| | 21 | 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 | |
| 22 | Author
| Kai Landskron, Stefan Horstmann, Wolfgang Schnick | Requires cookie* | | | Title
| Neue Tetraaminophosphonium-Salze durch Anionenaustausch in flüssigem Ammoniak Novel Tetraaminophosphonium Salts by Anion Exchange in Liquid Ammonia | | | | Abstract
| [P(NH2)4]Br and [P(NH2)41[N 03] have been prepared by anion exchange in liquid ammonia. Single crystals of [P(NH2)4]Br were obtained from an acetonitrile solution in a tempera ture gradient between 60 °C and room temperature while attempts to grow single crystals of [P(NH2)4][N 0 3] yielded [P(NH2)4][N 0 3](O P(N H 2)3). Both crystal structures were determined by single crystal X-ray methods at room temperature ([P(NH-))4]Br: P4/nbm, a = 809.2(1), c = 468.1(1) pm, Z = 2, R \ = 0.042, wR2 = 0.077; [P(NH2)4][NÖ3](OP(NH2)3): Pna2,, Z = 4, a = 1023.4(1), b = 1704.7(1), c = 618.0(1) pm, R \ =0.025', wR2 = 0.067. In the solid [P(NH2)4]Br forms a tetragonally distorted variant of the CsCl type of structure. [P(NH2)4][N 0 3](0P (N H 2)3) consists of [P(NH2)4]+cations, [N 0 3]_ anions, and OP(NH2)3 molecules which are interconnec ted by a complex system of hydrogen bonds. | | | |
Reference
| Z. Naturforsch. 54b, 1019—1026 (1999); eingegangen am 12. April 1999 | | | |
Published
| 1999 | | | |
Keywords
| Phosphorus, Ion Exchange, Liquid Ammonia, Crystal Structure | | | |
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| default:Reihe_B/54/ZNB-1999-54b-1019.pdf | | | | Identifier
| ZNB-1999-54b-1019 | | | | Volume
| 54 | |
| 23 | Author
| *. Sonderdruckanforderungen, ProfK. Dr, Dehnicke | Requires cookie* | | | Title
| D ie Kristallstruktur von Bis(bromo | | | | Abstract
| -triphenyl)arsen(V)-hexabromo-tellurat(IV), [Ph3A sB r]2[TeBr6] Crystal Structure o f B is(brom otriphenyl)-arsen ic(V)-h exab rom otellu rate(IV), [Ph3A sB r]2[TeBr6] S oheila Chitsaz, Bernhard N eum üller, Kurt D eh nick e* Yellow-orange single crystals of [Ph3AsBr]2[TeBr6] have been prepared from satu rated solutions of Ph3AsBr2 and TeBr4 in aceto nitrile and characterized by a crystal structure de term ination. Space group R3c, Z = 12, lattice di mensions at -7 0 °C: a = b = 1337.9(2), c = 7953.8(4) pm, R = 0.0691. The structure consists of discrete ions [Ph3A sBr]+ and nearly perfectly octahedral [TeBr6]2-. | | | |
Reference
| Z. Naturforsch. 54b, 1092—1094 (1999); eingegangen am 28. Mai 1999 | | | |
Published
| 1999 | | | |
Keywords
| Arsenic, Tellurium, Bromo Complex, Crystal Structure | | | |
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| default:Reihe_B/54/ZNB-1999-54b-1092_n.pdf | | | | Identifier
| ZNB-1999-54b-1092_n | | | | Volume
| 54 | |
| 25 | Author
| Birgit Fehrmann, Wolfgang Jeitschko | Requires cookie* | | | Title
| The Intermetallic Compounds GdRe2Al10 and TbRe2Al10, Crystallizing with a Stacking Variant of the YbFe2Al10 Type Structure | | | | Abstract
| The new compounds GdReaAlio and TbRe.Alio were obtained in well-crystallized form by reaction of the elemental components with an excess of aluminum after dissolving the matrix in hydrochloric acid. They crystallize with a new structure type which has been determined for TbReiAlio from single-crystal X-ray data: Cmcm, a = 932.2(1),/?= 1030.4(1),c= 1803.2(3)pm, Z = 8, R = 0.031 for 1159 structure factors and 77 variable parameters. Of the two terbium sites, one does not have full occupancy with terbium, however, it may have mixed Tb/Al occupancy. The resulting compositions are Tbo.948(5>Re2Alio or Tbo.936(3)Re:Alio.o64(3), respectively. The terbium atoms are coordinated by 4 Re and 16 Al atoms. The rhenium atoms are situated in distorted icosahedra formed by 2 Tb and 10 Al atoms. The nine different aluminum atoms have between 12 and 14 neighbors (1 or 2 Tb, 2 Re, and between 8 and 11 Al atoms). The structure may be viewed as consisting of two kinds of alternating layers. One of these is puckered, hexagonal close packed, with a mesh content of 4ReAl3; the other is planar and less densely packed. It has the mesh content 2TbAl4. The same kinds of atomic layers have been found in the structures of YbFe2Alio and LuRe2Alio. Thus, the three structure types may be considered as stacking variants of each other. The tetragonal CaC^Alio (ordered ThMni2) type structure also belongs to this structural family, although the CaAl4 layers somewhat differ from the layers TbAl4, YbAl4, and LuA14. | | | |
Reference
| Z. Naturforsch. 54b, 1277—1282 (1999); received May 27 1999 | | | |
Published
| 1999 | | | |
Keywords
| Intermetallic Compounds, Crystal Structure, Close Packed Layers | | | |
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| default:Reihe_B/54/ZNB-1999-54b-1277.pdf | | | | Identifier
| ZNB-1999-54b-1277 | | | | Volume
| 54 | |
| 26 | Author
| Qianfeng Zhanga, Jinxi Chena, Maochun Hongb, Xinquan Xina, Hoong-Kun Func | Requires cookie* | | | Title
| Crystal and Molecular Structure of the Copper(I)-thiolate-selenide Complex [Ph4P][Cu(SeS2CNC4H8)(S2CN2C4H8)] with an Unusual Se-S Bond | | | | Abstract
| Reaction of a DMF solution of Cu(S^CNC4 H8) with [Ph4 P]2 [WSe4 ] affords [Ph4 P b[W Se4 -(CuS2CNC4H8)3 ] (1) and [Ph4P][Cu(SeS2 CNC4 H8)(S2 CN2 C4 H 8)] (2) in which a Se atom from the decomposition of the W Se4 2~ anion has reacted with the pyrrolidyldithiocarbamate (C4 H8dtc) ligand anion to form the new ligand anion SeSiC N C +H s'. Complex 2 crystallizes with four formula units in the monoclinic space group P2\/c in a cell of dimensions a = 10.5824(2), b = 18.7575(3), c = 18.3268(4) A and ß = 109.0980(10)°. 6055 independent reflections above background were measured with a diffractometer and the structure was re fined anisotropically to R =0.073. The anion contains a three-coordinated copper(I) atom. The C4 H8 dtcö ligand is bonded to the Cu+ cation in a terminal fashion, while SeS2 CNC4 H8~ chelates the Cu+ cation. The Se-S bond length is 2.231 (4) A. | | | |
Reference
| Z. Naturforsch. 54b, 1313—1317 (1999); received April 4 1999 | | | |
Published
| 1999 | | | |
Keywords
| Crystal Structure, Copper Complex, Selenium Complex, Thiolate Ligand | | | |
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| default:Reihe_B/54/ZNB-1999-54b-1313.pdf | | | | Identifier
| ZNB-1999-54b-1313 | | | | Volume
| 54 | |
| 27 | Author
| Michael Becker, Martin Jansen, Martin Jansen Heisenbergstraße, D-70596, Stuttgart Sonderdruckanforderungen, Prof Dr, Martin Jansen | Requires cookie* | | | Title
| Darstellung und Charakterisierung von Rubidiumhydrogencyanamid Synthesis and Characterization of Rubidium Hydrogen Cyanamide | | | | Abstract
| The synthesis of RbHCN2 was carried out by reaction of cyanamide with rubidium amide in liquid ammonia. The crystal structure has been determinedo by x-ray powder methods (orthor-hombic, P2,2,2,, a = 7.299(1), b = 9.435(1), c = 9.420(1) Ä; Z = 8). The anion is slightly bent (174°) and exhibits two different bond lengths (C-N: 1.17, HN-C: 1.31 A). | | | |
Reference
| Z. Naturforsch. 54b, 1375—1378 (1999); eingegangen am 26. Juli 1999 | | | |
Published
| 1999 | | | |
Keywords
| Rubidium Hydrogen Cyanamide, Synthesis, Crystal Structure, IR Data | | | |
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| default:Reihe_B/54/ZNB-1999-54b-1375.pdf | | | | Identifier
| ZNB-1999-54b-1375 | | | | Volume
| 54 | |
| 28 | Author
| Stefan Dick | Requires cookie* | | | Title
| Uber die Struktur von synthetischem Tinsleyit K[A12 (P04)2(0H)(H20)]H 20 The Structure of Synthetic Tinsleyite K[A12 (P0 4)2 (0 H)(H2 0 )] H20 | | | | Abstract
| Synthetic tinsleyite KfAhCPO-ibCOHXFTO^TTO has been obtained by the reaction of gibb-site with a potassium-phosphate solution of pH = 7 at 423 K within five days. A single crystal X-ray structure analysis has shown that synthetic tinsleyite is isotypic with the mineral leucophosphite K[Fe2(P0 4)2(0 H)(H20)] H 20. Crystal data: monoclinic space group P2\/n, a = 949.9(2), b = 950.3(2), c = 953,5(2) pm, ß = 103,26(3)°, Z = 4. The structure of tinsleyite consists of tetranuclear A I4O 2 units formed by a central pair of edge sharing A1Ü6 octahedra, to which two additional A1C>6 octahedra are attached sharing corners. These units are crosslinked by phosphate ions to a three dimensional framework structure with tunnels along [010], occupied by potassium cations. While one type of water molecules is attached to Al, a second type is fixed in the structure by hydrogen bonds only. As a consequence two steps for thermal loss of water at 341 K and 471 K are observed. | | | |
Reference
| Z. Naturforsch. 54b, 1385—1390 (1999); eingegangen am 15. Juli 1999 | | | |
Published
| 1999 | | | |
Keywords
| Crystal Structure, Phosphate Mineral, Tinsleyite, Leucophosphite | | | |
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| default:Reihe_B/54/ZNB-1999-54b-1385.pdf | | | | Identifier
| ZNB-1999-54b-1385 | | | | Volume
| 54 | |
| 29 | Author
| Marcus Sigl, Annette Schier, Hubert Schmidbaur | Requires cookie* | | | Title
| Bis[(2-diphenyIphosphino)phenyl]phenylphosphine as an Inflexible Tridentate Ligand for Indium Trichloride | | | | Abstract
| Anhydrous indium trichloride reacts with [2-(Ph2P)C6H4]2PPh (TP) in the molar ratio 2:1 to give an ionic complex [(TP)InCl2]+ InC L-in almost quantitative yield. The structure of the product has been determined by a single crystal X-ray diffraction study. In the cation the TP molecule acts only as a bidentate ligand via its two terminal phosphorus atoms [In-Pl 2.5956(8), In-P2 2.5799o (7) A], Although the central phosphorus atom is also rather close to the metal atom [2.8259(8) A], the In-P3 interaction is inefficient because of an adverse orientation of the lone pair of electrons at P3 owing to the steric inflexibility of the ligand. Accordingly, the 11P N M R spectra of the compound in C D 2CI2 show large contact shifts and quadrupole broadening only for the signals of the two terminal phosphorus atoms, whereas the lines of the central phosphorus atom are less shifted and well resolved (A B2 spin system at -60°C). | | | |
Reference
| Z. Naturforsch. 54b, 1417—1419 (1999); received September 15 1999 | | | |
Published
| 1999 | | | |
Keywords
| Indium Trichloride, Tridentate Phosphine, Ligand Inflexibility, Crystal Structure | | | |
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| default:Reihe_B/54/ZNB-1999-54b-1417.pdf | | | | Identifier
| ZNB-1999-54b-1417 | | | | Volume
| 54 | |
| 30 | Author
| Wolfgang Jeitschko, HorstA. Mons, Ute Ch, Rodewald | Requires cookie* | | | Title
| Preparation and Crystal Structure of the Calcium Rhenate(VI, VII) Ca5Re30 15.x | | | | Abstract
| The title compound was prepared by reaction of elemental calcium with the calcium metaper-rhenate Ca(ReC>4)2. Its crystal structure was determined from single-crystal X-ray data: Amm2, a = 560.31 (5)pm, b = 1572.4(1)pm, c = 719.91 (6)pm ,Z = 2 ,R = 0.033 for 930 structure factors and 46 variable parameters. The calcium atoms occupy three atomic sites, all with seven oxygen neighbors. Of the two different rhenium atoms one has square-pyramidal oxygen coordination with an average oxidation number +6.25. The other rhenium site (oxidation number +7) was refined as a split position with trigonal-bipyramidal (75%) and tetrahedral oxygen coordination (25%). One oxygen site remains unoccupied, whenever the tetrahedral rhenium site is occupied, resulting in the composition Ca5Re3 0 i4.75. A test for superconductivity of this black compound down to 1.5 K was negative. | | | |
Reference
| Z. Naturforsch. 54b, 1483—1488 (1999); received August 16 1999 | | | |
Published
| 1999 | | | |
Keywords
| Crystal Structure, Mixed Valence, Rhenates, Perrhenates | | | |
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| default:Reihe_B/54/ZNB-1999-54b-1483.pdf | | | | Identifier
| ZNB-1999-54b-1483 | | | | Volume
| 54 | |
| 31 | Author
| KurtO. Klepp, Ferdinand Fabian, *. Sonderdruckanforderungen, Prof Kurt, O. Klepp | Requires cookie* | | | Title
| Darstellung und Kristallstruktur von Rb6Sn2S7 New Chalcogenometallates with Binuclear Anions, I: Preparation and Crystal Structure of Rb6Sn2S7 | | | | Abstract
| Colorless crystals of the new thiostannate Rb6Sn2S7 were obtained by reacting a stoichio metric melt of Rb2S, Sn and S at 700°C. The compound is orthorhombic, oP60, s.g. f '2,2,2, (No. 19) with a = 9.982(4), b = 13.45(1), c = 15.20(1) A; Z = 4. The crystal structure was determined from diffractometer data and refined to a conventional R of 0.043 (1380 Fo's, 137 variables). The crystal structure contains dimeric anions, [Sn2S7]2 -, which are built up by slightly distorted SnS4 tetrahedra sharing a common sulfur atom. The mean Sn-S bond length calculates as 2.384 Ä, the bond angle on the bridging S is 110.4°. The structure contains six independent Rb-cations which are coordinated to 5-6 sulfur atoms in irregular configurations. Neue Chalkogenometallate mit binuklearen Anionen, I: | | | |
Reference
| Z. Naturforsch. 54b, 1505—1509 (1999); eingegangen am 13. September 1999 | | | |
Published
| 1999 | | | |
Keywords
| Crystal Structure, Chalcogenides, Thiostannates, Rubidium, Tin, Sulfur | | | |
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| default:Reihe_B/54/ZNB-1999-54b-1505.pdf | | | | Identifier
| ZNB-1999-54b-1505 | | | | Volume
| 54 | |
| 35 | Author
| Barbara Wenzel, Peter Strauch | Requires cookie* | | | Title
| Synthesis, Structural and EPR Investigations on Bis(tetraphenylphosphonium)- bis(l,2-dithiosquarato)oxovanadate(IV), (Ph4P)2[VO(dtsq)2] | | | | Abstract
| The molecular structure and EPR studies of bis(tetraphenylphosphonium)bis(1,2-dithiosquarato)oxovanadate(IV) are reported. (Ph4P)2[VO(dtsq)2] crystallizes in the mono clinic spaceogroup P2,/n with the unit cell parameters a = 10,9820(2), b = 15,4620(3), c = 14,5050(3) Ä, ß = 95,700(8)°, Z = 2. The g and hyperfine coupling tensors Av obtained from the EPR spectra in liquid and frozen solution are used to characterize the properties of the molecular orbital containing the unpaired electron and are compared to those obtained from EHT-MO calculations. | | | |
Reference
| Z. Naturforsch. 54b, 165—170 (1999); eingegangen am 18. September 1998 | | | |
Published
| 1999 | | | |
Keywords
| Sulfur, Oxovanadate(IV), Synthesis, EPR Data, Crystal Structure | | | |
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| default:Reihe_B/54/ZNB-1999-54b-0165.pdf | | | | Identifier
| ZNB-1999-54b-0165 | | | | Volume
| 54 | |
| 36 | Author
| Karl Hensena>, Markus Kettner3, T., Peter Pickel3, Michael Bolteb | Requires cookie* | | | Title
| Neue dikationische Silicium-Komplexe mit N-Methylimidazol New Dicationic Silicon Complexes with N-M ethylimidazole | | | | Abstract
| The reactions of the dibromosilanes Et2SiBr2, Ph2SiBr2, EtHSiBr2, PhHSiBr2 and MeHSiBr2 with N-methylimidazole (NMI) led to white powders stable at room temperature (with Et2SiBr2 an 1:2 adduct, with EtHSiBr2 and Ph2SiBr2 1:3 adducts, and with PhHSiBr2 and MeHSiBr2 1:4 adducts). The compounds crystallize from solutions in chloroforme and acetonitrile. The X-ray single crystal investigations show in all five cases dicationic complexes. | | | |
Reference
| Z. Naturforsch. 54b, 200—208 (1999); eingegangen am 8. Oktober 1998 | | | |
Published
| 1999 | | | |
Keywords
| Dialkyldibromosilanes, Alkyldibromosilanes, N-Methylimidazol, Lewis-Acid-Base-Adducts, Crystal Structure | | | |
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| default:Reihe_B/54/ZNB-1999-54b-0200.pdf | | | | Identifier
| ZNB-1999-54b-0200 | | | | Volume
| 54 | |
| 37 | Author
| Karin Dölling, Kurt Merzweiler, Christoph Wagner, Horst Weichmann | Requires cookie* | | | Title
| 3-Triorganostannyl-N-diphenylmethylen-alaninestern Synthesis, Structure and Reactivity o f 3-Triorganostannyl-N-diphenylmethylene- alanine Esters | | | | Abstract
| The deprotonation of N-diphenylmethylene-glycine esters, obtained from glycine ester hy drochlorides and benzophenone imine, and reaction of the resulting carbanions with iodo-methyl triorganostannanes gives the 3-triorganostannyl-N-diphenylmethylene-alanine esters Me2RSnCH2CH(N=CPh2)COOR' (la -e\ R = Me, 'Bu; R' = Me, Et, 'Bu, Bz). These title compounds are transformed into their tin monochlorides MeR(Cl)SnCH2CH(N=CPh2)COOR' (2a -e) by a redistribution reaction with Me2SnCl2. IR and NMR data and the crystal structure of Me2(Cl)SnCH2CH(N=CPh2)COOEt (2b) reveal for 2a -e an intramolecular coordination of the ester C = 0 group at the tin atom. Mild two-phase hydrolysis of la -e with IN HC1 gives the 3-triorganostannyl-alanine ester hydrochlorides Me2RSnCH2CH(NH 2)COOR' • HC1 (3a -e). The transformation of 3a -e into the corresponding alanine esters Me2RSnCH2CH (N H 2)COOR' (4a -e) could be realized with NH3 in chloroform. 4a -e are of limited thermal stability. | | | |
Reference
| Z. Naturforsch. 54b, 293—299 (1999); eingegangen am 10. November 1998 | | | |
Published
| 1999 | | | |
Keywords
| Stannyl Alanine Ester Derivatives, Intramolecular Pentakoordination, NMR Data, Crystal Structure | | | |
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| default:Reihe_B/54/ZNB-1999-54b-0293.pdf | | | | Identifier
| ZNB-1999-54b-0293 | | | | Volume
| 54 | |
| 38 | Author
| Joachim Pickardt, Benedikt Staub | Requires cookie* | | | Title
| Metallkomplexe mit 2,2'-Dipyridylamin als Liganden: Kristallstrukturen der Komplexe mit CdX2 (X = Cl, Br, I) und CuCN Metal Complexes with 2,2'-Dipyridylamine as Ligand: Crystal Structures o f the Com plexes with CdX2 (X = Cl, Br, I) and CuCN | | | | Abstract
| Reactions of 2,2'-dipyridylamine (dpyam) with cadmium halides yield crystals of [Cd(dpyam)(H20)C l2] (1), [Cd(dpyam)Br2] (2), and [Cd(dpyam)I2] (3). With CuCl2 and KCN a complex [C u(dpyam)C N ]H 20 (4) is obtained. Depending on the size of the halide ions the coordination changes from octahedral in 1 to trigonal bipyramidal in 2 and tetrahedral in 3. The coordination in 4 is trigonal. Due to the geometric strain imposed by the ligand all coordination polyhedra show significant distortions. 1 and 2 form dimers by halide bridges. With the excep tion of 3 all compounds form "supramolecular" structures via hydrogen bonds, e.g. chains or networks. | | | |
Reference
| Z. Naturforsch. 54b, 329—336 (1999); eingegangen am 10. Dezember 1998 | | | |
Published
| 1999 | | | |
Keywords
| 2, 2'-Dipyridylamine Complexes, Cadmium Halides, Copper(I) Cyanide, Crystal Structure | | | |
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| default:Reihe_B/54/ZNB-1999-54b-0329.pdf | | | | Identifier
| ZNB-1999-54b-0329 | | | | Volume
| 54 | |
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