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121Author    K. Polborn, W. Steglich, J. D. Connolly, S. Huneck, To Prof, G. Antonio, GonzalezRequires cookie*
 Title    Structure of the Macrocyclic Bis-lactone Lepranthin from the Lichen Arthonia im polita; an X-Ray Analysis celebrating his half-century of involvement with natural products chemistry  
 Abstract    The structure and relative stereochemistry o f lepranthin from the lichen Arthonia impolita has been elucidated as 1 by NM R spectroscopy and X-ray analysis. 
  Reference    Z. Naturforsch. 50b, 1111—1114 (1995); received February 20 1995 
  Published    1995 
  Keywords    Lepranthin, Macrocyclic Bis-lactone, X-Ray, Lichen 
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 TEI-XML for    default:Reihe_B/50/ZNB-1995-50b-1111.pdf 
 Identifier    ZNB-1995-50b-1111 
 Volume    50 
122Author    R. Ainer PöttgenRequires cookie*
 Title    EuPdGe -a New Germanide with EuNiGe Type Structure  
 Abstract    The title compound was prepared from the elem ental com ponents in a tantalum tube at 1070 K and investigated by X-ray diffraction of both powder as well as single crystals. The crystal structure was refined from four-circle diffractometer data: P 2 xln, a = 618.1(1), b = 613.6(1), c = 743.9(1) pm, ß = 109.40(1)°, V = 0.2661(1) nm3, Z = 4 ,w R 2 = 0.0536 for 1564 F2 values and 29 variables. EuPdGe crystallizes with the E uN iG e type structure. Both Pd and G e atom s in EuPdGe have three germanium or palladium neighbors, respectively. They form two-dim ensionally infinite [PdGe] polyanions which consist o f corrugated 4.82 nets. These polyanions are separated by the europium atoms. 
  Reference    Z. Naturforsch. 50b, 1181—1184 (1995); received March 1 1995 
  Published    1995 
  Keywords    Germanide, Crystal Structure, X-Ray, Europium 
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 TEI-XML for    default:Reihe_B/50/ZNB-1995-50b-1181.pdf 
 Identifier    ZNB-1995-50b-1181 
 Volume    50 
123Author    Wolfgang Pohl, Ingo-Peter Lorenz, Heinrich Nöth, Martin SchmidtRequires cookie*
 Title    Offene und geschlossene Triferriophosphonium-Salze und Triferriophosphane O pen and Closed Triferriophosphonium Salts and Triferriophosphines  
 Abstract    The reaction of P(SiM e3)3 with an excess of C pFe(CO)2X (X = Cl, Br) through the action o f water gives the triferriophosphonium salt [{CpFe(CO)2}3PH]2FeX4 together with ferrocene as by-product. The cation of the salt can be deprotonated by D B U to afford the unstable triferriophosphine {CpFe(CO)2}3P. Its subsequent realkylation with RX (R = Me, CH2Ph; X = I, Br) leads to alkyltriferriophosphonium salts [{CpFe(CO)2}3PR]X. Photolysis of [{CpFe(CO)2}3PH]2FeX 4 induces the elimination of one CO group, and the CO-bridged and partly closed complex [{//-CO(CpFeCO)2}{CpFe(CO)2}PH]2FeX 4 is formed, the cation of which can also be deprotonated to give the corresponding m onobridged phosphine (w-CO(CpFeCO)2}{CpFe(CO)2}P. Both PH-phosphonium salts undergo a hydrogen-chlorine exchange reaction to give the P -C l analogues [{CpFe(CO)2}3PCl]2FeX4 and [{//-CO (CpFeCO)2}{CpFe(CO)2}PCl]2FeX 4. The IR and NM R spectra of all species as well as the X-ray structure analyses of the open and closed P -H functional com plexes are reported and discussed. 
  Reference    Z. Naturforsch. 50b, 1485—1493 (1995); eingegangen am 30. März 1995 
  Published    1995 
  Keywords    Iron, Tristrimethylsilylphosphine, Hydrogen Chlorine Exchange, X-Ray, Decarbonylation 
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 TEI-XML for    default:Reihe_B/50/ZNB-1995-50b-1485.pdf 
 Identifier    ZNB-1995-50b-1485 
 Volume    50 
124Author    YalcinE. Lerm Ana+, MehmetK. Abaka, Ingrid Svobodab, H. Artm Ut Fuessb-, KlausG. Riesarc, WolfgangH. AasecRequires cookie*
 Title    X-Ray Structure and Magnetic Properties of the Tetracupferronato-bis(//-methoxy)-diiron(III) Complex  
 Abstract    The tetracupferronato-bis(w-methoxy)-diiron(III) complex has been synthesized in aceto­ nitrile and its crystal structure determined. C i6H->6N80 1(>Fe2, monoclinic, space group C2/c, a =18.425(3), b = 12.999(2), c = 15.046(3) A, ß = 12 4 .6 6 (2)°,> = 2964(1) A , Z = 4, wR(2) = 0.097 from 1491 reflections (F2). Two iron(III) atoms are at special positions in six-fold co­ ordination, bridged by O with a F e -O -F e angle of 102.4(1)° and a distance between two iron(III) centers of 3.075(1) A. Temperature-dependent magnetic susceptibility measure­ ments reveal a antiferromagnetic exchange interaction (J = -1 4 cm -1) betw een the iron(III) centers. 
  Reference    Z. Naturforsch. 50b, 1587—1590 (1995); received January 11 1995 
  Published    1995 
  Keywords    X -Ray, Magnetic Properties, Antiferromagnetic Coupling 
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 TEI-XML for    default:Reihe_B/50/ZNB-1995-50b-1587.pdf 
 Identifier    ZNB-1995-50b-1587 
 Volume    50 
125Author    Dagmar Holthenrich, Imre Sóvágó, G. Erd Fusch, Andrea Erxleben, EddaC. Fusch, Ingo Rombeck, B.Ernhard LippertRequires cookie*
 Title    Heteronuclear Nucleobase Complexes as Tools for the Isolation of the Minor Rotamer of the Parent Compound: Synthesis and Crystal Structure Determination of H ead-H ead and H ead-Tail Forms of rrfl«5-[(CH3NH2)2Pt(l-MeC-Ar J)2]2+ (1-MeC = 1-methylcytosine)  
 Abstract    The two rotamers (head-tail, 1, and head-head, 2) of the bis(l-m ethylcytosine)com plex of f/ww-(CH3N H 2)2Pt(II), have been crystallized as C104-(1, 2a) and PF6-(2b) salts and characterized by X-ray crystal structure analysis and 'H and 19:iPt NMR spectroscopy. In aqueous solution, 1 is preferred over 2 by 70:30. Upon slow crystallization from H 2Ö, 1 is obtained as the only product. Isolation of 2a and 2b has now been accomplished via forma­ tion of the heteronuclear derivative rrans-[(CH3N H 2)2Pt(l-MeCv/V3,./W)2Hg]2+, in which the deprotonated 1-methylcytosinato ligands (1 -M eC) are oriented head-head, precipitation of Hg(II) by thiourea, and rapid crystallization of the parent compound. The solid state struc­ tures of 1 and 2b differ markedly in a number o f aspects. Isolation of pure 1 and 2 permits a detailed study of the kinetics and thermodynamics of the interconversion of the two rotam­ ers. From comparison with the behavior of 1 and 2 in H20 on the one hand and DM SO and DM F on the other a clear solvent effect on the rotamer distribution is seen which most likely relates to differences in H bonding between solvent and solute. 
  Reference    Z. Naturforsch. 50b, 1767—1775 (1995); received May 15 1995 
  Published    1995 
  Keywords    Transplatin, Nucleobase, 1-Methylcytosine, R otation, X-Ray 
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 TEI-XML for    default:Reihe_B/50/ZNB-1995-50b-1767.pdf 
 Identifier    ZNB-1995-50b-1767 
 Volume    50 
126Author    Jochen Ellermann, Peter Gabold, FalkA. Knoch, MatthiasM. Oll, Astrid Schmidt, Martin SchützRequires cookie*
 Title    Chemie polyfunktioneller Moleküle, 120 [1] Synthesen und Kristallstrukturanalysen von Tris(imido-tetraphenyl- diphosphinato-0,0')eisen(III) und des PP-verknüpften Phosphazens Ph2P-N=PPh2-PPh2=N-PPh2 Chemistry o f Polyfunctional M olecules, 120 [11 Syntheses and Crystal Structures o f Tris(imido-tetraphenyl-diphosphinato-0,0')iron(III) and o f the PP-Connected Phosphazene Ph2P-N=PPh2-PPh2=N-PPh2  
 Abstract    While the reaction of anhydrous iron(III) chloride with the chelate ligand [(C6H5)2P(0)]2NH (6) is an efficient way to synthesize the new tricyclic compound imido-tetraphenyl-diphosphinato-0,0'iron(III), [Fe{0-P(Ph2)=N-P(Ph2)= 0 }3] (4), treatment of [(C6H5)2P]2NLi (1) with anhydrous iron(III) fluoride in THF represents a simple route to obtain the phosphorus-phosphorus connected species Ph2P-N=PPh2-PPh2=N-PPh2(7). Both compounds were charac­ terized by X-ray crystallography, 'H ,31 P {1H}, 13C {1H} NMR, IR, Raman and mass spectra. 
  Reference    Z. Naturforsch. 51b, 201—208 (1996); eingegangen am 24. Juli 1995 
  Published    1996 
  Keywords    Phosphazene, Iron Complexes, Synthesis, X-Ray 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0201.pdf 
 Identifier    ZNB-1996-51b-0201 
 Volume    51 
127Author    Kuhn3, Thomas Kratz3, G. Erald, H. EnkelbRequires cookie*
 Title    N orbert  
 Abstract    The carbene adduct 5 is formed from the 2-tel-luroimidazoline 4 and iodine. The X-ray structure analysis reveals a dimeric structure in the solid state. 
  Reference    Z. Naturforsch. 51b, 295 (1996); eingegangen am 21. Juli 1995 
  Published    1996 
  Keywords    Tellurium, Carbene, Iodine Reaction, X-Ray 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0295_n.pdf 
 Identifier    ZNB-1996-51b-0295_n 
 Volume    51 
128Author    Yoshimitsu Yamazaki, MidoriG. Oto1, ^. Yu-Ichi, Takenori Kageyama, Hiroaki Tomohiro, OkunoRequires cookie*
 Title    Structure of Chloro(cyclopentadienone)- (cyclopentadienyl)ruthenium and its Cytotoxic Activity  
 Abstract    The structure of R u(cpO)(cp)C l com plex (3), which was precipitated from aqueous solutions of R u(cp)2Cl+PF6' (1), was determined by X-ray crystallographic analysis. The Ru-halogen bond distance was shorter and the dihedral angle be­ tween the rings was larger than the values re­ ported for the corresponding Br analogue, R u(cpO)(cp)Br (4). The com plex 3 (IC50 1 09 /iM) was more cytotoxic than 1 (IC50 163 //M) against mouse sarcoma S I80 cells, but less toxic than 4 (IC50 72 ,/M). 
  Reference    Z. Naturforsch. 51b, 301 (1996); received September 21 1995 
  Published    1996 
  Keywords    Ruthenium Complex, Cytotoxicity, X-Ray, Cyclic Voltammetry 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0301_n.pdf 
 Identifier    ZNB-1996-51b-0301_n 
 Volume    51 
129Author    Max Herberhold, Guo-Xin Jina, ArnoldL. RheingoldbRequires cookie*
 Title    Sulfur and Selenium Complexes of the Hydrido-tri(3,5-dimethyl-l- pyrazolyl)borate Nitrosylmolybdenum Fragment, [Tp*Mo(NO)]. An X-Ray Crystal Structure Determination of Tp*Mo(NO)(Se5)  
 Abstract    The reactions of hydrido-tri(3,5-dimethyl-l-pyrazolyl)borate nitrosylmolybdenum diiodide, Tp*Mo(NO)L (2), with the oligochalcogenides (N H ^Sio and (NEuteSeö in THF solution lead to mononuclear cvc/o-pentachalcogenido complexes, Tp*Mo(NO)(E5) (E = S (3a), Se (3b)). In the presence of either H2S or H^Se (generated by slow "in situ" hydrolysis of AI2E3 in moist THF solution) 2 is converted into binuclear chalcogenido-bridged products, Tp2Mo2(NO)2(//-E)2 (E = S (4a), Se (4b)) which are more conveniently obtained from 3a,b by dechalcogenation with tri(''butyl)phosphane (1:4,5). The new chalcogen complexes 3a,b and 4a,b were characterized by IR, NMR and mass spectroscopy and compared with the related chalcogen compounds derived from pentamethylcyclopentadienyl nitrosylmolybdenum diiodide, Cp*Mo(NO)l2. The molecular structure of Tp*Mo(NO)(Ses) (3b) has been determined; the complex contains a six-membered MoSe«; metallacycle in the chair conformation and a linearly coordinated nitrosyl ligand (angle M o -N -0 178.9(17)°). 
  Reference    Z. Naturforsch. 51b, 681—685 (1996); received August 28 1995 
  Published    1996 
  Keywords    Molybdenum-chalcogenido Complexes, Nitrosyl Compounds, X-Ray 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0681.pdf 
 Identifier    ZNB-1996-51b-0681 
 Volume    51 
130Author    Utzolino, Karsten BluhmRequires cookie*
 Title    A nne  
 Abstract    The compounds M nCo(B20 ?) (I) and M nM g(B20 5) (II) were prepared by using B20 3 flux techniques in an argon atmosphere. X-ray investigations on single crystals showed triclinic symmetry, space group C' -P i, I: a = 320.94(10), b = 619.20(11), c = 939.0(2) pm, a = 104.38(2)°, ß = 90.76(2)°, 7 = 92.046(14)° and II: a = 318.97(7), b = 619.8(2), c = 936.7(2) pm, q = 104.47(2)°, ß = 90.60(2)°, 7 = 91.98(2)° Z = 2. Their structures are isotypic with C o2(B20 5). All metal ions are octahedrally coordinated by six oxygen atoms. The structures contain diborate anions B ^ 4 -. Each boron atom is threefold coordinated by oxygen. Synthese und Kristallstruktur von manganhaltigen Pyroboraten: MnCo(B20 5) und MnMg(B20 5) 
  Reference    Z. Naturforsch. 51b, 912—916 (1996); eingegangen am 25. Januar 1996 
  Published    1996 
  Keywords    Manganese, Cobalt Magnesium, Pyroborate Crystal Structure, X-Ray 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0912.pdf 
 Identifier    ZNB-1996-51b-0912 
 Volume    51 
131Author    Stephan Von, B. Eckeratha, Ingo-Peter Lorenz, Riad Fawzib, M. Anfred, Steim AnnbRequires cookie*
 Title     
 Abstract    p(C O)2M nN (Bz)C H 2CH2 , der erste einzähnig koordinierte A ziridin-K om plex C p(C O)2M nN (B z)C H 2C H 2, the First M ono-C oordinate A ziridine Com plex The photolytically induced CO-substitution reaction of CpM n(CO b with N-benzyl-aziridine leads to the first mono coordinate aziridine complex, Cp(CO)2MnN(Bz)CH2CH2. It is stable against thermal C2H4 elimination up to 135°C. No nitrene complexes {Cp(CO)2Mn}"NBz (/? = 1, 2) were detected. The X-ray structure analysis of Cp(CO)2MnN(Bz)CH2CH2 shows the intact three-membered ring ligand and the pyramidal configuration of the nitrogen atom. 
  Reference    Z. Naturforsch. 51b, 959—962 (1996); eingegangen am 12. Januar 1996 
  Published    1996 
  Keywords    N-Benzyl-aziridine, Substitution, Cymantrene, X-Ray 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0959.pdf 
 Identifier    ZNB-1996-51b-0959 
 Volume    51 
132Author    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 
133Author    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 
134Author    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 
135Author    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 
136Author    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 
137Author    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 
138Author    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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 Identifier    ZNB-1997-52b-1194 
 Volume    52 
139Author    Z. NaturforschRequires cookie*
 Title    Kristallstruktur von MgS03*H20  
 Abstract    The crystal structure of M g S 0 3 H20 , space group P 2 \ln, Z = 4, Dx = 2.415 g em -3 , a = 4.699(1), b = 12.751(3), c = 5.618(1) Ä, ß = 90.49(3)°, was determined by single crystal X-ray diffraction. M g S 0 3 H20 crystallizes in the M n S 0 3 H20 type. The structure consists of buckled trans layers ^ [M gS03 H20 ], which are built up from strongly distorted M g 0 5(H20) octahedra sharing four equatorial vertices, and of trigonal pyramidal S 0 32-ions. It is close­ ly related to the structures of orthorhombic M nSe0s3 D 20 and monoclinic Z n S e 0 3 H20 . The M g -0 distances range from 2.051(3) to 2.175(4) A. The S-O distances (1.543(3), 1.547(3) and 1.493(3) Ä) and the O-S-O angles (98.4(2) and 2x 106.0(2)°) correspond to those in M n S 0 3 H20 . The distortion of the M 0 5(H20) octahedra (M = Mg, Mn) and of the S 0 32-ions is smaller in M g S 0 3 H20 , but with greater deviations from m symmetry. The distances between the H-connected ^ [M S 03 H20 ] layers are greater in M g S 0 3 H 20 , indicating weaker inter-layer hydrogen bonds. The lateral arrangement of the 2 [M S 0 3 H20 ] layers is nearly the same in both sulfite monohydrates. E in le itu n g 
  Reference    Z. Naturforsch. 53b, 131—134 (1998); eingegangen am 10. November 1997 
  Published    1998 
  Keywords    X-Ray, Sulfites, Hydrates, Magnesium, Pseudosymmetry 
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 Identifier    ZNB-1998-53b-0131 
 Volume    53 
140Author    Ingrid Pilz, K. Arin Goral, FriedrichV D HaarRequires cookie*
 Title    Phenylalanyl-tRNA Synthetase from Baker'Yeast: Structural Organization of the Enzyme and Its Complex with tRNAPhe as Determined by X-Ray Small-Angle Scattering  
 Abstract    The quaternary structure of the phenylalanyl-tRNA synthetase and its complex with tRNAPhe was studied in dilute solutions by small angle X-ray scattering. For the free synthetase the radius of gyration was determ ined as 5.5 nm, the volume 523 nm 3, the maximum diam eter 17.5 nm and the m olecular weight as 260 000 using an isopotential specific volume of 0.735. The overall shape could be best approxim ated by a flat cylinder with dimensions 18.2 n m X l l .5 n m X 4 nm ; the loose structure was approxim ated by building up the cylinder by spheres (diam eter 4.2 n m). The corresponding param eters of the enzyme tRN A complex were the following: radius of gyration 5.9 nm, volume 543 nm 3, maximum diam eter 21 nm and m olecular weight 290 000. These param eters suggest an 1:1 complex, whereby it m ust be assumed that the tRN A m olecule is attached in the extension of the longer axis. From the difference in the distance distribution functions of the free enzyme and the complex it is evident that we have to assume a change of conform ation (contraction) of the enzyme upon the binding of the specific tRNA. 
  Reference    Z. Naturforsch. 34c, 20 (1979); received November 20 1978 
  Published    1979 
  Keywords    X-Ray, Small-Angle, Scattering, Enzyme, Complex 
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 TEI-XML for    default:Reihe_C/34/ZNC-1979-34c-0020.pdf 
 Identifier    ZNC-1979-34c-0020 
 Volume    34 
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