| | 84 | Author
| Peter Schreiber, Karl Wieghardt, Ulrich Flörke, Hans-Jürgen Haupt | Requires cookie* | | | Title
| Synthese von Wolframkomplexen  | | | | Abstract
| des Typs [ L W (C O) 3X ] + (X = H , F, Br; L = 1,4,7-Triazacyclononan). Die Kristallstrukturen von [L W (C O) 3B r]B F 4 und [L W (C O) 3H ] 2[W O C l5] • h 2o Synthesis o f Tungsten Complexes o f the Type [L W (C O)3X ] + (X = H, F, Br; L = 1.4,7-triazacyclononane). The Crystal Structures o f [L W (C O)3Br]BF4 and [L W (C O)3H ]2[W O C l5] • H 20 The reaction of LW (C O), (L = 1,4,7-triazacyclononane) with Br2 in CHCl, yields orange [L W (C O)3Br](Br3) which was converted to its BF4~ salt. [L W (C O)3Br]BF4 crystallizes in the triclinic space group P 1 (a = 8.273(3), b = 8.628(2), c = 13.034(3) Ä , a = 80.10(2), ß = 72.69(2). y = 61.14(2)°, Z = 2); it consists of cations [L W (C O)3Br] + , with seven-coordinate W atoms, and BF4 -anions. The corresponding salt [L W (C O)3F](PFft) was obtained from L W (C O)3 with 20% aqueous HF in the presence of air and addition of NaPF6. The analogous reaction with 37% aqueous HC1 affords green crystals of [L W (C O)3H ]2[W OCl5] • H 20 which crystallize in the mono clinic space group P2,/c (a = 12.234(4), b = 18.853(7), c = 14.609(5) Ä . ß = 105.65(3)°, Z — 4). The W atoms in the [L W (C O)3H ]+ cations are seven-coordinate; the six-coordinate [W OCl5]: anions are not disordered. The W = 0 distance is short (1.72(1) Ä), the mean equatorial W —Cl distance is 2.390 Ä whereas the W —Cl bond distance trans to the W = 0 group is 2.562(5) Ä. | | | |
Reference
| Z. Naturforsch. 42b, 1391 (1987); eingegangen am 2. Juli 1987 | | | |
Published
| 1987 | | | |
Keywords
| Tungsten Complexes, X-Ray, Crystal Structure | | | |
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| default:Reihe_B/42/ZNB-1987-42b-1391.pdf | | | | Identifier
| ZNB-1987-42b-1391 | | | | Volume
| 42 | |
| 87 | Author
| T. Sogo, J. Romero, A. Sousa, A. De Blas, M. L. Durán, E. E. Castellano | Requires cookie* | | | Title
| The Electrochemical Synthesis of Neutral Zinc(II) Complexes of Schiff Base Ligands: The Crystal Structure of Bis[N-(4-methylphenyl)salicylaldiminato]zinc(II) | | | | Abstract
| The electrochemical synthesis and physico-chemical properties of neutral zinc(II) complexes of bidentate Schiff bases derived from salicylaldehydes are presented together with the X-ray struc-ture of bis[N-(4-methylphenyl)salicylaldiminato]zinc(II). The crystal is monoclinic, a = 21.877(3), b = 8.801(2), c = 12.027(5) Ä, ß = 96.55(3)°, space group C2/c. The complex is a monomer, and the zinc atom is tetrahedrally coordinated. | | | |
Reference
| Z. Naturforsch. 43b, 611—615 (1988); received November 5 1987/January 28. 1988 | | | |
Published
| 1988 | | | |
Keywords
| X-Ray, Zinc, Schiff Bases, Electrochemical Synthesis | | | |
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| default:Reihe_B/43/ZNB-1988-43b-0611.pdf | | | | Identifier
| ZNB-1988-43b-0611 | | | | Volume
| 43 | |
| 89 | Author
| Uwe Scholz, Mathias Noltemeyer, HerbertW. Roesky | Requires cookie* | | | Title
| Synthese und Struktur eines ungewöhnlichen Molybdän-Heterocyclus durch Substitution eines Phenylringes in ortho-Stellung Synthesis and Structure of an Unusual Molybdenum Heterocycle by Substitution of a Phenyl Ring in ortho-Position | | | | Abstract
| The new ligand (Me 3 Si) 2 NC(Ph)NP(Ph) 2 N(SiMe 3) (1) reacts with MOOC1 4 to yield the green metallacycle 4. 4 was characterized by X-ray diffraction. Crystals of 4 are monoclinic, space group P2,/n with a = 1061.2(10). b = 1590.5(10), c = 1737.4(20) pm, ß = 104.84(7)° and Z = 4. Mo is coordinated octahedrally by two nitrogens of the bifunctional ligand. by one oxygen and three chlorine atoms. The ligand undergoes cyclization, a bond being formed between N and one phenylic o-position. | | | |
Reference
| Z. Naturforsch. 43b, 937—940 (1988); eingegangen am 23. März 1988 | | | |
Published
| 1988 | | | |
Keywords
| X-Ray, Molybdenum, Heterocycle Phosphorus-Nitrogen Compound | | | |
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| default:Reihe_B/43/ZNB-1988-43b-0937.pdf | | | | Identifier
| ZNB-1988-43b-0937 | | | | Volume
| 43 | |
| 90 | Author
| Gisela Sawitzki, Wolfgang Einholz, Wolfgang Haubold | Requires cookie* | | | Title
| Kristall-und Molekülstruktur von N,N'-Bis(l,3-dimethylbenzo[b]-l,3?2-diazaboroIidin-2-yl)carbodiimid Crystal and Molecular Structure of N,N'-Bis(l,3-dimethylbenzo[b]-l,3,2-diazaborolidin-2-yl)carbodiimide | | | | Abstract
| Crystals of the title compound (2) are monoclinic with a = 905.5(3), b = 593.6(2). c — 3243.5(8) pm, ß = 95.63(2)°, Z = 4, space group P2 x ln. The molecule 2 neither has a C 2 -symmet-rical allene-type nor a D 2d -symmetrical cumulene-type structure, but it has a non-linear B-N = C=N —B arrangement and is nearly planar. The central N = C=N angle has a value of 171.9(3)°, the B —N = C angles are 145.9(2)° and 163.1(3)°. | | | |
Reference
| Z. Naturforsch. 43b, 1179—1183 (1988); eingegangen am 25. Mai 1988 | | | |
Published
| 1988 | | | |
Keywords
| Boron-Nitrogen Compounds, Borylated Carbodiimides, X-Ray | | | |
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| default:Reihe_B/43/ZNB-1988-43b-1179.pdf | | | | Identifier
| ZNB-1988-43b-1179 | | | | Volume
| 43 | |
| 92 | Author
| Susanne Maier, Wolfgang Hiller, Joachim Strähle, Christina Ergezinger, Kurt Dehnicke | Requires cookie* | | | Title
| | | | | Abstract
| The copper(I)amidinato complex Cu 2 [Ph-C(NSiMe 3) 2 ] ; has been prepared by the reaction of CuCl with N.N,N'-tris(trimethylsilyl)benzamidine in boiling acetonitrile. forming white crystals. The compound was characterized by its IR spectrum as well as by an X-ray structure determina-tion. Crystal data: space group PI, Z = 2 (2851 observed independent reflexions, R = 0.047). Lattice dimensions at 20 °C: a = 1135.0(3); b = 1219.6(4); c = 1372.4(4) pm; a = 106.74(3)°; ß = 107.92(4)°; y = 91.40(4)°. The compound forms dimeric molecules with a short Cu--Cu contact of 242 pm and two chelating amidinato ligands with Cu-N bond lengths of (averaged) 189.0 pm and bond angles N —C—N of 124.1°. | | | |
Reference
| Z. Naturforsch. 43b, 1628—1632 (1988); eingegangen am 11. August/30. September 1988 | | | |
Published
| 1988 | | | |
Keywords
| Synthesis, X-Ray, Copper(I) Amidinato Complex | | | |
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| default:Reihe_B/43/ZNB-1988-43b-1628.pdf | | | | Identifier
| ZNB-1988-43b-1628 | | | | Volume
| 43 | |
| 93 | Author
| Johannes Breker, PeterG. Jones, Reinhard Schmutzler, FrauM. Prof, Argot Becke | Requires cookie* | | | Title
| 4-Substituierte | | | | Abstract
| ,3,5,7-T etramethyl-1,3,5,7-tetraaza-4 A5-phosphaspiro-|3.3]heptan-2,6-dione; Röntgenstrukturanalyse von 1,3,4,6,7,9,10-Heptamethyl-5-oxa-l ,3>7,9,10-pentaaza-4 A5,6 A5-diphosphadispiro[3.1.3.1 ]decan-2,8-dion 4-Substituted l,3,5,7-Tetramethyl-l,3,5,7-tetraaza-4>3.5-phosphaspiro[3.3]heptane-2,6-diones; Crystal Structure of l,3,4,6,7,9,10-Heptamethyl-5-oxa-l,3,7,9,10-pentaaza-4A5, 6 / 5-diphospha-dispiro[3.1.3. l]decane-2,8-dione The reaction o f the tetrachlorophosphoranes RPC14 (R = Me, Ph) with N,N'-dimethylurea (dmh) (1), or o f the diazaphosphetidinone 0 = C (N M e)2PR (R = CC13) (3) and chlorine with N,N'-bis(trim ethylsilyl)-N,N'-dim ethylurea (2) furnished the spiro compounds | | | |
Reference
| Z. Naturforsch. 45b, 1407—1415 (1990); eingegangen am 19. Oktober 1989 | | | |
Published
| 1990 | | | |
Keywords
| Oxoazadiphosphetidine, N M R Spectroscopy, X-Ray | | | |
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| default:Reihe_B/45/ZNB-1990-45b-1407.pdf | | | | Identifier
| ZNB-1990-45b-1407 | | | | Volume
| 45 | |
| 94 | Author
| UlrichW. Annagat, Gabriele Bogedain, A. Drian Schervan, HeinrichC M Arsm Ann, DavidJ. Brauer, Hans Bürger, FrankD. Örrenbach, Gottfried Pawelke, Carl Krüger, Karl-Heinz Claus | Requires cookie* | | | Title
| Das Isosterenpaar S iO /P N , I Zur Isosterie von Perchlorcyclosiloxanen und Perchlorcyclophosphazenen. Schwingungsspektren und Röntgenstrukturanalyse von (Cl2SiO )3 und (Cl2SiO )4 The SiO/PN Isoelectronic Pair, I Perchlorocyclosiloxanes and Perchlorocyclophosphazenes. Vibrational Spectra and X-Ray Structure Analysis o f (Cl2SiO) 3 and (Cl2SiO) 4 | | | | Abstract
| Hexachlorocyclotrisiloxane (2) and octachlorocyclotetrasiloxane (4) were prepared by reac tion o f SiCl4 with 0 2 at 955 C. Their mass spectra are compared with those o f the isoelectronic cyclophosphazenes. The vibrational spectra o f 2 and 4 are very similar and closely related to that o f (PNC12)3, but clearly different from that o f the puckered (PNCU) 4 molecule. The X-ray examination o f 2 and 4 reveals planarity o f the (SiO)", n = 3 and 4 ring systems, with d (S i-O) on average 1.619(4) and 1.584(3) Ä, respectively. | | | |
Reference
| Z. Naturforsch. 46b, 931—9 (1991); eingegangen am 2. Novem ber 1990 | | | |
Published
| 1991 | | | |
Keywords
| Perchlorocyclosiloxanes, Perchlorocyclophosphazenes, Isoelectronic Relations, X-Ray, Vibrational Spectra | | | |
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| default:Reihe_B/46/ZNB-1991-46b-0931.pdf | | | | Identifier
| ZNB-1991-46b-0931 | | | | Volume
| 46 | |
| 95 | Author
| H. Erbert, W. Roesky, Birgit Meller-Rehbein, M. Athias Noltemeyer | Requires cookie* | | | Title
| Reactions of M e2NC(S)SN(SiMe3)2 with M etal Halides -Crystal Structure of M e2NCS2ZrCl3 * 3 Pyridine | | | | Abstract
| M e-,NC(S)SN(SiM e3)2 (1) reacts with TeCl4 and N bC lj to yield M e2N C (S)SN TeC l2 (4) and | | | |
Reference
| Z. Naturforsch. 46b, 1117—1121 (1991); eingegangen am 14. Februar 1991 | | | |
Published
| 1991 | | | |
Keywords
| Tellurium, Niobium, Zirconium, Hafnium, Complexes, X-Ray | | | |
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| default:Reihe_B/46/ZNB-1991-46b-1117_n.pdf | | | | Identifier
| ZNB-1991-46b-1117_n | | | | Volume
| 46 | |
| 96 | Author
| Yüniu Bai, M. Athias Noltemeyer, H. Erbert, W. Roesky | Requires cookie* | | | Title
| Synthese und Strukturen von Monoalkylamiden und -imiden des Titans Synthesis and Structures o f M onoalkylam ides and -imides of Titanium | | | | Abstract
| A new method for the preparation o f m onoalkylam ides o f com position Cp'TiCl2N H R is reported. M e3SnN H R (R = /Bu l a , CH/Pr-, lb) reacts with Cp'TiCl3 with elimination o f M e3SnCl to yield Cp'TiCLNHR (2) (2a: Cp' = C 5H 5, R = /Bu, 2b: Cp' = M e3SiC5H 4, R = t Bu, 2c: Cp' = (M e3Si)?C 5H 3, R = /Bu, 2d: Cp' = M e4C5H, R = /Bu, 2e: Cp' = M e5C5, R = t Bu, 2f: Cp' = C5H 5, R = CH/Pr2, 2g: Cp' = M e3SiC5H 4, R = CH/Pr2, 2h: Cp' = (M e3Si)2C5H3, R = CH/Pr2, 2i: Cp' = M e4C5H , R = CH/Pr2, 2j: Cp' = M e5C5, R = CH/Pr2). Compounds 2 a -2 j are stable and eliminate HC1 only in the presence o f a strong base to form (C5H 5T iC lN /B u)2 (3a) or (M e3SiC5H4T iC lN /B u)2 (3b) from 2 a and 2b, respectively. In 3a the chlorine atom s are substituted by N H /B u groups in boiling T H F by means o f L iN H /Bu to give (C5H 5T iN H /B uN /B u)2 (4). The reactions o f 2 e and 2b with L iN (SiM e3)2-Et20 in the presence o f pyridine yield M e5C5T iC lN /B u • Py (5 a) (Py = pyridine) and M e3SiC5H4T iC lN /B u P y (5 b), respectively. Com pounds 2 e and 5 a have been characterized by X-ray crystal structural analysis. | | | |
Reference
| Z. Naturforsch. 46b, 1357 (1991); eingegangen am 22. März 1991 | | | |
Published
| 1991 | | | |
Keywords
| X -Ray, Synthesis, Titanium, Amides, Imides | | | |
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| default:Reihe_B/46/ZNB-1991-46b-1357.pdf | | | | Identifier
| ZNB-1991-46b-1357 | | | | Volume
| 46 | |
| 97 | Author
| Dieter Sellmann+, Bernd Seubert, W. Olfgang Kern, Falk Knoch, M. Atthias, Moll | Requires cookie* | | | Title
| Übergangsmetallkomplexe mit Schwefelliganden, LXIX* and X-Ray Structure Analyses | | | | Abstract
| Chrom-und Wolfram-Nitrosyl-Komplexe mit schwefeldominierten Koordinationssphären: IC r(N O)XS4')]v (x = 1, y = 2; x = 2, y = 1), (NR4)2[W (NO)2(S 2)2] (R = M e, /i-Bu), [W(L)(NO)('S4)] (L = NO , N P M e3, NPEt3) und [//-0 { W (N 0)(S4)} 2] ('S2'2" = l,2-Benzoldithiolat(2-); 'S4'2-= l,2-Bis(2-mercaptophenylthio)ethan(2-)); Synthesen, Eigenschaften und Röntgenstrukturanalysen Transition M etal Complexes with Sulfur Ligands, LXIX* Chromium and Tungsten Nitrosyl Complexes with Sulfur Dom inated C oordination Spheres: [C r(N O)/S 4')]v(* = \ , y = 2 \x = 2 , y = 1), (N R 4)2[W(NO)2('S2')2] (R = Me, «-Bu), [W(L)(NO)('S4')] (L = NO, N PM e3, N P E t3) and [//-0{W (N 0)('s7)}2] ('S2'2-= 1.2-B enzenedithiolate(2-);'S4'2-= 1.2-Bis(2-mercaptophenylthio)ethane(2-)); Syntheses, Properties In order to study the properties o f sulfur coordinated metal centres, the chromium and tung sten complexes [Cr(NO)(//-'S4% (4), (N R 4),[W (N O)2('S 0 2] (1) (R = Me (la), «-Bu (lb)), [W (NO)2('S4')] (2), [^ -0 {W (N 0)('S 4')}2] (3) and [W (N PR 3)(N O)('S4')] (5) (R = Me (5a), Et (5b)) were synthesized ('S2'2 = 1,2-benzenedithiolate(2—) ; 'S4'2 = 1,2-bis(2-mercaptophenyl-th io)ethane(2-)). la and lb result from the reductive nitrosylation o f Li2[W('S2')3] which was prepared by reduction o f [W('S2')3] with rc-BuLi. la was also obtained from [W (NO)2(Cl)2]", 'S2'2-and N M e4+. Alkylation o f la or lb by 1.2-dibromoethane yields 2, whose X-ray structure | | | |
Reference
| Z. Naturforsch. 46b, 1435—5 (1991); eingegangen am 8. A pril/ 8. Juli 1991 | | | |
Published
| 1991 | | | |
Keywords
| Chromium, Tungsten, Nitrosyl Complexes, Sulfur Ligands, X-Ray | | | |
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| default:Reihe_B/46/ZNB-1991-46b-1435.pdf | | | | Identifier
| ZNB-1991-46b-1435 | | | | Volume
| 46 | |
| 98 | Author
| Dieter Sellmann, Peter Lechner, Falk Knoch, M. Atthias, Moll | Requires cookie* | | | Title
| Übergangsmetallkomplexe mit Schwefelliganden | | | | Abstract
| , LXXIII. Diastereospezifische Dichlormethylierung schwefelreicher IRu'^SRR XPPh^yS/j-Komplexe (SRR' = einzähniger Thioether-oder Thiol-Ligand; 'S4'2-= l,2-Bis(2-mercaptophenylthio)ethan(2-))* Transition Metal Complexes with Sulfur Ligands, LXXIII. Diastereospecific Dichlorom ethylation of Sulfur Rich [Run(SR R')(PPh3)'S4'] Complexes (SR R' = M onodentate Thioether or Thiol Ligand; 'S4': ~ = 1,2-Bis(2-m ercaptophenylthio)ethane(2-)) Under exclusion o f air the thioether and thiol complexes [Ru(SRR')(PPh3)'S4'] ('S4'2-= l,2-bis(2-m ercaptophenylthio)ethane (2 -)) easily react with C H C l, yielding [Ru(Cl)(PPh,)('S4'-C H C L)] in which one thiolato atom o f the 'S4' ligand is diastereospecifical-ly dichloromethylated. In the presence o f air, however, [Rum(Cl)(PPh3)'S4'] is formed. The molecular structures o f [Ru(Cl)(PPh3)('S4'-C H C l:)]-2C H C l3 and [Rum(Cl)(PPh3)'buS4'] have been determined by X-ray crystallography. 'buS4'2-(= 1,2-bis(3,5-di(/-butyl)-2-m ercaptophenylthio)ethane(2-)) is the r-butyl derivative o f the 'S4' ligand. Reasons for ob served diastereospecifity o f alkylation are discussed. | | | |
Reference
| Z. Naturforsch. 46b, 1585 (1991); eingegangen am 3. Mai 1991 | | | |
Published
| 1991 | | | |
Keywords
| Transition Metal Sulfur Complexes, Diastereospecifity, Alkylation, X-Ray | | | |
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| default:Reihe_B/46/ZNB-1991-46b-1585.pdf | | | | Identifier
| ZNB-1991-46b-1585 | | | | Volume
| 46 | |
| 99 | Author
| Dieter Sellmann, Stefan Fünfgelder, Falk Knoch | Requires cookie* | | | Title
| Übergangsmetallkomplexe mit Schwefelliganden, LXXV | | | | Abstract
| Synthese und Struktur von INi('NHS4)|2 und |N i(Py)2('S2')| * Py; Radikalische Templatalkylierungen von |Ni('S2')2l2~** Transition Metal Complexes with Sulfur Ligands, LXXV* Syntheses and Structure of [Ni('NHS4')]2 and [Ni(Py)2('S2')] • Py; Radical Alkylations of [Ni('S2')2]: ** [N i('N HS4')]2 ('N nS4'2~ = 2,2'-bis(2-m ercaptophenylthio)diethylam ine(2-)) was synthesized from Ni(ac)-, and N a2-' N HS4' and characterized by X-ray structure analysis. In the solid state [N i('N HS4')]2 contains two pseudooctahedral [N i('N HS4')] fragments bridged via thiolate d o nors, in D M F solution at 110 C it dissociates into mononuclear entities. The product o f the template reaction between [Ni('S2')2]2~ ('S2'2-= 1,2-benzenedithiolate) and (BrC\H4)2NH was shown to contain an as yet unidentified by-product in addition to [Ni('NnS4')]2. Pure [N i('N HS4')]2 does not react with pyridine, but the template product forms [N i(Py)2('S2')] which has a square planar coordination geometry with the pyridine rings perpendicular to the N iS2N 2 plane. Investigation o f the template formation o f [N i('N HS4')]2 provided evidence that the reaction o f [Ni('S,')J--with (BrC2H4)^NH involves radicals, suggesting a radical chain reaction m echa nism. | | | |
Reference
| Z. Naturforsch. 46b, 1593—1600 (1991); eingegangen am 13. Mai 1991 | | | |
Published
| 1991 | | | |
Keywords
| Nickel Sulfur Complexes, X -Ray, Template Reaction | | | |
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| default:Reihe_B/46/ZNB-1991-46b-1593.pdf | | | | Identifier
| ZNB-1991-46b-1593 | | | | Volume
| 46 | |
| 100 | Author
| Oligophosphine Ligands, Xxxiv, Lutz Dahlenburg | Requires cookie* | | | Title
| Oligophosphan-Liganden, XXXIV** Organoplatin(II)-Komplexe mit (+ )-(l *S)-l,2-Bis(diphenylphosphino)- 1 -phenylethan-Koordination | | | | Abstract
| O rganoplatinum (II) Complexes with (+)-(1 5)-1,2-Bis(diphenylphosphino)-1-phenylethane Coordination A ndrea Saare Reaction o f (C8H 12)P t(C H 2C M e3)2 with (+)-(l S)-Ph2P CH (Ph)C H 2P Ph2, S-PHEPHO S, gave (5'-PH EPH O S)Pt(C H2C M e3)2 (1). Cleavage o f one o f the P t -C bonds o f this com pound with m ethanolic HC1 yielded (5-PH EPH O S)PtC l(CH 2C M e3) (2) which could be converted to (5-PH EPH O S)PtH (C H 2C M e3) (3) by treatment with N a[H B (O M e)3], The com plexes so ob tained were characterized by N M R spectroscopy (preferentially 31P) as well as by an X-ray structure analysis performed on the dineopentyl derivative 1. While thermal generation o f (S'-PHEPHOS)Pt(O) from 3 in the presence o f H C = C C (0)0 C M e 3 produced the alkyne co | | | |
Reference
| Z. Naturforsch. 47b, 247 (1992); eingegangen am 24. Juli 1991 | | | |
Published
| 1992 | | | |
Keywords
| Chiral Bis(phosphine) Ligand, Platinum Complexes, X -Ray, Thermolysis | | | |
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| default:Reihe_B/47/ZNB-1992-47b-0247.pdf | | | | Identifier
| ZNB-1992-47b-0247 | | | | Volume
| 47 | |
|
