| 21 | Author
| K. Arl Hensen, PeterW. Ag, N. Er+ | Requires cookie* | | Title
| Die Kristallstruktur der Verbindung N-Trimethylsilyl-3,4-Dimethylpyridiniumbromid The C rystal Structure o f N -T rim ethylsilyl-3,4-dim ethylpyridinium Brom ide  | | | Abstract
| Trimethylbromosilane and 3,4-lutidine form a 1:1 com pound which is stable at room tem perature. Single crystals of this com pound can be isolated by sublimation. It crystallizes in the orthorhom bic space group P 2,2,2, with lattice constants a = 737,08(9) pm, b = 1295,7(1) pm, c = 1318,8(3) pm. The crystal structure was refined to Rw = 0,042 and proves an ionic struc ture. | | |
Reference
| (Z. Naturforsch. 48b, 79—81 [1993]; eingegangen am 21. Februar 1992) | | |
Published
| 1993 | | |
Keywords
| Trimethylbromosilane, 3, 4-Dimethylpyridine, Addition Com pound, Crystal Structure | | |
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| default:Reihe_B/48/ZNB-1993-48b-0079.pdf | | | Identifier
| ZNB-1993-48b-0079 | | | Volume
| 48 | |
22 | Author
| Michael Plate, Gerlinde Frenzen, K. Urt Dehnicke | Requires cookie* | | Title
| Synthese und Kristallstrukturen der ionischen Kronenetherkomplexe [TiCl3(15-Krone-5)(CH3CN)l[SbCl6l und | V Cl(OH)( 18-Krone-6)(CH3CN)2] [SbCl6l * V2(18-Krone-6 * CH3CN) Synthesis and Crystal Structures of the Ionic Crown Ether Complexes [TiCl3( 15-Crown-5)(CH3CN)][SbCl6] and [VCl(OH)( 18-Crown-6)(CH3C N )2][SbCl6] ■ 'A( 18-Crown-6 * C H 3CN)  | | | Abstract
| The title compounds were prepared by the reaction o f titanium tetrachloride with 15-crown-5 and antimony pentachloride, and by the reaction o f vanadium trichloride with 18-crown-6 and antimony pentachloride in the presence o f traces o f water in acetonitrile solution, respectively. The complexes were characterized by IR spectroscopy and by X-ray structure determinations. [TiCl3(15-crown-5)(CH1CN)][SbCl6]: Space group Pnma, Z = 4, 1355 observed unique reflec tions, R = 0.035. Lattice dim ensions at -8 0 °C: a = 1987(1), b = 1742.2(6), c = 111.0(2) pm. The com pound consists o f SbCl6~ anions and cations [TiCl3(15-crown-5)(CH3C N)]+, in which the titanium atom is coordinated octahedrally by three chlorine atom s in facial arrangement, by the nitrogen atom o f the acetonitrile m olecule, and by two oxygen atom s o f the crown ether molecule. [VCl(OH)(18 -crown-6)(C H 3C N)2][SbCl6] ■ 'A(18-crow n-6 • C H 3 CN); Space group P I, 3936 observed unique reflections, R = 0.014. Lattice dim ensions at -8 0 °C: a = 1194.2(6), b = 1349.8(6), c = 1365.5(6) pm, « = 93.55(4)°, ß = 111.23(4)°, y = 93.15(4)°. The com pound con sists o f SbCl6-anions, included 18-crown-6 and acetonitrile molecules, and cations [VCl(OH)(18-crown-6)(CH3C N)2]+, in which the vanadium atom is octahedrally coordinated by two nitrogen atoms o f the acetonitrile molecules in trans positions, by a chlorine atom and a hydroxyl group in cis position, and by two oxygen atom s o f the crown ether molecule. One o f the acetonitrile molecules forms weak hydrogen bridges with two oxygen atom s o f the includ ed crown ether molecule as well as with one chlorine atom o f the SbCl6" ion. | | |
Reference
| Z. Naturforsch. 48b, 149—155 (1993); eingegangen am 4. September 1992 | | |
Published
| 1993 | | |
Keywords
| Crown Ether Complexes, Titanium, Vanadium, IR Spectra, Crystal Structure | | |
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| default:Reihe_B/48/ZNB-1993-48b-0149.pdf | | | Identifier
| ZNB-1993-48b-0149 | | | Volume
| 48 | |
23 | Author
| Lothar Ohse, Mehmet Somer, Wolfgang Blase, Gerhard Cordier | Requires cookie* | | Title
| Verbindungen mit SiS2-isosteren Anionen i  | | | Abstract
| [AlX4/2 3 ] und i |InP4/23 ]: Synthesen, Kristallstrukturen und Schwingungsspektren von Na3|AlX2], K2Na[AlX2] und K3IInP2] (X = P, As) Com pounds with SiS2 Isoelectronic Anions l [A1X4 23-] and i [InP4/23-]: Synthesis, Crystal Structures and Vibrational Spectra of N a3[AlX2], K 2Na[AlX2] and K 3[InP2] (X = P, As) The title compounds were prepared from stoichiometric mixtures o f the elements or from alkali metals (Na, K), NaX (KX) and MX (M = Al, In; X = P, As) at 1000 K. The crystal structures (Ibam, No. 72) are characterized by infinite chains o f edge sharing tetrahedra j, [MX4;,3'] (M = Al, In; X = P, As) which are isoelectronic to SiS2. The vibrational spectra can be interpreted with respect to the symmetry P(2/m 2/c) 42/ m -D 4h of the isolated polymeric chain ][M X 4(23"]. The assignment of the observed frequen cies is supported by a normal coordinate analysis using the fragment method. | | |
Reference
| Z. Naturforsch. 48b, 1027—1034 (1993); eingegangen am 29. März 1993 | | |
Published
| 1993 | | |
Keywords
| Zintl Phases, Preparation, Crystal Structure, V ibrational Spectra, Force Constants | | |
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| default:Reihe_B/48/ZNB-1993-48b-1027.pdf | | | Identifier
| ZNB-1993-48b-1027 | | | Volume
| 48 | |
25 | Author
| Hans-Jörg Hemmerling, Margarete Janoschka, Hartmut Wunderlich | Requires cookie* | | Title
| Amidinadditionsprodukte des 1,2,3-Indantrionhydrats: Synthese und Strukturzuordnung durch Kristallstrukturanalyse, spektrale Daten und Blei(IV)acetatoxidation Products o f Am idinaddition to 1,2,3-Triketohydrindenhydrat: Synthesis and Determination by Crystal Structure, Spectral Data and Oxidation with Lead(IV)acetate  | | | Abstract
| The addition o f amidines to 1,2,3-triketohydrindenhydrat gives cyclic dihydroxyindenoimi-dazoles. From N-substituted amidines mixtures o f regioisomeric derivatives were obtained. Analysis o f crystals revealed the major product o f 2 k to be 4 k. They belong to the monoclinic space group P 2 ,/c (a = 889.1(2); b = 1186.6(3); c = 2783.5(7) pm; ß = 91.26(2)°) with Z = 8 molecules including four molecules o f ethanole per unit cell. These results were confirmed by oxidation with lead(IV)acetate, which lead to derivatives o f isoindols. | | |
Reference
| Z. Naturforsch. 48b, 1094—1104 (1993); eingegangen am 26. März 1993 | | |
Published
| 1993 | | |
Keywords
| Indeno[l, 2-d]im idazoles, Triketohydrinden, Crystal Structure, Amidines, Isoindoles | | |
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| default:Reihe_B/48/ZNB-1993-48b-1094.pdf | | | Identifier
| ZNB-1993-48b-1094 | | | Volume
| 48 | |
27 | Author
| Gerhard Müller, Joachim Lachmann | Requires cookie* | | Title
| Sterisch belastete cyclische Phosphanborane Sterically Crowded Cyclic Phosphine-Boranes  | | | Abstract
| A The anionic phosphine o-(diphenylphosphinomethyl)phenyl L has been used to prepare the sterically crowded cyclic phosphine-boranes BL3, 'BuBL2, and 'Bu2BL by reaction o f the lith-iated ligand LiL with B(OM e)3, 'BuB(OM e)2, and 'Bu2BOMe, respectively. In the new com pounds 'BuBL-, and 'Bu^BL one ligand L is bonded to the boron center by both its carbanionic and its phosptiino function with formation o f five-membered rings. In solution 11B and 31P N M R spectroscopy does not indicate substantial B -P dissociation, i.e., the existence o f three-coordinate boron. The steric bulk o f L in BL3 leads to the formation o f oligom ers in solution, presumably by a bridging coordination mode o f L to two boron centers. N o conclusive evi dence as to the monom eric or oligomeric nature o f BL3 in the solid state can be given, however. Five-membered ring form ation is proven for the solid state by X-ray structure determinations o f 'BuBL2 and 'Bu2BL which in addition confirm that the steric bulk o f L is superior to that o f a tert. butyl group. | | |
Reference
| Z. Naturforsch. 48b, 1248 (1993); eingegangen am 13. Mai 1993 | | |
Published
| 1993 | | |
Keywords
| nionic Benzylphosphines, Cyclic Phosphine-Boranes, Crystal Structure, Steric Hindrance | | |
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| default:Reihe_B/48/ZNB-1993-48b-1248.pdf | | | Identifier
| ZNB-1993-48b-1248 | | | Volume
| 48 | |
28 | Author
| DietrichM. Ootz, Dieter Stäben | Requires cookie* | | Title
| Die Hydrate von terf-Butanol: Kristallstruktur von Me3COH * 2 H20 und Me3COH * 7 H20 [ 1 ]  | | | Abstract
| The system /er/-butanol-water has been confirmed by X-ray powder diffraction and single crystal structure analysis to contain two hydrates, a dihydrate and a higher hydrate. The com position o f the latter, contradictory in the literature, could be resolved in favor o f the new one o f a heptahydrate. The dihydrate (m.p. 0.7 °C) is m onoclinic with space group P2, and Z = 2 formula units per unit cell o f dim ensions a = 6.017, b = 6.055, c = 10.377 A and ß -106.60° at -150 °C. The heptahydrate (m.p. -6 °C, dec.) is orthorhombic with space group Pnma, Z = 4, a -12.589, b = 15.251 and c = 6.645 A at -150 °C. Both hydrates contain characteristic layers o f hydrogen-bonded O atom s, which in the heptahydrate are further linked into a three-di-m ensional semi-clathrate structure. | | |
Reference
| Z. Naturforsch. 48b, 1325—1330 (1993); eingegangen am 17. Mai 1993 | | |
Published
| 1993 | | |
Keywords
| te/7-Butanol Hydrates, Melting Diagram, Crystal Structure, Hydrogen Bonding | | |
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| default:Reihe_B/48/ZNB-1993-48b-1325.pdf | | | Identifier
| ZNB-1993-48b-1325 | | | Volume
| 48 | |
29 | Author
| Henning Von Arnim, Kurt Dehnicke, Klaus Maczek, D. Ieter Fenske | Requires cookie* | | Title
| Ionische Kronenetherkomplexe von Thallium(I), Blei(II) und Indium(III). Die Kristallstrukturen von [Tl(12-Krone-4)2][SbCl6], [Pb(15-Krone-5)2][SbCl6]2* [SbCl3(15-Krone-5>] und [In(12-Krone-4)2][SbCl6]3* 3 CH3CN  | | | Abstract
| Ionic Crown E ther Complexes of Thallium(I), Lead(II), and Indium(III). Crystal Structures of [Tl(12-Crown-4)2][SbCl6], [Pb(15-Crown-5)2][SbCl6]2-[SbCl3(15-Crown-5)], and [In(12-Crown-4)2][SbCl6]3 -3 CH3CN T he ionic crown ether com plexes [Tl(12-crown-4)2][SbCl6] (1) and [In(12-crown-4)2][SbCl6]3-3 C H 3CN (3) have been prepared by reaction o f T1C1 and InCl3, respectively, with SbCl5 in the presence o f 12-crown-4 in acetonitrile solution. The lead com | | |
Reference
| Z. Naturforsch. 48b, 1331 (1993); eingegangen am 3. Juni 1993 | | |
Published
| 1993 | | |
Keywords
| Ionic Crown Ether Com plexes o f Thallium, Lead, Indium, Synthesis, Crystal Structure | | |
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| default:Reihe_B/48/ZNB-1993-48b-1331.pdf | | | Identifier
| ZNB-1993-48b-1331 | | | Volume
| 48 | |
30 | Author
| Hans Wolkers, Ralf Stegmann, G. Ernot, Frenking, Kurt Dehnicke, D. Ieter Fenske, G.Erhard Baum | Requires cookie* | | Title
| Das Methylviologen-Radikalkation. Synthese, Kristallstruktur und ab Rechnungen von N,N'-Dimethyl-4,4'-bipyridinium-chlorid-dihydrat The Methylviologen Radical Cation. Synthesis, Crystal Structure and ab initio Calculations of N,N' -Dimethyl-4,4'-bipyridinium Chloride Dihydrate  | | | Abstract
| The title compound has been prepared by the reduction of N,N'-dimethyl-4,4'-bipyridinium dichloride with dilithium tritelluride in dimethylformamide solution. It forms deep blue crystal needles, which were characterized by a crystal structure determination. Space group Pna21; Z -8, 3450 observed unique reflections, R = 0.045. Lattice dimensions at -70 °C: a = 1707.6(8), b = 2323.9(11), c -664.6(3) pm. The N,N'-dimethyl-4,4'-bipyridinium radical cations are planar and form ion pairs in the lattice. The chloride ions together with the water molecules form an infinite network of hydrogen bridges along the crystallographic «-axis. The structural parameters of the radical cation are in excellent agreement with ab initio calculations. | | |
Reference
| Z. Naturforsch. 48b, 1341—1347 (1993); eingegangen am 25. Juni 1993 N | | |
Published
| 1993 | | |
Keywords
| N'-Dimethyl-4, 4'-bipyridinium Chloride Dihydrate, Synthesis, Crystal Structure | | |
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| default:Reihe_B/48/ZNB-1993-48b-1341.pdf | | | Identifier
| ZNB-1993-48b-1341 | | | Volume
| 48 | |
31 | Author
| Indium Gallium, ThalliumG. Erhard Müller, Joachim Lachmann | Requires cookie* | | Title
| Vier-und fünffach koordinierte Organometall-Phosphankomplexe von Aluminium, Gallium, Indium und Thallium Four-and Five-Coordinate Organom etal Phosphine Complexes of Aluminum  | | | Abstract
| A The organom etal phosphine complexes M L3 (L = [o-(Ph2PCH2)C6H4]"; M = A l3+, G a3+, In3+) are obtained from MC13 and the lithiated ligand in diethyl ether. Tl[o-(Ph2PC H 2)C6H 4]3 is prepared from T1C1 by a disproportionation reaction. M 1 species could not be detected with L as ligand. Al[o-(Ph2PCH 2)C6H4]3 is the first triorganoaluminum bis(phosphine) adduct where C3P2 pentacoordination at aluminum has been definitely proven for both the solution (<5(27A1) = 131 ppm, w 1/2 = 12 kHz) and the solid state (d (A l-P) = 2.676(3)/2.782(2) Ä). The trigonal-bipyramidal coordination geometry (C3P2) at Al is achieved by two o f the anionic phosphines acting as chelating ligands, spanning equatorial (C atoms) and axial sites (P atom s), while the third phosphine is only carbon-bonded. Like A1L3, the heavier congeners M L3 (M = G a, In, Tl) are stereochemically nonrigid molecules in solution. Surprisingly, in the solid state only InL3 resembles the aluminum complex (C3P2 penta-coordination) while G aL 3 and T1L3 contain four-coordinate metal centers (C3P). This may be rationalized by the notice ably less polar G a -P bonds as compared to A l-P and I n -P bonds, while in T1L3 the span o f the ligand is not sufficient to allow for chelating coordination at a five-(or six-)coordinate Tl center. | | |
Reference
| Z. Naturforsch. 48b, 1544—1554 (1993); eingegangen am 12. Juli 1993 | | |
Published
| 1993 | | |
Keywords
| nionic Benzylphosphines, Main Group Metals, Phosphine Complexes, Crystal Structure | | |
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| default:Reihe_B/48/ZNB-1993-48b-1544.pdf | | | Identifier
| ZNB-1993-48b-1544 | | | Volume
| 48 | |
32 | Author
| Ekkehard Lindner, Walter Wassing, R. Fawzi, M. Steimann | Requires cookie* | | Title
| Zweikernige Mangan-und Rheniumkomplexe mit gemischt aliphatischen-aromatischen Kohlenwasserstoffbrücken Dinuclear Manganese and Rhenium Complexes with Mixed Aliphatic-Aromatic Hydrocarbon Bridges  | | | Abstract
| The symmetrically hydrocarbon-bridged complexes (OC)5M -(C H 2)n+1-X -(C H 2)n+|-M (CO)5 [n = 1, X = 1,4-C6H4, M = Mn (2a), M = Re (3a); n = 2, X = 1,4-C6H4, M = Mn (2b), M = Re (3b); n = 1, X = 1,3-C6H4, M = Mn (5a), M = Re (6a); n = 2, X = 1,3-C6H4, M = Mn (5b), M = Re (6b); n = 1, X = 1,2-C6H4, M = Mn (8a), M = Re (9a); n = 2, X = 1,2-C 6H4, M = Mn (8 b), M = Re (9b)] are obtained by the reaction of the bistriflates X[(CH2)"-C H 2-0 S 0 2CF3]2 [X = 1,4-C6H4, n = 1 (la), n = 2 (lb); X = 1,3-C6H4, n = 1 (4a), n = 2 (4b); X = 1,2-C6H4, n = 1 (7 a), n = 2 (7 b)] with the carbonyl metalates [M(CO)5]" (M = Mn, Re) in THF and dimethyl ether, respectively. According to an X-ray structural analysis 8a crystallizes in the triclinic space group PI with Z = 2. Depending on the solvent, the reaction of 7 a with [Mn(CO)5]" affords also the cyclic carbene complex 10 a. The behavior of the manganese compounds toward CO has been investigated exemplarily in the case of 8 a and leads to the diacyl complex l,2-C6H4[CH2CH2C (0)M n(C 0)5]2 (11). Upon reaction with Na2C 0 3/CH30 H 11 is con verted to give the corresponding diester 1,2-C6H4[CH2CH2C (0)0 C H 3]2 (12). | | |
Reference
| Z. Naturforsch. 48b, 1651—1660 (1993); eingegangen am 2. Juli 1993 | | |
Published
| 1993 | | |
Keywords
| Bistriflates, Hydrocarbon-Bridged Complexes, Manganese Complexes, Rhenium Complexes, Crystal Structure | | |
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| default:Reihe_B/48/ZNB-1993-48b-1651.pdf | | | Identifier
| ZNB-1993-48b-1651 | | | Volume
| 48 | |
33 | Author
| Hansjürgen Mattausch, Horst Borrmann, A.Rndt Simon, *. Sonderdruckanforderungen, ProfA. Dr, Simon | Requires cookie* | | Title
| Y 7I6C30 : Ein Carbidoxid mit kondensierten Y 6C -O ktaedem und Y 40-T etraed em Y7I6C30 : A Carbide Oxide with Condensed Y6C-Octahedra and Y40 -T etrahedra  | | | Abstract
| The new compound Y7I6C30 is prepared by re action of stoichiometric amounts of Y, YI3, Y20 3 and C in closed Ta capsules at 1370 K. Y,I6C30 forms bronze coloured, metallic, air and moisture sensitive crystals. It crystallizes in the space group Pmma (No. 51) with the lattice constants a = 2249.4(4), b = 383.7(1), c = 1079.1(1) pm. Within the crystal structure the C atoms and the O atoms are surrounded by Y atoms octahedrally and tetrahedrally, respectively. The Y6C octahedra and Y40 tetrahedra are condensed to form ondulated layers, which are separated by double layers of I atoms. Einleitung Metallreiche Halogenide der Seltenerdmetalle mit einem Halogen/M etallverhältnis kleiner als 2 [1] sind mit Ausnahm e der Sesquihalogenide SE2X3 [2,3,4] ternäre Verbindungen. In ihren Strukturen treten Nichtmetallatome wie H, B, C, N, Si oder Übergangsmetallatome wie zum Beispiel Fe, Co, Pt, Ru, A u durch SE-Atom e koordiniert auf. H [5] und N [6,7] bevorzugen tetraedrische, B, C, Si [1,8] und die Übergangsmetallatome [9,10,11] oktaedrische Plätze im Metallgerüst. Für Fe und Co wurde auch trigonal-prismatische Koordination durch SE-Atom e gefunden [12]. Ü ber den Einbau von O als interstitiellem Atom ist bisher nichts bekannt. Bei Untersuchungen im System Y/I/C erhielten wir durch Nebenreaktion bronzefarbene, lattenför | | |
Reference
| Z. Naturforsch. 48b, 1828—1830 (1993); eingegangen am 1. Juli 1993 | | |
Published
| 1993 | | |
Keywords
| Yttrium Iodide Carbide Oxide, Crystal Structure, Condensed Clusters, Metallic Behaviour | | |
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| default:Reihe_B/48/ZNB-1993-48b-1828_n.pdf | | | Identifier
| ZNB-1993-48b-1828_n | | | Volume
| 48 | |
34 | Author
| Axel Deeg, Dietrich Mootz | Requires cookie* | | Title
| Addukte Aromat/Chlorwasserstoff bei tiefen Temperaturen: Beiträge zu Bildung und Kristallstruktur [ 1 ] Adducts Arene/Hydrogen Chloride at Low Temperatures: C ontributions to Form ation and Crystal Structure [1]  | | | Abstract
| The melting diagrams o f the systems benzene-HCl, toluene-HCl and mesitylene-HCl have been established and the crystal structures o f two adducts determined. The adduct tolu ene-2 HC1, melting incongruently at -1 1 5 °C, is monoclinic with space group C 2 /c and Z = 4 formula units per unit cell; the adduct mesitylene-HCl, m .p. -6 4 °C, is orthorhom bic with space group P bca and Z = 8. The HC1 molecules are situated on both sides and one side, respectively, o f the plane o f the aromatic system and are linked to it by weak hydrogen bonds o f the type C l-H — it. | | |
Reference
| Z. Naturforsch. 48b, 571—5 (1993); eingegangen am 14. Dezember 1992 | | |
Published
| 1993 | | |
Keywords
| Adducts Arene/HCl, Melting Diagrams, Crystal Structure, Hydrogen Bonding C l-H — it | | |
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| default:Reihe_B/48/ZNB-1993-48b-0571.pdf | | | Identifier
| ZNB-1993-48b-0571 | | | Volume
| 48 | |
35 | Author
| Karlheinz Sünkel, Adrian Blum, Barbara Wagner | Requires cookie* | | Title
| Koordinationschemie perhalogenierter Cyclopentadiene und Alkine, XI [ 1 ]  | | | Abstract
| Darstellung einiger Cymantrenyl-mono-und bis-thioether mit einer weiteren funktionellen Gruppe am Cyclopentadienylring. Molekülstruktur von [C5Cl2(SM e)2(PPh2)lM n(CO)3 C oordination Chemistry of Perhalogenated Cyclopentadienes and Alkynes, XI [1] Synthesis of Some Cymantrene Mono-and Bis-Thioethers with One Additional Functional G roup on the Cyclopentadienyl Ring. M olecular Structure of [C5Cl2(SMe)2(PPh2)]Mn(CO)3 The reaction o f [C5Cl4(SM e)]M n(CO)3 (la) with «-butyllithium and the electrophiles SiM e3Cl, C 0 2, or PPh,Cl regiospecifically yields the chiral 1,3-disubstituted functional cym an trene thioethers [C5Cl3(SM e)R]M n(CO)3 (R = SiM e3 (2), COOLi (3a), PPh2 (4)). 3 a can be protonated to give the corresponding carboxylic acid (3 b), which in turn can be transformed to the acid chloride [C5Cl3(SM e)(COCl)]M n(CO)3 (3c). 3c reacts with N a N 3 to yield after work-up the urea derivative O C [[N H -C 5Cl3(SM e)]M n(CO)3]2 (3d). U sing the cymantrene bis-thioethers [C5Cl3(SR)2]M n(CO)3 (R = Me, 5a, Ph, 5b) as starting materials, the carboxyl de rivatives [C5Cl2(SM e)2(COR)]M n(CO)3 (R = OLi, 6a, OH, 6b, Cl, 6 c) and the potential organometallic S,P-chelate ligands [C5Cl2(SR)2(PPh2)]M n(CO)3 (R = Me, 7 a , Ph, 7b) can be obtained. The crystal structure determination o f 7a (C " H 160 3PS-,CLMn, m onoclinic, P 2,/c, a = 18.714(6) A, b = 9.506(3) A, c = 14.475(3) A, ß = 109.18(2)°, V = 2432.1(12) A \ Z = 4) shows an orientation o f the neighbouring PPh2-and SMe groups, that allows chelation o f an additional metal fragment. | | |
Reference
| Z. Naturforsch. 48b, 583—5 (1993); eingegangen am 16. N ovem ber 1992 | | |
Published
| 1993 | | |
Keywords
| M ultifunctional Cymantrene Thioethers, Organometallic P -S -C h elate Ligand, Chiral Cyclopentadienyl Complexes, Crystal Structure | | |
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| default:Reihe_B/48/ZNB-1993-48b-0583.pdf | | | Identifier
| ZNB-1993-48b-0583 | | | Volume
| 48 | |
36 | Author
| ". B. Preparation, 13cN., M. R., Vibrational Spectra, W. Preetz, A. Franken, M. R. Ath | Requires cookie* | | Title
| Darstellung, UB-, 13C-NM R-und Schwingungsspektren der c/öso-Hexaborate [B6H 5(C N )|2~ und m -[B 6H4(CN)2l2_ sowie Kristallstruktur von Cs2[B6H 5(CN)|  | | | Abstract
| of the c/oso-Hexaborates [B6H 5(CN)]2~ and c/s-[B6H 4(C N)2]2-, and the Crystal Structure o f Cs2[B6H 5(CN)] By reaction o f Cs2[B6H 6] with in situ generated dicyanogen in aqueous alkaline solution the m onocyanohydrohexaborate C s2[B6H5(CN)] and the dicyanohydrohexaborate cis-Cs,[B6H4(C N)2] are formed. The com pounds have been separated by ion exchange chrom atog raphy on diethylaminoethyl cellulose. The crystal structure o f Cs2[B6H5(CN)] was determined from single crystal X-ray diffraction analysis; monoclinic, space group P 2 Ja with a = 9.540(8), b = 9.977(3), c = 10.578(2) Ä, ß = 105.06(2)°. The B6 octahedron is compressed in the direction o f the nearly linear B -C N bond by about 5%, with bond lengths between 1.71 and 1.76Ä . The "B N M R spectra o f the two com pounds reveal the features o f substituted B6 cages with C4v and C2v point symmetry. In the l3C N M R spectrum o f Cs2[B6H 5(CN)] a quartet at -139 ppm with '/(C ,B) 92 Hz is observed. The IR and Raman spectra exhibit very strong CN stretching bands for Cs2[B6H5(CN)] at 2149, and for m -C s2[B6H4(C N)2] at 2170 c tr r 1. | | |
Reference
| Z. Naturforsch. 48b, 598—6 (1993); eingegangen am 7. Dezember 1992 | | |
Published
| 1993 | | |
Keywords
| M onocyanohydrohexaborate, m -Dicyanohydrohexaborate, Crystal Structure, 11B N M R Spectra, Vibrational Spectra | | |
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| default:Reihe_B/48/ZNB-1993-48b-0598.pdf | | | Identifier
| ZNB-1993-48b-0598 | | | Volume
| 48 | |
37 | Author
| Tetramethylammoniumfluorid Bildung, Wasserstoffbrückenbindung Struktur, Dieter Stäben, Dietrich Mootz | Requires cookie* | | Title
| Die kristallinen Hydrate  | | | Abstract
| The melting diagram of the system M e4N F -H 20 in the region 50-100 mol% H zO has been investigated for the first time, using D T A , D SC and tem perature-dependent X-ray powder diffraction. Four crystalline hydrates M e4N F\*H 20 were found, with x = 1 ,2 .3 3 ,4 and 5, which decom pose irreversibly above ca. 160 °C and m elt incongruently at 36 °C, congruently at 46 °C and again incongruently at 10 °C, respectively. The crystal structure o f each hydrate, except the already known one of the tetrahydrate, has b een determ ined with M oK a diffractom eter data. The monohydrate is rhombohedral with space group R3m and Z = 6 formula units per unit cell (hexagonal axes), the 2.33-hydrate m onoclinic with P2j/n and Z = 12, and the pen-tahydrate tetragonal with 142 m and Z = 2. The hydrogen-bonded H 20/F ~ structure is an iso lated centrosymmetric [F2(H 20) 2]2_ four-m em bered ring in the m onohydrate, a rather open three-dim ensional network in the 2.33-hydrate and a corrugated dense layer o f fused five-mem bered rings in the pentahydrate. | | |
Reference
| Z. Naturforsch. 48b, 1057—57 (1993); eingegangen am 5. April 1993 | | |
Published
| 1993 | | |
Keywords
| Tetramethylamm onium Fluoride, Fluoride Hydrates, M elting Diagram, Crystal Structure, Hydrogen Bonding | | |
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| default:Reihe_B/48/ZNB-1993-48b-1057.pdf | | | Identifier
| ZNB-1993-48b-1057 | | | Volume
| 48 | |
38 | Author
| Klaus Schulbert, R.Ainer Mattes | Requires cookie* | | Title
| Kupfer-und Goldkomplexe von Dithiocarbaminsäureestern. Strukturen von [CuC1(L1)3] * CH2C12, [AuC1(L1)2], [CuI(L1)(PPh3)]2 und [Cu2ICuIICl4(L2)2]IJ (L1 = N-Phenyl-S-methyldithiocarbaminsäureester, L2 = N,N-Dimethyl-S-methyldithiocarbaminsäureester) N-Phenyl-S-methyldithiocarbamate, L2 = N,N-Dimethyl-S-methyldithiocarbamate)  | | | Abstract
| Copper and Gold Complexes of Dithiocarbam ate Esters. X-Ray Structures of [CuC1(L1)3] ■ CH2C12, [A uC ^L 1^], [CuI(L1)(PPh3)]2 and [Cu2ICuIICl4(L2)2]n (L 1 = Reactions of N-phenyl-S-methyldithiocarbamate (L1) and N,N-dimethyl-S-methyldithio-carbamate (L2) with CuCl2, [CUjI^PPhj^] and HAuC14 yield the complexes [CuC1(L1)3] • CH2C12 (1), [AuCKL1),] (2), [CuI(L1)(PPh3)]2 (3) and [Cu2ICuIICl4(L2)2]" (4). Their structures have been determined by single crystal X-ray crystallography. 1 and 2 are monomeric, with Cu(I) tetrahedrally four-coordinate and Au(I) two-coordinate with an S-Au-S angle of 158.2(1)°. 3 is dimeric with a central CuI2Cu core, the Cu— Cu distance of which [314.9(1) pm] is rather large. The mixed valence complex 4 has a chain structure with the identity period CuI1(a-Cl)2CuI(a-S)2CuI(a-Cl)2. Cu1 is in a tetrahedral, Cu11 in a square planar environment. The (m-S)2 bridged Cu1---Cu1 distance is only 259.1(1) pm. The structures of the CuX2Cu cores of 3 and 4 are mainly determined by steric interactions of the donor atoms within the coordination spheres of the metal centers. | | |
Reference
| Z. Naturforsch. 48b, 1227—1233 (1993); eingegangen am 4. Mai 1993 | | |
Published
| 1993 | | |
Keywords
| Crystal Structure, Copper(I) Complexes, Dithiocarbamic Acid Esters, Gold(I) Complexes, Dithiocarbamic Acid Esters | | |
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| default:Reihe_B/48/ZNB-1993-48b-1227.pdf | | | Identifier
| ZNB-1993-48b-1227 | | | Volume
| 48 | |
39 | Author
| Hermann Irngartingera, Jochen Lichtenthälera, Dieter Fenskeb, Gerhard Baumb | Requires cookie* | | Title
| Synthesen und Strukturen von 2,5-Bis(2-arylvinyl)-l,4-benzochinonen und deren photochemisches Verhalten im Kristall Syntheses and Crystal Structures of 2,5-Bis(2-arylvinyl)-l,4-benzoquinones and their Photochemical Reactivity in the Crystalline State  | | |
Reference
| Z. Naturforsch. 48b, 1411—1418 (1993); eingegangen am 14. Mai 1993 | | |
Published
| 1993 | | |
Keywords
| 2, 5-D istyryl-l, 4-benzoquinones, Synthesis, Crystal Structure, Solid State Photochemistry | | |
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| default:Reihe_B/48/ZNB-1993-48b-1411.pdf | | | Identifier
| ZNB-1993-48b-1411 | | | Volume
| 48 | |
40 | Author
| Jörn Müller, Ke Qiao, Regina Schubert, M. Atthias Tschampel | Requires cookie* | | Title
| ;r-01efin-Iridium-Komplexe, XVIII [1] Reaktionen von Bis[cycloocta-l,5-dien-//-chloro-iridium] mit w-Propyllithium in Gegenwart von Alkinen yr-Olefin Iridium Complexes, XVIII [1] Reactions of Bis[cycloocta-l,5-diene-/z-chloro-iridium] with n -Propyllithium in the Presence of Alkynes  | | | Abstract
| The reaction of [(cod)IrCl]2 (cod = //4-cycloocta-l,5-diene) with n-C3H7Li gives non-isola-ble (cod)IrH species by /3-elimination of (cod)Ir-n-C3H7 intermediates; the stable final prod ucts of further reactions with RC = CR highly depend on the nature of the substituents R. With R = Me the 6-endo-H-hexamethylcyclohexadienyl complex 1 is obtained together with the iridacyclopentadienyl compound 2 and known }[(cod)IrH]4C3H4} (3). In case of R = Et steric effects cause transfer of the hydridic hydrogen to the cod ligand, and the hexaethyl-benzene species 4 is isolated which was characterized by crystal structure analysis. The reac tion system with tolane again yields a 6-enJo-H-cyclohexadienyl complex (5). In all cases free substituted benzenes are formed as cyclotrimerization products of the alkynes. | | |
Reference
| Z. Naturforsch. 48b, 1558—1564 (1993); eingegangen am 15. Juli 1993 | | |
Published
| 1993 | | |
Keywords
| Substituted Benzene, Cyclohexadienyl and Iridacyclopentadienyl Complexes, Synthesis, NMR Spectra, Crystal Structure | | |
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| default:Reihe_B/48/ZNB-1993-48b-1558.pdf | | | Identifier
| ZNB-1993-48b-1558 | | | Volume
| 48 | |
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