| 2 | Author
| A. Franken, W. Preetz | Requires cookie* | | Title
| Darstellung, n B-NMR-und Schwingungsspektren  | | | Abstract
| von Am inohexahydro-closo-hexaborat(l-), [B6H6(NH2)]~ sowie Kristallstruktur von Cs[B6H6(NH2)]*H 20 P rep aratio n , n B N M R and V ibrational Spectra of A m in o h e x a h y d ro -c lo so -h ex a b o ra te (l-), [B6H 6(N H 2)]' , and the C rystal S tructure of Cs[B6H 6(N H 2)] • H 20 By reduction of [B6H5(N0 2)]2_ with Fe2+ in aqueous alkaline solution [B6H6(NH2)]~ is formed. The compound has been separated by extraction with dichloromethane in the presence of tetrabutylammoniumbromid and precipitated from the organic phase by adding CsCH3COO/C2H5OH. The Crystal structure of Cs[B6H6(NH2)] H20 has been determined by single crystal X-ray diffraction analysis; monoclinic space group C2 with a = 22.1075(14), b = 6.491(2), c = 5.9570(4) Ä, ß = 100.168(6)°. The UB NMR spectrum is consistent with a mono-hetero-substituted octahedral B6 cage with local C4v symmetry. The IR and Raman spectra exhibit characteristic N -H , B -H and B6 vibrations. | | |
Reference
| (Z. Naturforsch. 50b, 11—14 [1995]; eingegangen am 9. August 1994) | | |
Published
| 1995 | | |
Keywords
| Aminohexahydro-closo-hexaborate(l-), Crystal Structure, UB NMR Spectra, Vibrational Spectra | | |
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| default:Reihe_B/50/ZNB-1995-50b-0011.pdf | | | Identifier
| ZNB-1995-50b-0011 | | | Volume
| 50 | |
4 | Author
| Z. Naturforsch | Requires cookie* | | Title
| K34[Zn2oIn85]: Eine ternäre Auffüllungsvariante des /?-rhomboedrischen Bors  | | | Abstract
| In the crystal structure of K34[Zn2()In85] (a = 1827.7(5) pm, c = 3980.5(8) pm, R3m , Nr. 166, Z = 3, R1 = 0.056, wR2 = 0.124) the In and Zn atoms form the /3-rhombohedral boron structure. The structure contains In84 Samson polyhedra, and clusters of 18 In and 10 Zn atoms, forming three In12 icosahedra sharing two common triangular faces. The potassium atoms occupy the centres of truncated tetrahedra -forming the Samson polyhedra -and Kasper polyhedra. | | |
Reference
| (Z. Naturforsch. 50b, 23 [1995]; eingegangen am 16. Juni 1994) | | |
Published
| 1995 | | |
Keywords
| Crystal Structure, Intermetallic Compound, Potassium, Zinc, Indium | | |
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| default:Reihe_B/50/ZNB-1995-50b-0023.pdf | | | Identifier
| ZNB-1995-50b-0023 | | | Volume
| 50 | |
6 | Author
| Z. Naturforsch | Requires cookie* | | Title
| Com plex F orm  | | | Abstract
| ation and M etal E x tractio n with H eterocyclic /3-Dicarbonyl C om pounds as C om parison. S tru ctu re of 3-Phenyl-4-benzoyl-5-isoxazolone E rh ard U hlem ann*, A lw in Friedrich, G erald H insche, W ulfhard M ickler, Acid constants and stability constants of nickel and zinc chelates with 2-thenoyltrifluoro-acetone, dibenzoylmethane, l-phenyl-3-methyl-4-benzoyl-5-pyrazolone and 3-phenyl-4-ben-zoyl-5-isoxazolone were compared. The extraction of copper was studied. Thermoanalytic measurements were made using the ligands and their copper compounds in the solid state. The molecular structure of 3-phenyl-4-benzoyl-5-isoxazolone was determined by X-ray analy sis. Crystal data: a = 874,7(2), b = 1959,2(7), c = 897,38(7) pm; ß = 101,030(7)°; space group P 12j/c 1; Z = 4; R = 0,043; 1920 observed, unique reflexions. | | |
Reference
| (Z. Naturforsch. 50b, 37—42 [1995]; eingegangen am 11. Juli 1994) | | |
Published
| 1995 | | |
Keywords
| 3-Phenyl-4-benzoyl-5-isoxazolone, Crystal Structure, Thermal Stability, Complex Stability Constants, Dioxane/Water-Mixtures | | |
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| default:Reihe_B/50/ZNB-1995-50b-0037.pdf | | | Identifier
| ZNB-1995-50b-0037 | | | Volume
| 50 | |
7 | Author
| J. Feldmann, Hk Miiller-Buschbaum | Requires cookie* | | Title
| Kristallstrukturuntersuchung an einem Strontium-Vanadyl-Vanadat: Sr2(V 0 )V 20 8 Crystal Structure Investigation of the Strontium Vanadyl-Vanadate: Sr2( V 0 ) V 20 8  | | | Abstract
| Single crystals of Sr2(V 0)V 20 8 have been prepared by quenching melts from higher tem peratures. This compound represents a new structure type and crystallizes with monoclinic symmetry, space group C |h-I 2 la, a = 6.929, b = 16.246, c = 7.260 A, ß = 115.82°, Z = 4. The point positions occupied by V5+ show tetrahedral coordination. The refinement of the V4+ position led to split positions with acentric orientations of V4+ in the octahedral O2-surrounding. It results in a square pyramidal coordination with one short V -O distance typically for vanadyl groups. | | |
Reference
| (Z. Naturforsch. 50b, 43—46 [1995]; eingegangen am 8. Juli 1994) | | |
Published
| 1995 | | |
Keywords
| Strontium, Vanadium Oxide, Crystal Structure | | |
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| default:Reihe_B/50/ZNB-1995-50b-0043.pdf | | | Identifier
| ZNB-1995-50b-0043 | | | Volume
| 50 | |
8 | Author
| H., M. Üller-Buschbaum, L. Walz | Requires cookie* | | Title
| Einkristallröntgenstrukturanalyse an Quecksilberchromat(VI)  | | | Abstract
| g 3 0 2 C r 0 4 Single C rystal X -Ray S tructure D eterm ination of a M ercury C hrom ate(V I): H g30 2C r 0 4 Th. H an sen , H k. Single crystals of Hg3C r0 6 have been prepared by high pressure techniques (3600 bar oxygen, 600 °C). Hg3C r06 crystallizes with trigonal symmetry, space group D |-P 3 212, a = 7.137(1), c = 10.017(2)Ä, Z -3. Nearly linear O -H g -O dumb-bells are connected in planes, forming strongly puckered nets of six-membered rings. Each Hg60 6 ring is centered by a C r04 tetrahedron; the C r04 tetrahedra are arranged in two equally occupied split positions. | | |
Reference
| (Z. Naturforsch. 50b, 47—5 [1995]; eingegangen am 2. August 1994) | | |
Published
| 1995 | | |
Keywords
| Mercury, Chromium, Oxide, Crystal Structure | | |
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| default:Reihe_B/50/ZNB-1995-50b-0047.pdf | | | Identifier
| ZNB-1995-50b-0047 | | | Volume
| 50 | |
9 | Author
| F.-DM. Artin, H.K M Üller-B, Uschbaum | Requires cookie* | | Title
| Eine synthetische Spezies zum Mineral Howardevansit mit Eisen anstelle von Kupfer: NaFe3V 30 12  | | | Abstract
| Single crystals of NaFe3V30 12 have been prepared by solid state reaction below the melt ing point of the reaction mixture. This compound is isotypic to the mineral Howardevansite but shows lower triclinic symmetry, space group C }-P 1 , a = 6.757(2), b = 8.155(2), c = 9.816(3) Ä, a = 106.05(2), ß = 104.401(9), y = 102.09(2)°, Z = 2. The acentric space group is caused by the sodium positions, all other atoms comply with the space group PI of Howarde vansite. The different ions are coordinated by O2-forming V 0 4 tetrahedra, FeOfi octahedra, trigonal FeOs bipyramids and irregular NaOs and NaOy polyhedra, respectively. The crystal chemistry is discussed with respect to Howardevansite. | | |
Reference
| (Z. Naturforsch. 50b, 51—55 [1995]; eingegangen am 5. August 1994) | | |
Published
| 1995 | | |
Keywords
| Sodium, Iron, Vanadium, Oxide, Crystal Structure | | |
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| default:Reihe_B/50/ZNB-1995-50b-0051.pdf | | | Identifier
| ZNB-1995-50b-0051 | | | Volume
| 50 | |
11 | Author
| E. Klüver, Hk Müller-Buschbaum | Requires cookie* | | Title
| Uber einen Lanthanoid-Mangan-Apatit: Nd4M n(Si04)30 On a Lanthanoid Manganese Apatite: Nd4M n(S i04)30  | | | Abstract
| Single crystals of Nd4M n (S i0 4)30 have been prepared by a Bi20 3 flux in closed copper tubes. The colourless crystals show hexagonal symmetry, space group C |h-P 6 3/m, a -9,4986(9), c = 6,944(2) A, Z = 2. Nd4M n (S i0 4)30 crystallizes in the A patite structure and shows Nd3+ and Mn2+ with partly statistical distribution. A s a consequence of this, 0 (2) and 0 (4) are occupying split positions. | | |
Reference
| (Z. Naturforsch. 50b, 61 [1995]; eingegangen am 25. Juli 1994) | | |
Published
| 1995 | | |
Keywords
| Neodymium, Manganese, Silicon, Apatite, Crystal Structure | | |
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| default:Reihe_B/50/ZNB-1995-50b-0061.pdf | | | Identifier
| ZNB-1995-50b-0061 | | | Volume
| 50 | |
12 | Author
| Inge Pabst3, Peter Sondergeld3, Mirjam Czjzekb, H. Artm, Ut Fuess3 | Requires cookie* | | Title
| Preparation and Crystal Structure Determination of [(C2H5 )4 N]2Hg3 Cl8  | | | Abstract
| X-Ray, Tetraethylammonium Chloromercurate, Cluster of [Hg3Cl8]2_ The title compound has been prepared in two different ways: First, by boiling single crystals of [(C2H 5)4N]H gC l3 in a mixture o f n-hexane/n-octane [4:1] at T = 350 K, and second, in a synthesis from stoichiometric quantities of the components. X-ray structure analysis gave the stoichiometry [(C2H 5)4N]?Hg3Cl8, monoclinic, space group P 2 1? a = 7.538(3), b = 19.909(6), c = 10.274(3) A , ß = 95.13(1)°, V = 1535.7(9) A 3, Z = 2. The basic [Hg3Cl8]2--units form broken zig-zag chains along [100]. The H g -C l distances within the [Hg3Cl8]2~ clusters range from 2.315(3) to 2.755(4) A. This is a new coordination type for halomercurates. | | |
Reference
| (Z. Naturforsch. 50b, 66—7 [1995]; received October 4 1994) | | |
Published
| 1995 | | |
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| default:Reihe_B/50/ZNB-1995-50b-0066.pdf | | | Identifier
| ZNB-1995-50b-0066 | | | Volume
| 50 | |
13 | Author
| Volker Lorenz3, Bernhard Neumiillerb, Karl-Heinz Thiele3 | Requires cookie* | | Title
| Synthese und Kristallstrukturen von Diazadien-Komplexen der Erdalkalimetalle Syntheses and Crystal Structures of Diazadiene Complexes of the Alkaline Earth Metals  | | | Abstract
| [C aN R -CPh=CPh-N R (D M E)2] 1 (R = C6H4-4 -C H 3; D M E = dim ethoxyethane) was pre pared by reaction of calcium with N R = C P h -C P h = N R in D M E solution. The compound forms orange, moisture sensitive crystals, which were characterized by an X-ray structure determination [space group orthorhombic, P 2 i2 12 1, Z = 4, 4634 observed unique reflections, R = 0.046; lattice dimensions at -7 0 °C: a = 1340.2(3), b = 1528.1(3), c = 1609.1(3) pm]. The calcium atom is coordinated by the four oxygen atoms of two chelating D M E molecules and two nitrogen atoms of the diazadiene ligand, bonded in its enediam ide form. [Ba2(D M E)3(N P h -C P h = C P h -N P h)2 DM E] 3 was obtained from barium metal and N Ph=C Ph-C Ph=N Ph in D M E solution as red crystals [space group monoclinic, P2!/c, Z = 4, 4000 observed unique reflections, R = 0.166; lattice dim ensions at -7 0 °C: a = 1704.5(3), b = 1786.1(4), c = 2177.4(4) pm, ß = 105.98(3)°]. The two barium atoms are bridged by two differently bonded diazadiene ligands (/<2-N ,N ';/i-N ,a -N '). Additionally, one of the barium atoms is coordinated to two DM E m olecules and the other one to only one of the ether molecules. A further DM E molecule is a constituent of the crystal lattice. | | |
Reference
| (Z. Naturforsch. 50b, 71—7 [1995]; eingegangen am 13. Juli 1994) | | |
Published
| 1995 | | |
Keywords
| Alkaline Earth Metal Complexes, Diazadiene Ligands, Enediamide Structure, X-Ray | | |
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| default:Reihe_B/50/ZNB-1995-50b-0071.pdf | | | Identifier
| ZNB-1995-50b-0071 | | | Volume
| 50 | |
14 | Author
| Christian Drost, Carsten Jäger, Uwe Klingebiel, Christina Freire-Erdbrügger, Regine Herbst-Irm, M. Er, Artina Schäfer | Requires cookie* | | Title
| Lithium-[N-di-terr-butylfluorsilyl-N' ,N ' -dimethyl-hydrazid] - Synthese, Kristallstruktur und Reaktivität Lithium (N-di-te/'f-butylfluorosilyl-N',N'-dimethyl)hydrazide - Synthesis, Crystal Structure and Reactivity  | | | Abstract
| Di-terf-butyldifluorosilane reacts with N-lithium -N',N'-dimethylhydrazine in a molar ratio 1:1 to yield the N-di-ferf-butylfluorosilyl-N',N'-dimethylhydrazine 1. The lithium derivative of 1 (2) forms a dimer with the nitrogen atoms coordinated "side-on" to the lithium atoms. The silylation with M e3SiCl gives product 3. Heating 2 in a vacuum leads to the cyclo-disilazane derivative 4. A bis(hydrazino)fluoroborane (5) is obtained in the reaction of 2 with trifluoroborane-etherate. | | |
Reference
| (Z. Naturforsch. 50b, 76—8 [1995]; eingegangen am 18. Juli 1994) | | |
Published
| 1995 | | |
Keywords
| Fluorosilylhyrazines, Lithium-Derivative, Crystal Structure, Side-on Coordination | | |
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| default:Reihe_B/50/ZNB-1995-50b-0076.pdf | | | Identifier
| ZNB-1995-50b-0076 | | | Volume
| 50 | |
15 | Author
| FrankW. Heinemann, Helm Ut, Hartung, NadjaM. Aier | Requires cookie* | | Title
| Kristall-und Molekülstruktur von 2-[3-(N,N-Diethylammonium)propylimino]-2-phenyl-dithioacetat Crystal and Molecular Structure of 2-[3-(N,N-Diethylammonium)propylimino]-2-phenyl-dithioacetate  | | | Abstract
| The title compound, formed by the reaction o f acetophenone with 3-diethylamino-1-propylamine and sulfur, crystallizes in the orthorhombic space group P 2 12 12 1 (Z = 4) with lattice constants a = 818.1(2) pm, b -1225.1(2) pm and c = 1622.4(4) pm. The characterization of the molecule as a zwitterion is established by the observed bond parameters. Both spec troscopic investigations and the results of the X-ray structure determination show that a hydrogen atom is bonded to the amino nitrogen rather than to the imino nitrogen. | | |
Reference
| (Z. Naturforsch. 50b, 81—8 [1995]; eingegangen am 9. August 1994) | | |
Published
| 1995 | | |
Keywords
| Dithioacetates, A cetophenone, Crystal Structure, Zwitterion, Betaine | | |
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| default:Reihe_B/50/ZNB-1995-50b-0081.pdf | | | Identifier
| ZNB-1995-50b-0081 | | | Volume
| 50 | |
17 | Author
| Andreas Puder3, Joachim Fuchs3, D. Ieter Lentz3, KlausR. Othb | Requires cookie* | | Title
| Das erste cyclische Isopolyoxoanion aus Oktaederbausteinen  | | | Abstract
| Synthese und Strukturbestimmung von Kaliumhexatellurat(VI) K8Te6O17(OH)10.1/2 KOH • 16 H20 The First Cyclic Isopolyoxo Anion Built from Octahedra. The Structure of the Potassium hexatellurate(VI) K8Te6O 1 7 (O H) 10 • 1/2 KOH • 16 H 20 The crystal structure of the potassium hexatellurate(VI) K8Te6O 17(O H)10-1/2K O H -16H 20 features a cyclic polyoxotellurate anion with six octahedral T e 0 6 units condensed through alternate sharing of edges and vertices. | | |
Reference
| (Z. Naturforsch. 50b, 91—9 [1995]; eingegangen am 13. April 1994) | | |
Published
| 1995 | | |
Keywords
| Polyoxo Anions, Tellurates(VI), Crystal Structure | | |
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| default:Reihe_B/50/ZNB-1995-50b-0091.pdf | | | Identifier
| ZNB-1995-50b-0091 | | | Volume
| 50 | |
18 | Author
| Thomas Albers, Joseph Grobe, Duc Le Van, Bernt Krebs, Mechtild Läge | Requires cookie* | | Title
| Reaktive  | | | Abstract
| E=C(p-p)^-Systeme, XL. Synthese und Struktur von Arsaalkenen des Typs F3CAs=C(F)NR2 Reactive E = C (p -p);r Systems, XL. Synthesis and Structure of Arsaalkenes of the Type F3 CAs=C(F)NR2 Bis(trifluoromethyl)arsane, Ammonolysis, Arsaalkenes The reaction of bis(trifluoromethyl)arsane 2 with secondary amines R2N H in a molar ratio of 1:3 at -6 0 °C allows the preparation of trifluoromethyl arsaalkenes o f the type F3C A s= C (F)N R 2 in moderate yields (1 5 -3 5 %) [N R 2 = N M e2 (3a), N M eEt (3b), N E t2 (3c)]. The main product of the reaction of 2 with M e2NH is the 1,1-diamino compound F3C A s=C (N M e2)2 (4a). With ethyl(isopropyl)-or di(isopropyl)am ine the corresponding de rivatives F3CAs=C(F)NEt(/Pr) (3d) and F3C A s=C (F)N (/Pr)2 (3e), respectively, are formed only in traces (3d), or not at all (3e). However, 3d and 3e can be prepared by reacting perfluoro-2-arsapropene with the corresponding secondary amines. The new compounds 3 a | | |
Reference
| (Z. Naturforsch. 50b, 94 [1995]; eingegangen am 21. Juli 1994) | | |
Published
| 1995 | | |
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| default:Reihe_B/50/ZNB-1995-50b-0094.pdf | | | Identifier
| ZNB-1995-50b-0094 | | | Volume
| 50 | |
19 | Author
| Michael Born, Dietrich Mootz, Sigrid Schaefgen | Requires cookie* | | Title
| Tautomere Wasserschichten. Bildung und Struktur tiefschmelzender Trihydrate von Triethylamin und 4-Methylpyridin [1] Tautomeric Water Layers. Formation and Structure of Low-Melting Trihydrates of Triethylamine and 4-Methylpyridine [1]  | | | Abstract
| Low-melting trihydrates of triethylamine (E t3N) and 4-methylpyridine (4-M ePy) have been confirmed and detected by phase analysis and the crystal structures determined. Both are monoclinic with space group P 2!/c and Z = 4 formula units per unit cell. The lattice parameters are a = 13.606, b = 6.291, c = 12.412 A , and ß = 99.47° at -1 0 0 °C for Et3N -3 H 20 , and a = 9.982, b = 6.877, c = 12.958 Ä , and ß = 103.50° at -9 0 °C for 4-M eP y-3 H20 . The water m olecules in the two structures are hydrogen-bonded in condensed four-, five-, and six-membered rings with 1:2:1 ratio, thus forming characteristic layers parallel (1 0 0) of identical topology and tautomeric to each other. The amine m olecules are linked to both sides of the layers by O -H — N bonds from different O atoms. | | |
Reference
| (Z. Naturforsch. 50b, 101—105 [1995]; eingegangen am 11. August 1994) | | |
Published
| 1995 | | |
Keywords
| Am ine Hydrates, Crystal Structure, Hydrates, Hydrogen Bonding, M elting Diagram, Water Layers | | |
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| default:Reihe_B/50/ZNB-1995-50b-0101.pdf | | | Identifier
| ZNB-1995-50b-0101 | | | Volume
| 50 | |
20 | Author
| M. Atthias Westerhausen, Wolfgang Schwarz | Requires cookie* | | Title
| Tetrakis(tetrahydrofuran-0)calcium-und -strontium-bis[bis(trimethylsilyl)- arsanid] -Vergleich der spektroskopischen Parameter sowie der Molekülstrukturen Tetrakis(tetrahydrofuran-0)calcium and Strontium Bis[bis(trimethylsilyl)- arsanide] -A Comparison of the Spectroscopic Param eters and the Molecular Structures  | | | Abstract
| Calcium-and strontium bis[bis(trimethylsilyl)amide] react with bis(trimethylsilyl)arsane in tetrahydrofuran to give the corresponding tetrakis(tetrahydrofuran-O) metal bis[bis(trime-thylsilyl)arsanides]. The calcium derivative crystallizes in the triclinic space group P I with a = 1191.7(2), b = 1232.0(2), c = 1655.0(2) pm, a = 102.46(1)°, ß = 107.92(1)°, y = 104.66(1)° and Z = 2, the strontium derivative in the orthorhombic space group Pbca with a = 2153.4(3), b = 1852.2(3), c -2182.4(3) pm and Z = 8. Both m olecules exist as frans-isomers with a nearly linear A s -M -A s moiety; however, the strontium analogue contains two remarkably different configurations for the arsenic atoms. One A s atom is surrounded nearly trigonally planar with a S r -A s bond length of 310 pm, whereas the other pnictogen atom has an angle sum of 338° with a S r -A s distance of 315 pm. | | |
Reference
| (Z. Naturforsch. 50b, 106 [1995]; eingegangen am 2. August 1994) | | |
Published
| 1995 | | |
Keywords
| Arsanide, Bis(trimethylsilyl)arsanide, Calcium, Strontium, NM R Spectra | | |
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| default:Reihe_B/50/ZNB-1995-50b-0106.pdf | | | Identifier
| ZNB-1995-50b-0106 | | | Volume
| 50 | |
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