| 1 | Author
| Moisés Morán, Miguel Gayoso | Requires cookie* | | Title
| Reactions of Dicyanogen and Cyanogen Halides with the Biscyclopentadienyls of Vanadium and Chromium  | | | Abstract
| The oxidative addition of dicyanogen, (CN)2, and of the cyanogen halides, XCN (X = Cl, Br or I), to the biscyclopentadienyl compounds of vanadium and chromium, (/y-C^Hs^M (M = V or Cr), leads to the formation of (/?-C5H5)2MX(CN) (X = CN, Cl, Br, I; M = V or Cr). The synthesized compounds have been characterized by elemental analyses, IR and EPR spectra, and determinations of the magnetic moments. | | |
Reference
| Z. Naturforsch. 38b, 177—180 (1983); received July 9/September 29 1982 | | |
Published
| 1983 | | |
Keywords
| Cyanogen Halides, Vanadium, Chromium | | |
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| default:Reihe_B/38/ZNB-1983-38b-0177.pdf | | | Identifier
| ZNB-1983-38b-0177 | | | Volume
| 38 | |
2 | Author
| Klaus Jonas, Volker Wiskamp, Professor Karl | Requires cookie* | | Title
| Olefin-, Aromaten-und Allylkomplexe des Vanadiums aus Vanadocen [1] Olefine, Arene, and Allyl Complexes of Vanadium from Vanadocene [1]  | | | Abstract
| Vanadocene (Cp2V) was reduced with potassium metal in tetrahydrofuran (THF) to give a 1:1 adduct K[Cp2V] which has been isolated as [K(THF)(Et20)][Cp2V]. The reactions of this compound with various molecules (L) capable of functioning as ligands were investigated. They cause the liberation of KCp and the formation of several new organovanadium compounds. The products of these reactions were: [K(THF)2 5][CpVCsHi2] for L = butadiene (C4H6), [K(THF)i.5][CpVC6H5P(C6H5)2] for L = P(C6H5)3, CpV(C4H6)P(CH3)3 for L = mixture of C4H6 and P(CH3)3. Vanadocene was reacted with allyllithium to yield LiCp and [LiTMEDA][CpV(C3H5)2] (TMEDA =: (CH3)2NCH2CH2N(CH3)2), which was transformed via allylbromide to CpV(C3Hö)2. Structures and reactivities of these new organovanadium complexes are discussed. I. Einführung Unlängst berichteten wir in Übersichtsaufsätzen [2, 3] zusammenfassend über eine von uns ent-wickelte Synthesemethode, durch die reaktive Über-gangsmetall-Olefin-und Alkalimetall-Übergangs-metall-Olefin-Komplexe des Nickels, Cobalts und Eisens auf einfache Weise zugänglich geworden sind, z.B. mit Ethen als Olefin: Et20 Cp2Co + K + 2 C2H4 • CpCo(C2H4)2 + KCp THF Cp2Co + 3K + 4C2H4 • K[Co(C2H4)4] + 2 KCp THF Cp2Fe + 2 Li + 2 C2H4 Li[CpFe(C2H4)2] + LiCp Wir haben nun überprüft, ob sich dieses Synthese-prinzip, das auf der reduktiven Ablösung der Cp-Ringe von den entsprechenden Metallocenen mittels Alkalimetall in Gegenwart von Olefinen beruht, auch auf das elektronenärmere Vanadocen über-tragen läßt. Überdies war zu klären, ob neben Olefinen auch andere Komplexbildner wie Kohlen-monoxid oder Phosphane oder gar Mischungen von Komplexbildnern eingesetzt werden können. Hier-über sowie über einen zweiten Synthese weg, der | | |
Reference
| Z. Naturforsch. 38b, 1113—1121 (1983); eingegangen am 7. März 1983 | | |
Published
| 1983 | | |
Keywords
| Vanadium, Potassium, Vanadocene, Allyllithium, Olefines | | |
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| default:Reihe_B/38/ZNB-1983-38b-1113.pdf | | | Identifier
| ZNB-1983-38b-1113 | | | Volume
| 38 | |
3 | Author
| J. Feldmann, Hk Müller-Buschbaum | Requires cookie* | | Title
| Kristallstrukturuntersuchung am Barium-Yanadyl-Vanadat: Ba2(V 0)V 20 8 Crystal Structure Investigation of the Barium Vanadyl-Vanadate: Ba2(V 0 )V 20 8  | | | Abstract
| Single crystals of Ba2(V 0)V 20 8 have been prepared by solid state reactions of Ba2V 20 7, V 9O 1 and V ^ 05 in sealed silica tubes. This compound crystallizes with monoclinic symmetry, space group C 1 -P 2 ,, a = 8.1174(9), b = 5.9699(9), c = 9.2903(9) A , ß = 113.94(1)°, Z = 2. V 5+ shows tetrahedral coordination. V 4+ inside ^ [V (3)0 4] chains is characterized by a square pyramidal coordination with a short apical V-O distance of 1.6 A typically for vanadyl groups. Ba2(V 0)V 20 8 represents a new structure type and is not isotypic to Sr2(V 0)V 20 8. | | |
Reference
| Z. Naturforsch. 51b, 489—4 (1996); eingegangen am 22. August 1995 | | |
Published
| 1996 | | |
Keywords
| Barium, Vanadium, Oxide, Crystal Structure | | |
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| default:Reihe_B/51/ZNB-1996-51b-0489.pdf | | | Identifier
| ZNB-1996-51b-0489 | | | Volume
| 51 | |
4 | Author
| Hans-Ulrich Meisch, JohannesA. Schmitt, Wolfgang Reinle | Requires cookie* | | Title
| Schwermetalle in Höheren Pilzen, III * Vanadium und Molybdän Heavy Metals in Higher Fungi, III. Vanadium and Molybdenum  | | | Abstract
| In several series of 212 samples, higher fungi, especially from the genus Amanita and related genera, were analyzed by atomic absorption spectroscopy on their content of the trace metals vanadium and molybdenum. Only vanadium was found to be present in high concentration in the fly agaric mushroom (Amanita muscaria), while 22 of its related species showed the normal V-content of the higher fungi tested. A correlation with the presence of molybdenum could not be detected. A special enrichment of Mo was not found in higher fungi. The analysis of several fruit bodies from A. muscaria showed that the highest V-content was present in the bulb and in the lamellae, both contents increasing with age, while the spores contained only 1 — 2% of the lamellar vanadium. | | |
Reference
| Z. Naturforsch. 33c, 1 (1978); eingegangen am 12. Dezember 1977/11. Januar 1978 | | |
Published
| 1978 | | |
Keywords
| Vanadium, Molybdenum, Higher Fungi, Amanitaceae | | |
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| default:Reihe_C/33/ZNC-1978-33c-0001.pdf | | | Identifier
| ZNC-1978-33c-0001 | | | Volume
| 33 | |
5 | Author
| A. Chrissanthopoulos3, C. Pouchan3, G. N. Papatheodorou5 | Requires cookie* | | Title
| Structural Investigation of Vanadium -Sodium Metaphosphate Glasses  | | | Abstract
| Paper presented a t the NATO A dvanced Study Institute, M ay 4-1 4 , 2001 (Kas, Turkey) The structure of the glass forming system (V20 5)x -(Na20 • P205)(1_^), (jc = 0-0.4), has been inves tigated using Raman spectroscopy. The stretching vibrations of various phosphate groups, connected to phosphorus or vanadium atoms, have been assigned. Variation o f the composition leads to structural changes where the sodium metaphosphate -P-O-P-chains break and then reconnect with the oxovana-dium units forming a -V-O-P-network structure. | | |
Reference
| Z. Naturforsch. 56a, 773—7 (2001); received August 8 2001 | | |
Published
| 2001 | | |
Keywords
| Vanadium, Phosphates, Vanadium Glass, Raman Spectroscopy, Metaphosphates | | |
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| default:Reihe_A/56/ZNA-2001-56a-0773.pdf | | | Identifier
| ZNA-2001-56a-0773 | | | Volume
| 56 | |
6 | Author
| D. Chales De Beaulieu, Hk Müller-Buschbaum | Requires cookie* | | Title
| Gemischtvalente Oxovanadate, I Ein neuer Strukturtyp für die Verbindung BaV10O15 Oxovanadates with Mixed Valence, I A New Crystal Structure of BaVioOis  | | | Abstract
| BaVioOis was prepared by high temperature reaction of BaO and V2O3 in H2-atmosphere (T > 1800°). X-ray investigations of single crystals show a new structure type with octa-hedral coordination of V 3+ /V 2+ (statistical distribution) and cuboctahedral surrounding of Ba 2+ . Orthorhombic symmetry, space group D^|-Ccmb, a = 995,8; b = 1161,8; c = 941,0; Z = 4. | | |
Reference
| Z. Naturforsch. 35b, 669—671 (1980); eingegangen am 5. Februar 1980 | | |
Published
| 1980 | | |
Keywords
| Barium, Vanadium, Oxide, Mixed Valence State, Crystal Structure | | |
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| default:Reihe_B/35/ZNB-1980-35b-0669.pdf | | | Identifier
| ZNB-1980-35b-0669 | | | Volume
| 35 | |
7 | Author
| D. Osterloh, Hk Müller-Buschbaum | Requires cookie* | | Title
| Zur Kenntnis von SrCo2V 208 und SrCo2(A s0 4)2 On SrCo2V20 8 and SrCo2(A s 0 4)2  | | | Abstract
| SrCo2V20 8 (I) and SrCo2(A s 0 4)2 (II) were prepared by crystallization from melts and investigated by X-ray single crystal technique. (I) is isotypic to the SrNi2V 20 8-type and crys tallizes with tetragonal symmetry, space group Cly-14-icd, a = 12.267; c = 8 .4 2 4 Ä ; Z = 8. (II) is iso ty p ic to th e la te ly fo u n d S r N i2(P 0 4) 2, sp a c e g ro u p C J -P 1 , a = 5.713; b = 6.903; c = 9.417 A ; a = 110.48; ß = 101.43; | | |
Reference
| Z. Naturforsch. 49b, 923 (1994); eingegangen am 28. Februar 1994 | | |
Published
| 1994 | | |
Keywords
| Strontium, Cobalt, Vanadium, Arsenic, Oxide, Crystal Structure | | |
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| default:Reihe_B/49/ZNB-1994-49b-0923.pdf | | | Identifier
| ZNB-1994-49b-0923 | | | Volume
| 49 | |
8 | Author
| S. Münchau, Hk Müller-Buschbaum | Requires cookie* | | Title
| Cd0,73 Cu0,27V2 O 6: A Com pound with Brannerite Structure  | | | Abstract
| Single crystals of Cd() 73Cu<,.27V 20 6 were prepared by solid state reactions. X-ray investiga tions lead to monoclinic symmetry, space group C \h-C2lm , a = 9.339, b = 3.5604, c = 6.893 A , ß = 111.85°, Z = 2. It belongs to the Brannerite structure, showing a statistical distribution of Cd2+ and Cu2+ on one point position. The crystal structure of Brannerites is discussed with respect to the distorted O 2-octahedra around V 5+ and the influence of the Jahn-Teller active Cu-+ ion to the shortened M2+Oa octahedra. | | |
Reference
| Z. Naturforsch. 49b, 927 (1994); eingegangen am 4. März 1994 | | |
Published
| 1994 | | |
Keywords
| Cadmium, Copper, Vanadium, Oxide, Brannerite Type | | |
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| default:Reihe_B/49/ZNB-1994-49b-0927.pdf | | | Identifier
| ZNB-1994-49b-0927 | | | Volume
| 49 | |
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 | |
10 | Author
| S. Münchau, Hk Müller-Buschbaum | Requires cookie* | | Title
| Zur Kristallchemie eines Silber-Cadmium-Oxovanadats: AgCdV04 On the Crystal Chemistry of a Silver Cadmium Oxovanadate: A gC dV 04  | | | Abstract
| Single crystals of A gC dV 04 have been prepared in closed silver tubes using V20 5 as a flux. The light-orange crystals sho\v orthorhom bic symmetry, space group D2h-Pnm a, a = 9.786(2), b = 6.994(1), c = 5.439(1) A, Z = 4. The hitherto unknown A gC dV 04 is related to the Olivine structure but isotypic to Ag2C r 0 4 and NaCd4(V 0 4)3 respectively. The differences in crystal chemistry between the Olivine type, NaCd4(V 0 4)3 and A gC dV 04 are discussed. | | |
Reference
| Z. Naturforsch. 50b, 703—706 (1995); eingegangen am 10. O ktober 1994 | | |
Published
| 1995 | | |
Keywords
| Silver, Cadmium, Vanadium, Oxide, Crystal Structure | | |
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| default:Reihe_B/50/ZNB-1995-50b-0703.pdf | | | Identifier
| ZNB-1995-50b-0703 | | | Volume
| 50 | |
11 | Author
| VerbindungC., S. Münchau, Hk Müller-Buschbaum | Requires cookie* | | Title
| Synthese und Kristallstruktur einer mit dem Johillerit verwandten  | | | Abstract
| Single crystals of C dC u^M gx.5Pbo.5V30 12 have been prepared in closed steel tubes using V 20 5 as a flux. The orange crystals show monoclinic symmetry, space group C2h-C 2 /c , a = 12.417(5), b = 12.983(6), c = 6.911(3) Ä , ß = 113.02(1)°, Z = 4. CdCu1.5Mg1.5PbojV30 12 reveals a relationship to the Johillerite type, but it is characterized by an additional point position for cadmium, situated betw een the square planar C u 0 4 polygons of the Johillerite structure. | | |
Reference
| Z. Naturforsch. 50b, 1158—1162 (1995); eingegangen am 22. D ezem ber 1994 | | |
Published
| 1995 | | |
Keywords
| Cadmium, Copper, Magnesium, Lead, Vanadium, Oxide, Crystal Structure | | |
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| default:Reihe_B/50/ZNB-1995-50b-1158.pdf | | | Identifier
| ZNB-1995-50b-1158 | | | Volume
| 50 | |
12 | Author
| J. Feldmann, Hk Müller-Buschbaum | Requires cookie* | | Title
| Kristallstrukturuntersuchung an einem bismuthaltigen Hollandit: Crystal Structure Investigation of the Bismuth Containing Hollandite: Bij 9Cu4V40 16  | | | Abstract
| Single crystals of B^ 9Cu4V 4O i6 have been prepared by quenching of CO2-LA SER heated samples. They were investigated by X-ray techniques. The compound^ crystallizes with tetra gonal symmetry, space group C4h-I 4 /w , a = 9.945(2) A, c = 2.915(3) A, Z = 1, and is isotypic to the mineral Hollandite. B^ 9Cu4V4O i6 is the first Hollandite with a statistical distribution of vanadium and copper in the network o f octahedra. Calculations of the Coulomb terms of lattice energy led to a distance o f bismuth to the lone pair of 1.07 A. Considering the lone pair as part of the coordination sphere of Bi3+ a square pyramidal polyhedron is obtained. | | |
Reference
| Z. Naturforsch. 50b, 1163—1166 (1995); eingegangen am 22. D ezem ber 1994 | | |
Published
| 1995 | | |
Keywords
| Bismuth, Copper, Vanadium, Oxide, Crystal Structure | | |
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| default:Reihe_B/50/ZNB-1995-50b-1163.pdf | | | Identifier
| ZNB-1995-50b-1163 | | | Volume
| 50 | |
13 | Author
| C. W. Adewitz, HkM. Üller-Buschbaum | Requires cookie* | | Title
| Synthese und Struktur eines Strontium -V anadyl-Phosphats: Sr2( V 0 ) (P 0 4)2 Synthesis and Structure o f a Strontium Vanadyl Phosphate: Sr2(V 0 )(P 0 4)2  | | | Abstract
| Dark green single crystals of Sr2(VO)P2Ox have been prepared by solid state reactions in closed quartz tubes. X-ray investigations led to monoclinic symmetry, space group C2h-I2/c/, a = 6.744(4), b = 15.866(4), c = 7.032(2) Ä, ß = 115.41(2), Z = 4. Sr2(VO)P2O s is isotypic to Sr2(VO)V2Os and shows V4+ in split positions. The split positions are in non-centric octahedral coordination forming a short vanadium to oxygen distance typical for the vanadyl group. The crystal chemistry of the monovanadyl orthophate Sr2(VO)P2O x is discussed considering related divanadyl phosphates. | | |
Reference
| Z. Naturforsch. 51b, 929—933 (1996); eingegangen am 17. Januar 1996 | | |
Published
| 1996 | | |
Keywords
| Strontium, Vanadium, Phosphorus, Oxygen, Crystal Structure | | |
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| default:Reihe_B/51/ZNB-1996-51b-0929.pdf | | | Identifier
| ZNB-1996-51b-0929 | | | Volume
| 51 | |
14 | Author
| C. Wadewitz, Hk Müller-Buschbaum | Requires cookie* | | Title
| Strukturelle Unterschiede zwischen Sr2(V 0)(A s04)2 und Ba2(V 0)(P 04)2 Strucural Differences between Sr2(V 0 )(A s0 4)2 and Ba2(V 0 )(P 0 4)2  | | | Abstract
| Two new alkaline earth vanadyl compounds, Sr2(V 0)(A s 0 4)2 (I) and Ba2(V 0)(P 0 4)2 (II), have been prepared by solid state reactions in closed quartz tubes and characterized by sin gle crystal X-ray diffraction methods. Crystal data: (I): monoclinic, C ,h -12/a, a = 6.873(2), b = 16.307(4), c = 7.196(2) A, ß = 115.67(2), Z = 4; (II): monoclinic, C^-I2, a = 9.471(2), b = 5.443(1), c = 16.972(4) Ä, ß = 101.65(2), Z = 4. (I) is isotypic to Sr2(V 0)V 20 8 and Sr2(V 0)(P 0 4)2. (II) shows significant differences to the strontium compounds as well as to Ba2(V 0)(V 0 4)2. The differences of the crystal chemistry and the similarity of (II) to Ba2(V 0)(P 0 4)2 H20 are discussed. | | |
Reference
| Z. Naturforsch. 51b, 1290—1294 (1996); eingegangen am 26. April 1996 | | |
Published
| 1996 | | |
Keywords
| Barium, Strontium, Vanadium, Phosphorus, Arsenic, Oxygen, Crystal Structure | | |
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| default:Reihe_B/51/ZNB-1996-51b-1290.pdf | | | Identifier
| ZNB-1996-51b-1290 | | | Volume
| 51 | |
15 | Author
| Thomas Miekisch, Klaus Harms, Sigrid Wocadlo, Werner Massa, Bernhard Neumüller, Christoph Frommen, Kurt Dehnicke, Herrn Prof, J. Dr, Lorberth | Requires cookie* | | Title
| [TiJv Cl8(NPMe3)3]Cl und [Vnw vCl4(NPPh3)3] Crystal Structures of the Phosphoraneiminato Complexes [Ti3v Cl8(NPMe3)3]Cl and [vl"/IVCl4(NPPh3)3]  | | | Abstract
| [Ti3Cl8(NPMe3)3]Cl has been prepared by the reaction of TiCl3(THF)3 with Me3SiNPMe3 in dichloromethane forming green moisture sensitive crystals. According to the crystal structure determination the titanium atoms of the cation [Ti3Cl8(NPMe3)3]+ are linked by two /x3-N atoms of two NPMe3~ groups forming a distorted trigonal-bipyramidal arrangement. The third NPMe3_ group and two of the chlorine atoms have /i2-bridging functions. The mixed-valence complex [V2Cl4(NPPh3)3] is formed as dark green moisture sensitive crystals by the reaction of vanadium trichloride with Me3SiNPPh3 in boiling toluene. According to the crystal structure determination the vanadium atoms are linked by two /z2-N atoms of two NPPh3_ groups forming a nonplanar V2N2 four-membered ring with a V-V distance of 266.8(1) pm which corresponds to a (a, 1/27r) bond type. This is confirmed by the measurement of the magnetic susceptibility which leads to a magnetic moment of 1.45(5) B. M., corresponding to the remaining d 1 -electron. | | |
Reference
| Z. Naturforsch. 52b, 1484—1490 (1997); eingegangen am 8. September 1997 | | |
Published
| 1997 | | |
Keywords
| Phosphoraneiminato Complexes, Titanium, Vanadium, Crystal Structure | | |
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| default:Reihe_B/52/ZNB-1997-52b-1484.pdf | | | Identifier
| ZNB-1997-52b-1484 | | | Volume
| 52 | |
16 | Author
| Max Herberhold, Silke Köppl, Wolfgang Milius | Requires cookie* | | Title
| Mixed-Sandwich rflry Vanadium Complexes. The Molecular Structure of (?75-2-Methyl-indenyl)-(777-cycloheptatrienyl)-vanadium  | | | Abstract
| The diamagnetic halfsandwich complexes [V(?^7-C7H7)(CO)3] and [V(7/5-L5)(CO)4] have been used as intermediates in the conversion of hexcarbonylvanadium, V(CO)6, to the para magnetic trovacene derivatives, [V(775-L5)(r77-C7H7)] [L^ = cyclopentadienyl ligand, C5H4-R (R = H (1), Me (la), 'Bu (lb)) and CsMes (lc); indenyl (2) and 2-methylindenyl (2a)]. The molecular structure of 2a has been determined: the distances between vanadium and the center Z of the (nearly parallel) ring ligands are 193.0 pm | | |
Reference
| Z. Naturforsch. 54b, 899—903 (1999); received April 8 1999 | | |
Published
| 1999 | | |
Keywords
| Sandwich Compounds, Cycloheptatrienyl Complexes, Vanadium, Crystal Structure | | |
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| default:Reihe_B/54/ZNB-1999-54b-0899.pdf | | | Identifier
| ZNB-1999-54b-0899 | | | Volume
| 54 | |
17 | Author
| Hans-Ulrich Meisch, Wolfgang Reinle, Bernd-Arwed Richter | Requires cookie* | | Title
| Zur Frage biogener Anreicherungen von Vanadium und Nickel in Pflanzen des Karbonzeitalters The Question of Biogenous Enrichments of Vanadium and Nickel in Plants of the Carbon Age  | | | Abstract
| O riginal carbonaceous m aterial of fossile carbon plants from the divisions of the Equisetophyta (Calam ariaceae), Lycophyta (Lepidodendraceae, S igillariacea e), Filicophyta (F ilicatae), and Sper-matophyta (Pteridospermatae, Cordaitidae) was analyzed by atomic absorption spectroscopy on its content of the trace metals vanadium and nickel. The average V-content was found to be 1 0 to 100 fold higher than that of the neighbouring coal beds or that of the embedding materials, while the Ni-concentrations were found to be almost in the same range. The highest contents of V and N i were found in the Calamariaceae and in the Pteridospermatae. The V-and Ni-contents of the fossile carbon plants are compared to those of related recent plant genera (clubmosses, horse tails, fern s), which were analyzed by 46 representative samples. A possible biogenous enrichment of V and N i in plants of the carbon age is discussed. | | |
Reference
| Z. Naturforsch. 33c, 616 (1978); eingegangen am 7. Juni/21. Juni 1978 | | |
Published
| 1978 | | |
Keywords
| Vanadium, Nickel, Carbon, Carbon Plants, Ferns, Horsetails, Clubmosses | | |
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| default:Reihe_C/33/ZNC-1978-33c-0616.pdf | | | Identifier
| ZNC-1978-33c-0616 | | | Volume
| 33 | |
19 | Author
| Fausto Calderazzo, Guido Pam, M. Artin Sperrlea, Ulli Englertb | Requires cookie* | | Title
| Electron-and Ligand-Transfer Reactions Involving N,N-Dialkylcarbamates. Synthesis and Molecular Structure of V jIf^ -C C sH ^ yC ^ C N t^ H ^ h  | | | Abstract
| Electron-and ligand-transfer reactions o f low-valent organom etallic com pounds o f titanium and vanadium with N,N-dialkylcarbam ates o f titanium(IV) are reported. The reaction o f VCp2 (Cp = ^-cyclopentadienyl) with T i(0 2C N E t2)4 affords, inter alia, the dimeric vana-dium(III) N ,N-diethylcarbam ato derivative V2Cp2(0 2C N E t2)4 which has been studied by X-ray diffraction methods. Crystal data; triclinic, space group P i; a = 10.802(2), b = 11.004(1), c = 8.960(1) Ä; a = 112.879(9), ß = 102.66(1), y = 102.42(1)°; V = 902.3(6) A 3; Z = 1; F(000) = 368, gcalc = 1.282 g em -3; n = 5.47 cm -1. It consists o f a centrosymmetric dimer, the two vanadium atom s being surrounded by four oxygen atom s o f the bridging N,N-diethylcar-bamato groups and by the cyclopentadienyl ligand. The metal atom exhibits a distorted square-pyramidal coordination geometry with the oxygen atom s occupying the basal plane. The reaction o f TiCp2(CO)2 or Vmes2 (mes = //6-l,3 ,5 -M e3C6H 3) with T i(0 2C N E t2)4 affords Ti(III) and V(III) N,N-diethylcarbam ato derivatives by a simultaneous ligand-and electron-transfer reaction. M agnesium N ,N-diisopropylcarbam ate, M g (0 2CNPr'2)2, has been obtained by a ligand-transfer reaction between M gCp2 and T i(0 2CNPr'2)3. | | |
Reference
| Z. Naturforsch. 47b, 389 (1992); received A ugust 9 / October 16 1991 | | |
Published
| 1992 | | |
Keywords
| N, N-D ialkylcarbam ates, Vanadium, Titanium, Cyclopentadienyl, Electron Transfer | | |
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| default:Reihe_B/47/ZNB-1992-47b-0389.pdf | | | Identifier
| ZNB-1992-47b-0389 | | | Volume
| 47 | |
20 | 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 | |
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