| 61 | Author
| Marcos Luján, Frank Kubel, Hans Schmid | Requires cookie* | | Title
| Crystal Growth, Room Temperature Crystal Structure and Phase Transitions of K M nP04  | | | Abstract
| Single crystals of K M nP 04 grown in a KC1 flux show ferroelastic domains. The structure was determ ined on an optically controlled single domain crystal by X-ray diffraction methods. The cell is triclinic with dimensions a = 5.4813(5), b = 8.627(1), c = 8.887(1), in A, a = 87.73(1)°, ß = 89.10(1)°, y = 88.01(1)°, VM = 419.6(1) A 3 and Z = 4. The structure is closely related to the stuffed /3-tridymite type. DTA experiments between room tem perature and 1000 °C and polarized light microscopy observations showed four phase transitions: at 165, 330, 353 and 707 °C. | | |
Reference
| Z. Naturforsch. 50b, 1210—1214 (1995); received February 20 1995 | | |
Published
| 1995 | | |
Keywords
| Manganese Potassium Orthophosphate, Crystal Structure, Crystal Growth, Phase Transitions | | |
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| default:Reihe_B/50/ZNB-1995-50b-1210.pdf | | | Identifier
| ZNB-1995-50b-1210 | | | Volume
| 50 | |
62 | Author
| Z. Naturforsch | Requires cookie* | | Title
| In2.24(NCN)3 and NaIn(NCN)2: Synthesis and Crystal Structures of New Main Group Metal Cyanamides  | | | Abstract
| Single crystals of In2.24(N C N)3 and N aIn(N C N)2 can be synthesized from a reaction be tween InBr and NaCN at 400 °C, followed by chemical transport at 4 0 0 -5 0 0 °C. The X-ray crystal structure determinations of In2.24(N C N)3 (rhombohedral R 3c, a = 606.09(4), c -2884.4(2) pm, Z = 6) and N aIn(N C N)2 (orthorhombic Cmcm, a = 961.30(6), b = 716.84(5), c = 603.65(4) pm, Z = 4) reveal ionic layer structures built from sheets of cationic and anionic (cyanamide) motifs. While N aIn(N C N)2 contains In3+ and N a+ ions, In2 24(N C N)3 is a mixed-valence compound, incorporating a m onovalent In+ ion besides trivalent indium. The N CN 2~ units of both In2,24(N C N)3 and N aIn(N C N)2 reflect perfect D xll point group symmetry within the limits of experimental accuracy. Furthermore, an evaluation of all presently available crystallographic data on metal cyanamide crystal structures manifests that there is no evi dence for a non-centrosymmetric description o f any of these. Likewise, we propose an alter native centrosymmetric structural model for lead cyanamide, PbNCN, and question the evi dence of the unsymmetrical, non-D xh shaped cyanamide anion in the latter structure. | | |
Reference
| Z. Naturforsch. 50b, 1245—1251 (1995); received April 11 1995 | | |
Published
| 1995 | | |
Keywords
| Indium Cyanamide, Indium Sodium Cyanamide, Crystal Structure, Cyanamide Molecular Symmetry | | |
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| default:Reihe_B/50/ZNB-1995-50b-1245.pdf | | | Identifier
| ZNB-1995-50b-1245 | | | Volume
| 50 | |
65 | Author
| Frank Steffen, G. Erd, Meyer | Requires cookie* | | Title
| [Er14(C2)2 (N )2 ] l24 -ein Iodid mit einem oligom eren, heterointerstitiellen Cluster [E r14(C2)2(N)2]l24 -an Iodide with an Oligomeric, H eterointerstitial Cluster  | | | Abstract
| [Er14(C2)2(N)2]l24 (triclinic, P I, a = 966.3(4) pm. b = 1027.6(2) pm. c = 1663.4(4) pm, « = 101.374(9)°, ß = 92.853(14)°, y = 112.83(2)°, Z = 2) is obtained as red-brown single crystals through a conproportionation reaction of E rl3 and erbium in the presence of carbon and N aN 3 in a sealed niobium container. It contains discrete, tetrameric [Er14(C2)2(N)2] clusters that are built from two octahedra and two tetrahedra connected via com mon edges. The octahedral voids are filled with C2 units and the tetrahedral voids with N atoms. Each discrete [Erj4(C2)2(N)2] cluster is surroun ded by 32 iodide ligands which connect six clu sters via i-a and a-a bridges. | | |
Reference
| Z. Naturforsch. 50b, 1570—1573 (1995); eingegangen am 7. April 1995 | | |
Published
| 1995 | | |
Keywords
| Rare Earth Elements, Halides, Cluster, Erbium Iodide Dicarbide Nitride, Crystal Structure | | |
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| default:Reihe_B/50/ZNB-1995-50b-1570_n.pdf | | | Identifier
| ZNB-1995-50b-1570_n | | | Volume
| 50 | |
66 | Author
| Anne Utzolino, Karsten Bluhm | Requires cookie* | | Title
| Cox 5Ti0 5(B 0 3) 0 and Co! 5Zro.5(B 0 3) 0  | | | Abstract
| Single crystals of Co15Tio.5(B 0 3)0 (I) and Coj 5Zr0 5(BO3)O (I I) were obtained by a B20 3 flux technique. Both compounds crystallize with orthorhombic symmetry, space group D -Pnma (Nr. 62), I a = 928.1; b = 311.1; c = 940.1 pm; Z = 4 and I I a = 949.5; b = 323.42; c = 934.7 pm; Z = 4. The compounds are isotypic to the mineral warwickite. All metal ions are octahedrally coordinated by oxygen ions. The structure contains isolated, trigonal planar B 0 3 units and oxygen that is not coordinated to boron. Die Synthese und Kristallstruktur von cobalthaltigen Boratoxiden: Coi^Tio,5(B03)0 und C o i?5Zr<),5(B03)0 | | |
Reference
| Z. Naturforsch. 50b, 1653—1657 (1995); eingegangen am 4. Mai 1995 | | |
Published
| 1995 | | |
Keywords
| Cobalt, Titanium, Zirconium, Borate Oxide, Crystal Structure, X-Ray | | |
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| default:Reihe_B/50/ZNB-1995-50b-1653.pdf | | | Identifier
| ZNB-1995-50b-1653 | | | Volume
| 50 | |
67 | Author
| Oliver Seidelmann, Lothar Beyer, Rainer Richter | Requires cookie* | | Title
| N,N-Disubstituierte N'-Ferrocenoylthioharnstoffe als zweizähnige Komplexliganden für Übergangsmetallionen. Kristallstruktur von Bis-(N,N-diethyl-N'-ferrocenoylthioureato)nickel(II) N,N-Disubstituted N'-Ferrocenoyl Thioureas as Bidentate Ligands for Transition Metal Ions. Crystal Structure of Bis-(N,N-diethyl-N'-ferrocenoylthioureato)nickel(II)  | | | Abstract
| N,N-diethyl-N'-ferrocenoyl-thiourea and N-(morpholino-thiocarbonyl)ferrocenecarboxylic amide have been prepared by the reaction of ferrocenoyl chloride with potassium thiocyanate and the respective amine in dry acetone. These bidentate ligands yield neutral heterometal-lic complexes with Ni(II), Cu(II), Mn(II) and Co(III). The dark brown air stable crystals of bis-(N,N-diethyl-N'-ferrocenoylthioureato)nickel(II) were characterized by X-ray structure de termination. Lattice dimensions: a = 1870.9(1), b = 1161.5(1), c = 1491.4(1) pm; space group Pca2!, Z = 4, R = 0.030 for 5707 observed reflections. | | |
Reference
| Z. Naturforsch. 50b, 1679—1684 (1995); eingegangen am 23. März 1995 | | |
Published
| 1995 | | |
Keywords
| Ferrocene Complexes, Thiourea, Hetero Metal Complexes, Synthesis, Crystal Structure | | |
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| default:Reihe_B/50/ZNB-1995-50b-1679.pdf | | | Identifier
| ZNB-1995-50b-1679 | | | Volume
| 50 | |
68 | 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 | |
69 | 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 | |
70 | Author
| AndreasF. Stange, Eberhard Waldhör, Michael Moscherosch, Wolfgang Kaim | Requires cookie* | | Title
| Variable Structure of the Cu2S2 Core in Doubly Thiolate-Bridged Dicopper(I) Complexes. An X-Ray Crystallographic, Electrochemical and EPR Study of (dmp)2 (o-CH3 C6H4S)2Cu2 , dmp = 2,9-Dimethyl-l,10-phenanthroline, and a Comment on the Nature of Phenanthroline-Containing "Cu(0)" Complexes  | | | Abstract
| The molecular and crystal structure of the dicopper(I) complex (dm p)2(M-o-CH3C6H4S)2Cu2 (1), dmp = 2,9-dim ethyl-l,10-phenanthroline, has been deter mined. With Cu/S/Cu and S/Cu/S bond angles between 80 and 100°, the planar structure of the central CuSCuS four-membered ring is much more symmetric for 1 as compared to the analogous complex 2 of unsubstituted 1,10-phenanthroline which has a folded Cu2S2 core with bond angles between 67 and 108°. This result illustrates a considerable structural flexi bility of the LCu(m-SR)2CuL entity which is being discussed as a possible model for CuA centers of cytochrome c oxidase or nitrous oxide reductase. Oxidation of both com plexes 1 and 2 remains irreversible even at cyclovoltammetric scan rates o f 1 V/s. However, the methyl substitution in complex 1 causes increased reversibility of the electronically coupled dmp-based reduction processes. Accordingly, the EPR spectrum of l -* is characterized by hyper-fine splitting from dmp--and a relatively small 63 " Cu coupling of 0.53 mT. The stabilization of 2,9-disubstituted 1,10-phenanthroline radical anions by coordination to Cu(I) is also dem onstrated by detection of a single broad EPR line at g 2.0028 for the formal "C u(0)" complex Cu(dpp)2 = CuI(dpp_-)(dpp), dpp = 2,9-diphenyl-l,10-phenanthroline. While the EPR signal of Cu(dpp)2 loses intensity on cooling, possibly due to dimerization and spin-pairing, the distorted tetrahedral configuration with essential orthogonal arrangement of dpp jz systems seem s to disfavour an intramolecular electron hopping. | | |
Reference
| (Z. Naturforsch. 50b, 115—122 [1995]; received July 25 1994) | | |
Published
| 1995 | | |
Keywords
| Crystal Structure, Copper Complexes, Sulfur Ligands, 1, 10-Phenanthrolines, EPR Spectra | | |
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| default:Reihe_B/50/ZNB-1995-50b-0115.pdf | | | Identifier
| ZNB-1995-50b-0115 | | | Volume
| 50 | |
71 | Author
| Peter Dierkes, Gerlinde Frenzen, Sigrid Wocadlo, W. Erner Massa, Stefan Berger, Jürgen Pebler, Kurt Dehnicke | Requires cookie* | | Title
| Komplexe des Typs [MCl4(SEt2)2] mit M = Mo und W. Kristallstrukturen, NMR-Spektren und magnetisches Verhalten [MCl4(SE t2)2] Complexes with M = Mo and W. Crystal Structures, NMR Spectra, and Magnetic Behaviour  | | | Abstract
| The crystal structures of the thioether complexes [MCl4(SEt2)2] with M = Mo and W have been solved by X-ray methods. Both compounds crystallize isotypically in the triclinic space group P I with two formula units per cell unit. The metal atoms are octahedrally coordinated by four chlorine atoms and by the two sulfur atoms of the thioether molecules in trans position (symmetry Q) with bond lengths (average): M o -C l 233.1, M o -S 253.4, W -C l 233.1, and W -S 251.7 pm. Both complexes were also characterized by !H and 13C NM R spectro scopy as well as by measurement of the magnetic susceptibilities in the tem perature range from 1.8 to 350 K. | | |
Reference
| Z. Naturforsch. 50b, 159—167 (1995); eingegangen am 23. August 1994 | | |
Published
| 1995 | | |
Keywords
| D iethylthioethers of Molybdenum and Tungsten, Crystal Structure, NMR Spectra, Magnetic Susceptibility | | |
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| default:Reihe_B/50/ZNB-1995-50b-0159.pdf | | | Identifier
| ZNB-1995-50b-0159 | | | Volume
| 50 | |
72 | Author
| Hans Bock, Sabine Nick, Christian Näther, Wolfgang Bensch | Requires cookie* | | Title
| Wechselwirkungen in Kristallen, 63 [1, 2]  | | | Abstract
| Kristallisation und Strukturbestimmung von 1,2-Dimesitoylbenzol und von Bis(hydrogen-l,2-dimesitoylbenzol)-dinatrium-bis(ethylendiamin) Interactions in Crystals, 63 [1, 2] Crystallization and Structure Determ ination of 1,2-Dimesitoylbenzene and of Bis(hydrogen-l,2-dimesitoylbenzene)-disodium-bis(ethylendiamine) | | |
Reference
| Z. Naturforsch. 50b, 605 (1995); eingegangen am 18. August 1994 | | |
Published
| 1995 | | |
Keywords
| 1, 2-Dimesitoylbenzene, Radical A nion Sodium Salt, Single Crystal Structures, M N D O Calculations | | |
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| default:Reihe_B/50/ZNB-1995-50b-0605.pdf | | | Identifier
| ZNB-1995-50b-0605 | | | Volume
| 50 | |
73 | Author
| Konstantina Kehagia, Alexander Dömling, Ivar Ugi, Wolfgang Hiller, Jürgen Riede | Requires cookie* | | Title
| N e w Synthesis and Structure Determination o f 13-Aza-4,-trioxatricyclo[7,3>l?05'13]tridecane  | | | Abstract
| A new 13-Aza-4,4,8,8,12,12-hexamethyl-2,6,10-trioxatricyclo[7,3,l,05'13]tridecane synthesis and the crystal structure are reported. It crystallizes in the monoclinic space group P2Jn with a = 1201.9(1) pm, b = 1436.6(1) pm, c = 1726.2(2) pm, ß = 90.74(1)° and Z = 8. | | |
Reference
| Z. Naturforsch. 50b, 667—670 (1995); received August 2 1994 | | |
Published
| 1995 | | |
Keywords
| Asinger Condensation, C3-Symmetric Heterocycle, 5, 6-Dihydro-2//-l, 3-oxazine, Crystal Structure | | |
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| default:Reihe_B/50/ZNB-1995-50b-0667.pdf | | | Identifier
| ZNB-1995-50b-0667 | | | Volume
| 50 | |
74 | Author
| Z. Naturforsch | Requires cookie* | | Title
| Organosubstituierte  | | | Abstract
| l,6,2,5-Azoniathiasilaboratabicyc!o[3.3.0]oct-3-ene -Herstellung und Kristallstruktur [1] O rg anosubstituted 1,6,2,5-A zoniathiasilaboratabicyclo[3.3.0]oct-3-enes -P rep aratio n and Crystal Structure [1] R oland K östera *, G ü n te r Seidel3, B ernd W rackm eyerb, R oland B oesec The heterocycles MeNSi(Me2)C(R3)=C (Et)B Et [R3 = Me: A; R3 = C(M e)=CH 2: B] react with 2-aminoethanet'nioi (i) by elimination of M eNH 2 to give the monocyclic H N CH 2CH2SSi(Me2)C (R)=C (Et)B Et [R = Me: 3a; R = C(M e)=CH 2: 3b] and the ther-mically more stable bicyclic compounds H NSi(Me2)C (R)=C (E t)B (E t)SC H 2CH 2 [R = Me: 4a; R = C(M e)=CH2: 4b], 4a crystallizes in the monoclinic space ^ ro u p P2i/c [lattice con stants (at 120 K) a = 9.3239(10), b = 8.9225(11), c = 17.3958(23) A; ß = 92.207(9)°] with a folded bicyclic ring system. c/s-ClB(Et)C=C(M e)Si(M e2)Cl (C) and Na2-lB E t3 (prepared from 1 and N aH BEt3) form by elimination of M eNH2 preferentially 3 a and minor amounts of 4a. A reacts with o-aminothiophenol (2) via H NSi(Me2)C(M e)=C (Et)B (Et)S(oC 6H 4) (5) to NSi(Me2)C(M e)=C(Et)BS(oC6H 4) (6) and the products 7-10. | | |
Reference
| Z. Naturforsch. 50b, 959—968 (1995); eingegangen am 24. November 1994 | | |
Published
| 1995 | | |
Keywords
| 2, 5-Dihydro-l, 2, 5-azasilaboroles, Am inothioalkanes(arenes), Bicyclic Heterocycles, Crystal Structure | | |
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| default:Reihe_B/50/ZNB-1995-50b-0959.pdf | | | Identifier
| ZNB-1995-50b-0959 | | | Volume
| 50 | |
75 | Author
| Hans-Christian Böttcher3-, Helmut Hartungb, Andre Krugb | Requires cookie* | | Title
| Synthese und Kristallstruktur des koordinativ ungesättigten Komplexes [FeRu(CO)5(//-P B u92] Synthesis and Crystal Structure of the Coordinatively Unsaturated Complex [FeR u(C O )5Cu-PBu92]  | | | Abstract
| [{Ru(CO)3C12}2] reacts with the in situ prepared reagent Li2[Fe(CO)3(PBu2)2] to give the new heterobinuclear complex [FeRu(CO)5(w-PBu92] (!) • Crystals of 1 are isomorphous to those of the known compound [Fe2(CO)5(a-PBu2)2] (2) and crystallize in the triclinic space group P 1 with a = 867,5(1), b = 1181,0(2), c = 1373,1(2) pm; a = 76,64(1), ß = 79,72(1) and y = 76,48(1)°. A double bond between the two metal atoms concluded for 2 from the results of EHMO calcula tions is also proposed for 1 (Fe=Ru: 259,8(1) pm). | | |
Reference
| Z. Naturforsch. 50b, 1175—1180 (1995); eingegangen am 19. Januar 1995 | | |
Published
| 1995 | | |
Keywords
| Iron-Ruthenium Complex, H eterobinuclear Carbonyl Complex, Iron-Ruthenium Double Bond, Crystal Structure, Molecular Structure | | |
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| default:Reihe_B/50/ZNB-1995-50b-1175.pdf | | | Identifier
| ZNB-1995-50b-1175 | | | Volume
| 50 | |
77 | Author
| Béla Baján, H.-Jürgen Meyer | Requires cookie* | | Title
| Neue Niob-und Tantalchloride der  | | | Abstract
| Zusammensetzung A4[M6C118] (A = (Ga,) In, TI; M = Nb, Ta) New Niobium and Tantalum Chlorides of the Composition A4[M6C118] (A = (Ga,) In, TI; M = Nb, Ta) The syntheses of new compounds of the general formula A4[Nb6Cli8] (A = Ga, In, Tl) and A4[TaöCli8] (A = In, Tl) are reported. The indexing of their X-ray powder patterns was performed isotypically with K^NböClis]-A single-crystal structure refinement on In4[Ta6Clis] gave the space group C2/m, Z -2, a = 1077.7(3) pm, b = 1542.3(5) pm, c = 960.2(2) pm, ß = 117.68(2) . The structure contains [TaöCliiClö] strongly distorted coordination sphere of Cl -. | | |
Reference
| Z. Naturforsch. 50b, 1373—1376 (1995); eingegangen am 16. Januar 1995 | | |
Published
| 1995 | | |
Keywords
| Niobium and Tantalum Chloride Clusters, Monovalent Ga, In, TI, Synthesis, Crystal Structure | | |
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| default:Reihe_B/50/ZNB-1995-50b-1373.pdf | | | Identifier
| ZNB-1995-50b-1373 | | | Volume
| 50 | |
78 | Author
| W. S. Sheldrick, B. Schaaf | Requires cookie* | | Title
| Ditelluridogermanaten(IV) der Alkalimetalle K -C s M ethanolotherm al Synthesis and Crystal Structure of Diselenido-and Ditelluridogerm anates(IV ) of the Alkali Metals K -C s  | | | Abstract
| Methanolothermal reaction of M2C 0 3 (M = K, Rb) with Ge and Se yields respectively the diselenidogerm anates(IV) K2G eS e4 and Rb2G eSe4, both of which contain chain anions ro[GeSe42_] in which G eS e4 tetrahedra are linked via S e -S e bonds. A similar structural principle is found in the ditelluridogermanates(IV) Rb2GeTe4 and Cs2GeTe4, prepared by reaction of M2C 0 3 (M = Rb, Cs) with Ge and Te in methanol at temperatures o f respectively 200 and 160 °C. The effect of cation size on the chain conformation is discussed. Rb4G e4S eU)CH3O H , which is formed together with Rb2G eSe4, exhibits isolated anions [G e4S e 10]4_ with an adamantane-like structure. Methanolothermale Synthese und Kristallstruktur von Diselenido-und | | |
Reference
| Z. Naturforsch. 50b, 1469—1475 (1995); eingegangen am 31. März 1995 | | |
Published
| 1995 | | |
Keywords
| Selenidogerm anates(IV ), Telluridogermanates(IV), Alkali Cations, Methanolothermal Synthesis, Crystal Structure | | |
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| default:Reihe_B/50/ZNB-1995-50b-1469.pdf | | | Identifier
| ZNB-1995-50b-1469 | | | Volume
| 50 | |
|