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1997[X]
41Author    Stefan Fuchs, JoséM. López-De-Luzuriaga, M.Elena Olmos, Alexander Sladek, Hubert SchmidbaurRequires cookie*
 Title    Gold Coordination by a Tertiary Phosphine with Three Thioether Functions  
 Abstract    Gold(I) Coordination, Tris(phenylthiomethyl)phosphine, Ambidentate P/S3-Ligand The reaction of tris(phenylthiomethyl)phosphine with equimolecular amounts of [AuPPh3]+[BF4]~ affords the complex (tris(phenylthiomethyl)phosphine)(triphenylphosph-ine)-gold(I) tetrafluoroborate 1 in good yield. The X-ray diffraction analysis of this prod­ uct shows an unusual conformation with the three ChLSPh arms of the phosphine folded back towards the metal atom shielding the P-Au-P' unit. The reaction of the same substrate with Bis(tetrahydrothiophene)gold(I) perchlorate in a 1:1 molar ratio leads to the displacement of both weakly coordinated tht ligands, and a dimeric product [AuP(CH2SPh)3]2(C104)2 2 is obtained. 
  Reference    Z. Naturforsch. 52b, 217—220 (1997); received December 16 1996 
  Published    1997 
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 Identifier    ZNB-1997-52b-0217 
 Volume    52 
42Author    Wolfgang Einholz, Ronald Schäfer, Willi Keller, Bernhard VoglerRequires cookie*
 Title    Zwölfgliedrige Heteroborancluster durch Copyrolyse von Tetrachlordiboran(4) mit Elementhalogeniden Twelve-Vertex Heteroborane Clusters by Copyrolysis of Tetrachlorodiborane(4) and Element Halides  
 Abstract    The perchlorinated arsaboranes c/o5o-l,2-As2B 10Cl10 and As4B8C16 are formed in the co­ pyrolysis of B2C14 and AsC13 at temperatures of 330-450°C. The icosahedral structure of closo-1,2-As2B |0C110 is confirmed by 1 B-"B-COSY-NMR spectroscopy. As4B8C16 is suppo­ sed to be a conjuncto-borane (As2B4Cl3)2 with two boron-boron linked As2B4C13 octahedra. The copyrolysis of B2C14 andSbCl3 or SbCl5 yields Sb2B l0C l10, and the corresponding reaction of B2C14 with S2C12 gives the icosahedral thiaborane cluster SBn C ln . 
  Reference    Z. Naturforsch. 52b, 221—226 (1997); eingegangen am 24. Oktober 1996 
  Published    1997 
  Keywords    Perchlorinated Arsaboranes, Stibaboranes, Thiaboranes 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0221.pdf 
 Identifier    ZNB-1997-52b-0221 
 Volume    52 
43Author    Borate Anion, A. Wiesch, K. BluhmRequires cookie*
 Title    AgSrfByO^]: Das erste wasserfreie quaternäre Silber(I)-Borat mit vierfach koordiniertem Silberion und einem neuartigen Boratanion AgSr[B70 12]: The First Anhydrous Quaternary Silver(I)-Borate with Fourfold Coordinated Silver Ion and a New  
 Abstract    Single crystals of AgSr[B70 , 2] were obtained by using a B20 3 flux-technique and Ag2C 0 3 and SrC 03 as starting materials in a silver ampoule at 800 °C. X-ray investigations on single crystals led to the space group C 2/c with a = 664.2(5); b = 1153.6(3); c = 2198.0(6) pm; ß = 92,52(3)°; Z = 8. Ag+ is fourfold coordinated by oxygen atoms and forms distorted A g04 tetrahedra while Sr2+ has nine nearest neighbours. The compound contains a hitherto unknown two dimensional borate anion [B70 i 2]3-which contains four trigonal planar B 0 3 groups and three B 0 4 tetrahedra per unit. 
  Reference    Z. Naturforsch. 52b, 227—230 (1997); eingegangen am 9. September 1996 
  Published    1997 
  Keywords    Silver, Strontium, Borate, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0227.pdf 
 Identifier    ZNB-1997-52b-0227 
 Volume    52 
44Author    R. Pöttgen, K. H. Wachtmann, W. Jeitschko, A. Lang, T. EbelRequires cookie*
 Title    Er5Re2C7, Tm5Re2C7, and Lu5Re2C7 with Sc5Re2C7 Type, and Yb2ReC2 with Pr2ReC2 Type Structures  
 Abstract    ErsReiCy, TmsRe2C7, and LusReaC? were prepared by arc-melting of the elemental compo­ nents and subsequent annealing at 800 °C. ErsRe^Cy forms only after the annealing process, whereas the other two carbides were already present in the as cast samples. They crystallize with a ScsReiC? type structure, which was refined from single-crystal X-ray data of LusRe2C7: Cmmm, a = 791.44(5), b = 1418.08(8), c = 332.79(2) pm, Z = 2, R = 0.037 for 544 structure factors and 21 variable parameters. The structure contains linear centrosymmetric C3 units with a C-C bond length of 133(2) pm and isolated carbon atoms in octahedral coordination of four lutetium and two rhenium atoms. The rhenium atoms within the two-dimensionally infinite polymeric sheets [ReiC-tln are electronically saturated as is indicated by the diamagnetism and the semiconductivity of this carbide. Yf>2ReC2 was prepared by reacting the elements in a sealed tantalum tube with a high-frequency furnace. It crystallizes with a Pr2ReC2 type structure: Pnma, a = 645.91(6), b = 498.64(6), and c = 966.05(6) pm. Magnetic susceptibility measurements indicate the ytterbium atoms to be trivalent in this compound. 
  Reference    Z. Naturforsch. 52b, 231—236 (1997); received November 15 1996 
  Published    1997 
  Keywords    Crystal Structure, Magnetic Properties, Rare Earth Metal Rhenium Carbides, Polymeric Rhenium-Carbon Polyanions 
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 Identifier    ZNB-1997-52b-0231 
 Volume    52 
45Author    Z. NaturforschRequires cookie*
 Title    Zinn(IV)  
 Abstract    Komplexe mit diaciden Azo(hydrazono)verbindungen. Kristallstruktur von Bis[4-(2'-hydroxyphenylazo)-3-methyl-l-phenyl-pyrazol-5-onato(2-)]zinn(IV) Tin(IV) Complexes with Diacidic Azo(hydrazono) Compounds. Crystal Structure of Bis[4-(2'-hydroxyphenylazo)-3-methyl-l-phenyl-pyrazol-5-onato(2-)]tin(IV) Wolfgang Banße3, Tin(IV) complexes of diacidic azo and hydrazono compounds were synthesized by the reaction of these ligands with SnCl2acac2 and SnCl2 • 2H20 , respectively. The complexes were further characterized by Mössbauer spectroscopy. For bis[4-(2'-hydroxyphenylazo)-3-methyl-l-phenyl-pyrazol-5-onato(2-)]tin(IV) force field calculations have been performed and the crystal structure was determined by X-ray analysis. 
  Reference    Z. Naturforsch. 52b, 237—242 (1997); eingegangen am 16. Oktober 1996 
  Published    1997 
  Keywords    Tin(I V) Complexes, Diacidic Azo Compounds, Mössbauer Spectroscopy, Molecular Mechanics Study, Crystal Structure 
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 Identifier    ZNB-1997-52b-0237 
 Volume    52 
46Author    Matthias Krieger3, Klaus Harms3, Jörg Magullb, Kurt Dehnicke3Requires cookie*
 Title    Phosphanimin-und Phosphaniminato-Komplexe des  
 Abstract    Zinks. Kristallstrukturen von [ZnCl2(Me3SiNP(CH2)4CMe3)]2, [ZnI2(Me3SiNPEt3)]2, [ZnI2{Me2Si(NPEt3)2 }] und [ZnBr(NPMe3)]4 CH2Cl2 Phosphaneimine and Phosphoraneiminato Complexes of Zinc. Crystal Structures of [ZnCl2(M e3SiNP(CH2)4CM e3)]2, [ZnI2(Me3SiNPEt3)]?, [Znl2{Me2Si(NPEt3)2}], and [ZnBr(NPMe3)]4 CH2Cl2 The donor-acceptor complexes [ZnCl2(Me3SiNP(CH2)4CMe3)]2 (l)and [ZnI2(Me3SiNPEt3)]2 (2) have been prepared from the zinc dihalides and the corresponding silylated phosphaneimi-nes in CH2C12. Thermolysis of 2 leads to the formation of [ZnI2(Me2Si(NPEt3)2)] (3). Znl2 and ZnBr2 react with the silylated phosphaneimines Me3SiNPR3 (R = Me, Et) in the presence 
  Reference    Z. Naturforsch. 52b, 243—250 (1997); eingegangen am 1. August 1996 
  Published    1997 
  Keywords    Zinc Compounds, Phosphoraneiminato Complexes, Synthesis, Crystal Structure 
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 Identifier    ZNB-1997-52b-0243 
 Volume    52 
47Author    W. SchnickRequires cookie*
 Title    Synthesen, Kristallstrukturen und Eigenschaften von Trisilber-und Trikalium-tri-/x-imido-cyclotriphosphat, Ag3(P 0 2NH)3 und K3(P 0 2NH)3 Syntheses, Crystal Structures, and Properties of Trisilver and Tripotassium Tri-^-im ido Cyclotriphosphate, Ag3(P 0 2N H)3 and K3(P 0 2N H)3 N. Stock  
 Abstract    Coarse crystalline Ag3(P 0 2NH)3 (1) and K3(P 0 2NH)3 (2) are obtained by addition of an aqueous solution of A gN 03 to an acidified solution of Na3(P 0 2NH)3 • 4H20 and by diffusion controlled addition of ethanol to a solution of K3(P 0 2NH)3 in water, respectively. The crystal structures of 1 and 2 have been determined by single crystal X-ray methods (Ag3(P 0 2NH)3: P2,/c; a = 1166.6(1), b = 786.4(1), c = 997.8(1) pm, ß = 106.91(1)°; Z = 4. K3(P 0 2NH)3: R3; a = 1271.4(2), c = 1017.9(2) pm, Z = 6). In Ag3(P 0 2NH)3 the cyclic anion is markedly distorted because of interactions between Ag+ and one nitrogen atom of the anion. In K3(P 0 2NH)3 the trimetaphosphimate ring shows a chair conformation and two cyclic anions are connected to each other by hydrogen bonds. DTA/TG investigations show thermal decomposition above 275 and 250 °C for 1 and 2, respectively. 
  Reference    Z. Naturforsch. 52b, 251—255 (1997); eingegangen am 14. November 1996 
  Published    1997 
  Keywords    Trimetaphosphimate, Synthesis, Crystal Structure, Thermal Property 
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 Identifier    ZNB-1997-52b-0251 
 Volume    52 
48Author    EvgeniV. Avtomonov3 ', Rainer Griiningb, Jörg LorberthaRequires cookie*
 Title    Crystal and Molecular Structure of 3-Iodo-2-propynyl-N-butylcarbamate  
 Abstract    The crystal structure of the title compound has been determined by X-ray diffraction methods. Due to the Lewis acidic character of the iodine substituent a "zig-zag" chain is formed via intermolecular interactions (2.933(4) A) between iodine and oxygen atoms of theocarbamate moiety. A three-dimensional network is formed through hydrogen-bridging (2.04 A) between NH-groups and the oxygen atoms of the neighbouring carbamate group of the next molecule. 
  Reference    Z. Naturforsch. 52b, 256—258 (1997); received October 15 1996 
  Published    1997 
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 Identifier    ZNB-1997-52b-0256 
 Volume    52 
49Author    Z. NaturforschRequires cookie*
 Title    Electroreduction of Organic Compounds  
 Abstract    , 30 [1] Cathodic Formation of 4,4,8-Trichlorodispiro[2.1.2.1] octane from 4,4,8,8-Tetrachlorodispiro[2.1.2.1] octane D irk N ü n n eck e3, Jü rg en Voss3 *, G unadi A diw idjajab, 1996 Electrochemical Reduction. Dechlorination, X-Ray, Dispiro[2.1.2.1.]octanes Bicyclo[1.1.0]butane The formation of the highly strained r ,3 '-Dichlorodispiro[cyclopropane-l,2'-bicyclo[1.1.0]-butane-4', l "-cyclopropane] (2) by electrochemical reduction of the title compound 1, pub­ lished by Strelow, Voss and Baum [2], turned out to be erroneous and has to be corrected. Instead of the formation of 2 a substitution of one chloro substituent by hydrogen takes place and the trichlorodispiro[2.1.2.1]octane 3 results. The structure of 3 is confirmed by an X-ray structural analysis. 
  Reference    Z. Naturforsch. 52b, 259—262 (1997); received August 22 
  Published    1997 
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 Identifier    ZNB-1997-52b-0259 
 Volume    52 
50Author    K. Laus, A. Lb, E. Rt3, N. Ter, H. Äfelinger, -A, P. Iotr, M. Ilartb, TadeuszM. Arek, K. Rygow Skic, TillK., M. Atthias, P. Ursch, Sabine Strohschein3, Prof Dr, ErnstRequires cookie*
 Title    Conformational Aspects of the p-Nitrosophenolate Anion and Related Compounds: NMR Study and ab initio 6-31G Optimizations of Molecular Structures  
 Abstract    , 1996 p-Nitrosophenolate Anion, NMR Spectra, Conformational Aspects The p-nitrosophenolate anion, PNPA (3), represents an excellent example of variable rc-electron transfer demanded by a network of different hydrogen bonds. The limiting structures of mono-protonation in the solid state and in solution are either the p-nitrosophenol (1) or the p-quinonoxime (2) molecules. For the systems 1 to 3 and the related compounds 4 to 7 are results of ab initio 6-31G HF MO optimizations of molecular structures presented which are calculated additionally in variously rotated conformations. Solid state 13C-CP/MAS NMR spectra of two PNPA salts 8 and 9 have been recorded at 7.0 Tesla. The protonation of 8 and 9 was studied in solution using a 400 MHz NMR spectrometer recording the variations in 'H and 13C NMR chemical shifts on changing the solvent from DMSO-d6 to D20 in steps of 25%. The 2D *H-13C correlated spectrum leads to unambigous assignment of NMR signals. From the coalescence temperature of 'H signals of 9 the experimental barrier of rotation in D20 was determined as 16.9 ± 0.1 kcal mol-1. The calculated gas phase rotational barrier for free PNPA is with 26.9 kcal mol"1 much higher, but is lowered by calculations for the Li-salt 6 c to 14.5 kcal mol-1 and to 11.8 kcal mol-1 for the protonated PNP If. The in-plane inversion of PNPA through 3c is calculated to be extremely high with 52.4 kcal mol-1. The effects of rotation of substituents to orthogonal conformations on calculated energies and on intramolecular distances were studied thoroughly. 
  Reference    Z. Naturforsch. 52b, 263—280 (1997); received October 11 
  Published    1997 
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 Identifier    ZNB-1997-52b-0263 
 Volume    52 
51Author    Prof Dr, ErnstRequires cookie*
 Title    Zur Festphasenpeptidsynthese des Makrophagen-migrationsinhibierenden Faktors der Maus (mMIF): Ein Vergleich verschiedener Syntheseansätze zur Darstellung der schwierigen C-terminalen Sequenz mMIF(93-115)  
 Abstract    Solid Phase Peptide Synthetic A ppro ach es to M ouse M acrophage M igration Inhibitory Factor (m M IF): C om parison of D ifferent Strategies Producing the C-Terminal D ifficult Sequence P eptide m M IF (9 3 -1 1 5) Thom as Kaiser, W olfgang V oelter* From solid phase peptide synthetic approaches of mMIF(93-115) the C-terminal sequence turned out to be a typical "difficult sequence" peptide. Various stepwise syntheses were performed with different resins and coupling reagents. The Peptide was synthesized in 90% yield by solid phase fragment condensation of protected mMIF(93-108) to mMIF(109-115) '2-Chlorotrityl' resin bound. 
  Reference    Z. Naturforsch. 52b, 281—295 (1997); eingegangen am 4. Dezember 1996 MIF 
  Published    1997 
  Keywords    Solid Phase Peptide Synthesis, Difficult Sequence, Fragment Condensation, Coupling Conditions 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0281.pdf 
 Identifier    ZNB-1997-52b-0281 
 Volume    52 
52Author    A. Rn, VasiliIvanovitch Sokolov3, H. Ans, V. Idar Volden, H. Ans, JoachimB. Reunigb, M. Ichael, D., K. Erb, R. Oland, R. ÖslerbRequires cookie*
 Title    The Molecular Structures and Conformational Preferences of Bis(dimethylstibyl)- Oxane, -Sulfane and -Selane, E(SbMe2)2? E = O, S or Se, Me = CH3, by Density Functional Theory Calculations and Gas Electron Diffraction  
 Abstract    Density Functional Theory calculations on E (SbM e2)2, E = O, S or Se, Me = CH3, indicate that the equilibrium structures are syn-syn or near syn-syn conformers with over-all C2 sym­ metry. The barriers restricting rotation about E-Sb bonds are very low, the equilibrium values for the dihedral angles 0(Sb-E-Sb-lp) where lp denotes the direction of the electron lone pair on one of the Sb atoms are probably less than 45°. The calculations further indicate the existence of syn-anti conformers som e 4 kJ m ol-1 above the more stable syn-syn. Gas elec­ tron diffraction data show that both conformers are present in gaseous Ö (SbM e2)2, while the presence of the syn-anti conformer in gaseous Se(SbM e2)2 is uncertain; least-squares refinements yielded the mole fraction % = 0.27(18). The Sb-O and Sb-Se bond distances are 197.6(14) and 255.1(5) pm respectively, the valence angles of the syn-syn conformers are <SbOSb = 122.3(16)° and <SbSeSb = 96.3(11)°. It is suggested that the wide <SbOSb angle is due to across-angle repulsion betw een the Sb atoms. 
  Reference    Z. Naturforsch. 52b, 296 (1997); received Septem ber 30 1996 
  Published    1997 
  Keywords    Distibyloxane, Distibylsulfane, Distibylselane, D ensity Functional Theory Calculations, Gas Electron Diffraction 
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 Identifier    ZNB-1997-52b-0296 
 Volume    52 
53Author    A.Lexander Sladek, H. Ubert SchmidbaurRequires cookie*
 Title    Bridging of Trigoldsulfonium Clusters by a Silver(I) Ion  
 Abstract    Treatm ent of tris[(triphenylphosphine)gold(I)]-sulfonium tetrafluoroborate with AgBF4 (molar ratio 2:1) in tetrahydrofuran affords a hepta-nuclear mixed-metal cluster trication {[(Ph3P)6Au6AgS2](thf)}3+ as the tetrafluorobor­ ate salt. The crystal structure of the compound has been determ ined by X-ray diffraction. The sil­ ver atom is found in a bridging position between the two Au3S units with short contacts to both sulfur atoms and to three out of six gold atoms. The coordination sphere of the silver atom is com plem ented by a tetrahydrofuran molecule. In di(tri)chlorom ethane solutions there is rapid site exchange of the silver coordination as shown by virtual equivalence of the phosphine ligands on the NM R time scale at ambient temperature. 
  Reference    Z. Naturforsch. 52b, 301—303 (1997); received January 3 1997 
  Published    1997 
  Keywords    Gold Clusters, Silver Bridging, Sulfonium Cations, Mixed Gold/Silver Cluster 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0301_n.pdf 
 Identifier    ZNB-1997-52b-0301_n 
 Volume    52 
54Author    H. Oppermann, S. Ehrlich, C. HennigRequires cookie*
 Title    Calorimetrie an Yttriumtrihalogeniden und Yttriumoxidhalogemden Calorimetry of Yttrium Trihalides and Yttrium Oxyhalides  
 Abstract    The heats of solution of Yttrium, YOC1, YOBr, YOI, YC13, YBr3, YI3 and Y20 3 were determined in 4n HX. From those the enthalpies of formation of Yttrium Trihalides YX3 and Yttrium Oxyhalides YOX at 298 K were derived: Z\Hb(YC13j 298) = -2 4 0 .4 ± 0.6 kcal/mol, Z\H^(YBr3,f,298) = -2 0 2 .1 ± 1.5 kcal/mol, _\H £(YI3,f '298) = -147.0 ± 1.7 kcal/mol, ^ H ^ (Y O c if,298) = -2 4 0 .2 ± 1.0 kcal/mol. _AHß(YOBrf 298) = -229.7 ± 2.0 kcal/mol, AH 
  Reference    Z. Naturforsch. 52b, 305—310 (1997); eingegangen am 28. November 1996 
  Published    1997 
  Keywords    Synthesis, Yttrium Oxyhalides, Yttrium Halides, Heat of Solution, Enthalpy of Formation 
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 Identifier    ZNB-1997-52b-0305 
 Volume    52 
55Author    S. Ehrlich, H. Oppermann, C. HennigRequires cookie*
 Title    Calorimetrie an Ammoniumyttriumhalogeniden Calorimetry of Ammonium Yttrium Halides  
 Abstract    The heat o f solution of all solid phases in the system YX3-NH4X with X = Cl, Br, I in 4 n HX was investigated. The enthalpies of formation of the ammonium yttrium halides are derived from the enthalpies of formation of Y X 3 and of NH4X and their heats of solution in An HX: Z\H^(NH4 Y 2Cl7,f,298) = — 561,5 ± 1,7 kcal/mol, Z\H^((NH4)3 YCl6,f,298) = -474,5 ± 1,3 kcal/mol, ziH ß((N H 4)3YBr6 f 298) = -400,8 ± 2,6 kcal/mol, _AH£((NH4)3 YI6,t-298) = -291,9 ± 3,0 kcal/mol. 
  Reference    Z. Naturforsch. 52b, 311—314 (1997); eingegangen am 24. Januar 1997 
  Published    1997 
  Keywords    Synthesis, Ammonium Yttrium Halides, Ammonium Halides, Heat of Solution, Enthalpy of Formation 
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 Identifier    ZNB-1997-52b-0311 
 Volume    52 
56Author    W. Preetz, A. KrullRequires cookie*
 Title    Kristallstrukturen, Schwingungsspektren und Normalkoordinatenanalysen von Tetrahalogenooxalatoosmaten (IV), [OsX4(ox)]2', X = Cl, Br, I Crystal Structures, Vibrational Spectra and Normal Coordinate Analyses of Tetrahalogenooxalatoosmates (IV), [OsX4(ox)]2~, X = Cl, Br, I  
 Abstract    The crystal structures of [(C5H5N)iC H 2][OsCl4(ox)] (monoclinic, space group I2/m, a = 10.260(5), b = 13.841(5), c = " 12.273(5) Ä, ß = 92.050(5)°, Z = 4), [(C5H5N)2CH2j[O sBr4(o x)]H 20(m onoclinic, space g ro u p P 2 ,/n ,a = 11.666(3),b = 11.591(5), c = 14.926(2) A, ß = 102.45(2)°, Z = 4) and [P(C6H5)4M O sI4(ox)]-2CH2C12 (triclinic, space group P i, a = 14.597(2), b = 11.9185(9), c = 22.5624(14) A, a = 80.284(8), ß = 78.903(8), 7 = 69.432(8)°, Z = 2) have been determined by single crystal X-ray diffraction analysis. The IR and Raman spectra of the three complexes were measured at room temperature. Using the molecular parameters of the X-ray determinations normal coordinate analyses based on a modified valence force field have been performed and the normal modes o f vibration are assigned. With a set of 25 force constants and taking into account the innerligand vibrations a good agreement between observed and calculated frequencies has been achieved. The valence force constants of the X-Os-X axis are fd(OsCl) = 1.77, fd(OsBr) = 1.48, fd(OsI)o= 1.0 mdyn/A, of the X'-Os-O* axes are fd(O sCl') = 1.88, fd(OsBr') = 1.6, fd(OsI') =1.1 mdyn/A and fd(OsO*) ranges from 2.7 to 2.8 mdyn/A. 
  Reference    Z. Naturforsch. 52b, 315—322 (1997); eingegangen am 27. November 1996 
  Published    1997 
  Keywords    Tetrachlorooxalatoosmate(IV), Tetrabromooxalatoosmate(IV), Tetraiodooxalatoosmate(IV), Crystal Structure, Vibrational Spectra 
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 Identifier    ZNB-1997-52b-0315 
 Volume    52 
57Author    KonstantinV. Domasevitch3, VeraV. Ponomarevaa, AndreyA. Mokhir3, EduardB. Rusanov3, Joachim Sielerb, Eberhard HoyerbRequires cookie*
 Title    The Phenomenon of Intramolecular Attractive S— O Interactions: Synthesis and Structure of (l,10-Phenanthroline)copper(II) Complexes with Isonitroso-(4-methylthiazol-2-yl)acetamide and Isonitroso-(4-methylthiazol-2-yl)-(benzothiazoI-2-yl)methanide  
 Abstract    Isonitroso-(4-methylthiazol-2-yl)acetamide H (L '), isonitroso-(4-methylthiazol-2-yl)(benzo-thiazol-2-yl)methanide H(L2) and their copper(II) complexes of composition [C u(Phen){L'}(C 104)] (1) and [Cu(Phen){L2}Cl]*C2H5 0 H (2) have been prepared. Crys­ tal and molecular structures of the complexes have been determined from X-ray diffractioon data (1: monoclinic, space group P2]/c, with a = 11.611(2), b = 10.259(2), c = 17.869(4) Ä, ß = 104.67(3)°, V = 2059.1(7) Ä3, Z = 4; R\ = 0.046 for the 2522 unique reflections with I > 2a(I). 2: triclinic, space group PI, with a = 8.351(1), b = 10.876(1), c = 14.891(2) Ä, a = 96.170(8)°, ß = 94.201(9)°, 7 = 106.721(9)°, V = 1280.1(2) A3, Z = 2; R\ = 0.034 for the 4038 unique reflections with I > 2a(I)). In the structure of 1 the coordination polyhedron of Cu2+ is a distorted square pyramid with an oxygen atom of the CIO4 counter anion in the apex (C u -0 2.505(3) A); in complex 2 the copper atom adopts fivefold coordination of a slightly distorted trigonal-bipyramidal geometry with a chlorine atom in the equatorial plane (Cu-Cl 2.3504(9) A). Ethanol of crystallization gives rise to a hydrogen bond at the chlorine atom. In both structures the oximic anions are coordinated to the metal center in a bidentate chelate manner via the nitrogen atom of the nitroso group and the carbonyl oxygen atom (1) or via the benzothiazole nitrogen atom (2) (Cu-O, Cu-N in the range 1.963(2) -2.031 (2) Ä). The thiazole group of the ligands takes no part in the coordination. The nitroso oxygen atoms possess short intramolecular contacts with thiazole sulphur atoms, with d(S— O) at 2.605(3) (1) and 2.676(3) A (2), which may be attributed to a strong intraligand interaction. 
  Reference    Z. Naturforsch. 52b, 323—330 (1997); received September 16 1996 
  Published    1997 
  Keywords    Copper(II), Oximes, Thiazoles, Benzothiazoles, X-Ray 
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 Identifier    ZNB-1997-52b-0323 
 Volume    52 
58Author    SvitlanaR. Petrusenkoa, Joachim Sielerb, VladimirN. Kokozay3 'Requires cookie*
 Title    Direct Synthesis of Zinc and Nickel(II) Complexes with l,4-Diazabicyclo[2.2.2]octane  
 Abstract    The peculiarities of the formation of zinc and nickel(II) complexes by interaction of metal powder or metal oxide with ammonium salts (halides, nitrate, thiocyanate) were investigated in non-aqueous solutions (methanol, acetonitrile, N,N-dimethylformamide=DMF, dimethylsulf-oxide=DMSO) in presence of l,4-diazabicyclo[2.2.2]octane. The stoichiometry of the com ­ plexes was found to depend on the initial reagent ratio Ni/ZnOiNfLX and Ni/ZnO:Ten. The compounds of compositions Z n(H Ten)(H 20)(N 03)3 and Ni(HTen)(Ten)Cb were character­ ized by X-ray crystallography. Both complexes contain five-coordinate metal atoms. The zinc compound possesses monomeric molecular structure whilst the nickel complex is polymeric. 
  Reference    Z. Naturforsch. 52b, 331—336 (1997); received July 30 1996 
  Published    1997 
  Keywords    Synthesis, Zinc, Nickel(II), Triethylenediamine, X-Ray 
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 Identifier    ZNB-1997-52b-0331 
 Volume    52 
59Author    LarisaA. Kovbasyuk3, Olga Yu, Vassilyeva3, VladimirN. Kokozay3, Wolfgang LinertbRequires cookie*
 Title    Crystal Structure of the Di-bromo-bis(2-dimethylaminoethanolato)(dime- thylsulfoxide)-copper(II)-lead(II) Dimer Obtained by Direct Synthesis  
 Abstract    A heterotetranuclear C unPbu complex containing 2-dimethylaminoethanol has been synthesized, using copper powder and PbB n as starting materials, and character­ ized by X-ray crystallography. The crystal is composed of centrosymmetric molecules [C uP b B ^ K C H ^N C F b C F L O j^ d m so h . The central strictly planar fragment is a Pb2Ü2 paral­ lelogram completed by bridging oxygen atoms of chelating 2-dimethylaminoethoxo groups. The Pb atom forms four quite short bonds with oxygen atoms of the three 2-dimethylaminoethoxo groups and of the dmso molecule and assumes a six-coordinate structure also involving two bromine atoms. The two oxygen and two nitrogen atoms of two 2-dimethylaminoethoxo groups form the copper coordination environment, which possesses a somewhat distorted square planar geometry. 
  Reference    Z. Naturforsch. 52b, 337—339 (1997); received July 30 1996 
  Published    1997 
  Keywords    Heteronuclear Complexes, Crystal Structure, Direct Synthesis 
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 Identifier    ZNB-1997-52b-0337 
 Volume    52 
60Author    Olaf Reckeweg, H.-Jürgen MeyerRequires cookie*
 Title    Unsymmetrische BN23'-Ionen in den Strukturen von Ca2ClBN2 und Sr2ClBN2. Unsymmetric BN23~-Ions in the Structures of Ca2ClBN2 and Sr2ClBN2  
 Abstract    The new compounds Ca2ClBN2 (1) and Sr2ClBN2 (2) were prepared from the respective metal, its dihalide and h-BN in sealed tantalum ampoules at 1200 °C. The crystals obtained were transparent yellow (1) and blue (2), respectively. The crystal structures were determined from single crystal X-ray data. Ca2ClBN2 and Sr2ClBN2 are isotypic and crystallize in the orthorhombic space group Pnma (No. 62), Z = 4 (Ca2ClBN 2: a = 1166.7(2), b = 390.26(4), c = 899.8(1) pm, R 1 = 0.043, wR2 = 0.115 for 554 independent reflections; Sr-,C1BNT: a = 1242.8(1), b = 416.75(4), c = 920.8(1) pm, R\ = 0.031, wR2 = 0.054 for 6 6 2 'independent reflections). The structures contain two different layers of M 2+, C P and BN23~ alternating along the [010] direction. The bond angles N-B-N are 177.2(4)° for (1) and 176,6(5)° for (2), the bond distances of the BN23_ ions are dB_ N] = 134.6(5) pm for (1), 136,3(7) pm for (2) and dg_N2 = 132.4(5) pm for (1) and 131,3(7) pm for (2). The unsymmetric structure of the BN23~ ion, as is manifested particularly in the Sr compound (2), is caused by the coordination of N 1 to four cations while N2 is coordinated only to three. 
  Reference    Z. Naturforsch. 52b, 340—344 (1997); eingegangen am 12. November 1996 
  Published    1997 
  Keywords    Boronitrides, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0340.pdf 
 Identifier    ZNB-1997-52b-0340 
 Volume    52 
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