| | 101 | Author
| Ekkehard Lindner, Günter Von Au | Requires cookie* | | | Title
| Darstellung und Eigenschaften von und Reaktionen mit metallhaltigen Heterocyclen, VII [1] Heterolytische Spaltung der Re-Re-Bindung in den Zweikern-Anionen [(OC)4ReP(R2 )0] 2 2 ~ mit Elektrophilen - ein Weg zu Heterocyclen mit Re-C-o-Bindung Preparation and Properties of, and Reactions with, Metal-Containing Heterocycles, VII [1] Heterolytic Cleavage of the Re-Re Bond in the Binuclear Anions [(0C)4ReP(R2)0]2 2_ with Electrophiles -a Pathway to Heterocycles with Re-C a Bonds  | | | | Abstract
| The preparation of the six-membered rhenacyclohexanes (OC)4ReP(R2)OCH2C(CH3)2CH2 (la, b) [R = CH3 (a), C6H5 (b)J is accomplished by heterolytic cleavage of the Re-Re bond in the binuclear anions [(0C)4ReP(R2)0]2 2 -with strong electrophiles like the alkane-diylbis(triflate) (CH3)2C(CH2Y)2 (Y= OSO2CF3), followed by an attack of the a>-positioned carbenium-like C atom on the phosphinite oxygen of the anion. 1 a, b insert SO2 under ring I I | | | |
Reference
| Z. Naturforsch. 35b, 1104—1110 (1980); eingegangen am 9. Mai 1980 | | | |
Published
| 1980 | | | |
Keywords
| Rhenacyclohexanes, Mechanism, S02-Insertio", X-ray, IR spectra, NMR spectra : | | | |
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| default:Reihe_B/35/ZNB-1980-35b-1104.pdf | | | | Identifier
| ZNB-1980-35b-1104 | | | | Volume
| 35 | |
| 102 | Author
| Ahmet Keçeci, Dieter Rehder | Requires cookie* | | | Title
| IR, 31 P-, 55 Mn-und 185 187 Re-NMR spektroskopische Untersuchungen an einigen Carbonylmangan-und -rhenium-Komplexen | | | | Abstract
| The IR and NMR spectra of the complexes [M(CO)e]Cl • HCl (M = Mn: 1, M = Re: 2), M(C0)5C02Et (M = Mn: 3, M = Re: 4), [Mn(CO)5PR3][PF6] (5; PR3 = PPh(OPh)2: a, P(n-Pr)3: b, PHPh2: c, PPh(NEt2)2: d, P(p-C6H4F)3: e), [Be(CO)5PHPh8][FF6] (6 c), Mn2(CO)s(PR3)2 (7) and Re2(CO)g(PHPh2)2 (8c) are discussed in the context of a-and ^-interactions in the metal-ligand system and compared with 51 V NMR data of the analogous isoelectronic and isostructural carbonylvanadates (—I). On the basis of these results, the phosphines are arranged in the order of decreasing integral ligand strength according to a>b>c>d. The 55 Mn shielding of 5 is greater than that of 1, which is explained by strong (x-interactions and correspondingly large e-ai* splitting dominating the paramagnetic deshielding term in the pseudooctahedral complexes of type 5. The only rhenium compound accessible to NMR is 2, for which the 185 Re and 187 Re resonances were obtained. 31 P coordination shifts are positive for all complexes. Spectroscopic data for 7c show that this complex presumably has the structure (CO)sMn-Mn(CO)3(PHPh2)2, contrasting 7 a, 7 b, 7d and 7e (local D4d symmetry). | | | |
Reference
| (Z. Naturforsch. 36b, 20—26 [1981]; eingegangen am 6. Oktober 1980) | | | |
Published
| 1981 | | | |
Keywords
| Carbonylphosphinemanganese, Car bony lphosphinerhenium, IR Spectra, Manganese NMR Spectra, Rhenium NMR Spectra | | | |
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| default:Reihe_B/36/ZNB-1981-36b-0020.pdf | | | | Identifier
| ZNB-1981-36b-0020 | | | | Volume
| 36 | |
| 104 | Author
| W. Preetz, H. Schulz | Requires cookie* | | | Title
| Darstellung und spektroskopische Charakterisierung von Tetrakis (chlor o -iodo ) oxalato -osmaten (IV ) | | | | Abstract
| On treatment of [OsLjox] 2-with Cl~ the mixed complexes [OsClnI4_nox] 2 -, n = 1, 2, 3, are formed. The isolation and complete separation of the differently coloured geometric isomers is achieved by ion exchange chromatography on diethylaminoethyl cellulose. The IR and Ra spectra are assigned according to point groups Czv, Cs, Ci. The mutual influence of ligands, especially by the high trans effect of I, is indicated by shifts of the distinct vibrational and electronic bands. The observed splittings of I -> Os transitions are attributed to the different groupings I-Os-I, I-Os-Cl, and I-Os-O, important for the distinction of stereoisomers. The CT-bands as well as the d-d-transitions show batho-chromic shifts with increasing number of I-ligands. Up to five spin-orbit components in the NIR region are well resolved. The assignment is improved by the electronic Ra spectra. The fine structure of some d-d-bands originates from coupling with symmetric vibrational modes. | | | |
Reference
| (Z. Naturforsch. 36b, 62—69 [1981]; eingegangen am 10. Oktober 1980) | | | |
Published
| 1981 | | | |
Keywords
| Tetrakis(chloro-iodo)oxalato-osmates(IV), UV-VIS-NIR Spectra, IR Spectra, Raman Spectra | | | |
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| default:Reihe_B/36/ZNB-1981-36b-0062.pdf | | | | Identifier
| ZNB-1981-36b-0062 | | | | Volume
| 36 | |
| 105 | Author
| Jürgen Hanich, Wolfgang Willing, Ulrich Müller, Kurt Dehnicke, Dieter Rehder | Requires cookie* | | | Title
| Cyclothiazeno-Vanadiumdibromid, VBr2(N3S2) Cyclo-Thiazeno Vanadium Dibromide, V B r2(N 3 S2) | | | | Abstract
| V B r 2(N 3S2) was synthesized by reaction o f VC12(N 3S2) with M e 3SiBr. It reacts with PPh4B r in dibromomethane solution to form (P P h 4) 2[V B r 3(N 3S2) ] 2. The compounds were characterized by their IR and 51V N M R spectra. The crystal structure o f V B r 2(N 3S2) was determined by X-ray diffraction (2060 reflexions, R = 0.114). Crystal data: triclinic, space group P I , a — 586.4, b = 794.2, c — 744.6 pm, a = 89.25, ß = 108.58, y — 99.67°, Z = 2. The vanadium atoms form planar, six-membered rings with the N 3S2 groups, with short V N distances (172 and 185 pm). Bromine-bridged dimers are associated via V —N links to form chains in a similar way as in some tetrahalides. The structure is similar to that o f VC12(N 3S2), but the chains are rotated by 17° along their axes. | | | |
Reference
| Z. Naturforsch. 40b, 1457—1462 (1985); eingegangen am 2. Juli 1985 | | | |
Published
| 1985 | | | |
Keywords
| Cyclo-Thiazeno Vanadium Dibrom ide, Synthesis, IR Spectra, 51V N M R Spectra, Crystal Structure | | | |
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| default:Reihe_B/40/ZNB-1985-40b-1457.pdf | | | | Identifier
| ZNB-1985-40b-1457 | | | | Volume
| 40 | |
| 106 | Author
| Wolfgang Willing, Ulrich Müller, Udo Dem, Kurt Dehnicke | Requires cookie* | | | Title
| Synthesen und Kristallstrukturen von PPh4[RuCl4(NO)(NSCl)] und (PPh4)2[RuCl4(NS)]2-4C H 2CI2 Syntheses and Crystal Structures of PPh4[RuCl4(NO)(NSCl)] and (PPh4)2[RuCl4(NS)]2-4 CH 2C12 | | | | Abstract
| By reaction o f trithiazylchloride, (NSC1)3, with PPh4[RuCl4(N O)]2 in dichlorom ethane the thiazylchloridenitrosyl com plex PPh4[RuCl4(N O)(N SC l)] is obtained; its vacuum pyrolysis at 2 0 0 -2 2 0 °C yields the thionitrosyl com plex (PPh4)2[RuCl4(N S)]2 which crystallizes from C H 2C12 solution with four m olecules o f CH 2C12. Both com pounds were charaterized by their IR spectra and by X-ray crystal structure determ inations. Crystal data: PPh4[RuCl4(N O)(N S C l)], m on o clinic, space group P 2 xln, Z = 4, a = 982.6, b = 1700.0, c = 1772.3 pm , ß = 104.79° (2548 observed reflexions, R = 0.046); (PPh4)2[RuCl4(N S)]2-4 C H 2C12, triclinic, P I , Z = 1, a = 952.9, b = 1380.0, c — 1458.5 pm , a — 112.91, ß = 106.67, y = 92.61° (3760 observed reflexions, R = 0.053). In the [RuCl4(N O)(N S C l)]e ion the nitrosyl and thiazyl chloride ligands occupy e x positions; bond lengths indicate double bonds in the linear Ru = N -0 group, while the NSC1 m olecule is attached by a donor-acceptor interaction R u -N = S -C l , although with a rather short Ru —N bond o f 198 pm (N = S 144 pm, S —Cl 213 pm). The centrosymm etric [RuC14(N S)]220 ions have chloro bridges and NS ligands in axial positions; the nearly linear R u = N = S group has bond lengths R u = N 175 pm and N = S 147 pm. | | | |
Reference
| Z. Naturforsch. 41b, 560 (1986); eingegangen am 29. Januar 1986 | | | |
Published
| 1986 | | | |
Keywords
| Thionitrosyl and Thiazylchloride C om plexes o f Ruthenium, Syntheses, IR Spectra, Crystal Structure | | | |
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| default:Reihe_B/41/ZNB-1986-41b-0560.pdf | | | | Identifier
| ZNB-1986-41b-0560 | | | | Volume
| 41 | |
| 108 | Author
| Hans-Günter Hauck, W. Olfgang, Willing, Ulrich Müller, Kurt Dehnicke | Requires cookie* | | | Title
| Brom-und Chlorthionitrenkomplexe des Rheniums Die Kristallstruktur von (PPh4)2[ReBr4(N S)(N SBr)] *CH2Br2 Bromo-and Chlorothionitrene Complexes of Rhenium The Crystal Structure of (PPh4)2[ReBr4(NS)(NSBr)] ■ C H 2B r2 | | | | Abstract
| The thionitrosyl-halothionitrene com pounds (PPh4)2[R eX 4(N S)(N S X)]-2 C H 2X 2, X = Cl or Br, are obtained by nucleophilic ring cleavage o f the R e(N 2S2) rings o f com plexes [R eX 4(N 2S2)]e with PPh4X in C H 2X 2. (A sP h4)2[R eC l4(N S)(N SC l)] • C H 2C12 can also be obtained by the reaction | | | |
Reference
| Z. Naturforsch. 41b, 825 (1986); eingegangen am 7. März 1986 | | | |
Published
| 1986 | | | |
Keywords
| Bromo- and Chlorothionitrene Complexes of Rhenium, Synthesis, IR Spectra, Crystal Structure | | | |
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| default:Reihe_B/41/ZNB-1986-41b-0825.pdf | | | | Identifier
| ZNB-1986-41b-0825 | | | | Volume
| 41 | |
| 109 | Author
| Somluck Ruangsuttinarupap, Claus Friebel, Kurt Dehnicke | Requires cookie* | | | Title
| Synthese, IR-, EPR-und Elektronenspektren der Dischwefel-dinitrid-Komplexe [CUC1 2 (CH 3 CN)] 2 -(/I-S 2 N 2 ) und [CuCl 2 ] 2 * (/I-S 2 N 2 ) Synthesis, IR, EPR, and Electronic Spectra of the Disulfur Dinitride Complexes [CUC1 2 (CH 3 CN)] 2 * (w-S 2 N 2 ) and [CuCl 2 ] 2 -(w-S 2 N 2 ) | | | | Abstract
| [CuCl 2 (CH 3 CN)] 2 -(W-S 2 N 2) is prepared by the reaction of trithiazyl chloride with CuCl in acetonitrile solution. Thermolysis at 120 °C yields [CuCl 2 ] 2 -(W-S 2 N 2). The complexes are charac-terized by their IR, EPR, and electronic spectra. | | | |
Reference
| Z. Naturforsch. 42b, 337—340 (1987); eingegangen am 24. November 1986 | | | |
Published
| 1987 | | | |
Keywords
| Disulfur Dinitride Complexes of Copper(II), EPR Spectra, Electronic Spectra, Synthesis, IR Spectra | | | |
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| default:Reihe_B/42/ZNB-1987-42b-0337.pdf | | | | Identifier
| ZNB-1987-42b-0337 | | | | Volume
| 42 | |
| 110 | Author
| W. Preetz, H.N V Allwörden | Requires cookie* | | | Title
| Darstellung und Schwingungsspektren von Chloro-Bromo-Ruthenaten(IV) einschließlich der Stereoisomeren Preparation and Vibrational Spectra of Chloro-Bromo-Ruthenates(IV) Including Stereoisomers | | | | Abstract
| The mixed chloro-bromo complexes [RuCl"Br 6 _"] 2_ , n = 1—5, have been separated for the first time by ion exchange chromatography on diethylaminoethylcellulose. Due to the stronger trans-effect of Br compared with Cl, on treatment of [RuBr 6 ] 2 ~ with Cl" in the presence of Br 2 nearly pure ciy//ac-isomers,andbyreactionof [RuCl 6 ] 2 " withBr"/Br 2 nearlypurerran5/mer-isomersforn = 2,3,4 are formed. The vibrational spectra of the mixed ligand complexes are completely assigned according to point groups D 4h , C 4v , C 3v and C 2v , respectively. The bands are observed in the characteristic regions: v(RuCl): 340-270 > v(RuBr): 245-190 > <3(ClRuCl): 170-140 > ö(ClRuBr) > <3(BrRuBr): 125—90 > v L : < 100 cm" 1 . The lower stability of the hexahalogeno complexes of Ru(IV), 4d, compared with the homologous complexes of Os(IV), 5d, is confirmed by a decrease of the force field constants by approximately 15%. | | | |
Reference
| Z. Naturforsch. 42b, 381—386 (1987); eingegangen am 18. Dezember 1986 | | | |
Published
| 1987 | | | |
Keywords
| Chloro-Bromo-Ruthenates(IV), Stereoisomers, r/wis-Effect, IR Spectra, Raman Spectra | | | |
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| default:Reihe_B/42/ZNB-1987-42b-0381.pdf | | | | Identifier
| ZNB-1987-42b-0381 | | | | Volume
| 42 | |
| 111 | Author
| Guido Effinger, WolfgangH. Iller, Ingo-Peter Lorenz | Requires cookie* | | | Title
| Reaktionen | | | | Abstract
| von Silylphosphanen mit Halogenokomplexen von Übergangsmetallen: Synthese, Struktur und Eigenschaften von Komplexen des Typs cis-X(CO)4Mn{PPh3 _"(SiMe3)/I} (n = 1 -3) und [{Cp(CO)2Fe}2PPhR]X (R = Ph, H) bzw. [{Cp(CO)2Fe}3PH]X (X = CI, Br, I) Reactions of Silylphosphanes with Halogeno Complexes of Transition Metals: Synthesis, Structure and Properties of Complexes c«-X (C O)4 M n{PPh3 _"(SiMe3)"} (n = 1 -3) , [{Cp(CO)2Fe}2 PPhR]X (R = Ph, H) and [{Cp(CO)2Fe}3 PH]X (X = Cl, Br, I) The reactions o f pentacarbonylm anganese halides (C O)5M nX (X = Cl, Br, I) with the silyl phosphanes Ph3_"P(SiMe3)" (n = 1—3) at am bient temperature result in the elimination o f one CO ligand and the formation o f cw-configurated substitution products X (C O)4M n{PPh3_"(SiMe3)"}. N o CO -substitution, but M e3SiX-elim ination is observed in the reaction of Ph3_"P(SiMe3)" with the dicarbonylcyclopentadienyliron halides C pFe(C O)2X to give the di-and triferriophosphonium halides [{C p (C O)2F e}2P PhR ]X (R = Ph, H) and [{C p(C O)2F e }3PH]X (X = Cl, Br, I). The mass, IR and NM R spectra are reported and discussed. The crystal structures o f cz's-I(CO)4M nPPh2SiM e3 and [{C p (C O)2F e}2PPh2]I have been determined. | | | |
Reference
| Z. Naturforsch. 42b, 1315 (1987); eingegangen am 30. April 1987 | | | |
Published
| 1987 | | | |
Keywords
| Trimethylsilyl Phosphanes, Substitution R eactions, T etracarbonylhalogenom anganese C om plexes, H alogenosilane Elim ination, IR Spectra | | | |
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| default:Reihe_B/42/ZNB-1987-42b-1315.pdf | | | | Identifier
| ZNB-1987-42b-1315 | | | | Volume
| 42 | |
| 112 | Author
| Dieter Fenske, Karin Völp, Kurt Dehnicke | Requires cookie* | | | Title
| N-Chlor-Nitrenokomplexe des Molybdäns: M oF4(NC1) und [C H 3C N -M oF4(N C 1)] N-Chloro-Nitrene Complexes o f Molybdenum: M oF 4(NC1) and [C H 3C N -M o F 4(NC1)] | | | | Abstract
| MoF4(NC1) has been prepared as a yellow crystal powder by the reaction of diluted fluorine with MoCl3(N 3S2) at room temperature. The compound is associated via fluorine bridges, accord ing to the IR spectrum. With acetonitrile, the monomeric complex [CH3CN —MoF4(NC1)] is obtained, which was characterized by its IR and l9F N M R spectra as well as by an X-ray structure determination. Crystal data: space group Pm, Z — 2 (1068 observed, independent reflexions, R — 0.03). Lattice dimensions at —90 °C: a — 507.1. b = 704.8, c = 995.8 pm, ß — 102.02°. The unit cell contains two crystallographically independent molecules [CH3CN —MoF4(NC1)], the M o = N —Cl groups being linear (bond angles 176°, 178°) with bond lengths MoN = 172 and NCI = 159. 162 pm. In the trans position to the MoNCl group, the nitrogen atom of the acetonitrile molecule is coordinated. | | | |
Reference
| Z. Naturforsch. 42b, 1398—1402 (1987); eingegangen am 2. Juli 1987 | | | |
Published
| 1987 | | | |
Keywords
| IR Spectra, I9F N M R Spectra, X-Ray, N-Chloro-Nitrene-Molybdenum Tetrafluoride, Acetonitrile Adduct | | | |
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| default:Reihe_B/42/ZNB-1987-42b-1398.pdf | | | | Identifier
| ZNB-1987-42b-1398 | | | | Volume
| 42 | |
| 113 | Author
| Astrid Görge, Kurt Dehnicke, Dieter Fenske | Requires cookie* | | | Title
| N-Chlornitrenokomplexe des Wolframs: WC1 4 (NC1) und [CH 3 CN-WC1 4 (NC1)] N-Chloro-Nitrene Complexes of Tungsten: WC1 4 (NC1) and [CH 3 CN-WC1 4 (NC1)] | | | | Abstract
| WC1 4 (NC1) has been prepared as a red-brown crystal powder by the reaction of tungsten hexacarbonyl with excess nitrogen trichloride in boiling CC1 4 . The complex is associated via chloro bridges, forming dimeric units, according to the IR spectrum. Thermal decomposition at 200 °C leads to tungsten nitride trichloride, WNC1,. With acetonitrile, WC1 4 (NC1) reacts with formation of the monomeric complex [CH,CN-WC1 4 (NC1)], which was characterized by its IR spectrum as well as by an X-ray structure determination. Crystal data: space group P2,/m, Z = 2 (1387 independent observed reflexions, R — 0.07). Lattice dimensions at 20 °C: a = 590.4(3), b = 729.0(3), c = 1124.6(4) pm, ß = 100.63(2)°. The complex forms monomeric molecules, in which the tungsten atom has a distorted octahedral environment of four chlorine atoms in equatorial positions, and the acetonitrile molecule in fram-position to the W=N —Cl group. Bond lengths WN = 172 and NCI -161 pm; bond angle WNC1 = 175.5°. | | | |
Reference
| Z. Naturforsch. 43b, 677—681 (1988); eingegangen am 26. Januar 1988 | | | |
Published
| 1988 | | | |
Keywords
| Synthesis, IR Spectra, X-Ray, N-Chloro-Nitrene-Tungsten Tetrachloride, Acetonitrile Adduct | | | |
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| default:Reihe_B/43/ZNB-1988-43b-0677.pdf | | | | Identifier
| ZNB-1988-43b-0677 | | | | Volume
| 43 | |
| 114 | Author
| Karin Völp, Gerhard Baum, Werner Massa, Kurt Dehnicke | Requires cookie* | | | Title
| [Na-15-Krone-5][MoF 2 Cl2(N 3 S2)]; Synthese und Kristallstruktur [Na-15-Crown-5][MoF 2 Cl 2 (N 3 S 2 )]; Synthesis and Crystal Structure | | | | Abstract
| The cyclothiazeno complex [Na-15-crown-5][MoF 2 Cl 2 (N 3 S 2)] has been prepared by the reaction of sodium fluoride with [MOC1 3 (N 3 S 2)] 2 in acetonitrile solution in the presence of [15-crown-5], The compound was characterized by its IR spectrum as well as by an X-ray structure determina-tion (3560 observed independent reflexions, R = 0.039). Crystal data: monoclinic, P2,//?, Z = 4; a = 1044.8(2); b = 1513.7(2); c = 1363.8(3) pm; ß = 104.33(2)°. The structure consists of ion pairs, in which the sodium atom is seven-coordinated by the oxygen atoms of the crown ether molecule and by the two fluorine ligands of the [MOF 2 C1 2 (N 3 S 2)]~ unit. The molybdenum atom is a member of the planar MON 3 S 2 ring; the fluorine atoms are coordinated in trans position to the nitrogen atoms of the cyclothiazeno ring. | | | |
Reference
| Z. Naturforsch. 43b, 1235—1239 (1988); eingegangen am 7. Juni 1988 | | | |
Published
| 1988 | | | |
Keywords
| Fluoro-Chloro-Cyclothiazeno Complex of Molybdenum(VI), Synthesis, IR Spectra, Crystal Structure | | | |
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| default:Reihe_B/43/ZNB-1988-43b-1235.pdf | | | | Identifier
| ZNB-1988-43b-1235 | | | | Volume
| 43 | |
| 115 | Author
| P. E. Rlhöfer, W. Preetz | Requires cookie* | | | Title
| Darstellung und Schwingungsspektren der 35CI/37Cl-markierten Fluoro-Chloro-Platinate(IV) Preparation and Vibrational Spectra of 35C1/ Cl Labelled Fluoro-Chloro-Platinates(IV) | | | | Abstract
| A ll com ponents of the two series Cs2[PtF"35Cl6_"] and Cs2[PtF"37ClA_"], including the pairs of geom etric isomers for n = 2 ,3 , 4, have been prepared and isolated by ion exchange chrom atogra phy on D E A E cellulose. The highly resolved low temperature (80 K) IR and Raman spectra of the pure isotopom ers show distinctive isotopic shifts for different vibrational m odes up to 10 cm -1 . The excellent agreem ent o f the observed values with Teller-R edlich calculations verifies the assignm ent of all stretching and especially o f the narrow deform ation bands. For trans -com plexes containing C l—P t— Cl axes, the lowered of mutual exclusion. | | | |
Reference
| Z. Naturforsch. 44b, 619 (1989); eingegangen am 8. Februar 1989 | | | |
Published
| 1989 | | | |
Keywords
| Fluoro-C hloro-Platinates(IV ), Isotopom ers, Teller-Redlich Calculation, IR Spectra, Raman Spectra | | | |
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| default:Reihe_B/44/ZNB-1989-44b-0619.pdf | | | | Identifier
| ZNB-1989-44b-0619 | | | | Volume
| 44 | |
| 116 | Author
| JohnDavid Kildea, Wolfgang Hiller, Beatrice Borgsen, Kurt Dehnicke | Requires cookie* | | | Title
| Synthese, IR-Spektrum und Kristallstruktur des Amidinatokomplexes [N a(15-K rone-5)][Ph—C(NSiM e3)2SnCl3F] Synthesis, IR Spectrum, and Crystal Structure of the Amidinato Complex [N a(15-Crow n-5)][Ph-C(N SiM e3)2SnCl3F] | | | |
Reference
| Z. Naturforsch. 44b, 889 (1989); eingegangen am 30. März 1989 | | | |
Published
| 1989 | | | |
Keywords
| N, N '-Bis(trim ethylsilyl)am idinato C om plex, Synthesis, IR Spectra, Crystal Structure | | | |
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| default:Reihe_B/44/ZNB-1989-44b-0889.pdf | | | | Identifier
| ZNB-1989-44b-0889 | | | | Volume
| 44 | |
| 117 | Author
| PeterH. Ofacker, Claus Friebel, Kurt Dehnicke, Petra Bäuml, Wolfgang Hiller, Joachim Strähle | Requires cookie* | | | Title
| Über die Reduktion von Alkinkomplexen des Molybdäns und Wolframs in hohen Oxidationsstufen. Die Kristallstruktur von MoCI3(THF)3 On the Reduction of Alkyne Complexes of M olybdenum and Tungsten in High Oxidation States. The Crystal Structure of MoC13(T H F)3 | | | | Abstract
| The reduction of the tungsten alkyne complexes [WC14(R C = C R)]2 (R — Ph. SiMe3) with cobaltocen in T H F solutions leads to the complexes [CoCp2]2[WCl4(R C = C R)]2 (R = Ph (i); R — SiMe3 (2)), as green, oxygen sensitive crystalline powders. Reduction of [WCl4(M e3SiC =C SiM e3)]2 and of[M oC l4(P hC = C P h)]2 with sodium naphthalide in T H F solutions in the presence of 15-crown-5 gives [Na-15-crown-5]3[W2Cl9], and MoC13(T H F)3, respectively. All compounds have been characterized by IR spectroscopy, and 1 and 2, in addition, by their E PR spectra. The crystal structure of MoC13(T H F)3 was determ ined by X-ray m ethods. Space group P2,/c, Z — 4, 2642 observed unique reflexions, R = 0.050. Lattice dim ensions at 20 °C: a = 888.4(2), b = 1281.5(3), c = 1535.2(3) pm, ß = 92.17(2)°. The com pound forms m onom eric octahedral molecules with a meridional arrangem ent of the ligands. | | | |
Reference
| Z. Naturforsch. 44b, 1161 (1989); eingegangen am 28. Juni 1989 | | | |
Published
| 1989 | | | |
Keywords
| Alkyne Complexes of Molybdenum and Tungsten, R eduction, E PR Spectra, Crystal Structure, IR Spectra | | | |
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| default:Reihe_B/44/ZNB-1989-44b-1161.pdf | | | | Identifier
| ZNB-1989-44b-1161 | | | | Volume
| 44 | |
| 119 | Author
| Fluoro, Petra Neumann, K. Urt Dehnicke, Dieter Fenske, G.Erhard Baum | Requires cookie* | | | Title
| Fluoro-, Chloro-und Bromo-Wolfram(VI)-Alkinkomplexe. Die Kristallstrukturen von [K(18-Krone-6)l[WF5( P h -C = C -H ) | * CH3CN und | WCl4( P h -C = C -S e -/ i -C 4H 9)(C H 3CN)| | | | | Abstract
| -, Chloro-, and Bromo-Tungsten(VI) Alkyne Complexes. The Crystal Structures of [K(18-Crown-6)][WF5(P h ~ C = C -H)] • C H 3CN and [WCl4(P h -C = C -S e -w -C 4 H9)(CH 3CN)] Several tungsten alkyne complexes o f the type [WC14(R -C = C -H) ] 2 and [WC14(R -C = C -R') ] 2 have been prepared by reactions o f WC16 with the alkynes in the presence o f C2C14. Treat ing with BrSiMe3 leads to corresponding bromo com plexes, whereas reactions o f N aF and KF, respectively, in acetonitrile solution in the presence o f crown ethers yield the fluoro complexes [N a(l 5-crown-5)][WFs(R -C = C -R ') ] and [K(18-crown-6)][W F5(R -C = C -R ') ] , respectively. All complexes were characterized by IR and l3C N M R spectroscopy. The crystal structures o f [K(18-crown-6)][W F5(P h -C = C -H) ] C H 3CN and [WCl4(P h -C = C -S e -« -C 4 H9)(C H 3C N)] have been determined by X-ray methods. [K(18-crown-6)][W F5(P h -C = C -H ] C H 3 CN: Space group P 2,, Z = 2, 8555 observed unique reflections, R = 0.034. Lattice dim ensions at -7 0 °C: a = 1199.4(3), b = 893.4(2), c = 1351.8(3) pm, ß = 109.73(3)°. The com pound forms ion pairs via three K -F contacts with bond lengths o f 262.0, 282.7, and 293.3 pm; the potassium ion is thus nine-fold coordinated by the six oxygen atoms o f the crown ether molecule and by three fluoride ligands. The alkyne ligand is bonded side on to the tungsten atom o f the [W F5(P h -C = C —H)] unit with WC bond lengths o f 202.4 and 202.6 pm, respectively. [WCl4(P h -C = C -S e -t t -C 4 H9)(C H 3C N)]: Space group P 2 Ja, Z = 4, 4595 observed unique reflections, R = 0.058. Lattice dim ensions at -7 0 °C: a = 1030.3(5), b = 1596.3(9), c = 1170.9(7) pm, ß = 104.28(3)°. The com pound has a molecular structure, in which the tungsten atom is seven-fold coordinated by four chloride ligands, by the two alkyne carbon atom s (WC bond lengths 200 and 203 pm), and in trans position to the latter by the nitrogen atom o f the acetonitrile molecule with a W -N bond length o f 226 pm. | | | |
Reference
| Z. Naturforsch. 46b, 999—1010 (1991); eingegangen am 4. Februar 1991 | | | |
Published
| 1991 | | | |
Keywords
| Tungsten Alkyne Complexes, Synthesis, IR Spectra, 13C N M R Spectra, Crystal Structure | | | |
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| default:Reihe_B/46/ZNB-1991-46b-0999.pdf | | | | Identifier
| ZNB-1991-46b-0999 | | | | Volume
| 46 | |
| 120 | Author
| Alfred Zinn, Henning Von Arnim, Werner Massa, Michael Schäfer, Jürgen Pebler, K. Urt Dehnicke | Requires cookie* | | | Title
| [P h -C ( | | | | Abstract
| N S iM e3)2]2FeO ; ein Amidinatokomplex von Eisen(III) mit verzerrt trigonal-bipyramidaler Struktur [P h -C (N S iM e3)2]2FeCl; an Amidinato Complex o flro n (III) with a Distorted Trigonal-Bipyramidal Structure The am idinato complex [P h -C (N S iM e3)2]2FeCl has been prepared by the reaction o f FeOCl with the amidine P h -C (N S iM e3)[N(SiM e3)2] in acetonitrile/THF in the form o f dark red m ois ture sensitive single crystals. The complex was characterized by IR spectroscopy, by its 57Fe-M össbauer spectra, as well as by an X-ray structure determination. Space group P i, Z = 2, 3180 observed unique reflections, R = 0.068. Lattice dimensions at -8 0 C: a = 1210.4(2), b = 1272.7(3), c = 1316.0(3) pm; a = 67.81(3)°, ß = 76.14(3)°, y = 67.19(3)°. The com plex has a molecular structure in which the iron atom is surrounded in a distorted trigonal-bipyramidal fashion with the chlorine ligand and two nitrogen atoms o f different amidinato chelates in equatorial positions. The remaining nitrogen atom s occupy the apical positions. | | | |
Reference
| Z. Naturforsch. 46b, 1300 (1991); eingegangen am 28. Februar 1991 | | | |
Published
| 1991 | | | |
Keywords
| Am idinato Complex o f Iron, Synthesis, IR Spectra, 57Fe M össbauer Spectra, Crystal Structure | | | |
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| default:Reihe_B/46/ZNB-1991-46b-1300.pdf | | | | Identifier
| ZNB-1991-46b-1300 | | | | Volume
| 46 | |
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