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41	Author	Anne-Kathrin Duhme, Henry Strasdeit	Requires cookie*
	Title	Ligandenmangelkomplexe des Cadmiums. Synthese und spektroskopische Charakterisierung molekularer (Pentafluorphenyl)cadmium-Thiolate und die Struktur des Cubankomplexes [{Cd(C6F5)(SBur)}4] Ligand-Deficient Complexes of Cadmium. Synthesis and Spectroscopic Characterization o f Molecular Pentafluorophenyl Cadmium Thiolates and the Structure o f the Cubane Complex [{Cd(C6F5)(SBuf)}4]
	Abstract	In toluene, bis(pentafluorophenyl)cadmium(II) and thiols RSH (R = Bu', 2,4,6-Pr'3C6H2, 2,4,6-Bu'3C6H2) react to give soluble pentafluorophenyl cadmium thiolates [(Cd(C6F5)(SR)} J. The compounds [{Cd(C6F 5)(SBu')}4] (1)0 .5 C6H5CH3, [ {Cd(C6F5)(SC6H2Pr'3-2,4,6)} J (2)-ca. 0.25n C6H 5CH3, and [{Cd(C6F5)(SC6H2Bu'3-2,4,6)} J (3) ca. 0.25« C6H5CH3 have been prepared in 65, 59 and 78% yield, respectively. 1-0.5 C6H5CH3 crystallizes in the triclinic space group PI with a = 11,635(1)Ä, b = 11.583(1)Ä, c = 21.480(2)Ä, a = 82.12(1)°, ß = 76.26(1)°, y — 89.35(1)°, and Z = 2. 1 is a cubane-type complex with a {Cd4(/z3-SBur)4}4+ core. Each Cd atom is coordinated by three bridging thiolato ligands and one terminal C6F5 group (C d -S 2.62 A, C d -C 2.15Ä (mean values)). The central C atoms of the Bu'S" ligands of 1 show a remarkable low-field shift o f their 13C N M R resonance (12.3 ppm relative to the value of the free thiol). A characteristic spectral feature of (Cd(C6F5) } + complexes is the large value of the coupling constant 2/ (19F ,13C) o f the ipso-C atom (1, 2: 68 Hz; 3: 67 Hz). The complexes [Cd(C6F5)(SR) + H]+, [Cd(SR)2 + H]+, and [Cd2(SR)3]+ were identified in the Cl mass spectra (/50-butane) of 2 and 3.
	Reference	(Z. Naturforsch. 49b, 119—127 [1994]; eingegangen am 17. August 1993)
	Published	1994
	Keywords	Cadmium Complexes, Thiolates, Crystal Structure, NMR Spectra, Mass Spectra
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	TEI-XML for	default:Reihe_B/49/ZNB-1994-49b-0119.pdf
	Identifier	ZNB-1994-49b-0119
	Volume	49

42	Author	Dietrich Mootz, Michael Born	Requires cookie*
	Title	Niedere Hydrate von Aminen. Kristallstrukturen der Hemihydrate von Ethyl-und Diethylamin sowie des Hemi-und Monohydrats von 1-Butylamin [1] Lower Hydrates of Amines. Crystal Structures of the Hemihydrates of Ethyl-and Diethylamine and the Hemi-and M onohydrate of 1-Butylamine
	Abstract	The melting diagrams of three systems alkylamine-water have been reexamined and the crystal structures of four lower hydrates determined for the first time. The hydrate EtNH2 -0.5 H20 , m.p. -72 °C, is triclinic with space^roup P 1 and Z = 4 formula units per unit cell of dimensions a = 5.104, b = 8.137, c = 9.394 Ä, a = 100.41, ß = 98.41 and y = 97.96° at -150°C. The O and N atoms are hydrogen-bonded into a two-dimensional array l[ON6/3] analogous to the layer of the Cdl2 structure type. The hydrate Et2NH • 0.5 H20 , m.p. -20 °C, is monoclinic with 12/a, Z = 8 , a -8.324, b = 15.090, c = 10.006 Ä and ß -103.34° at -100 °C. The O and N atoms are linked into a four-membered ring spiro chain ifON^] analogous to that in SiS2. The hydrate l-BuNH2 0.5H20 (m.p. -57 °C, monoclinic, P 2x/c, Z = 8,a = 14.994, b = 5.086, c = 16.15 A .,ß -103.45° at -81 °C) contains essentially the same hydrogen-bonded array as the hydrate EtNH,-0.5H20 (see above). l-BuNH2-H20 , the only monohydrate in vestigated besides the three hemihydrates (m.p. -60 °C, monoclinic, C 2/m, Z = 4, a = 9.68, b = 4.238, c = 15.58 A, ß = 94.9° at -81 °C), has also a two-dimensional H20/N H 2 partial structure, similar to a subset of the three-dimensional network of the adduct NH3 H20 of analogous composition. Z ur Bildung kristalliner Hydrate von einfachen Alkylaminen gibt es eine Reihe von z. T. schon recht frühen Untersuchungen mit allerdings nicht immer eindeutigen und widerspruchsfreien Ergebnissen. Die Bestimmung von Kristallstrukturen be schränkte sich bisher auf einige höhere Hydrate mit W assergehalten oberhalb denen von Pentahydra-ten. Solche wasserreichen Phasen wurden als Cla-thrathydrate oder Semiclathrate charakterisiert. Sie enthalten nämlich dreidimensional vernetzte W irtsstrukturen aus den W assermolekülen und in deren m ehr oder weniger gestörten polyedrischen H ohlräum en die fast immer auch noch H-brücken-aktiven (N -H — O und/oder O -H -N) Am in moleküle als Gastspezies [2]. Gegenstand der vorliegenden A rbeit sind nun erstmals K ristallstrukturen niederer Hydrate von * Sonderdruckanforderungen an Prof. Dr. D. Mootz.
	Reference	Z. Naturforsch. 49b, 243—249 (1994); eingegangen am 27. Oktober 1993
	Published	1994
	Keywords	Amine Hydrates, Lower Hydrates, Melting Diagram, Crystal Structure, Hydrogen Bonding
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	TEI-XML for	default:Reihe_B/49/ZNB-1994-49b-0243.pdf
	Identifier	ZNB-1994-49b-0243
	Volume	49

43	Author	P. Souza, M. A. Mendiola3, A. Arquerob, V. Ferná, E. G Utiérrez-Pueblac, C. Ruiz-Valeroc	Requires cookie*
	Title	Copper(II) Complexes of Hydrazone Derivatives
	Abstract	Three benzil based, macrocyclic oxygen-, nitrogen-, and sulfur-containing ligands, (3,4,10,11 -tetraphenyl-1,2,5,6,8,9,12,13-octaazacyclotetradeca-7,14-dithione-2,4,9,11 -tetraene) ethanol (L 1), 10,1 l-diethoxy-3,4,10,11-tetraphenyl-1,2,5,6,8,9,12,13-octaazacyclotetradeca-7.14-dithione-2,4-diene (L2), (3,4,10,11 -tetraphenyl-1,2,5,6,8,9,12,13-octaazacyclotetradeca-7.14-dione-2,4,9,l 1-tetraene) ethanol (L3); a cyclic ligand, 6-ethoxy-l,6-diphenyl-4-oxo-3,4,5,6-tetrahydro-2,3,5-triazine (L5) and two open chain ligands, benzilsemicarbazone (L6) and benzilbisthiosemicarbazone (L4) are reported. These ligands react with copper(II) chlor ide, nitrate and acetate. The complexes obtained have been characterized on the basis o f N M R , IR, electronic and mass spectral studies, conductance and analytical data. The sto-ichiometry and the spectroscopic data o f the complexes indicate that the copper ions are coor dinated by neutral ligands or by ligand anions formed by loss o f protons from the ligand. The molecular and crystal structure o f 6-ethoxy-l,6-diphenyl-4-oxo-3,4,5,6-tetrahydro-2,3,5-triazine (L 5) was determined by X-ray diffraction; the space group is triclinic, P 1 with a = 7.865(1), b = 14.101(6), c = 15.733(9) A, a = 69.10(3)°, ß = 75.62(2)°, y = 86.69(2)°, V = 1578(1) A 3, Z = 4.
	Reference	Z. Naturforsch. 49b, 263—2 (1994); received June 2/October 4 1993
	Published	1994
	Keywords	Benzil, Hydrazones, Copper(II), M acroligands, Crystal Structure
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	Identifier	ZNB-1994-49b-0263
	Volume	49

44	Author	Meyer Zu Köcker, Andreas Behrendt, K. Urt Dehnicke, Dieter Fenske	Requires cookie*
	Title	Phosphaniminato-Cluster des
	Abstract	Kupfers. Synthese und Kristallstrukturen von ICu6Cl6(NPM e3)4\|Cl[Me3SiNPM e3\| • CH2C12 und ICu6Cl6(NPM e3)4l[Cu(Me3SiNPM e3)2lCl2 Phosphoraneim inato Clusters o f Copper. Syntheses and Crystal Structures of [Cu6Cl6(N PM e3)4]Cl[Me3SiNPM e3] • C H 2C12 and [Cu6Cl6(NPM e3)4][Cu(Me3SiNPM e3)2]Cl2 R olf The title com pounds have been prepared as black-blue crystals with metallic lustre by the reaction o f CuCl2 and CuCl, respectively, with M e3SiN P M e3 in C H 2C12 suspensions. The com plexes have been characterized by cyclic voltammetry and by crystal structure determinations. [Cu6Cl6(N P M e3)4]Cl[M e3SiN P M e3] • C H 2C12: Space group P 2,2,2,, Z = 4, structure solution with 4407 unique observed reflections, R = 0.057. Lattice dimensions at -7 0 °C: a -1159.3(8), b = 2027.1(14), c = 2063.3(12) pm. The compound consists o f cluster ions [Cu6Cl6(N P M e3)4]+, in which the copper atom s form a regular octahedron. Four planes o f the octahedra are capped by //3-nitrogen atom s o f the (N P M e3)~ groups. Each o f the Cu atom s is connected with a terminal chlorine atom . Another chloride ion serves for charge com pensa tion; this ion occupies another Cu3 plane o f the octahedron. W ithout bonding interaction one M e3SiN P M e3 molecule and one C H 2C12 molecule are included in the lattice. [Cu6Cl6(N P M e3)4][Cu(M e3SiN P M e3)2]Cl2: Space group Pna2,, Z = 4, structure solution with 5676 unique observed reflections, R = 0.071. Lattice dimensions at -7 0 °C: a = 3117.2(21), b = 1927.4(11), c = 1002.7(8) pm. The compound consists o f cluster ions [Cu6Cl6(N P M e3)4]+, the com plex ion [Cu(M e3SiN PM e3)2]+, and chloride ions. In the cation [Cu(Me3SiN P M e3)2]+ the copper atom is linearly coordinated by the nitrogen atom s o f the phosphaneimine m olecules.
	Reference	Z. Naturforsch. 49b, 301—3 (1994); eingegangen am 18. November 1993
	Published	1994
	Keywords	Phosphoraneim inato Clusters o f Copper, Synthesis, Cyclic Voltammetry, Crystal Structure
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	Identifier	ZNB-1994-49b-0301
	Volume	49

45	Author	Holger Szillat, Hanskarl Müller-Buschbaum	Requires cookie*
	Title	Synthese und Kristallstruktur von KCuHo2Mo40 16 Synthesis and Crystal Structure of K C uH o2M o40 I6
	Abstract	Single crystals o f K C uH o2M o40 16 have been prepared by recrystallisation from melts and investigated by X-ray diffractometer techniques. The compound crystallizes with m onoclinic symmetry, space group C 2/c, a = 521.6(1), b = 1251.3(2), c = 1953.1(2) pm, ß = 92.903(18)°, Z -4. K C uH o2M o40 16 represents a new structure type characterized by H oO s and alternate CuO6/K O 10 polyhedra chains. The connection o f these polyhedra chains to each other and by M o 0 4 tetrahedra is described and the crystal structure discussed with respect to related com pounds o f the C uLnM o2Os and K L nM o20 8 types.
	Reference	Z. Naturforsch. 49b, 350 (1994); eingegangen am 10. Dezember 1993
	Published	1994
	Keywords	Crystal Structure, Copper, H olm ium, M olybdenum, Potassium
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	Identifier	ZNB-1994-49b-0350
	Volume	49

46	Author	Mitra Ghassemzadeh, Kurt Dehnicke, Helmut Goesmann, Dieter Fenske	Requires cookie*
	Title	//2-Halogenokomplexe von N-Iodsuccinimid. Die Kristallstrukturen von PPh4[X(N-Iodsuccinimid)2] * CH3CN mit X = Cl, Br, I /^2-Halogeno Complexes of N-Iodosuccinimide. The Crystal Structures of PPh4 [X(N-Iodosuccinimide)2] * CH 3CN with X = Cl, Br, I
	Abstract	The ,a2-halogeno complexes PPh4[X(N-Iodosuccinimide)2] • CH 3CN with X = Cl. Br, I have been prepared by reactions of N-Iodosuccinimide with the corresponding tetraphenylphos-phonium halides PPh4X in acetonitrile solutions. The compounds form pale yellow crystal needles, which were characterized by IR spectroscopy and by crystal structure determina tions. PPh4[Cl(N-Iodosuccinimide)2] C H 3CN (1): Space group Pna2!, Z = 4, 4461 observed unique reflections, R -0.027. Lattice dimensions at -6 0 °C: a = 1840.5(9), b = 2589(1), c = 728.2(4) pm.
	Reference	Z. Naturforsch. 49b, 602—608 (1994); eingegangen am 22. Dezember 1993
	Published	1994
	Keywords	Halogeno Complexes of N-Iodosuccinimide, Synthesis, IR Spectra, Crystal Structure
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	Identifier	ZNB-1994-49b-0602
	Volume	49

47	Author	M. Ahm, Shakibaie-M Oghadam, Ulrich Timper, Gert Heller	Requires cookie*
	Title	Darstellung und Struktur dreier verschiedener Bis(ethylendiamin)-kupfer(II)-tetraborate Preparation and Structure o f Three Different Bis(ethylenediamine) Copper(II) Tetraborates
	Abstract	Three different bis(ethylenediamine) Copper(II) tetraborates have been prepared: Cu(en),[B40 5(0 H)4]-2 B (0 H)3 (A), 2{Cu(en),B (0H)3 H 20[B 40 5(0 H)4]} H ,0 (B) and
	Reference	Z. Naturforsch. 49b, 627—634 (1994)
	Published	1994
	Keywords	Bis(ethylenediamino) Copper Tetraborates, Boric Acid Molecules, Preparation, Crystal Structure
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	Identifier	ZNB-1994-49b-0627
	Volume	49

48	Author	IrinaB. Ecker, M. Arcus, W. Indhaus, R. Ainer, M. Attes	Requires cookie*
	Title	Synthesen, 121Sb-Mößbauer-Spektren und
	Abstract	Strukturen von [SbF3(18-Krone-6)], [SbF3(18-Krone-6)]*CH3CN und [(SbF3)2(12-Krone-4)] Synthesis, 121Sb-M ößbauer Spectra and S tructures of [SbF3(18-Crown-6)], [SbF3(18-Crown-6)] C H 3CN, and [(SbF3)2(12-Crow n-4)] The crown ether complexes SbF3(18-crown-6) (1), SbF3(18-crown-6) • CH3CN (2) and (SbF3)2(12-crown-4) (3), have been prepared by reactions of SbF3 and the corresponding crown ether. They have been characterized by IR. Raman and 121Sb-Mößbauer spectroscopy, and by X-ray structure determinations. The s electron density at the Sb atom is diminished in these complexes. 1 and 2 show a symmetrical half-sandwich structure, with coplanar O atoms and S b -O distances ranging from 298 to 321 pm. 3 has a band-like structure. The two metal centers adopt different stereochemistries. The S b -O distances are in the range from 269 to 325 pm. One oxygen atom of 12-crown-4 has a bridging function. Crystal data for 1: space group P 21212i, a = 823,1(1), b = 1146,1(2), c = 1807,0(3) pm, Z = 4; 2: space group P2,/c. a = 1257,7(3), b = 828,9(2), c -1895,5(5) pm, ß = 93,68(2). Z = 4; 3: space group P2j/c, a = 805,6(1), b = 2143,1(4), c = 836,4(2) pm, ß = 90,98(1), Z = 4.
	Reference	Z. Naturforsch. 49b, 870—876 (1994); eingegangen am 30. Dezember 1993
	Published	1994
	Keywords	Crown Ether Complexes of SbF3, 121Sb-Mößbauer Spectra, Crystal Structure
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	Identifier	ZNB-1994-49b-0870
	Volume	49

49	Author	Birgit Bäck, H. An, S. Preut	Requires cookie*
	Title	Uber die Reaktionen von Molekülen
	Abstract	(R2CS)2 (R = CF3, CI) und C12CS mit XeF+MF6-(M = As, Sb) und Kristallstruktur von (CF3)2CSC(CF3)2SF+SbF6-[1] O n th e R eactions of M olecules (R 2C S)2 (R = C F 3, Cl) and C12CS with X eF +M F6_ (M = As, Sb) and C rystal Structure of (C F3)2C SC (C F3)2SF+SbF6~ [1] R olf M inkwitz XeF+MF6_ (M = As, Sb) reacts with ((CF3)2CS)2 and C12CS to form the corresponding monofluorinated sulfonium hexafluorometalates. The salts have been characterized by vibra tional and 19F NMR spectroscopic measurements. (CF3)2CSC(CF3)2SF+SbF6^ crystallizes in the monoclinic space group C2/c with a =o 14.791(10), b = 11.093(6), c -10.356(6)Ä, ß -119.83° and Z = 4. With a value of 1.51(1) A d (S -F) is comparable to the SF-bond distance in (CF3)(C1)CSC(CF3)(C1)SF+AsF6-.
	Reference	Z. Naturforsch. 49b, 881—888 (1994); eingegangen am 10. November 1993
	Published	1994
	Keywords	Monofluorosulfonium Salts, Preparation, Vibrational Spectra, 19F NMR Data, Crystal Structure
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	Identifier	ZNB-1994-49b-0881
	Volume	49

50	Author	Blaschette, PeterG. Jones, Karin Linoh, Ilona Lange, M. Artina Näveke, Dagmar Henschel, Axel Chrapkowski, Dietm Ar, Schomburg	Requires cookie*
	Title	Arm
	Reference	Z. Naturforsch. 49b, 999—1011 (1994); eingegangen am 1. Februar 1994
	Published	1994
	Keywords	Polysulfonylamines, 18-Crown-6-Dimesylamine (3/2), Synthesis, Crystal Structure, Coronand Conformation
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	Identifier	ZNB-1994-49b-0999
	Volume	49

51	Author	H. Bocka, T. H. Auck3, C. N. Äthera, Z. Havlasb	Requires cookie*
	Title	Wechselwirkungen in Kristallen, 35 [ 1, 2]
	Abstract	Einkristallzüchtung von Na0 ^C(NO2)3 [*] aus Etherlösungen zu einem polymeren Band [(Na" 9 C (N 0 2)3) D io x a n ^ und einem Lösungsmittel-getrennten Ionenpaar [(Na0 /18-Krone-6)(THF)2]0 [(Na0 /18-K rone-6)(O N O -C e (NO 2)2)2]e Interactions in Crystals, 35 [1, 2] Single Crystal Growths of Na0 e C (N O 2)3 [] from Ether Solutions to a Polymer Band [(Na0 e C (N O2)3)Dioxane]TO and to a Solvent-Separated Ion Pair [(Na0 /18-Crown-6)(THF)2]0 [(Na0 /18-C row n-6)(O N O -C e (N O 2)2)2]e The sodium salt of the most simple polynitro-substituted hydrocarbon anion, Na0 e C (N O 2)3, (for a hazard warning cf. [**]) crystallizes from ether solutions without and with addition of 18-crown-6 either in a polymer band, [(Na®0 C (N O 2)3)dioxane]oo, or as a solvent-separated ion pair, [(Na®/18-crown-6)(THF2]0 [(Na®/18-crown-6)(O2N -C e (N O 2)2)2]e . The Na® cations are each 8-fold coordinated in hexagonal bipyramidal arrangement. According to extensive quantum-chemical calculations based on the structure coordinates, the formation of these novel salts can be traced back to the charge distribution in the anions e C (N 0 2)3, which due to negatively charged oxygen centers are favorable complex ligands. The structure determining effects of solvation are discussed.
	Reference	Z. Naturforsch. 49b, 1012—1020 (1994); eingegangen am 31. Januar 1994
	Published	1994
	Keywords	Trinitromethanide Salts, Single Crystal Structure, M N DO Calculations, Solvation Effects
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	Identifier	ZNB-1994-49b-1012
	Volume	49

52	Author	Hans Bocka, Sabine Nicka, ChristianN. Äthera, JanW. Bats3, Professor Franz-Gustav	Requires cookie*
	Title	Strukturen ladungsgestörter Moleküle, 47 [1 , 2 ] Dinatrium-und Dikalium-Nitranilate: Die Cyanin-Verzerrung der Kohlenstoff-Sechsringe Structures of Charge-Perturbed Molecules 47 [1,2] Disodium and Dipotassium Nitranilates: The Cyanine Distortion of the Six-Membered Carbon Ring
	Abstract	Crystals of lemon yellow dipotassium nitranilate and of yellow disodium nitranilate di hydrate have been grown and their structures determined at 290 and 200 K. The six-member-ed, 0 2N-disubstituted rings show a pronounced cyanine distortion with all four CO bonds identical and the two (0 C C (N 0 2) C 0) e chains connected by single CC bonds of each 156 pm length. In the anhydrous K® salt, the ring is planar, but in the Na® hydrate salt it exhibits a twist conformation. Quantum chemical calculations allow to reproduce the structure in every detail, demonstrate strong charge alternation along the cyanine chains with considerable delocalization into the 0 2N acceptor substituents, and suggest that the rather long connecting CC bonds contain positively charged carbon centers on both ends. In addition, metal ion coordination effects as well as the rather high pKa value of nitranilic acid are rationalized.
	Reference	Z. Naturforsch. 49b, 1021—1030 (1994); eingegangen am 17. März 1994
	Published	1994
	Keywords	Cyanine Distortion of C6-Rings, Single Crystal Structures, Semiempirical Calculations
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	Identifier	ZNB-1994-49b-1021
	Volume	49

53	Author	W. Lübbe, A. Franken, W. Preetz	Requires cookie*
	Title	Darstellung, n B-, 13C-, 'H-NMR-und Schwingungsspektren
	Abstract	von 1.2-Trimethylenpentahydro-closo-Hexaborat(l -) , c i s -[B6H5(CH2)3]" und 1.2-TetramethyIenpentahydro-closo-Hexaborat(l-), cjs-[B6H5(CH2)4]_ sowie Kristallstrukturen von [P(C6H5)4][B6H5(CH2)3] und [P(C6H5)4][B6H5(CH2)4] Preparation, n B, 13C, 'H NMR and Vibrational Spectra of 1.2-Trim ethylenepentahydro-closo-hexaborate(l-), ds-[B 6H 5(C H 2)3]_, and 1.2-Tetram ethylenepentahydro-closo-hexaborate(l-), ds-[B 6H 5(CH 2)4]~, and the Crystal Structures of [P(C6H 5)4][B6H 5(CH 2)3] and [P(C6H 5)4][B6H 5(C H 2)4] 1.2-Trimethylenepentahydro-closo-hexaborate(l -) , 1.2-Tetram ethylenepentahydro-closo-hexaborate(
	Reference	Z. Naturforsch. 49b, 1115—1122 (1994); eingegangen am 17. Januar 1994
	Published	1994
	Keywords	), Crystal Structures, 'H NM R Spectra, Vibrational Spectra
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	Identifier	ZNB-1994-49b-1115
	Volume	49

54	Author	M. Arcos, L. Uján, FrankKubel H Ans Schmid	Requires cookie*
	Title	Crystal Growth and X-Ray Structure of Metastable «-KC0 PO 4
	Abstract	Crystals o f KC0PO4 were obtained by growth in a gel of tetramethoxysilane/water at 64 °C. The hexagonal crystals have space group P 63, a = 18.206(1), c = 8.5135(8) [Ä], V = 2443.8(4) [A 3]. Z = 24. The structure was solved by single crystal X-ray diffraction methods. The struc ture is isotypic with a -K Z n P 0 4. It comprises an ordered three dim ensional network o f alter nating C oÖ 4 and P 0 4 tetrahedra. which has rings of six tetrahedra in the xy plane. These rings form tunnels in the [001] direction, where the potassium ions are located. U pon heating, the compound undergoes a phase transition at about 565 °C; on cooling, the phase transition occurs at 449 °C, where it transforms into another structure which is yet unknown. This indicates that the hexagonal structure is a metastable phase.
	Reference	Z. Naturforsch. 49b, 1256—1262 (1994); received May 4. 1994
	Published	1994
	Keywords	Potassium Cobalt Orthophosphate Crystal Structure, Crystal Growth, Metastable Phase Phase Transition
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	Identifier	ZNB-1994-49b-1256
	Volume	49

55	Author	Hendrik Möller, Ellen Suchanek, HeinzDieter Lutz, Werner Paulus	Requires cookie*
	Title	Neutronenbeugungs-Untersuchung von M g(I03)2*4H 20 -Einkristallen Neutron Diffraction Studies on M g (I0 3 )2 -4H 20 Single Crystals
	Abstract	The crystal structure of M g (I 0 3)2-4 H 20 has been determined by neutron single crystal diffraction (P2j/c, Z = 2, R = 2,2% on the basis of 1107 observed reflections). M g (I 0 3)2-4 H 20 forms a layered structure built up of octahedral M g(H 20) 4(I 0 3)2 units linked by hydrogen bonds. The two crystallographically different water m olecules are in volved in asymmetric, nearly linear hydrogen bonds to adjacent iodate ions (vOD of matrix isolated HDO: 2480, 2475, 2425 und 2412 cm -1, IR spectroscopic data, 90 K). The strength of the hydrogen bonds as well as that of other iodate hydrates is discussed in terms o f both the synergetic effect and Brown's bond valences.
	Reference	Z. Naturforsch. 49b, 1334—1338 (1994); eingegangen am 2. Mai 1994
	Published	1994
	Keywords	Magnesium Iodate Tetrahydrate, Crystal Structure, Neutron Diffraction Studies, Hydrogen Bonds
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	TEI-XML for	default:Reihe_B/49/ZNB-1994-49b-1334.pdf
	Identifier	ZNB-1994-49b-1334
	Volume	49

56	Author	Stefan Horstmann, Wolfgang Schnick	Requires cookie*
	Title	Synthese, Kristallstruktur und Eigenschaften von Tetraaminophosphoniumiodid [P(NH2)4]I Synthesis, Crystal Structure, and Properties of Tetraaminophosphonium Iodide [P(NH2)4]I
	Abstract	The title compound has been prepared starting from phosphorothionic triamide SP(N H 2)3 by methylation of the sulfur atom and subsequent ammonolysis reaction in dry acetonitrile and dichloromethane, respectively, both at room temperature. Suitable single crystals are obtained from an acetonitrile solution in a temperature gradient between 70 °C and room temperature. The crystal structure o f [P(N H 2)4]I has been determined by single crystal X-ray methods (P 4!nbm\ a = 842.6(2), c = 486.7(2) pm, Z = 2). In the solid [P(NH2)4]+-and I~-ions are found with significant N -H -I -h y d r o g e n bonding interactions between anions and cations (H —I: 276.4 pm). The P -N -b o n d length in the cation (160.7(2) pm) represents the shortest P -N H 2 bond distance reported to date indicating a significant electrostatic strengthening. The condensation behaviour of [P(N H 2)4]I in solution and in the solid has been investigated.
	Reference	Z. Naturforsch. 49b, 1381—1386 (1994); eingegangen am 5. Mai 1994
	Published	1994
	Keywords	Tetraaminophosphonium Salt, Synthesis, Crystal Structure, Hydrogen Bonding, Condensation Reactions
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	TEI-XML for	default:Reihe_B/49/ZNB-1994-49b-1381.pdf
	Identifier	ZNB-1994-49b-1381
	Volume	49

57	Author	Roland Boese3, RolandK. Österb, M. Ohamed Yalpanib	Requires cookie*
	Title	Produkte der Carbodiimid-Hydroborierung mit (9H -9-BBN)2 [1] Hydroboration Products of Carbodiimides with (9H-9-BBN) 2 [1]
	Abstract	The hydroboration of H n C6N=C=NC6H n (A) with (9H -9-B B N)2 (C2) gives H n C6N=
	Reference	Z. Naturforsch. 49b, 1453—1458 (1994); eingegangen am 13. Mai 1994
	Published	1994
	Keywords	Carbodiimides, Addition of 9-BBN, Formamidine, Crystal Structure, Formaminal
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	Identifier	ZNB-1994-49b-1453
	Volume	49

58	Author	M. Anfred Fild, PeterG. Jones, Karsten Ruhnau, Carsten Thöne	Requires cookie*
	Title	Darstellung und Strukturen von 2,2,4,4-Tctrafluor-l,3-diphosphctancn und -1,3-diphosphetan-disulfiden Synthesis and Structures of 2,2,4,4-Tetrafluoro-l,3-diphosphetanes and of -1,3-diphosphetane Disulfides
	Abstract	A simple route to 1,3-diphosphetanes [RPCF2]2 [R = Ph, Me, Bu'] is described. The phos-phaalkene intermediates RP=CF2, as well as the corresponding disulfides [R (S)PC F2]2 have been characterized. The crystal structures of [PhPCF2]2, and of the sulfides [Ph(S)PCF2]2 and [Bu'(S)PCF2]2 are reported.
	Reference	Z. Naturforsch. 49b, 1361—1367 (1994); eingegangen am 6. Juni 1994
	Published	1994
	Keywords	Phosphaalkenes, 1, 3-Diphosphetanes, 1, 3-Diphosphetane Disulfides, NM R Spectra, Crystal Structure
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	TEI-XML for	default:Reihe_B/49/ZNB-1994-49b-1361.pdf
	Identifier	ZNB-1994-49b-1361
	Volume	49

59	Author	Peter Dierkes, Kurt Dehnicke, Dieter Fenske	Requires cookie*
	Title	Diinkomplexe
	Abstract	von Wolfram(VI). D ie Kristallstruktur von [(Et2S)WCl4(Me3S i-C = C -(C H 2)4 -C = C -S iM e 3)WCl4(SEt2)] Diyne Complexes of Tungsten(VI). The Crystal Structure of [(Et2 S)WCl4 (M e3Si -C = C -(C H 2)4-C ^ C -SiMe3) WCl4 (SEt2)] The diyne complexes [(Et2S)W C l4(R -C ^ C -(C H 2)" -C = C -R)W C l4(SEt2)] (R = SiM e3, n = 3, 4, 8; R = C6H 5, n = 4, 8) have been prepared by the reaction o f /rarcs-[WCl4(SEt2)2] with the corresponding diyne in toluene solutions. The com plexes form green or orange, diamagne tic, moisture sensitive crystal powders, which were characterized by their IR and 13C NM R spec tra. The crystal structure of the com plex with R = SiM e3 and n = 4 has been determined. [(Et2S)WCl4(M e3S i-C = C -(C H 2)4-C = C -S iM e 3)W Cl4(SE t2)]: Space group P2j/c, Z -2, 3620 observed unique reflections with I>2a(I), R = 0.027. Lattice dimensions at -7 0 °C: a -1431.8(11), b -839.6(8), c = 1731.3(11) pm, ß = 112.74(2)°. The structure consists o f m ole cules in which both tungsten atom s are surrounded by four chlorine atoms in equatorial positions, both alkyne groups are bonded side on (rj2) to the tungsten atoms, whereas the sulfur atoms of the diethylsulfide molecules are located trans to the alkyne groups.
	Reference	Z. Naturforsch. 49b, 1391—1396 (1994); eingegangen am 17. Mai 1994
	Published	1994
	Keywords	Diyne Complexes of Tungsten(VI), Synthesis, IR Spectra, NM R Spectra, Crystal Structure
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	TEI-XML for	default:Reihe_B/49/ZNB-1994-49b-1391.pdf
	Identifier	ZNB-1994-49b-1391
	Volume	49

60	Author	Hansjürgen Mattausch, Thomas Gulden, R. Einhard, K. Kremer, Jörg Horakh, A.Rndt Simon	Requires cookie*
	Title	H o4 C7, Y4 C7: Carbides with C34-and C4" Ions
	Reference	Z. Naturforsch. 49b, 1439—1443 (1994); eingegangen am 17. Mai 1994
	Published	1994
	Keywords	Holm ium Carbide, Yttrium Carbide, Crystal structure, Allenylide Ions, Paramagnetic Behaviour
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	TEI-XML for	default:Reihe_B/49/ZNB-1994-49b-1439_n.pdf
	Identifier	ZNB-1994-49b-1439_n
	Volume	49

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