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1997[X]
1Author    M. Onoheteroarylborates [, Norbert Kuhn3, Heike Kotowski3, Dieter Bläserb, Roland BoesebRequires cookie*
 Title    Monoheteroarylborate [1]  
 Abstract    The heteroaryl borates Li[C4Me4NBH3] (6) and Na[C3H 3N2(BMe3)2]* 2 C4HgO (8) are ob­ tained by treatment of Li[C4Me4N] and Na[C3H3N2] with Me2S • BH3 and BMe3, respectively. The X-ray structure of [Na(C4H 80) 6][C3H 3N 2(BM e3)2] (10) is reported. 
  Reference    Z. Naturforsch. 52b, 351—354 (1997); eingegangen am 28. Oktober 1996 
  Published    1997 
  Keywords    Borates, Pyrroles, Imidazoles, X-Ray 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0351.pdf 
 Identifier    ZNB-1997-52b-0351 
 Volume    52 
2Author    N. Orbert Kuhn, Riad Faw, M. Anfred, Steim Ann, JörgW. Iethoff, HerrnRequires cookie*
 Title    Zur Reaktion von Derivaten des l,3-Dimethyl-2-iminoimidazolins mit CS2 [1]  
 Abstract    1,3-Dimethyl-2-iminoimidazoline (4, ImNH) reacts with CS2 to give the imidazolium salt [ImNH2][(ImNCS2)2H] (7) in which two dithioformimide fragments are linked by a hydrogen bridge. From the trimethylsilyl derivative ImNSiMe3 (11) and CS2 the adduct ImNSiMe3 • CS2 (12) is obtained which reacts with oxygen to give the disulfide (ImNCS2) (14). The X-ray structures of 7 and 14 were determined. 
  Reference    Z. Naturforsch. 52b, 609—614 (1997); eingegangen am 19. Februar 1997 
  Published    1997 
  Keywords    Imidazoles, Carbon Disulfide, X-Ray 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0609.pdf 
 Identifier    ZNB-1997-52b-0609 
 Volume    52 
3Author    G. Alina, S. Z. Aitseva11 ', SergeyS K Arlova, ElenaS A Lekseyevaa, LeonidA A Slanova, EvgeniV A Vtom Onovb, JörgL. OrberthbRequires cookie*
 Title    -Allylgermatrane. Synthesis, Structure and Reaction with Diazomethane  
 Abstract    Reaction of allyltribromogermane (2), readily available from dibrom o(l,4-dioxane)ger-manium(II) (1) and allylbromide, with tris(2-tributylstannoxyethyl)-amine (4) gives 1-allylgermatrane (3) in almost quantitative yield. 3 crystallizes from /7-pentane as a colourless crystalline solid which was characterized by 'H and ,3C NMR spectroscopy and by an X-ray crystal structure study. The "atrane" skeleton shows a strong conformational disorder; the Ge-N distance of 2.208(3) A suggests the presence of a coordinative Ge-N bond. Treatment of 1 -allylgermatrane (3) with CH2N2 in the presence of catalytic amounts of Pd(OAc)2 affords 1-cyclopropylmethylgermatrane (5) in high yield. 
  Reference    (Z. Naturforsch. 52b, 30—34 [1997]; received August 16 1996) 
  Published    1997 
  Keywords    Germanium, Germatrane, Cyclopropanation, X-Ray, NMR Spectra 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0030.pdf 
 Identifier    ZNB-1997-52b-0030 
 Volume    52 
4Author    Atthias Lemke, Falk Knoch, Horst KischRequires cookie*
 Title     
 Abstract    The dication of tetrakis(dimethylamino)ethene (TDAE2+) forms ion pair complexes with [M(mnt)2]2~, mnt2-= maleonitrile-2,3-dithiolate, M(II) = Ni, Pd, Pt, and Zn. According to X-ray analysis the structure of {TDAE2+[Pt(mnt)2]2~ } consists of a chain-like arrangement o f planar dianions and twisted (71°) dications. Shortest interionic contacts are 11 pm longer than the corresponding van der Waals radii. In the UV-VIS diffuse reflectance spectra of the complexes with a d8 central metal there is no unambiguous evidence for the presence of an ion pair CT band. This band is observed, however, at 450 nm when the d 10 metal Zn(II) is present. Application of the Hush-Marcus model affords a reorganization energy of 110 kJ / mol for electron transfer from [Zn(mnt)2]2-to TDAE2+. This value is 40 kJ / mol higher than the one reported for the analogous complex wherein TDAE2+ is replaced by a 2,2'-bipyridinium acceptor of similar reduction potential. 
  Reference    (Z. Naturforsch. 52b, 65—68 [1997]; received April 1 1996) 
  Published    1997 
  Keywords    Ion Pair Charge-Transfer, Optical Electron Transfer, X-ray 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0065.pdf 
 Identifier    ZNB-1997-52b-0065 
 Volume    52 
5Author    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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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0323.pdf 
 Identifier    ZNB-1997-52b-0323 
 Volume    52 
6Author    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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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0331.pdf 
 Identifier    ZNB-1997-52b-0331 
 Volume    52 
7Author    J. Dautel, S. Abele, W. SchwarzRequires cookie*
 Title    Synthese von 2,2-DiphenylethyI-substituierten Silanen -Molekülstruktur von Trichlor-2,2-diphenylethylsilan Syntheses of 2,2-Diphenylethyl-Substituted Silanes -Molecular Structure of Trichloro-2,2-diphenylethylsilane  
 Abstract    Hydrosilylation of 1,1-diphenylethylene with trichlorosilane leads in high yields to trichloro-2.2-diphenylethylsilane (1), which was investigated spectroscopically as well as by X-ray structure determination. The compound crystallizes monoclinically in the acentric space group Cc {a = 1002.4, b = 1573.8, c = 979.7 pm, ß = 106.27°, Z = 4}; the bonding parameters show no special features. By fluorination with zinc(II) fluoride in diethylether and by reduction with "Red-Al" in toluene, the corresponding SiF3 (2) and SiH3 derivatives (3) are received, respectively. 
  Reference    Z. Naturforsch. 52b, 778—784 (1997); eingegangen am 13. März 1997 
  Published    1997 
  Keywords    22-Diphenylethyl-Substituted Silanes, Fluorination, X-Ray 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0778.pdf 
 Identifier    ZNB-1997-52b-0778 
 Volume    52 
8Author    VeraV. Ponomareva3, VictorV. Skopenkoa, KonstantinV. Domasevitcha, Joachim Sielerb, Thomas GelbrichbRequires cookie*
 Title    Synthesis and Crystal Structure of a Caesium Hydrogen Benzoylcyanoximate Complex with 18-Crown-6: Cs(18-Crown-6){H(L)2}  
 Abstract    The caesium hydrogen benzoylcyanoximate (L_) complex with 18-crown-6 of composition Cs(18-crown-6){H(L)2} has been prepared and studied by means of X-ray diffraction [mon­ oclinic, space group P2)/n, with a = 9.906(1), b = 18.387(3), c = 18.855(3)Ä, ß = 90.13(1)°, V = 3434.3(9) Ä, Z = 4; final R1 = 0.043 for the 6431 independent reflections used. The lattice consists of C s(18-crown-6)+ cations and complex hydrogen oximate anions {H(L)2}~, formed via strong hydrogen bonding between the oxygen atoms of nitroso-groups [O— O ca. 2.456(5)A], The caesium atom deviates by 1.492(3) A from the mean plane of the oxygen atoms of the macrocyclic ether (dominant orientation of disordered ligand, 60%) and adopts a typical "sunrise coordination" [C s-0 (ether) 3.040(9)-3.312(7) A], The hydrogen oximate groups are bonded to the metal center only on one side of the crown ether plane via the oxygen atoms of nitroso-groups and the nitrogen atoms of cyano groups (C s-0 ca. 3.040(9), 3.312(7) A; Cs-N ca. 3.469(5), 3.679(6) A). The coordination polyhedron of Cs+ can be described as a distorted bicapped tetragonal prism. 
  Reference    Z. Naturforsch. 52b, 901—905 (1997); received February 28 1997 
  Published    1997 
  Keywords    Caesium Macrocyclic Complexes, Crown Ether Complexes, Benzoylcyanoxime, X-Ray 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0901.pdf 
 Identifier    ZNB-1997-52b-0901 
 Volume    52 
9Author    VladimirM. Amirkhanov3, Joachim Sielerb, VictorA. Trusha, VladimirA. Ovchynnikov3, KonstantinV. DomasevitchaRequires cookie*
 Title    Synthesis, IR and X-Ray Studies of a Dioxouranium(VI) Nitrate Complex with N,N'-Tetraethyl-NM -trichloracetylphosphortriamide  
 Abstract    A new dioxouranium(VI) nitrate complex with N,N'-tetraethyl-N"-trichloracetylphosphor-triamide (HL = CCl3C(0)N(H)P(0)(NEt2)2) of composition U0 2 (HL)2(N0 3)2 (1) has been synthesised. The IR spectroscopic data reveal that the ambidentate ligand is coordinated to the metal center in a monodentate manner via the phosphoryl oxygen atom. The crystal and molecular structure of 1 has been determined from X-ray diffraction data (triclinic, space group Pi with a = 9.225(2), b = 10.360(2), c = 12.249(2) A, a = 100.02 (1),/3 = 103.81(1), 7 = 108.80 (1)°, Z = 1; R = 0.037 for 4092 unique reflections. The structure is made up of centrosymmetric molecules in which the neutral ligands HL are monocoordinated. Phosphoryl and carbonyl groups of the HL moieties are in the trans positions to each other. The axial vertices of the distorted hexagonal bipyramid of uranium are occupied by two oxo ligands [U-0 1.753(5) A] while six oxygen atoms of phosphoryl and nitrate groups lie in the equatorial plane [U-0 2.347(5)-2.547(6)A], 
  Reference    Z. Naturforsch. 52b, 1194—1198 (1997); received February 24 1997 
  Published    1997 
  Keywords    Dioxouranium(VI), Carbacylamidophosphates, X-Ray 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-1194.pdf 
 Identifier    ZNB-1997-52b-1194 
 Volume    52 
10Author    Ayhan Elmali3, Yalcin Elermana, Ingrid Svobodab, Hartmut Fuessb, Klaus Griesar0, Wolfgang HaasecRequires cookie*
 Title    Structure and Magnetic Properties of a Dinuclear Copper(II) Complex  
 Abstract    [Cu2L] (L=N-2-hydroxy-4-methylphenyl-4-oxo-2-pentalketimine) was synthesized and its crystal structure determined. C24H?6Cu2N204 monoclinic space group P2|/n with a= 10.978(2), 17.045(3), c= 11.958(2) Ä, ß = 101.89(1)°, V = 2189.6(7) A3,Z = 4. Two copper(II) atoms in a distorted square-planar coordination are bridged by two oxygen atoms to form a dinuclear unit. The copperfll) centers are separated by 3.025(1) A and antiferro-magnetically coupled (7=-222.3 cm), which follows from temperature-dependent magnetic susceptibility measurements in the range 4.2 to 300 K. 
  Reference    Z. Naturforsch. 52b, 157—161 (1997); received September 30 1996 
  Published    1997 
  Keywords    Dinuclear Cu(II) Complex, X-Ray, Structure, Magnetic Properties, Antiferromagnetic Coupling 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0157.pdf 
 Identifier    ZNB-1997-52b-0157 
 Volume    52 
11Author    JuliaA. Manskaya, VolodimirN. Kokozay, KonstantinV. DomasevitchRequires cookie*
 Title    Crystal Structure of an Ammonium Dithiocyanatocuprate(I) Complex with 18-Crown-6, [NH4(18-Crown-6){Cu(NCS)2}] Obtained from Zero Valent Metal  
 Abstract    The new macrocyclic dithiocyanatocuprate(I) complex [NH4(18-crown-6){Cu(NCS)2}] has been prepared using a direct method of interaction and characterized by X-ray crystallogra­ phy (orthorhombic, space group Cmc2i, with a = 12.453(2), b = 21.650(4), c = 8.151(2) A, V = 2197.6(8) Ä3, Z = 4 , 1 (F) = 0.054; wR2(F2) = 0.141 for 972 unique reflections with I > 2<r(I) and /?1(F) = 0.082; w/?2(F2) = 0.210 for all 1098 unique reflections). The lattice comprises complex cations [NH4(18-crown-6)]+ and infinite polymeric anions [Cu(NCS)2]-of a one-dimensional zig-zag structure. The copper atoms adopt three-fold coordination [CuN^S] (Cu-N 1,89(1), 1,90(1) A; Cu-S 2.278(4) A). 
  Reference    Z. Naturforsch. 52b, 1311—1314 (1997); received 
  Published    1997 
  Keywords    18-Crown-6, Copper(I), Thiocyanate, Synthesis, X-Ray 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-1311.pdf 
 Identifier    ZNB-1997-52b-1311 
 Volume    52 
12Author    Z. NaturforschRequires cookie*
 Title    Synthese und Reaktivität von 7-Triphenylstannyl-a-am inobuttersäure- derivaten  
 Abstract    Ph3SnCH2CH 2C H (NHCOOCH 2P h)COOCH3 (1) is synthesized by hydrostannation of methyl N-(benzyloxycarbonyl)vinylglycinate with Ph3SnH. The reaction o f 1 with HC1 in CH 3OH and with bromine in CHC13 yields the halostannylsubstituted compounds Ph3_"X,?SnCH2CH 2C H(NHCOOCH 2Ph)C OOCH3 (2 -4) (n = 1, 2; X = Cl, Br). By sapo­ nification with one equivalent of NaOH and subsequent acidification with HCl 1 is transformed into the free acid Ph3SnCH2C H 2C H(NHCOOCH2Ph)COOH (5) that undergoes cyclization into the 1,2-oxastanninane 6 with intramolecular elimination of benzene. IR, NMR data and the determination of the crystal structure of Ph2BrSnCH2CH2CH(NHCOOCH2Ph)COOCH3(3) reveal for 2 and 3 an intramolecular coordination of the N C (0)0-group at the tin atom to form a seven-membered ring. 
  Reference    (Z. Naturforsch. 52b, 9—16 [1997]; eingegangen am 20. August 1996) 
  Published    1997 
  Keywords    Triphenylstannyl Aminobutyric Acid Derivatives, Halostannyl Aminobutyric Acid Derivatives, IR Spectra, NMR Spectra, X-Ray 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0009.pdf 
 Identifier    ZNB-1997-52b-0009 
 Volume    52 
13Author    Lothar BeyerRequires cookie*
 Title    Substituierte l,2,4-Thiadiazolium-dichloroaurate(I) und -tetra- chloroaurate(III) als Reaktionsprodukte von N-Thiocarbamoyl- benzamidinen mit TetrachIorogold(III)-Verbindungen  
 Abstract    Substituted 1,2,4-T hiadiazolium dichloroaurates(I) and -tetrachloroaurates(III) as Products o f the R eaction o f N -T hiocarbam oyl-benzam idines w ith Tetrachlorogold(III) Com pounds U w e Schröder3, R ainer R ichter3, Jürgen H artung3, U lrich A bram b, 
  Reference    Z. Naturforsch. 52b, 620—628 (1997); eingegangen am 12. März 1997 
  Published    1997 
  Keywords    1, 2, 4-Thiadiazoliumchloroaurates(I/III), Synthesis, X-Ray, EM Spectra, N-Thiocarbamoylbenzamidines 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0620.pdf 
 Identifier    ZNB-1997-52b-0620 
 Volume    52 
14Author    Jochen Ellermann3, Martin Schütz3, FrankW. Heinemann3, Matthias Moll3, Walter BauerbRequires cookie*
 Title    Chemie polyfunktioneller Moleküle, 127 [1] PPh2-Eliminierung aus dem PP-verknüpften Phosphazen Ph2P-N=PPh2-PPh2=N-PPh2 mit [C5H5Fe(CO)(/x-CO)]2; Kristallstrukturanalyse des Phosphazen-Derivats Chemistry of Polyfunctional Molecules, 127 [1] PPh2 Elimination from the PP Connected Phosphazene Ph2P-N=PPh2-PPh2=N-PPh-, with [C5H5Fe(CO)(^-CO)]2; Crystal Structure of the Phosphazene Derivative  
 Abstract    The reaction of Ph2P-N=PPh2-PPh2=N-PPh2 (Ph = C6H5, 2) with [CpFe(CO)(^-CO)]2 (Cp = C5H5, 3) yields under elimination of a PPh2-group from 2 and cleavage of the Fe-Fe bond in 3 the monocyclic ferraphosphazene complex Cp(OC)Fe-Ph2P-N=PPh2=N-PPh2 (4) and Ph2P-PPh2 (5). In a side reaction the P-P bond of 2 is also cleaved in a redox process to give Cp(OC)Fe-Ph2P-N-PPh2 (7). Compound 4 has been characterized by a crystal structure determination. 
  Reference    Z. Naturforsch. 52b, 795—800 (1997); eingegangen am 7. April 1997 
  Published    1997 
  Keywords    Phosphazene, Iron Complexes, X-Ray, Elimination of PPh2, Cleavage of PP 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0795.pdf 
 Identifier    ZNB-1997-52b-0795 
 Volume    52