 an 1:2 adduct, with EtHSiBr2 and Ph2SiBr2 1:3 adducts, and with PhHSiBr2 and MeHSiBr2 1:4 adducts). The compounds crystallize from solutions in chloroforme and acetonitrile. The X-ray single crystal investigations show in all five cases dicationic complexes. | | |
Reference
| Z. Naturforsch. 54b, 200—208 (1999); eingegangen am 8. Oktober 1998 | | |
Published
| 1999 | | |
Keywords
| Dialkyldibromosilanes, Alkyldibromosilanes, N-Methylimidazol, Lewis-Acid-Base-Adducts, Crystal Structure | | |
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| default:Reihe_B/54/ZNB-1999-54b-0200.pdf | | | Identifier
| ZNB-1999-54b-0200 | | | Volume
| 54 | |
33 | Author
| Christoph Elschenbroich, Steffen Voß, Klaus Harms | Requires cookie* | | Title
| Metal Complexes of Heteroarenes, X [1]. 7 7 1 -Coordination of Phosphinine: Synthesis and Structure of cis-Dichloro-bis(2,6-dimethyl-4-phenyI-phosphinine)platinum  | | | Abstract
| C/5-Dichloro-bis(2 ,6 -dimethyl-4 -phenyl-77'-phosphinine)platinum (3) has been prepared by ligand substitution from cis -dichloro(2,5-cyclooctadiene)platinum and characterized by spec troscopy ('H , 13C, 31P NMR, IR, UV-Vis), CV and X-ray diffraction (space group P2|/c, a = 14.998, b = 16.540, c -11.506 Ä, a = 7 = 90°, ß = 92.46°, Z = 4). In line with findings for simi lar P hybridization states, the Pt-P bond length (221 pm) in 3 equals that in 771 -phosphaalkene Pt complexes and falls short of the respective parameters in Pt phosphane species. The stretching frequencies u^c\ and the bond length Pt-Cl indicate that phosphinines and phosphaalkenes, relative to phosphanes, adopt a lower position on the rram'-influence scale. This gradation is also suggested by the coupling constants 1 J (195Pt,31P). | | |
Reference
| Z. Naturforsch. 54b, 209—213 (1999); received September 9 1998 | | |
Published
| 1999 | | |
Keywords
| Phosphinine Complex, Platinum, X-Ray Data, NMR Data, frans-Influence | | |
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| default:Reihe_B/54/ZNB-1999-54b-0209.pdf | | | Identifier
| ZNB-1999-54b-0209 | | | Volume
| 54 | |
36 | Author
| U. Petasch, C. Hennig, H. Oppermann | Requires cookie* | | Title
| U  | | | Abstract
| n te r s u c h u n g e n z u m q u a s ib in ä r e n S y s te m B i2T e3 /B iC l3 Investigations on the Pseudobinary System Bi2Te3/BiCl3 The phase diagram of the pseudobinary sytem Bi2Te3/BiCl3 was investigated by DTA, total pressure measurements, and X-ray phase analysis. Only BiTeCl exists as a ternary phase in this system. The compound melts incongruently at 430 °C. The heat of formation and the standard entropy of BiTeCl were calculated from vapor pressure data: AH°b (BiTeCl, f, 298) = (-39,5 ± 1,6) kcal/mol; S° (BiTeCl, f, 298) = (34,4 ± 2,7) cal/K mol. The heat of formation of BiCl3 was determined on the basis of the heat of solution of BiCl3 and Bi20 3, and the heat of formation of Bi20 3: z\Hß (BiCl3, f, 298) = (-95,9 ± 0,9) kcal/mol. | | |
Reference
| Z. Naturforsch. 54b, 234—238 (1999); eingegangen am 9. Oktober 1998 | | |
Published
| 1999 | | |
Keywords
| Bismuth Telluride Chloride, Phase Diagram, Total Pressure Measurements, Calorimetry, Thermodynamic Data | | |
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| default:Reihe_B/54/ZNB-1999-54b-0234.pdf | | | Identifier
| ZNB-1999-54b-0234 | | | Volume
| 54 | |
38 | Author
| N. | Requires cookie* | | Title
| Untersuchungen zum ternären System Bi/Te/O, III. Bestimmung thermodynamischer Daten der ternären Verbindungen  | | | Abstract
| In v estig atio n s o n th e T ern ary S ystem B i/T e/O , III. D e te rm in a tio n o f T h e rm o d y n a m ic D a ta o f T e rn a ry C o m p o u n d s P. S chm idt, C. H en n ig , H . O p p e rm a n Bismuth-Tellurium-Oxides, H eat of Solution, Enthalpy of Formation The phase relations in the ternary system Bi/Te/O have been determ ined in previous stu dies by solid state reactions. Thermodynamical data have now been obtained for the pertinent equilibria. The heats of solution of Bi20 3, Bi12T e 0 2o, Bi,()Te20 19, Bi16Te50 34, Bi2T e 0 5, Bi2Te20 7, Bi2Te4O n and TeCl4 were determ ined in 4N HC1. From these the enthalpies of formation of bismuth tellurites at 298 K have been derived: zIH°b (B i12TeO20, f, 298) = -901,6 ± 8 kcal/mol, z1H°b (B i10Te2O i9, f, 298) = -856,1 ± 9 kcal/mol, zIH°b (Bi16T e ,0 34, f, 298) = -1519,5 ± 17 kcal/mol, z1H°b (BioTeO,, f, 298) = -222,8 ± 3 kcal/mol, z1H°b (Bi2Te2Ö 7, f, 298) = -299,4 ± 4 kcal/mol, ZIH°b (Bi2Te4O u , f, 298) = -448,2 ± 7 kcal/mol. | | |
Reference
| Z. Naturforsch. 54b, 252—260 (1999); eingegangen am 2. O ktober 1998 | | |
Published
| 1999 | | |
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| default:Reihe_B/54/ZNB-1999-54b-0252.pdf | | | Identifier
| ZNB-1999-54b-0252 | | | Volume
| 54 | |
39 | Author
| Z. Naturforsch | Requires cookie* | | Title
| Thermochemische Untersuchungen am System Bi/Se/O III. Zum quasibinären System Bi20 3 -B i2Se3 und zum ternären Bereich Bi20 3-Bi20 2Se -Se -S e 0 2  | | | Abstract
| T h erm o c h em ical In v e stig a tio n s on th e S ystem B i/S e/O III. T he Q u asy B in ary S ystem B i20 3-B i 2S e3 a n d th e T ern ary R a n g e B i20 3-B i 20 2S e -S e -S e 0 2 H . O p p e rm a n n 3 *, H . G ö b e la, P. S c h m id t3, H . S c h a d o w +a, V. V assilevb, I. M a rk o v a -D e n e v a b Ternary System Bi/Se/O, Bi20 2Se, Total Pressure M easurements, Enthalpy of Formation, Standard Entropy Only the ternary phase Bi20 2Se is shown to exists in the thermodynamical equilibrium in the investigated ternary system on the binary line Bi20 3-B i2Se3. Its thermal decomposition was measured in a quartz membrane zero manometer. The enthalpy of formation and the standard entropy were derived from the tem perature function of the decomposition equi librium: A H°(Bi20 2Ses.298) = -104,6 ±4,0 kcal/mol S°(Bi20 2Ses298) = 43 ± 3 cal/K mol. The coexistence ranges in the ternary region Bi20 3-S e 0 2-B i20 2S e-S e were followed by X-ray diffraction, IR spectroscopy and total pressure measurements of binary and ternary compositions. | | |
Reference
| Z. Naturforsch. 54b, 261—269 (1999); eingegangen am 9. November 1998 | | |
Published
| 1999 | | |
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| default:Reihe_B/54/ZNB-1999-54b-0261.pdf | | | Identifier
| ZNB-1999-54b-0261 | | | Volume
| 54 | |
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