| | 21 | Author
| S. Meyer, Hk Müller-Buschbaum | Requires cookie* | | | Title
| Zur Kenntnis eines Vanadyl-Oxocuprat-Phosphats CaCu  | | | | Abstract
| (V0)(P0 4) 2 mit Cu2+ auf Positionen der V 0 2+-Ionen und einer kupferreicheren Phase CaCulvt3(VO)o,87(P04)2 On an Vanadyl Oxocuprate Phosphate C aC u(V 0)(P 04)2 Containing Cu2+ at Positions of V 0 2+ Ions and a Copper Rich Phase CaCu, !3(VO)0 g7(P04)2 Single crystals of CaCu(V 0)(P04)2 (I) and CaCu,.i3(VO)o.87(P04)2 (II) have been prepared using solid state reactions in closed and evacuated quartz tubes. X-ray characterization led to | | | |
Reference
| Z. Naturforsch. 53b, 521—526 (1998); eingegangen am 4. Februar 1998 | | | |
Published
| 1998 | | | |
Keywords
| Calcium, Copper, Vanadyl-Phosphate, Crystal Structure | | | |
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| default:Reihe_B/53/ZNB-1998-53b-0521.pdf | | | | Identifier
| ZNB-1998-53b-0521 | | | | Volume
| 53 | |
| 23 | Author
| Tristram Chivers, Xiaorong Li, Masood Parvez | Requires cookie* | | | Title
| Preparation and X-Ray Structure of 3,5-Dimethyl-1,4-dichloro-1,2,6- thiadiazine-1 -oxide | | | | Abstract
| The title compound was obtained by the reaction of 3,5-dimethyl-2//-l,2,6-thiadiazine-l,l-dioxide with PCI5 in chloroform. It crystallizes in the monoclinic system, space group P2\/c, a = 7.521(7) A, b = 8.400(4) A, c = 13.908(4) Ä, ß = 100.35(4)°, V = 864.4(8) A3, and Z = 4. The S(VI) atom lies 0.43 A out of the plane of the 7r-delocalized NCCCN unit. The mean S-N bond distance is 1.569(3) A. | | | |
Reference
| Z. Naturforsch. 53b, 532—534 (1998); received December 18 1997 | | | |
Published
| 1998 | | | |
Keywords
| Crystal Structure, 1, 2, 6-Thiadiazines, Sulfanuric Chloride | | | |
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| default:Reihe_B/53/ZNB-1998-53b-0532.pdf | | | | Identifier
| ZNB-1998-53b-0532 | | | | Volume
| 53 | |
| 25 | Author
| MikeR. Kopp, Bernhard Neumüller | Requires cookie* | | | Title
| Benzylgallium-Verbindungen. Die Kristallstrukturen von [Mg3Br2 | | | | Abstract
| ,4Cl1,6(OEt2)6][Ga(CH2Ph)4]2 • 0,5 Toluol und [(3,5-Me2C6H3CH2)2GaBr]2 Benzylgallium Compounds. The Crystal Structures of [Mg3Br2 4C1 j 6(OEt2)6][Ga(CH2Ph)4]2 • 0.5 Toluene and [(3,5-Me2C6H3CH2)2GaBr]2 [Mg3Br2 4C1] 6(OEt2)6][Ga(CH2Ph)4]2-0.5 toluene (1) can be obtained by the reaction of one equivalent of GaCl3 with four equivalents of PhCH2MgBr in Et20 . Recrystallization of the crude product from toluene at 60°C gives colorless crystals of 1. Treatment of GaCl3 with two equivalents 3,5-Me2C6H3CH2MgBr in Et20 gives after recrystallization from toluene the diorganogallium bromide [(3,5-Me2C6H3CH2)2GaBr]2 (2). 1 and 2 were characterized by NMR, IR and MS techniques as well as by X-ray structure analyses. 1 consists in the dication [Mg3Br2 4C1, 6(OEt2)6]2+, two gallate units [Ga(CH2Ph)4]_ and a toluene molecule, disordered around a center of inversion. 2 forms centrosymmetric dimers [(3,5-Me2C6H3CH2)2GaBr]2. | | | |
Reference
| Z. Naturforsch. 53b, 545—551 (1998); eingegangen am 5. Februar 1998 | | | |
Published
| 1998 | | | |
Keywords
| Gallium Compounds, Magnesium Compound, Crystal Structures | | | |
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| default:Reihe_B/53/ZNB-1998-53b-0545.pdf | | | | Identifier
| ZNB-1998-53b-0545 | | | | Volume
| 53 | |
| 26 | Author
| V. Erena, M.T T Hiede, W. Olfgang, Jeitschko | Requires cookie* | | | Title
| Ternary Intermetallic Compounds L«Mn2Ali0 (Ln = Y, La-Nd, Sm, Gd-Dy) and L«Re2Al10 (Ln = Ce, Pr, Sm) with CaCr2Al10-Type Structure | | | | Abstract
| The twelve title compounds have been prepared for the first time. Their CaCnA lio-type structure (PA/nm m, Z = 4) was refined from single-crystal X-ray data for the three representatives TbM mAlio (a = 1274.3(2) pm, c = 511.4(2) pm, R = 0.025 for 680 structure factors F and 43 variable parameters VO, CeRe2Alio (a -1295.5(5) pm, c -517.2(4) pm, R = 0.054 for 810 F a n d 46 V), and SmReaAlio (a = 1291.5(2) pm, c = 516.5(1) pm, R = 0.021 for 622 F and 46 V). The atomic positions of the lanthanoid and transition metal atoms are fully occupied. Significant deviations from the full occupancies were observed for two aluminum sites in TbM mAlio and for all five aluminum sites of the two rhenium-containing compounds, resulting in the compositions TbMn2Al9.63(2), CeRe2Al9.52(8), and SmRe2Al9.i6< 9)-The cell volume of CeRe2Alio and to a smaller extent also that of CeMm A1 io indicate mixed or intermediate +III/+IV valencies of the cerium atoms in these compounds. The structural relationships between the three closely related body-centered tetragonal structures of ThM ni2, CeMn-iAlx, DyFeöAU, and the primitive tetragonal structure of CaCnA lio are briefly discussed. | | | |
Reference
| Z. Naturforsch. 53b, 673—678 (1998); received February 2 1998 | | | |
Published
| 1998 | | | |
Keywords
| Intermetallic Compounds, Crystal Structure, X-Ray Data | | | |
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| default:Reihe_B/53/ZNB-1998-53b-0673.pdf | | | | Identifier
| ZNB-1998-53b-0673 | | | | Volume
| 53 | |
| 27 | Author
| Francoanellite K^alschpo^cpo, Stefan Dicka, Thomas Zeiskeb | Requires cookie* | | | Title
| Francoanellit K3A15HP04)6(P04)2*12H20: Struktur und Synthese durch topochemische Entwässerung von Taranakit-I 2 H2O: Structure and Synthesis by Topochemical Dehydration of Taranakite | | | | Abstract
| Single crystals of synthetic francoanellite K3Al5(HP0 4)6(P0 4)2-12H20 could be obtained for the first time by topochemical dehydration of taranakite crystals. An X-ray structure de termination showed francoanellite to be the mineral with the second longest crystallographic axis described hitherto. Crystal data: space group R3c, a = 869.0(2), c = 8227(1)pm, Z = 6 , R g = 0.042. Francoanellite is a layer structure mineral having six layers of composition [K3Al5(HP04)6(P04)2(H2 0)i2], connected by hydrogen bonds. The rigid layer is formed by columns of corner sharing hydrogen phosphate tetrahedra and AIOö-octahedra which are inter connected by additional six-coordinated A1 ions. In trigonal holes of the layer orthophosphate ions are situated. The structure of francoanellite is very similar to the structure of taranakite K3H6Al5(P04)8-18H20 which has planar water interlayers between the Al-phosphate layers. A neutron scattering experiment with subsequent Rietveld refinement of the powder pattern gave the H-atom positions. Hydrogen bonds in francoanellite are formed within the rigid layers and between them. During the reaction taranakite —► francoanellite crystals in an intermediate stage of dehy dration could be obtained. From the c-axis of 8858 pm and one-dimensional electron density projections it can be proposed that in these crystals every second water interlayer was lost and a first order staging product of the deintercalation of water from taranakite was formed. | | | |
Reference
| Z. Naturforsch. 53b, 711—719 (1998); eingegangen am 2. März 1998 | | | |
Published
| 1998 | | | |
Keywords
| Crystal Structure, Neutron Scattering, Francoanellite, Taranakite, Topochemical Reaction | | | |
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| default:Reihe_B/53/ZNB-1998-53b-0711.pdf | | | | Identifier
| ZNB-1998-53b-0711 | | | | Volume
| 53 | |
| 28 | Author
| Andreas Mommertz, Roland Leo, Werner Massa, Kurt Dehnicke | Requires cookie* | | | Title
| Uber die Reaktion von Bis(f-butylamino)dimethylsilan mit Titantetrachlorid. Kristallstrukturen des Imido-Komplexes [TiCl2 (N-CMe3 )(H2 N-CMe3 )(CH3CN)]2 und des Ketimido-Komplexes [TiCl3 {NC(Me)N(H)CMe3}(CH3CN)2 ] | | | | Abstract
| On the Reaction of Bis(f-butylamino)dimethylsilane with Titanium Tetrachloride. Crystal Structures of the Imido Complex [TiCl->(N-CMe3)(H-,N-CMe3)(CH3CN)]2 and of the Ketimido Complex [TiCl3{NC(Me)N(H)CMe3}(CH3CN)2] The reaction of bis(f-butylamino)dimethylsilane with titanium tetrachloride in dichloro methane solution leads to a mixture of compounds from which the imido complex (H3N-CMe3)2[TiCl3(N-CMe3)]2 (1) and by extraction of the residue with acetonitrile the imido complex [TiCl2(N-CMe3)(H2N-CMe3)(CH3CN)]2 (2) can be isolated. 1 reacts with acetonitrile to give the ketimido complex [TiCl3{NC(Me)N(H)CMe3}(CH3CN)2] (3). According to crystal structure determinations 2 consists of centrosymmetric dimeric molecules containing TiCl2Ti bridges, the N-CMe3~ ligands being in equatorial positions with TiN bond lengths of 168.8(4) pm which corresponds to double bonds. In the monomeric complex 3 the chloro ligands are in meridional positions of the distorted octahedrally coordinated titanium atom with a TiN bond length of 175.7(2) pm of the ketimido ligand. | | | |
Reference
| Z. Naturforsch. 53b, 887—892 (1998); eingegangen am 27. April 1998 | | | |
Published
| 1998 | | | |
Keywords
| Titanium, Imido Complex, Ketimido Complex, Crystal Structure | | | |
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| default:Reihe_B/53/ZNB-1998-53b-0887.pdf | | | | Identifier
| ZNB-1998-53b-0887 | | | | Volume
| 53 | |
| 29 | Author
| Werner Urland, Helmut Person | Requires cookie* | | | Title
| Zur Kristallstruktur von Ho2Se3 On the Crystal Structure of Ho2Se3 | | | | Abstract
| Starting from HoSe2_ t powder and holmium metal bright brownish-yellow, plate-like single crystals of Ho2Se3 could be prepared by chemical transport with A1C13. Holmium sesquiselenide crystallizes in the Sc2S3-type structure, space group Fddd, with lattice constants a = 1140,7(2), b -812,6(1) and c = 2423,9(3) pm. | | | |
Reference
| Z. Naturforsch. 53b, 900—902 (1998); eingegangen am 9. April 1998 | | | |
Published
| 1998 | | | |
Keywords
| Holmium Sesquiselenide, Chemical Transport, Crystal Structure | | | |
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| default:Reihe_B/53/ZNB-1998-53b-0900.pdf | | | | Identifier
| ZNB-1998-53b-0900 | | | | Volume
| 53 | |
| 30 | Author
| Isabel Díaza, Vicente Fernández, José Luis, M. Artínezb, Lothar Beyer0, Astrid Pilzd, Ulrich Müllerd | Requires cookie* | | | Title
| Thermochrome Chloro-und Bromocuprate | | | | Abstract
| [C(NH2)3]2[CuBr4], (H3CC2N2SNH3)2[Cu2Br6], (C7N3H14)2[CuC14], (C7N3H14)2[CuBr4], [(Cl, Br)C3N2H6][CuCl3OH2] und (BrC3N2H6)2[CuBr4] Thermochromic Chloro-and Bromocuprates: [C(NH2)3]2CuBr4, (H3CC2N9SNH3)2[Cu2Br6], (C7N 3H 14)2[CuC14], (C7N3H 14)2[CuBr4], [(Cl, Br)C3N2H6][CuCl3OH2] and (BrC3N2H6)2[CuBr4] CuCl2 and CuBr2 were reacted in water-ethanol solutions containing HC1 or HBr, re spectively, with the following organic bases or their chlorides or bromides: guanidine (1), 2-amino-5-methyl-l,3,4-thiadiazol (2), hexahydro-2//-pyrimidine-(1,2A)-pyrimidine (3), and 2-hydrazino-2-imidazoline (4). With 1 and 3 the tetrahalocuprates (lH)2[CuBr4], (3H)2[CuCl4] and (3H)2[CuBr4] were obtained having flattened tetrahedral anions. 2 and CuBr2 form (2H)2[Cu2Br6], with nearly planar [Cu2Br6]2-ions that are associated to chains with square-pyramidal coordination of Cu. 2 and CuCl2 yield the hydrate (2H)C1H20 . 4 undergoes substitution of the hydrazine group for halogen, yielding the 2-halo-2-imidazolinium salts (5H)0 2(6H)o,8[CuCl3OH2] and (6H)2[CuBr4] in addition to [H3NCH2CH2NH3][CuCl4] (5 = 2-chloro-, 6 = 2-bromo-2-imidazoline). The planar [CuCl3(OH2)]_ ions are associated to chains. Crystal structure determinations were performed with (lH)2[CuBr4], (2H)2[Cu2Br6], (3H)2[CuCl4], (5H)0 2(6H)o 8[CuCl3OH2] and (6H)2[CuBr4]; the latter three at 298 K and at 166 K or 173 K. The known crystal structure of [H3N(CH2)2NH3][CuCl4] was redetermined at 166 K. In all cases small differences of bond lengths and bond angles are observed between room temperature and low temperature. The magnetic properties and electrospray mass spectra were measured. The products show thermochromic behavior. | | | |
Reference
| Z. Naturforsch. 53b, 933—938 (1998); eingegangen am 6. Mai 1998 | | | |
Published
| 1998 | | | |
Keywords
| Chloro Cuprates, Bromo Cuprates, Crystal Structures, Thermochromism | | | |
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| default:Reihe_B/53/ZNB-1998-53b-0933.pdf | | | | Identifier
| ZNB-1998-53b-0933 | | | | Volume
| 53 | |
| 31 | Author
| Steffen Runge, M. Athias, O. Senge | Requires cookie* | | | Title
| Electron Donor-Acceptor Compounds. Synthesis and Structure of 5-(l,4-Benzoquinone-2-yl)-10,15,20-trialkylporphyrins | | | | Abstract
| A series of 5-(benzoquinone)-10,15,20-trialkylporphyrins was synthesized via cross conden sation of the respective aldehydes, 2,5-dimethoxybenzaldehyde and pyrrole followed by de-methylation with BBr3 and oxidation with P b 0 2. This method worked reasonably well for compounds bearing the benzoquinone substituent and butyl, isopropyl, 1 -methylpropyl and 2-ethylpropyl residues (2a-d). The free base porphyrin quinones were converted into the zinc(II) complexes (3a-d) all of which showed remarkable stability for porphyrin quinones. The zinc(II) complex 3c bearing isopropyl residues was investigated by X-ray crystallography and showed a supramolecular structure consisting of polymeric chains facilitated by coordina tion of a benzoquinone oxygen to a neighboring zinc(II) center. Attempts to synthesize a 5-(benzoquinone)-10,15,20-tris(terr-butylporphyrin) resulted in the formation of a yellow por-phomethene (4), which could not be oxidized further. A crystal structure analysis of 4, the first for a free base porphomethene, shows an extremely twisted conformation with syn-orientation of the three rm-butyl groups. The results indicate that new methods will have to be developed for the synthesis of nonplanar porphyrin quinones. | | | |
Reference
| Z. Naturforsch. 53b, 1021—1030 (1998); received June 15 1998 | | | |
Published
| 1998 | | | |
Keywords
| Porphyrins, Quinones, Electron Transfer Compounds, Crystal Structure, Conformation | | | |
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| default:Reihe_B/53/ZNB-1998-53b-1021.pdf | | | | Identifier
| ZNB-1998-53b-1021 | | | | Volume
| 53 | |
| 32 | Author
| M. Sm, B. Ern, H. Ard, N. Eum Üller, K. Urt, D. Ehnicke | Requires cookie* | | | Title
| ClPb[N(SiMe3)2]3 C rystal S tructure of C lPb[N (SiM e3 ) 2 ]3 | | | | Abstract
| Pale brown single crystals of the title compound have been obtained by the reaction of Pb[N(SiMe3) 2] 2 with molybdenum pentachloride in ether solution as a result of a redox reaction. ClPb[N(SiMe3) 2] 3 crystallizes in the trigonal space group R3 with three formula units per unit cell. Lattice dimensions at -50 °C: a = b -1828.7(2), c = 854.5(1) pm. The compound forms monomeric molecules with bond lengths P b-C l = 247.9(4) pm and P b -N = 213(2) pm. | | | |
Reference
| Z. Naturforsch. 53b, 1074—1076 (1998); eingegangen am 3. Juli 1998 | | | |
Published
| 1998 | | | |
Keywords
| Lead(IV), Amido Complex, Crystal Structure | | | |
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| default:Reihe_B/53/ZNB-1998-53b-1074_n.pdf | | | | Identifier
| ZNB-1998-53b-1074_n | | | | Volume
| 53 | |
| 33 | Author
| Frank Wendland, Christian Näther, Michael Schur, Wolfgang Bensch | Requires cookie* | | | Title
| Solvothermal Synthesis and Crystal Structure Determination of Tris- (ethyleneamine-ammonium) Tetraselenoantimonat: Non-Centrosymmetry Mediated by an Extended Unusual N-H***N Hydrogen Bonded Network? | | | | Abstract
| The title compound has been synthesized under solvothermal conditions by the reaction of elemental chromium, antimony and selenium in a solution of 40% 1,2-ethanediamine (en) in methanol. The crystal structure consists of tetrahedral SbSe,*3 --anions which are connected by monoprotonated 1,2-ethanediamine (enH+) cations via N-H--Se hydrogen bonding. The enH+ cations are joined via strong N-H -N hydrogen bonds between the ammonium hydrogen and the amino nitrogen atom forming four distinct chains, each built up of three crystallographically independent enH+ cations. Two of these chains are running parallel to [100], the other two are parallel to [010]. Based on this arrangement different centrosymmetric or non-centrosymmetric hydrogen bonding patterns are possible, but only in one chain the sequence of NH2 and NH3+ groups was determined by X-ray diffraction. | | | |
Reference
| Z. Naturforsch. 53b, 1144—1148 (1998); received June 15 1998 | | | |
Published
| 1998 | | | |
Keywords
| Selenoantimonates, Solvothermal Synthesis, Crystal Structure, Hydrogen Bonding | | | |
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| default:Reihe_B/53/ZNB-1998-53b-1144.pdf | | | | Identifier
| ZNB-1998-53b-1144 | | | | Volume
| 53 | |
| 34 | Author
| Markus Tampier, Dirk Johrendt | Requires cookie* | | | Title
| B aC u 6G e2S8 -Ein Thiogermanat als Variante der L i3Bi-Struktur BaCu6Ge2S8 -A Thiogermanate as a Variant of the Li3Bi Structure | | | | Abstract
| BaCu6Ge2S8 was synthesized by direct reaction of the elements at 750°C and characteri zed by X-ray single crystal techniques. The thiogermanate crystallizes in a new orthorhombic structure type (a = 6.122(1) A, b = 12.084(3) A , c = 17.614(5) A; Pbcm, Z = 4). Isola ted [GeS4]4_ tetrahedra form a slightly distorted cubic face-centered (fee) arrangement. Ba-and Cu-atoms each occupy half the octahedral gaps (O G) of this " tetrahedra packing" . Fur ther Cu atoms fill the tetrahedral gaps (T G) completely. The compound can be written as Ba2<l/2 0 G,(Cu2)2<l/2<:)G)Cu8<7G)(GeS4)4 . Thus the structure o f BaCu6Ge2S8 can be derived from the Li^Bi type. The sulfur coordination o f the metal atoms (Cu tetrahedral or trigonal, Ba with CN 8) are realized by the spatial orientation of the [GeS4]4~ tetrahedra. Their centers nearly maintain the fcc-arrangement. This structure interpretation of BaCu6 Ge2S8 from the viewpoint o f a " filled tetrahedra packing" is discussed for further known thiogermanate compounds. | | | |
Reference
| Z. Naturforsch. 53b, 1483—1488 (1998); eingegangen am 9. Juli 1998 | | | |
Published
| 1998 | | | |
Keywords
| Chalcogenides, Germanium, Copper, Preparation, Crystal Structure | | | |
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| default:Reihe_B/53/ZNB-1998-53b-1483.pdf | | | | Identifier
| ZNB-1998-53b-1483 | | | | Volume
| 53 | |
| 35 | Author
| Yoshitaka Matsushitab, MercouriG. Kanatzidis | Requires cookie* | | | Title
| Synthesis and Structure of I ^ G e S | | | | Abstract
| The compound Li4 GeS4 has been prepared as transparent, light yellow moisture-sensitive crystals. Li.(GeS4 belongs to the space group Pnma with a = 14.107(6) A, b = 7.770(3) A and c = 6.162(2) A. The crystal structure was solved by direct-methods. The final R and /?H-values are 1.85 and 1.65% for 866 observed reflections. The Li4 GeS4 structure has three crystallographically independent lithium sites and one germanium site. The lithium atoms adopt two different coordination types. The Lil atom is coordinated to five sulfur atoms in a square pyramidal geometry, while the Li2 and Li3 atoms have distorted tetrahedral coordination. The Ge atom is tetrahedrally coordinated by four sulfur atoms and is found as [GeS4 ]4-units. The anisotropic three-dimensional crystal structure of Li4 GeS4 is described. | | | |
Reference
| (Z. Naturforsch. 53b, 23—30 [1998]; received October 10 1997) | | | |
Published
| 1998 | | | |
Keywords
| Lithium, Germanium, X-Ray Data, Crystal Structure, Raman Spectra | | | |
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| default:Reihe_B/53/ZNB-1998-53b-0023.pdf | | | | Identifier
| ZNB-1998-53b-0023 | | | | Volume
| 53 | |
| 36 | Author
| Vibrational Spectra, Sandra Loss, Caroline Röhr | Requires cookie* | | | Title
| RbAsF6, CsA sF 6 und RbSbF6: Kristallstrukturen, Thermische Phasenumwandlungen und Schwingungsspektren RbAsF6, CsAsF6 and RbSbF6: Crystal Structures, Thermal Phase Transitions | | | | Abstract
| The title compounds are isostructural to CsSbFö and crystallize with the KOsFö structure type (space group RS, Z = 3) with the lattice constants a = 749.7(1) pm, c = 758.9(1) pm (RbAsFö), a = 772.3(1) pm, c = 805.0(1) pm (CsAsFö) and a = 767.0(1) pm, c = 786.1(2) pm (RbSbF6). The structures exibit nearly ideal [MFö]-octahedra, the alkaline cations are coordinated by 12 fluorine ions in a distorted cuboctahedral geometry. Cations and complex anions form a slightly distorted CsCl arrangement. On heating, the arsenates transform to a NaCl arrangement with disordered [AsF6] ions, whereas the antimonates of Rb and Cs form the corresponding disordered CsCl type at higher temperatures. The phase transitions and the i. r. and Raman spectra as well as the structural relations to the remaining hexafluoropnictates A![MVF6] are discussed. | | | |
Reference
| (Z. Naturforsch. 53b, 75—80 [1998]; eingegangen am 14. Oktober 1997) | | | |
Published
| 1998 | | | |
Keywords
| Alkaline Hexafluoropnictates, Crystal Structure, Thermal Phase Transitions, Vibrational Spectra | | | |
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| default:Reihe_B/53/ZNB-1998-53b-0075.pdf | | | | Identifier
| ZNB-1998-53b-0075 | | | | Volume
| 53 | |
| 37 | Author
| Gabriele Korus, Martin Jansen | Requires cookie* | | | Title
| Kristallstruktur von Natriumtrifluormethylsulfonat- Trifluormethylsulfonsäure (1/3) Studies on Sodium Trifluoromethanesulfonate. Crystal Structure of Sodium Trifluoromethanesulfonate-Trifluoromethanesulfonic Acid (1/3) | | | | Abstract
| Single crystals of sodium trifluoromethanesulfonate-trifluoromethanesulfonic acid (1/3) (N aS 0 3CF3 • 3 H S 0 3CF3) have been prepared by reaction of sodium trifluoromethanesulfonate with anhydrous trifluoromethanesulfonic acid at 60 °C. N aS 0 3CF3 • 3 H S 0 3CF3 crystallizes in space group 1 2 ^ (No. 199) with a = 16.210(1) A, Z = 8. Sodium is coordinated by six oxygen atoms from six different trifluoromethanesulfonic acid molecules, each acid molecu le connecting two sodium ions. The 3-dimensional network resulting from the edge sharing octahedra corresponds to the cubic (10, 3) net, not realised otherwise, so far. The trifluorome thanesulfonate anion is bonded to three trifluoromethanesulfonic acid molecules by hydrogen bonds. | | | |
Reference
| Z. Naturforsch. 53b, 438—442 (1998); eingegangen am 19. Dezember 1997 | | | |
Published
| 1998 | | | |
Keywords
| Sodium Trifluoromethanesulfonate, Sodium Triflate, Trifluoromethanesulfonic Acid, Synthesis, Crystal Structure | | | |
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| default:Reihe_B/53/ZNB-1998-53b-0438.pdf | | | | Identifier
| ZNB-1998-53b-0438 | | | | Volume
| 53 | |
| 38 | Author
| Dirk Steinbom, Olaf Gravenhorst, Henrik Junicke, FrankW. Heinemann | Requires cookie* | | | Title
| Synthese und Charakterisierung von kronenetherstabilisierten Platin(IV)- Komplexen mit Aminosäureliganden Synthesis and Characterization of Amino Acid Complexes of Platinum(IV) Stabilized by Crown Ethers | | | | Abstract
| Crown ether complexed pentachloro(aqua)platinic acid, (H30)[PtCl5(H20)]-2(18-cr-6) • 6H20 (1) reacts with glycine, L-alanine, and DL-2-aminobutyric acid to give ds-[PtCl4(0-glyH)(H20)](1 8 -cr-6)H 20 (4a)1 and ds-[PtCl4(0-amacH)(H2O)](18-cr-6) (amacH = alaH 4b, abuH 4c), respectively, as well as (amacH2)2[PtCl6]-2(18-cr-6) (amacH = glyH 5a, alaH 5b, abuH 5c). The crown ether complexed hexachloroplatinic acid, (H30) 2[PtCl6]-2(18-cr-6) (2), reacts with glycine to afford (glyH2)[PtCl4(yV,0-gly)]-2(18-cr-6)1.25H20 (6). The structures of 4b and 6 were determined by X-ray diffraction. The alanine ligand in 4b is a zwitterion that is coordinated to platinum by one oxygen atom of the carboxylate group only. The other oxygen atom is engaged in a strong hydrogen bond to the ds-coordinated aqua ligand. The glycinato ligand in 6 is /V,(9-coordinated at platinum forming an anion [PtCl4(/V,0-gly)]_ . The other oxygen atom of the carboxylate group is involved in a strong hydrogen bridge to the cation (glyH2)+. In both complexes hydrogen bridges are formed between the -N+H3 and -NH2 groups of the amino acid ligands and the oxygen atoms of the crown ether molecules. 1 Abbreviations: amacH = amino acid, glyH = glycine, alaH = L-alanine, abuH = DL-2-amino-butyric acid. | | | |
Reference
| Z. Naturforsch. 53b, 581—586 (1998); eingegangen am 16. Januar 1998 | | | |
Published
| 1998 | | | |
Keywords
| Platinum(IV) Complexes, Crown Ethers, Amino Acids, Crystal Structure | | | |
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| default:Reihe_B/53/ZNB-1998-53b-0581.pdf | | | | Identifier
| ZNB-1998-53b-0581 | | | | Volume
| 53 | |
| 39 | Author
| JuliaA. Manskayaa, KonstantinV. Domasevitcha ', VeraV. Ponomareva2, Joachim Sielerb, VolodimirN. Kokozay2 | Requires cookie* | | | Title
| Crystal Engineering towards Design of Macrocyclic Coordination Compounds: Crystal Structure of Rubidium Tetrachloro-and Tetracyanoaurate(III) Complexes with 18-Crown-6 | | | | Abstract
| The new macrocyclic complexes of composition Rb(18-crown-6)AuX4 (X = Cl (1) and CN (2)) have been prepared and characterized by X-ray crystallography (1: monoclinic, space group P2\/n, with a = 8.747(1), b = 8.366(1), c = 15.404(1) Ä; ß = 104.37(1)°, V = 1092.0(3) A , Z = 2; final R 1 =0.025 for 2030 independent reflections used; 2: monoclinic, space group P2\/c, with a = 14.765(3), 6 = 17.134(3), c = 8.855(2) k \ ß = 90.20(1)°, V = 2240.2(8) Ä3, Z = 4; final R 1 = 0.080 for 2034 independent reflections used). Both structures consist of Rb(18-crown-6)+ cations (A) and complex aurate(III) anions AuX4_ (B). Complex 1 has a linear polymeric array -A-B-A-B-(Rb-Cl 3.604(3), 3.654(3) Ä) with the rubidium ions disordered 0.276(2) A above and below the crown ether plane (Rb-O 2.819(5)-2.884(5) A, av. 2.846(5) A). The positioning of the rubidium atom away from the center of the 18-crown-6 is effected by the packing of the Rb(18-crown-6)+ and AuCU-moieties, and by the resemblance in the charge and symmetry of the cationic and anionic parts of the structure. Complex 2 has a zig-zag polymeric array -A-B-A-B-(Rb-N 2.92(2), 2.94(1) A) with orthogonal disposition of Rb(18-crown-6)+ and Au(CN)4-planes. The rubidium atom is situated 0.90(2) A above the mean plane of the macrocyclic oxygen atoms (Rb-O 2.93(5)-3.15(4) A) and adopts a typical "sunrise coordination". | | | |
Reference
| Z. Naturforsch. 53b, 683—688 (1998); received January 5 1998 | | | |
Published
| 1998 | | | |
Keywords
| 18-Crown-6, Rubidium Macrocyclic Complexes, Gold(III), Crystal Structure | | | |
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| default:Reihe_B/53/ZNB-1998-53b-0683.pdf | | | | Identifier
| ZNB-1998-53b-0683 | | | | Volume
| 53 | |
| 40 | Author
| Wolfgang Banße, Jana Fliegner, Stefan Sawusch, Uwe Schilde, Erhard Uhlemann | Requires cookie* | | | Title
| Dioxomolybdän(VI)-Komplexe mit dreizähnigen diaciden Liganden Dioxomolybdenum(VI) Complexes with Tridentate Diacidic Ligands | | | | Abstract
| Dioxomolybdenum(VI) complexes have been synthesized by ligand exchange reactions o f M o(CO)6, M o(NO)2(acac)2 and M o 0 2(acac)2 with tridentate diacidic ligands. X-ray structure analyses were performed on single crystals. The complexes salicylaldehyde-2-hydroxyanilato(2-)-triphenylphosphaneoxide-dioxomolybdenum(VI) (lb) and 2,2'-dihydroxy-azobenzenato(2-)-triphenylphosphaneoxide-dioxomolybdenum(VI) (2) are isomorphous. In all chelates the Mo atom is in a distorted octahedral environment. Structural data: Salicylaldehyde-2-hydroxyanilato(2-)-tetrahydrofurane-dioxomolybdenum (VI) (la): a = 23.381(6) Ä, b = 6.756(2) A, c = 28.380(8) A, ß = 124.47(2)°; Salicylaldehyde-2-hydroxyanilato(2-)-triphenylphosphaneoxide-dioxomolybdenum (VI) (lb): a = 9.4208(14) A, b = 30.550(5) A, c = 10.461(2) Ä, ß = 111.005(17)°; 2,2'-Dihydroxy-azobenzenato(2-o)-triphenylphosphaneoxide-dioxomolybdenum(VI) (2): a = 9.392(2) A, b = 31.012(13) A, c = 10.350(2) Ä, /3 = 110.968(17)°; Salicylaldehyde-salicylhydrazonato(2-0)-triphenylphosphaneoxide-dioxomolybdenum(VI) (3): a = 9.321(2) A, b = 12.048(2) A, c — 13.858(3) A, a = 101.90(2)°, ß = 94.94(2)°, 7 = 105.479(17)°. | | | |
Reference
| Z. Naturforsch. 53b, 689—693 (1998); eingegangen am 6. März 1998 | | | |
Published
| 1998 | | | |
Keywords
| Ligand Exchange Reactions, Dioxomolybdenum(VI) Complexes, Tridentate Diacidic Ligands, Crystal Structure | | | |
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| default:Reihe_B/53/ZNB-1998-53b-0689.pdf | | | | Identifier
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| 53 | |
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