| | 1 | Author
| Dieter Fenske, Eberhard Böhm, Kurt Dehnicke, Joachim Strähle | Requires cookie* | | | Title
| N-TrimethylsilyMminotriphenylphosphoran-Kupfer(II)-chlorid, (Me 3 SiNPPh 3 * CuCl 2 ]2 Synthese und Kristallstruktur N-Trimethylsilyl-iminotriphenylphosphorane Copper(II) Chloride, [Me 3 SiNPPh 3 * CuCl : ] 2 Synthesis and Crystal Structure  | | | | Abstract
| The title compound has been prepared by the reaction of N-trimethylsilyl-iminotriphenylphos-phorane with copper(II) chloride in boiling CCl 4 /C 2 H 5 OH, and forms moisture sensitive crystals, which are green in transmittance and black in reflexion. [Me 3 SiNPPh 3 • CuCl 2 ] 2 was characterized by its IR spectrum as well as by a crystal structure determination (4197 observed, independent reflexions, R = 0.049). The lattice dimensions are at 20 °C: a = 1102.7. b = 1407.3. c = 1560.2 pm; ß = 94.27°; space group P2,/« with two formula units in the unit cell. The complex consists of centrosymmetric, dimeric molecules with a planar Cu 2 Cl 2 ring (Cu —CI bond lengths 229 and 231 pm). A terminally bonded CI atom (Cu —CI = 221 pm) and the N atom of the Me,SiNPPh 3 ligand (Cu —N = 198.5 pm) complete the coordination number four of the nearly planar surroundings of the Cu atoms. | | | |
Reference
| (Z. Naturforsch. 43b, 1 [1988]; eingegangen am 4. September 1987) | | | |
Published
| 1988 | | | |
Keywords
| N-Trimethylsilyl-iminotriphenylphosphorane Copper(II) Chloride, Synthesis, IR Spectra, Crystal Structure | | | |
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| default:Reihe_B/43/ZNB-1988-43b-0001.pdf | | | | Identifier
| ZNB-1988-43b-0001 | | | | Volume
| 43 | |
| 2 | Author
| Andrea Maurer, Dieter Fenske, Johannes Beck, Wolfgang Hiller, Joachim Strähle, Eberhard Böhm, Kurt Dehnicke | Requires cookie* | | | Title
| Kupfer(I)-chlorid-Addukte von Phosphoraniminen Die Kristallstrukturen von Ph 3 PNPh * CuCl und von 2,3-Bis(triphenylphosphoranylidenamino)maIeinsäure-N-methylimid- Kupfer(I)-chlorid Copper(I) Chloride Adducts of Phosphoranimines The Crystal Structures of Ph 3 PNPh-CuCl and of 2,3-Bis(triphenylphosphoranylideneamino)maleic Acid N-Methylimide Copper(I) Chloride | | | | Abstract
| The title compounds Ph,PNPhCuCl (1) and (Ph,P) 2 N : C 4 0 2 (NMe) CuCl (2) have been prepared by the reactions of CuCl with the corresponding phosphoranimines Ph 3 PNPh and 2.3-bis(triphenylphosphoranylideneamino)maleic acid N-methylimide, respectively. Both com-plexes were characterized by their IR spectra as well as by crystal structure determinations. PhiPNPh • CuCl (1): space group PI, Z = 4, 3639 independent observed reflexions, R = 0.038. Lattice dimensions (18 °C): a = 1047.6; b = 1251.5; c = 1755 pm; a = 103.43°; ß = 97.24°; y = 101.30°. The compound forms monomeric molecules; the asymmetric unit contains two crystallo-graphically independent molecules. The CuCl molecule is bonded via the N atom of the phos-phoranimine. Bond lengths: Cu—N = 189 pm; Cu —CI = 209 pm; bond angle N —Cu —CI = 177°. (PhiP),NiC 4 Oi(NMe) CuCl (2): space group Pbca, Z = 8, 5611 independent, observed reflex-ions, R = 0.069. Lattice dimensions (25 °C): a = 1224.3; b = 1962.5: c = 2994.0 pm. The compound forms monomeric molecules with the CuCl molecule bonded via one of the N atoms of the phosphoranimine groups. Bond lengths: Cu—N = 194 pm; Cu—CI = 212 pm; bond angle N—Cu —CI -175°. | | | |
Reference
| (Z. Naturforsch. 43b, 5—11 [1988]; eingegangen am 4. September 1987) | | | |
Published
| 1988 | | | |
Keywords
| Copper(I) Chloride Adducts of Phosphoranimines, Synthesis, IR Spectra Crystal Structure | | | |
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| default:Reihe_B/43/ZNB-1988-43b-0005.pdf | | | | Identifier
| ZNB-1988-43b-0005 | | | | Volume
| 43 | |
| 3 | Author
| Dieter Fenske, Thomas Godemeyer, Kurt Dehnicke | Requires cookie* | | | Title
| |i-Nitridokomplexe von Wolfram(V) | | | | Abstract
| Die Kristallstruktur von (PPh^^CM/fj-NMOM^-NCl)^-1,5 CH 2 C1 2 w-Nitrido Complexes of Tungsten(V) The Crystal Structure of (PPh 4) 2 [W 3 Cl 9 (wrN)(0)(/< 2 -NCl)] 2 • 1,5 CH 2 C1 2 /<-Nitrido Complexes of Tungsten(V), Synthesis, IR Spectra, Crystal Structure W ; NC1 7 has been prepared by the reaction of tungsten pentachloride with the bromide of Millon's base, [Hg 2 N]Br, in boiling CC1 4 . The product forms a dark brown, moisture sensitive crystal powder (« eff = 0.7 B.M. at 21 °C). With phosphoryl chloride, the complex W 2 NCl 7 -2 POCl 3 is formed. The reaction with chlorine leads to the mixed-valenced W(V)/W(VI) complex W 2 NC1 8 (// eff = 0.5 B.M. at 22 °C), which reacts with tetraphenylphosphonium chloride in CH 2 C1 2 to form (PPh 4) 2 [W 2 NCl 10 ] -2CH 2 C1 2 . The reactions of W 2 NC1 7 with PPh 4 Cl in molar ratios in CH^C1 2 solution lead to several complexes; one of them was identified bv X-ray diffraction methods to be"(PPh 4) 2 [W,Cl 9 (w 3 -N)(0)(« 2 -NCl)] 2 -1,5 CH 2 C1 2 , which forms black crystals. The compound crystallizes monoclinically in the space group P2 Jn with two formula units per unit cell (7318 observed, independent reflexions, R = 0.083). The lattice dimensions are (20 °C): a = 994.4; b = 2673; c = 1518.2 pm; ß = 101.00°. The compound consists of PPh 4 ® cations and centrosymmetric anions [W,Cl 9 Cu 3 -N)(0)(« 2 -NCl)] 2 2e . The tungsten atoms form a scalene tri-angle with WW bond lengths of 282 and 278 pm, respectively. The hypothenuse of this triangle is a nearly linear W-N —W bridge with WN distances of 199 and 182 pm. One of the WW edges is bridged by a //-NCI group with WN bond lengths of 196 und 189 pm. respectively. | | | |
Reference
| (Z. Naturforsch. 43b, 12—20 [1988]; eingegangen am 21. September 1987) | | | |
Published
| 1988 | | | |
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| default:Reihe_B/43/ZNB-1988-43b-0012.pdf | | | | Identifier
| ZNB-1988-43b-0012 | | | | Volume
| 43 | |
| 4 | Author
| A. Schliephake, H. Falius, H. Buchkremer-Hermanns, P. Böttcher | Requires cookie* | | | Title
| Darstellung und Kristallstruktur des Bis(triethylammonium)octasulfids, [HN(C 2 H 5 ) 3 ] 2 S 8 Preparation and Crystal Structure of the Bis(triethylammonium)octasulfide, [HN(C 2 H 5 ) 3 ] 2 S 8 | | | | Abstract
| The preparation and crystal structure of the first octasulfide is described. The reaction of triethylamine, sulfur and dihydrogen sulfide in a solution of formamide yields orange-red crystals of bis(triethylammonium)octasulfide. The crystals are orthorhombic, space group Pbcn. with 4 molecules per unit cell. The cell constants are a = 23.709(4) Ä. b = 13.276(4) Ä. c = 7.388(2) A. The chains of sulfur, S 8 2 ^, do not show the common helical all-trans conformation, but a mixed sequence with the signs of the dihedral angles (-M h+ and 1). | | | |
Reference
| (Z. Naturforsch. 43b, 21—24 [1988]; eingegangen am 12. August/14. Oktober 1987) | | | |
Published
| 1988 | | | |
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| default:Reihe_B/43/ZNB-1988-43b-0021.pdf | | | | Identifier
| ZNB-1988-43b-0021 | | | | Volume
| 43 | |
| 5 | Author
| Christiane Löwe, Gottfried Huttner, Laszlo Zsolnai, Heinz Berke | Requires cookie* | | | Title
| Acetalisierte Formylmangan-Komplexe Acetals of Formyl Manganese Complexes | | | | Abstract
| Acetal complexes of the type (OC) 5 MnCH(XR) 2 , RX = PhO (la), (RX) 2 = 1,2-dioxybenzene (lb), (RX), = S-(CH,),-S (2) and (OC),[P(OCH,),],MnCHS-(CH,),-S (5) were synthesized. Glyoxyloyl acetal derivatives (0C) 5 MnC(0)CH(XR) 2 . RX = PhO (3a), (RX) 2 = 1,2-dioxyben-zene (3b), (RX) 2 = S-(CH 2),-S (4) were obtained by the action of NaMn(CO) 5 upon the corresponding acid chlorides or anhydrides, la can be transformed to 3a by CO insertion, la has been characterized by an X-ray structure determination. | | | |
Reference
| (Z. Naturforsch. 43b, 25—30 [1988]; eingegangen am 31. Juli/9. Oktober 1987) | | | |
Published
| 1988 | | | |
Keywords
| Acetals, Thioacetals, Formyl and Glyoxyloyl Manganese Carbonyl Complexes X-Ray | | | |
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| default:Reihe_B/43/ZNB-1988-43b-0025.pdf | | | | Identifier
| ZNB-1988-43b-0025 | | | | Volume
| 43 | |
| 6 | Author
| Franjo Gol, Gerd Hasselkuß, PeterC. Knüppel, Othmar Stelzer | Requires cookie* | | | Title
| Lineare Oligophosphaalkane, XX [1] Alkalimetall-und Trimethylsilylderivate PH-funktioneller Methylenbisphosphane Linear Oligophosphaalkanes, XX [1] Alkali Metal and Trimethylsilyl Derivatives of PH-Functional Methylenebisphosphanes | | | | Abstract
| The synthesis of the trimethylsilyl derivatives of the PH-functional methylenebisphosphanes, R 2 ^"(Me 3 Si)"P—CH 2 —PR(SiMe 3) (R = Me. /Pr. tBu. Ph. 2.4.6-Me 3 C (,H 2 ; n = 0. 1) is reported. In the Li-phosphides R 2 _"Li"P — CH 2 — PUR used as reactive intermediates, a monomer-oligomer association equilibrium causes a rapid Li-exchange as indicated by the solvent and temperature dependent ^PI'H} and 7 Li NMR spectrum of (/Pr) 2 P-CH 2 -P(/Pr)Li in various solvents (Et : 0. THF and MTHF) in the temperature range from 30 to -110 °C. For the syntheses of the Me-and Ph-substituted PH-functional methylenebisphosphanes R 2 P-CH 2 -PRH and RHP-CH 2 -PRH (R = Me, Ph) the chlorophosphane CKP —CH 2 —PC1 2 is used as a starting material. Bifunctional substituents (Ph —N—N —Ph and Me —N—CO —N—Me) are employed for the first time as protect-ing groups to block one or two PCl-functions in C1T—CIL—PCI-,. Cleavage of the PN-bonds in the five membered ring systems RP-CH 2 -PR-N(Ph)-N (Ph) (R = Me. Ph) with HCl affords the P-substituted methylenebis-chlorophosphanes RC1P—CH 2 — PC1R in satisfactory yields. The compounds have been characterized by 'H. I3 C{ 'H} and 3! F*{'H}NMR spectroscopy. With-in homologous substitution series of methylenebisphosphanes, e.g. R 2 P—CH 2 —PR 2 _"H" the coupling constants 2 /(PP) seem to reflect conformational changes at the PCP-skeleton. | | | |
Reference
| (Z. Naturforsch. 43b, 31—44 [1988]; eingegangen am 15. Juni 1987) | | | |
Published
| 1988 | | | |
Keywords
| Functional Methylenebisphosphanes Bifunctional Protecting Groups, Lithium and Trimethylsilyl Derivatives, Dynamic Li-Exchange, NMR Spectra | | | |
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| default:Reihe_B/43/ZNB-1988-43b-0031.pdf | | | | Identifier
| ZNB-1988-43b-0031 | | | | Volume
| 43 | |
| 7 | Author
| Chr Zybill, G. Müller | Requires cookie* | | | Title
| Synthese und Kristallstruktur von f-Butyloxyzinn(II)chlorid Synthesis and Crystal Structure of /-Butyloxytin(II) Chloride | | | | Abstract
| r-Butyloxytin(II) Chloride. NMR Spectra f-Butyloxytin(II) chloride (1) is prepared from SnCU and KO-r-Bu at -60 °C in tetrahydrofuran. Above —30 °C a reversible dismutation into SnCl 2 and [(/-BuO) 2 Sn] is observed in THF. For this process AG = +38 kJ/mol is estimated from NMR data. Compound 1 is a centrosymmetric dimer in the solid state with bridging O atoms (Sn — O 2.153(2)/2.156(2) A. O-Sn-O 73.0(1)°, Sn-O-Sn 107.0(1)°). Due to the acute intraring bond angles at Sn, the 0---0 distance across the four-membered ring is relatively short (2.563(3) Ä). The dimers are very loosely connected to chains by bridging THF molecules. | | | |
Reference
| (Z. Naturforsch. 43b, 45—48 [1988]; eingegangen am 22. September 1987) | | | |
Published
| 1988 | | | |
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| default:Reihe_B/43/ZNB-1988-43b-0045.pdf | | | | Identifier
| ZNB-1988-43b-0045 | | | | Volume
| 43 | |
| 8 | Author
| Hubert Schmidbaur, Jan Ebenhöch, Gerhard Müller | Requires cookie* | | | Title
| Synthese und Eigenschaften einiger Silylethinylsilane; Molekülstruktur von Tetrakis(trimethylsilylethinyl)silan Synthesis and Properties of Some Silylethynylsilane; Molecular Structure of Tetrakis(trimethylsilylethynyl)silane | | | | Abstract
| Silylethynylsilane. Molecular Structure, Tetrakis(trimethylsilylethynyl)silane Trimethylsilylethine (1) has been prepared from C 2 H 2 , sodium and Me,SiCl in anisole. The product can be converted into a Grignard reagent Me 3 SiC=CMgCl using /PrMgCl. This reagent yields the compounds Me 3 SiC=CSiH 3 , (Me 3 SiC=C) 2 SiH 2 , (Me 3 SiC=C) 3 SiH, and (Me 3 SiC=C) 4 Si (2—5) when treated with equivalent amounts of H,SiBr. H 2 SiBr 2 , HSiCl 3 , or SiCl 4 . respectively. The new silanes have been characterized by NMR data. The crystal structure of (Me 3 SiC=C) 4 Si has been determined by single crystal X-ray diffraction. It shows the expected tetrahedral geometry at the central silicon atom with four linear SiC^CSi linkages. | | | |
Reference
| (Z. Naturforsch. 43b, 49—52 [1988]; eingegangen am 2. Oktober 1987) | | | |
Published
| 1988 | | | |
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| default:Reihe_B/43/ZNB-1988-43b-0049.pdf | | | | Identifier
| ZNB-1988-43b-0049 | | | | Volume
| 43 | |
| 9 | Author
| St Böck, H. Nöth, P. Rahm | Requires cookie* | | | Title
| Lithium-dimethylamino-hydrido-aluminate: Lösungszustand in Diethylether, Tetrahydrofuran und Dimethyldiglykolether Lithium Dimethylamino Hydrido Aluminates: The Solution State in Diethylether, Tetrahydrofuran and Dimethyldiglycol Ether | | | | Abstract
| The reaction of LiAlH 4 with dimethylamine has been studied in THF, diglyme and diethyl ether solution covering the molar ratios 1:0.5 to 1:4. In all cases the stoichiometric amount of H : is evolved. With the exception of LiAl[N(CH 3) 2 ] 4 all other members of the series LiAlH 4 _"[N(CH 3) 2 ]" cannot be isolated. They are in equilibrium with one another in solution. These equilibria are independent of the solvent used. The structure of compound LiAl[N(CH 3) 2 ] 4 -2(OC 4 H 8) has been determined by X-ray diffrac-tion. The anion acts as a bidentate ligand to Li which is also bonded to the oxygen atoms of two THF molecules. | | | |
Reference
| (Z. Naturforsch. 43b, 53—60 [1988]; eingegangen am 19. August 1987) | | | |
Published
| 1988 | | | |
Keywords
| Lithium Dimethylaminohydrido Aluminates, 27 A1 NMR Spectra, Solution State, X-Ray, 7 Li NMR Spectra | | | |
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| default:Reihe_B/43/ZNB-1988-43b-0053.pdf | | | | Identifier
| ZNB-1988-43b-0053 | | | | Volume
| 43 | |
| 10 | Author
| Karl-Heinz Van Bonn, Theo Von Bennigsen-Mackiewicz, Jutta Kiesgen, Christoph Von Plotho, Peter Paetzold | Requires cookie* | | | Title
| Neue Iminoborane und ihre Reaktionen Novel Iminoboranes and their Reactions | | | | Abstract
| The iminoboranes RB=NR', 2a—f, are formed by the elimination of Me 3 SiHal from the corresponding aminoboranes la—f. Stabilization occurs either through cyclodimerisation (^ • 3b—d,f), cyclotrimerisation (—>4e), bicyclotrimerisation (—»-5b) or cyclotetramerisation (-*6a). Trialkylboranes BX 3 are added to give the diboryl amines RXB—N(R')—BX 2 , 7a—f. The zl : -tetraazaborolines [—(R)B—(R')N-N=N-N(X')—], 8a-f, are the (3+2)-cycloaddition products from 2a—f and azides X'N V A CH-bond of cyclopentadiene adds to one of the BN bonds of 2f, giving a mixture of the corresponding 1,3-and 1,4-cyclopentadienyl boranes, 9f, 9'f. | | | |
Reference
| (Z. Naturforsch. 43b, 61—68 [1988]; eingegangen am 9. September 1987) | | | |
Published
| 1988 | | | |
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| default:Reihe_B/43/ZNB-1988-43b-0061.pdf | | | | Identifier
| ZNB-1988-43b-0061 | | | | Volume
| 43 | |
| 12 | Author
| HerbertW. Roesky, Bertel Nobert, Edelmann Frank, GeorgeM. Mathias Noltemeyer, Sheldrick | Requires cookie* | | | Title
| Darstellung und Struktur des Bis(triphenylarsoranyliden)ammoniumchlorids Preparation and Structure of Bis(triphenvlarsoranylidene) Ammonium Chloride | | | | Abstract
| The reaction of Ph,AsCl 2 (1) and N(SiMe,) 3 (2) yields [Ph,As-N-AsPh,] + Cl (3) as a crystal-line white solid, soluble in CH,OH and acetone. 3 might be used to stabilize unusual anions. It crystallizes as a 1:1 toluene adduct in the space group C2/c with a = 1585.3(3), b = 1058.7(2). c = 2266.3(4) pm, ß -94.40(2)° and Z = 4. The cation in 3 lies on a crystallographic two-fold axis with As-N-As 123.9(1)°. As-N 174.9(3). and As-C 196.7(5), 197.6(5). 193.2(5) pm. | | | |
Reference
| (Z. Naturforsch. 43b, 72—74 [1988]; eingegangen am 7. September 1987) | | | |
Published
| 1988 | | | |
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| default:Reihe_B/43/ZNB-1988-43b-0072.pdf | | | | Identifier
| ZNB-1988-43b-0072 | | | | Volume
| 43 | |
| 13 | Author
| Helmut Blum | Requires cookie* | | | Title
| Synthese, Eigenschaften und Struktur neuer 1,1-Diphosphonsäuren Synthesis, Properties and Structure of New 1,1-Diphosphonic Acids | | | | Abstract
| 3-rm-Alkyl-3-oxo-l-aminopropane-l,l-diphosphonic Acids, 3-terf-Alkyl-3-oxo-l-hydroxypropane-l,1-diphosphonic Acids, 3-ter/-Alkyl-3-oxo-prop-l-ene-1,1-diphosphonic Acids, Diphosphonocyanohydrin, Preparation The synthesis of 3-/m-alkyl-3-oxo-l-arninopropane-l,l-diphosphonic acids and of 3-fm-alkyl-3-oxo-prop-l-ene-l,l-diphosphonic acids as two new groups of metal complexing agents and their chemical properties are described. Evidence is given for their suggested structures. In addition, the first known example of a diphosphonic acid with a cyano group attached to the geminal carbon atom was prepared from 3-oxo-l-aminoalkane-l,l-diphosphonic acids and 3-terr-alkyl-3-oxo-l-hydroxypropane-1,1-diphosphonic acids from 3-oxo-l-aminopropane-l,l-diphosphonic acids. | | | |
Reference
| (Z. Naturforsch. 43b, 75—81 [1988]; eingegangen am 4. August/23. September 1987) | | | |
Published
| 1988 | | | |
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| default:Reihe_B/43/ZNB-1988-43b-0075.pdf | | | | Identifier
| ZNB-1988-43b-0075 | | | | Volume
| 43 | |
| 14 | Author
| Olefine, Hans-Dieter Hausen, Wolfgang Kaim | Requires cookie* | | | Title
| Elektronenreiche | | | | Abstract
| Zusammenhang zwischen Struktur, Spektroskopie und Reaktivität von Tetrakis(trimethylsilylmethyl)ethen Electron Rich Olefins, 1 The Relationship between Structure, Spectroscopy, and Reactivity of Tetrakis(trimethylsilylmethyl)ethene Crystal and molecular structure analysis of the electron rich title compound exhibits an un-distorted, yet sterically shielded tetra(primary alkyl)-substituted double bond system with alter-nating anti-periplanar CH : SiMe 3 substituents. The diastereotopic methylene protons have been located and their position correlated to the 'HNMRdataandtotheESRhyperfinecouplingconstants of the corresponding radical cation. In contrast to the highly inert all-carbon derivative, tetraneopentylethene, the more electron-rich and more flexible organosilicon title compound reacts with bromine. Close to orthogonal arrangement between the C—C(H :)—Si planes and the ethene plane ensures effective, fourfold a/jr-hyperconjugation. | | | |
Reference
| (Z. Naturforsch. 43b, 82—88 [1988]; eingegangen am 3. Juli/29. September 1987) | | | |
Published
| 1988 | | | |
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| default:Reihe_B/43/ZNB-1988-43b-0082.pdf | | | | Identifier
| ZNB-1988-43b-0082 | | | | Volume
| 43 | |
| 16 | Author
| W. Preetz, C. Sartori | Requires cookie* | | | Title
| Darstellung und Schwingungsspektren des 13 C-und 18 0-markierten rrans-Dioxotetracyanoosinats(VI), [0s0 2 (CN) 4 ] 2 ~ Preparation and Vibrational Spectra of 13 C and ls O Labelled mms-Dioxotetracyanoosrnate(VI), [0s0 2 (CN) 4 ] 2 | | | | Abstract
| Through careful acidification of the aqueous solution of [0s0 2 (0H) 4 ] 2 ~ in the presence of CN or 13 CN~ with acetic acid, [0s0 2 (CN) 4 ] 2 " or [OsO : (13 CN) 4 ] 2:: are formed, respectively. The reaction of 0s 18 0 4 and tetrabutylammonium cyanide with glacial acetic acid in anhydrous methanol yields [0s 18 0 2 (CN) 4 ] 2 ~. The shifts of the infrared and Raman bands of the isotopically labelled complexes are in good agreement with Teller-Redlich calculations. The degenerate E modes, expected for tetragonal symmetry, are split by approx. 15 cm ', indicating an orthorhombic distortion of the complex ion in the solid state. Therefore, all the observed IR-and Raman frequencies are assigned according to point group D 2h . For the complex containing an 16 0 = 0s= 18 0 axis, the symmetry is lowered to C 2v , and the rule of mutual exclusion is restricted. This results in a weak absorption in the infrared spectrum of the Raman active symmetric OsO stretching vibration and vice versa a weak band in the Raman spectrum for the antisymmetric infrared active mode. | | | |
Reference
| (Z. Naturforsch. 43b, 94—98 [1988]; eingegangen am 11. September 1987) | | | |
Published
| 1988 | | | |
Keywords
| /rans-Dioxotetracyanoosmate(VI) Isotopic Labeling, IR Spectra, Raman Spectra | | | |
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| default:Reihe_B/43/ZNB-1988-43b-0094.pdf | | | | Identifier
| ZNB-1988-43b-0094 | | | | Volume
| 43 | |
| 17 | Author
| Christian Robl | Requires cookie* | | | Title
| Erdalkaliquadratate, VI [1] SrC 4 0 4 -3H 2 0, Typ III Alkaline-earth Squarates, VI [1] SrC 4 0 4 -3H 2 0, Type III | | | | Abstract
| SrC 4 0 4 -3H 2 0, type III, was obtained in an aqueous silica gel besides crystals of SrC 4 0 4 • 3 H 2 0, type I. X-ray crystal structure analysis showed close relationship to BaC 4 0 4 -3H 2 0, but no iso-typism. Sr 2+ is coordinated by four water molecules and four oxygen atoms of the squarate dianion. The connection of Sr 2+ with C 4 0 4 2 leads to layers. The geometry of C 4 0 4 2 is typical for delocalized jr-systems. The O squarate atoms are not equally bound to Sr 2+ . One O squarate atom (0(4)) is bound to two Sr 2+ , two (O(l), 0(2)) are bound to one Sr 2+ , respectively, and the fourth O squaraIe atom (0(3)) shows no bonding contact to Sr 2+ . These differences are compensated for by inter-molecular hydrogen bonds which involve 0(3) three times, O(l) and 0(2) once each, but not 0(4). | | | |
Reference
| (Z. Naturforsch. 43b, 99—103 [1988]; eingegangen am 21. September 1987) | | | |
Published
| 1988 | | | |
Keywords
| Strontium Squarate Type III, Preparation, Crystal Structure, Hydrogen Bonding | | | |
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| default:Reihe_B/43/ZNB-1988-43b-0099.pdf | | | | Identifier
| ZNB-1988-43b-0099 | | | | Volume
| 43 | |
| 18 | Author
| Ulrich Wannagat, Dietmar Wiese | Requires cookie* | | | Title
| Synthese des 9,9-DimethyI-9-silaacridans sowie einiger Derivate mit variierter Seitenkette Synthesis of 9,9-Dimethyl-9-silaacridane and of Some Derivatives with Varied N-Side Chains | | | | Abstract
| 9-Silaacridane. Tricyclic Psychopharmaca, Silasubstitution 9,9-Dimethyl-9-silaacridane 3a was synthesized by ringclosing reactions of N-trimethylsilyl-bis(2-halogenophenyl)amines with dichlorodimethylsilane and acid cleavage of the silyl groups (eqs (6—9)). Syntheses of N-organyl-substituted 9.9-dimethyl-9-silaacridanes 13 occurred by ring closure of N-organyl-bis(2-halogenophenyl)amines 12 with dichlorodimethylsilane. organyl groups here being dimethylaminoethyl. pyrrolidinoethyl, piperidinoethyl, 3-dimethylamino-2-methyl-propyl and (l-methylpiperidin-3-yl)methyl. 13 were transformed to their hydrochlorides and methoiodides 14. Structures of 13 are compared with those of analogous compounds bearing aminopropyl-side chains and discussed in the light of psychopharmacological effects of tricyclic ring systems. | | | |
Reference
| (Z. Naturforsch. 43b, 104—112 [1988]; eingegangen am 25. August 1987) | | | |
Published
| 1988 | | | |
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| default:Reihe_B/43/ZNB-1988-43b-0104.pdf | | | | Identifier
| ZNB-1988-43b-0104 | | | | Volume
| 43 | |
| 19 | Author
| Karl Brunn, Helmut Endres, Johannes Weiss | Requires cookie* | | | Title
| Ein Chelatligand mit einer -NSSSN-Kette: Bis(oxamido)trisulfan und sein Kupferkomplex A Chelate Ligand with a -NSSSN-Chain: Bis(oxamido)trisulfane and its Copper(II) Complex | | | | Abstract
| Chelate Ligand, Copper(II) Complex, Structure Bis(oxamido)trisulfane was obtained first as a by-product in the synthesis of 3,4-dihydroxy-I,2,5-thiadiazole, later in direct syntheses from 3,4-diethoxy-l,2,5-thiadiazole. Reaction with anhydrous CuCL gave bis(oxamido)trisulfane copper(II). Bis(oxamido)trisulfane is monoclinic P2 x /n, a = 8.975(2) A. b = 8.875(1) Ä, c = 12.781(2) Ä. ß = 94.40(2)°, V = 1015.05(4) Ä 3 , Z = 4, M r = 270.31, D r = 1.76 gem" 3 , MoK", A = 0.7107 Ä, ju = 7.0 cm -1 , wR = 0.038 for 1371 observed independent reflections. Bis(oxamido)trisulfane copper(II) is triclinic PI, a = 5.279(1) Ä, b = 11.388(3) Ä, c = II.943(4) Ä, a = 89.08(2)°, ß = 82.62(2)°, y = 86.44(2)°, V = 710.8(3) A 3 , Z -2, M r = 331.83, D v = 1.56 gem" 1 , MoK", Ä = 0.7107 Ä, ft = 19.89 cm" 1 , wR = 0.039 for 1974 observed inde-pendent reflections. | | | |
Reference
| (Z. Naturforsch. 43b, 113—116 [1988]; eingegangen am 9. Juli/18. August 1987) | | | |
Published
| 1988 | | | |
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| default:Reihe_B/43/ZNB-1988-43b-0113.pdf | | | | Identifier
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| 43 | |
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