| 1 | Author
| Enno Lork, Ulrich Behrens, G. Ünter Steinke, Rüdiger Mews | Requires cookie* | | Title
| Die Kristallstruktur von trans-l,3?5-Trichloro-l,3>5-trioxo  | | | Abstract
| 1 A6, 3 A6, 5 A6,2,4,6-trithiatriazin (/?-Sulfanurchlorid) The Crystal Structure o f /raws-1,3,5-Trichloro-1,3,5-trioxo-1 X6, 3/i6, 516, 2,4,6-trithiatriazine (/?-Sulfanuric Chloride) The crystal structure o f /?-(N S(0)C l)3 is reported. | | |
Reference
| Z. Naturforsch. 49b, 437 (1994); eingegangen am 22. November 1993 | | |
Published
| 1994 | | |
Keywords
| Trichlorotrioxotrithiatriazines, Sulfanuric Chlorides, Crystal Structure | | |
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| default:Reihe_B/49/ZNB-1994-49b-0437.pdf | | | Identifier
| ZNB-1994-49b-0437 | | | Volume
| 49 | |
4 | Author
| Jörn Müller, PetraEscarpa Gaede, Ke Qiao | Requires cookie* | | Title
| ^-Olefin-Iridium-Komplexe, XXII [1] C -H -Aktivierung von aromatischen und aliphatischen Solvensmolekülen RH bei der Reaktion von [Cp*IrCI2 ] 2 mit Butadienmagnesium unter Bildung von [Cp*Ir(773-C4H 7)R] sowie Kristallstruktur von [Cp*Ir(i/3-C4H 7)C6H 5] jr-Olefin Iridium Complexes, XXII [1] C -H Activation of Aromatic and Aliphatic Solvent Molecules RH in the Reaction of [Cp*IrCl2 ] 2 with Butadienemagnesium with Formation of [Cp*Ir(?;3 -C4 H 7 )R], and Crystal Structure of [Cp*Ir(773 -C4 H 7 )C6 H 5] Activation of C -H , (l-Methylallyl)(pentamethylcyclopentadienyl)iridium-a-organyl Com plexes  | | | Abstract
| Reactions of [Cp*IrCl2]2 (Cp* = ^3-C5M e5) with [MgC4H6 -2 THF]" at low temperature give [Cp*Ir(^4-C4H6)] together with [Cp*Ir(/73-C4H 7)R] compounds, the latter being formed via C -H activation of solvent molecules RH (RH = benzene, toluene, anisole, thiophene, furane, N-methylpyrrole, pentane, cyclohexane. THF). In the case of pyrrole, C -N -activation occurs. The ratio of syn and anti isomers of the 1-methylallyl com plexes as well as the sites o f C -H activation of RH were investigated by NM R spectrometry. An enantiomorphous crystal of [Cp*Ir(773-C4H7)C6Hs] was characterized by X-ray diffraction analysis which reveals trigonal planar coordination at the Ir atom and an exo, syn conformation o f the 1-methylallyl ligand. A mechanism of the reaction which involves 16-electron intermediates is discussed. The corresponding system [Cp*RhCl2]2/butadienemagnesium/RH gives only [Cp*Rh(>/4-C4H6)], and no C -H activation is observed. | | |
Reference
| Z. Naturforsch. 49b, 1645—1653 (1994) | | |
Published
| 1994 | | |
Keywords
| Synthesis, NMR Spectra, Crystal Structure | | |
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| default:Reihe_B/49/ZNB-1994-49b-1645.pdf | | | Identifier
| ZNB-1994-49b-1645 | | | Volume
| 49 | |
5 | Author
| Thom As Schleid, Falk Lissner | Requires cookie* | | Title
| Oxidsulfidchloride der Lanthanide vom Typ M 4OS4Cl2 (M = L a-N d ) M 4OS4Cl2-Type Oxysulfide Chlorides of the Lanthanides (M = L a -N d )  | | | Abstract
| Oxysulfide chlorides, M4OS4Cl2, o f the lanthanides (M = L a -N d) are obtained upon the oxi dation o f the metals with sulfur in the presence o f MOC1 (or M 20 3) and MC13 in appropriate molar ratios. Additional NaCl or an excess o f MC13 serving as a flux provide even single crys talline material after reactions at 850 °C for seven days in sealed tantalum capsules. The crys tal structure o f M4OS4Cl2 (hexagonal, P 6 3mc, no. 186, Z = 2; M = La: a = 933.19(3), c = 701.22(4) pm, c/a = 0.7514, R = RH = 0.020; M = Ce: a = 925.49(3), c = 694.13(3) pm, c/a = 0.7500; M = Pr: a = 919.72(4), c = 688.53(4) pm, c/a = 0.7486; M = Nd: a = 914.25(4), c = 683.12(4) pm, c/a = 0.7472, R = 0.022, Rw = 0.019) contains isolated 0 2--centered (M 3+)4 te-trahedra which are surrounded by twelve S2-and six Cl-, capping vertices, edges, and faces o f each tetrahedron and linking to other [OM4] units. Basically, the structure is identical to that o f Ba4OCl6 if Ba2+ is substituted by M 3+ and 2/3 o f the CL anions are replaced by S2-to secure charge neutrality in M4OS4Cl2. Different models for the C L /S 2-replacement are presented on the basis o f comparisons o f the Madelung part o f the lattice energy (M A PLE) with the M APLE sum o f the binaries (M 20 3, M 2S3, and MC13). | | |
Reference
| Z. Naturforsch. 49b, 340 (1994); eingegangen am 27. September 1993 | | |
Published
| 1994 | | |
Keywords
| Lanthanides, Oxysulfide Chlorides, Synthesis, Crystal Structure | | |
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| default:Reihe_B/49/ZNB-1994-49b-0340.pdf | | | Identifier
| ZNB-1994-49b-0340 | | | Volume
| 49 | |
6 | Author
| Enno Lork, Ulrich Behrens, Detlef Viets, Rüdiger Mews | Requires cookie* | | Title
| Die Kristallstruktur von A sF5 0 S C F 2S (0 2)CF2 The Crystal Structure of A sF 5 * 0& C F2S (0 2)C F 2  | | | Abstract
| The crystal structure of AsF5 • 0$C F2S(02)CF2 is reported. It crystallizes in the orthorhombic space group Pnma with a = 749.1(3) pm, b = 770.6(3) pm and c = 1630.0(5) pm, V = 960.9(6)-106 pm3, Z = 4. Einleitung Intensiv ist in den letzten Jähen die Chemie der Dithietane F 2tS (O x)FyC F 2S(Ov)Fw im Arbeitskreis Sundermeyer [1] und von uns [2] untersucht wor den. Ein Ziel unserer Arbeiten war es, das D onor verhalten dieser Systeme gegenüber Fluor-Lewis-Säuren (AsF5, SbF5, BF3) zu untersuchen und die Grenzen zwischen Carbenium-, Sulfoniumsalz-und Addukt-Bildung zu erkennen. Durch Strukturun tersuchungen konnte belegt werden, daß AsF5 aus F2CSCF2S F " abstrahiert unter Bildung des cycli schen Carbeniumions FCSC F2S+ [lb]; nach IR-und 1' 9F-N M R -U ntersuchungen führt die analoge Umsetzung von F 7SCF?S(0")C F7 (n = 0 -2) zu Sul-foniumsalzen FSC F2S(0")CF2+ [lc], während in Sulfoxid-Derivaten die Lewis-Säure an den Sauer stoff unter Bildung von F 2CS(0")CF2S 0 • M F 5 (n = 0 -2) addiert wird. In der vorliegenden Arbeit be richten wir über die Struktur des Adduktes F2C S 0 2C F2S 0 • A sF5 (2 a). | | |
Reference
| Z. Naturforsch. 49b, 422—424 (1994); eingegangen am 21. Oktober 1993 | | |
Published
| 1994 | | |
Keywords
| Dithietanes, Sulfoxides, Adducts with Lewis-Acids, Crystal Structure | | |
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| default:Reihe_B/49/ZNB-1994-49b-0422_n.pdf | | | Identifier
| ZNB-1994-49b-0422_n | | | Volume
| 49 | |
7 | Author
| Andreas Ahle, K. Urt Dehnicke, CäciliaM. Aichle-Mössmer, Joachim Strähle | Requires cookie* | | Title
| Synthesis and Crystal Structure of [Na( 12-Crown-4)2]2[Fe4Se4Cl4]  | | | Abstract
| [N a(12-crow n-4)2]2[Fe4Se4Cl4] has been pre pared by the reaction o f FeCl2 with N a2Se4 in di-methylform amide solution in the presence o f 12-crown-4 as dark red crystals, which were char acterized by a_ crystal structure determination. Space group P 1, Z = 2, 6295 observed unique re flections, R = 0.085. Lattice dim ensions at 20 °C: a = 1397.3(3), b = 1501.8(4), c = 1570.1(4) pm, a = 85.86(2)°, ß = 64.06(2)°, y = 65.01(2)°. The structure consists o f [Na(12-crown-4)2]+ cations and cuban-like anions [Fe4Se4Cl4]2" with Fe — Fe contacts o f 282.8(3) pm. | | |
Reference
| Z. Naturforsch. 49b, 434 (1994); eingegangen am 30. September 1993 | | |
Published
| 1994 | | |
Keywords
| Tetranuclear Iron Selenium Cluster Dianion, Synthesis, Crystal Structure | | |
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| default:Reihe_B/49/ZNB-1994-49b-0434_n.pdf | | | Identifier
| ZNB-1994-49b-0434_n | | | Volume
| 49 | |
9 | Author
| S. Möhr, Hk Müller-Buschbaum | Requires cookie* | | Title
| Ein gemischtvalentes Oxometallat mit Cr3+ anstelle von Ti3+: Ba2Ti4+Cr20 13  | | | Abstract
| Single crystals of Ba2Ti4+C r20 13 w ere p rep a red by C 0 2-L A S E R h igh te m p era tu re r ea ctio n s and in v estig a te d by X -ra y w o rk . T h e c o m p o u n d c ry sta llize s w ith m o n o c li nic sym m etry, a = 15.0 1 8 5 , b = 3 .9 4 1 9 , c -9 .0 7 6 4 Ä , ß = 9 8 .1 3 7 °, Z = 2. B a 2T i4Cr20 13 is iso ty p ic to N a 2T i60 13. T h e crystal stru ctu re is d isc u sse d w ith r e sp e ct to o rd ered or d iso rd ered d istrib u tio n s o f T i4+ and C r3+ u sin g c a lc u la tio n s o f C o u lo m b term s o f la ttice energy. It is sh o w n , th at th e sta b ility o f th is stru ctu re ty p e w ill b e d e c r e ased by rep la ce m en t o f N a + by io n s w ith h ig h er o x id a tio n sta tes. | | |
Reference
| Z. Naturforsch. 49b, 911 (1994); eingegangen am 17. Februar 1994 | | |
Published
| 1994 | | |
Keywords
| Barium, Titanium, Chromium, Oxide, Crystal Structure | | |
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| default:Reihe_B/49/ZNB-1994-49b-0911.pdf | | | Identifier
| ZNB-1994-49b-0911 | | | Volume
| 49 | |
11 | Author
| Hk Müller-Buschbaum, S. Frenzen | Requires cookie* | | Title
| Zur  | | | Abstract
| Kenntnis von EuBeGd20 5 mit einem Beitrag über Phasen der Zusammensetzung M1 _xM'A .BeLn20 5 : Ca0,4Sr0,6BeSm2O5, Ba0,25Ca0,75BeNd2O5 und Ba0,36Sr0,64BeNd2O5 On E uB eG d20 5 and on Phases of the Composition M 1_^M'xBeLn20 5: Ca0,4Sr06BeSm2O 5, Bao,2sCao,75 BeNd2 0 5 and Ba0 3 6 Sr0,64BeNd2O5 Single crystals of (I): E uB eG d20 5, (II): Ca0,4Sr0ABeSm 20 5, (III): Ba0,25 Ca()75B eN d2O 5 and (IV): Ba<)3 6Sr()64B eN d2O s were prepared by (I): plasma torch and (II)-(IV): C 0 2-LASER technique. X-Rayo investigations lead to (I) monoclinic (space group C 2h-P2j/c, a = 7.126, b = 6.457, c = 9.394 A, ß = 90.40°) and (I I)-(I V) orthorhombic symmetry (D ^ -P n m a). (II: a = 9.454, b = 7.142, c = 6.490 A; III: a = 9.508, b = 7.188, c = 6.531 A; IV: a = 9.642, b = 7.295, c = 6.614 A). In contrary to the phases M j^ M '^ B eL ^ O s, E uBeG d2Os is characterized by an ordered distribution of Eu2+ and G d3+ inside o f the Kagome network. | | |
Reference
| Z. Naturforsch. 49b, 919 (1994); eingegangen am 28. Februar 1994 | | |
Published
| 1994 | | |
Keywords
| Alkaline Earth, Beryllium, Rare Earth, Oxide, Crystal Structure | | |
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| default:Reihe_B/49/ZNB-1994-49b-0919.pdf | | | Identifier
| ZNB-1994-49b-0919 | | | Volume
| 49 | |
12 | 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 | |
13 | Author
| Z. Naturforsch | Requires cookie* | | Title
| NaK9Tl13: Eine neue Verbindung an der Zintl-Grenze mit isolierten, von Thallium besetzten Tl17-Ikosaedern  | | | Abstract
| NaK9T l13 (a = 1152.0(1) pm, Im 3, Z = 1, RI -0.029, wR2 = 0.0724) has been prepared from the elements and characterized by single crystal X-ray diffraction. The title compound contains isolated T l12 icosahedra, which are centered by T1 atoms. The icosahedra are in an a-W-type arrangement. | | |
Reference
| Z. Naturforsch. 49b, 935 (1994); eingegangen am 14. Februar 1994 | | |
Published
| 1994 | | |
Keywords
| Crystal Structure, Intermetallic Compound, Sodium, Potassium, Thallium | | |
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| default:Reihe_B/49/ZNB-1994-49b-0935.pdf | | | Identifier
| ZNB-1994-49b-0935 | | | Volume
| 49 | |
14 | Author
| W. S. Sheldrick, B. Schaaf | Requires cookie* | | Title
| Schichtstruktur £, [Te6~] RbTe6, a Polytelluride with Layer Structure ^,[Te6_]  | | | Abstract
| Reaction of Rb2C 0 3 with Te in M ethanol at 160 °C in the presence of G e yields the polytellu ride RbTe6, the structure o f which has been deter mined by X-ray structural analysis. The poly anions (£,[Te6~] contain Te6 rings with a chair conformation, which are connected via four T e-T e bonds into a layer structure. A T structure is exhibited by the resulting TeTe3 units. The Rb cations adopt positions betw een neighbouring parallel anion layers and are surrounded by 12 Te atoms in their first coordination sphere. | | |
Reference
| Z. Naturforsch. 49b, 993—9 (1994) | | |
Published
| 1994 | | |
Keywords
| Rubidium Polytelluride, Methanolothermal Synthesis, Crystal Structure | | |
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| default:Reihe_B/49/ZNB-1994-49b-0993_n.pdf | | | Identifier
| ZNB-1994-49b-0993_n | | | Volume
| 49 | |
15 | Author
| F.-D Martin, Hk Müller-Buschbaum | Requires cookie* | | Title
| Synthese und Kristallstruktur von NaM g1?64Cu0 ,36^3^10 Synthesis and Crystal Structure of NaM glt64Cuoi36V 3 0 1o  | | | Abstract
| Single crystals of NaMg] 64Cu().36V 3O 10 have been prepared by heating mixtures of Na2C 0 3, M gC 03, CuO and V 20 5 above the melting point. The yellow crystals show triclinic symmetry, space group Cj-PT, a = 6.726(8), b = 6.743(7), c = 9.625(2) Ä , a = 100.705(9), ß -104.57(1), y = 101.700(9)°, Z = 2. N aM g164Cu0.36V 3O 10 represents a new structure type showing V 3O 10 groups, a statistical distribution of Mg2+ and Cu2+ on two point positions, and N a+ in an irregular coordination. | | |
Reference
| Z. Naturforsch. 49b, 1329—1333 (1994); eingegangen am 6. Mai 1994 | | |
Published
| 1994 | | |
Keywords
| Sodium Magnesium, Copper, Vanadium Oxide, Crystal Structure | | |
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| default:Reihe_B/49/ZNB-1994-49b-1329.pdf | | | Identifier
| ZNB-1994-49b-1329 | | | Volume
| 49 | |
17 | Author
| D. Frerichs, Hk Müller-Buschbaum | Requires cookie* | | Title
| Ein Beitrag zur Kristallchemie von Verbindungen mit Johillerit-Struktur: On the Crystal Chemistry of Compounds with Johillerite Structure: KCo3 Cu(As2 5 8 V0 4 2 )O i2  | | | Abstract
| Single crystals of KCo3Cu(As2.58Vo42) 0 12 were prepared by solid state reactions below the melting point of the reaction mixture (K 2C 0 3, CuO, CoC20 4, V 20 5 and 3 A s20 5 -5 H 20) . It crystallizes with m onoclinic symmetry, space group C |h-C 2 lc, a = 12.207, b = 12.730, c = 6.811 A , ß = 113.69°, Z -4. The structure type is characterized by isolated twisted-square C u 0 4-polygons, C o 0 6-octahedra and a special 4+4-coordination o f the potassium ion. A s5+ and V*+ are in tetrahedral coordination with a partly statistical distribution of these ions. | | |
Reference
| Z. Naturforsch. 49b, 1463—1466 (1994); eingegangen am 13. Juni 1994 | | |
Published
| 1994 | | |
Keywords
| Potassium, Cobalt, Arsenic, Vanadium Oxide, Crystal Structure | | |
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| default:Reihe_B/49/ZNB-1994-49b-1463.pdf | | | Identifier
| ZNB-1994-49b-1463 | | | Volume
| 49 | |
18 | Author
| Christian Robl, VolkerG. Öbner | Requires cookie* | | Title
| Kristallstruktur und hydrothermale Darstellung der Schichtverbindung B e2( P 0 4)(0 H )* 2 H 20 Crystal Structure and Hydrotherm al Synthesis of the Layered Com pound Be2 ( P 0 4 ) (0 H ) * 2 H 20  | | | Abstract
| Colourless monoclinic single crystals of B e2(P 0 4) (0 H) -2 H 20 (space group P 2 Jn) have been prepared under hydrothermal conditions in aqueous solution. Crystal data: a = 631.7(1), b = 1108.7(2), c = 812.7(2) pm, ß = 105.83(2)°, 910 unique reflections, 108 parameters, Rg = 0.0233. P is tetrahedrally coordinated by 4 oxygen atoms. Each of the two crystallographically unique Be atoms has two phosphate oxygen atoms, one water molecule, and one OH group as coordination partners. The tetrahedra share common vertices and build up a two-dim ensionally infinite pattern. The OH group links the two unique Be centered tetrahedra. Loss of water com m ences at 300 °C and is finished at 580 °C. | | |
Reference
| Z. Naturforsch. 49b, 1499—1502 (1994); eingegangen am 23. Juni 1994 | | |
Published
| 1994 | | |
Keywords
| Beryllophosphate, Crystal Structure, Differential Thermal Analysis, Layered Compound | | |
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| default:Reihe_B/49/ZNB-1994-49b-1499.pdf | | | Identifier
| ZNB-1994-49b-1499 | | | Volume
| 49 | |
19 | Author
| S. Mann, M. Jansen | Requires cookie* | | Title
| Ein neuer Zugang zu ionischen Thionylimiden. Einkristallstruktur von N(CH3)4NSO A New Access to Ionic Thionylimides. Single Crystal Structure of N(CH3)4NSO  | | | Abstract
| Single crystals of N (C H 3)4NSO have been prepared via ion exchange from RbNSO or CsNSO and tetraalkylammonium halides in liquid ammonia and investigated by X-ray single crystal techniques (14, a = 1137.6(1), c = 1134.9(2) pm, Z = 8, T = -1 0 0 °C). The crystal structure of N (C H 3)4NSO is related to the CsCl-type of structure. Using the same preparative route N M e3B zN SO has been obtained. Its lattice powder data (orthorhombic primitive; a = 896.3(2) | | |
Reference
| Z. Naturforsch. 49b, 1503—1506 (1994); eingegangen am 13. Juni 1994 | | |
Published
| 1994 | | |
Keywords
| Thionylimide, Ion Exchange, Tetramethylammonium, Crystal Structure, Benzyltrimethylammonium | | |
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| default:Reihe_B/49/ZNB-1994-49b-1503.pdf | | | Identifier
| ZNB-1994-49b-1503 | | | Volume
| 49 | |
20 | Author
| Oliver Heilmann, Hans-Dieter Hausen, Wolfgang Kaim | Requires cookie* | | Title
|  | | | Abstract
| The crystal structure determination of the new rhodium(III)-complex [(DM L)(C5Me5)ClRh](PF6). DML = 1,3-dimethyllumazine, reveals 0 4,N5 coordination of the metal to DML with not very different bond lengths of 213.0(2) pm (R h -N) and 219.2(2) pm (R h -O). This result stands in contrast to the previously reported structure of a cationic dihydrobiopterin bound to [Mo(0)C13] which exhibited a very unsymmetrical chelate ar rangement. Chemical and electrochemical two-electron reduction of the Rh(III) complex led to a very labile Rh(I) species (DM L)(C5Me5)Rh which is distinguished by an intense charge transfer band in the visible. The results confirm the characterization of DML as a weak o donor In acceptor ligand with a rather low-lying tc* orbital. | | |
Reference
| Z. Naturforsch. 49b, 1554—1560 (1994); received July 8 1994 | | |
Published
| 1994 | | |
Keywords
| Crystal Structure, Pteridine Heterocycles, Rhodium, Electrochemistry, Coordination | | |
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| default:Reihe_B/49/ZNB-1994-49b-1554.pdf | | | Identifier
| ZNB-1994-49b-1554 | | | Volume
| 49 | |
|