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1994[X]
21Author    S. Möhr, Hk Müller-BuschbaumRequires cookie*
 Title    Uber ein gemischtvalentes Oxoniobat mit planaren Polygonen um Niob und Barium: BaNb2+Nb2+0 6 On a Mixed Valent Oxoniobate Containing Planar Polygons A round Niobium and Barium: BaNb2 +N b^+0 6  
 Abstract    Single crystals of B aN b30 6 were prepared by C 0 2-LA SER high temperature technique. The compound crystallizes with trigonal symmetry C fv-R 3 m , a = 11.4333, c -3.4949Ä , Z = 3. The new structure type is characterized by planar N b 0 4 and planar B a 0 6 polygons. The results are discussed with respect to related compounds like Ca0.75 Nb3O6 or N aNb30 6. 
  Reference    Z. Naturforsch. 49b, 915 (1994); eingegangen am 17. Februar 1994 
  Published    1994 
  Keywords    Barium, Niobium, Oxide, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-0915.pdf 
 Identifier    ZNB-1994-49b-0915 
 Volume    49 
22Author    Hk Müller-Buschbaum, S. FrenzenRequires 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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 Identifier    ZNB-1994-49b-0919 
 Volume    49 
23Author    D. Osterloh, Hk Müller-BuschbaumRequires 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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 Identifier    ZNB-1994-49b-0923 
 Volume    49 
24Author    Z. NaturforschRequires 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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 Identifier    ZNB-1994-49b-0935 
 Volume    49 
25Author    W. S. Sheldrick, B. SchaafRequires 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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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-0993_n.pdf 
 Identifier    ZNB-1994-49b-0993_n 
 Volume    49 
26Author    FrankW. Heinem, Helmut Hartung, NadjaM. Aier3, HermannM. Atschiner3Requires cookie*
 Title    Molekül-und Kristallstruktur der Verbindung 8-(n-Butylamino- phenyl-methyliden)  
 Abstract    -l,2,3?4,5,6,7-heptathiocan Molecular and Crystal Structure of 8-(«-Butylamino-phenyl-methylidene)-l,2,3,4,5,6,7-heptathiocane By the reaction of acetophenone with sulfur and primary amines yellow-coloured crystals of the title compound are formed. It crystallizes in the monoclinic space group P 2 x!n with lattice constants a = 1309.9(2) pm, b = 926.5(2) pm, c -1582.2(2) pm and ß -114.00(1)°. The structure of the eight-membered heptathiocane ring is characterized by a crown confor­ mation. The range of the S -S distances [204.4(1)-207.3(1) pm], the S -S -S bond angles [107.2(1) — 109.0(1)°] and the S-S-S-S torsion angles [93.2(1)-97.7(1)°] is comparable to those observed in a-, ß-and y-sulfur. 
  Reference    Z. Naturforsch. 49b, 1063—1066 (1994); eingegangen am 3. Februar 1994 
  Published    1994 
  Keywords    Heptathiocane, Acetophenone, Sulfur, Crystal Structure, Crown Conformation 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-1063.pdf 
 Identifier    ZNB-1994-49b-1063 
 Volume    49 
27Author    Rainer Pöttgen, G. Ünter Block, Wolfgang Jeitschko, RonaldK. BehrensRequires cookie*
 Title    Preparation and Crystal Structure of the Carbides Ln12Re5C15 (Ln = Y, L a-N d, G d-E r)  
 Abstract    The title compounds were prepared by arc-melting of the elem ental components and sub­ sequent annealing. Their crystal structure is hexagonal P 6 2 m with one formula unit per cell. It was determined from single-crystal X-ray data o f La12R e5C i5 (a = 1116.8(1) pm. c = 545.3(1) pm. R = 0.060 for 287 structure factors and 27 variable parameters) and H o 12R e5C i5 (a = 1066.7(1) pm, c -504.2(1) pm, R = 0.018 for 392 F's and 31 variables). The structures correspond to the formula Ln12[ReC 3]2[R e3C3(C2)3], where the brackets indicate two differ­ ent trigonal planar anionic rhenium-carbon groups. The coordination of the rhenium atoms in these polyanions seem s to be compatible with the 18-electron rule. 
  Reference    Z. Naturforsch. 49b, 1081—1088 (1994); received February 22 1994 
  Published    1994 
  Keywords    Crystal Structure, Lanthanoid-Rhenium-Carbides, 18-Electron Rule 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-1081.pdf 
 Identifier    ZNB-1994-49b-1081 
 Volume    49 
28Author    F.-D Martin, Hk Müller-BuschbaumRequires 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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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-1329.pdf 
 Identifier    ZNB-1994-49b-1329 
 Volume    49 
29Author    YueQing Zheng, Arnold AdamRequires cookie*
 Title    Ein neues Carbonat mit Baylissit-Struktur: Rb2[M g(C 03)2(H 20 )4] A New Carbonate with Baylissite Structure: Rb2 [Mg(C0 3 )2(H 2 0 )4]  
 Abstract    The new complex carbonate Rb2[M g (C 0 3)2(HoC))4] crystallizes in the Baylissite-tvpe structure with a = 1130,4(3), b = 641,9(1), c = 703,3(2) pm, ß = 99,62(1)°, V EZ = 503,2(2), space group P2l/n (No. 14) and Z = 2. In comparison with the isostructural potassium compound the cell dimensions increase in b-and c-and decrease in ö-direction. This effect depends on the greater coordination number of Rb+ and the rigidity of strong hydrogen bonds. The carbonate anion exhibits significant deviations from D 3h-symmetry (C -O : 127,1(5)-130,2(5) pm, Z_ O -C -O : 117.9(4)-121,1(3)°). 
  Reference    Z. Naturforsch. 49b, 1368—1372 (1994); eingegangen am 25. April 1994 
  Published    1994 
  Keywords    M etal-Carbonato-Complex, Baylissite Type, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-1368.pdf 
 Identifier    ZNB-1994-49b-1368 
 Volume    49 
30Author    Stefan Peschel, Dietrich BabelRequires cookie*
 Title    Zur Kristallstruktur der Cyanoelpasolithe [N(CH3)4]2CsCo(CN)6 und [H3NCH3]2NaFe(CN)6 Concerning the Crystal Structures of the Cyano-Elpasolites [N(CH3 )4]2CsCo(CN) 6 and [H3NCH3]2NaFe(CN) 6  
 Abstract    Single crystals of the cyano com plexes [N (C H 3)4]2C sC o(C N)6 and [H3NCH 3]2N aFe(C N)6 were prepared and their structures determined by X-ray methods. The cobalt compound is monoclinic, a -885.5(1), b = 892.6(2), c = 1259.9(5) pm, ß = 90.29(4)°, space group 12Im, Z = 2; R l = 0.048 for 861 independent reflections. The resulting average distances in the nearly undistorted octahedra are C o -C = 189.8, C -N = 114.1, C s -N = 325.6 pm. The iron compound exhibits a cubic elpasolite type structure, a = 1105.2(1) pm, space group Fm 3m , Z = 4; R l = 0.040 for 127 independent reflections; F e -C = 193.4(6), N a -N = 247.7(8) pm. The orientation of the librating tetramethyl-ammonium group within the cages of the cobalt compound and the disorder of the monomethyl-ammonium cation around the special site (1/4, 1/4, 1/4) of the iron complex are discussed. 
  Reference    Z. Naturforsch. 49b, 1373—1380 (1994); eingegangen am 31. März 1994 
  Published    1994 
  Keywords    Hexacyanometallates(III), Crystal Structure, Elpasolite 
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 Identifier    ZNB-1994-49b-1373 
 Volume    49 
31Author    F.-D Martin, Hk Müller-BuschbaumRequires cookie*
 Title    Zur Kenntnis von K4CuV50 15C1 On K4 CuV5 0 1 5 C1  
 Abstract    Single crystals of K4CuV50 15C1 were prepared by crystallization from the melt. The yellow brown crystals show tetragonal symmetry, space group C 4-P 4, a = 8.8690, c = 5.4196 A , Z = 1. K4CuV50 15C1 is strongly related to KBaCuV20 7Cl and K2V 30 8. V (l) shows V 20 7 double tetrahedra connected by square V 0 5 and C u 0 4Cl pyramids. The crystal structure is discussed with respect to the related compounds. 
  Reference    Z. Naturforsch. 49b, 1459—1462 (1994); eingegangen am 9. Juni 1994 
  Published    1994 
  Keywords    Potassium, Copper, Vanadium Oxide-Chloride, Crystal Structure 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-1459.pdf 
 Identifier    ZNB-1994-49b-1459 
 Volume    49 
32Author    D. Frerichs, Hk Müller-BuschbaumRequires 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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 Identifier    ZNB-1994-49b-1463 
 Volume    49 
33Author    Christian Robl, VolkerG. ÖbnerRequires 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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 Identifier    ZNB-1994-49b-1499 
 Volume    49 
34Author    S. Mann, M. JansenRequires 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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 Identifier    ZNB-1994-49b-1503 
 Volume    49 
35Author    Oliver Heilmann, Hans-Dieter Hausen, Wolfgang KaimRequires 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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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-1554.pdf 
 Identifier    ZNB-1994-49b-1554 
 Volume    49 
36Author    M. Arkus Wieber, Stefan Lang, StefanRalph Rohse, Christian Habersack, BurschkaRequires cookie*
 Title    Synthese und Kristallstruktur von Triphenyltelluroniumsulfid Synthesis and Crystal Structure of Triphenyltelluroniumsulfide  
 Abstract    The synthesis of triphenyltelluroniumsulfide (Ph3TeS)4 is described together with a NMR-spectroscopic characterization. The structure of the title compound was determined by single crystal X-ray diffraction. Crystals of triphenyltelluroniumsulfide are triclinic (space group P I) with the cell parameters a = 1178.0(3) pm. b = 1295.8(6) pm. c = 1298.7(4) pm, a = 77.67(3)°, ß = 82.18(2)°, y = 66.00(2)° (V = 1766(1) x 106 pm3) and Z = 2. The compound appears to form a step-like structure of two [Ph3TeS]2 units and crystallizes with two m ole­ cules of CH2C12 per unit cell. 
  Reference    Z. Naturforsch. 49b, 1654—1658 (1994); eingegangen am 5. Mai 1994 
  Published    1994 
  Keywords    Triphenyltelluroniumsulfide, Synthesis, NMR Data, Crystal Structure, Secondary Bonding 
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 Identifier    ZNB-1994-49b-1654 
 Volume    49 
37Author    SundaraR. Am Aprabhu, EdwinA C Lucken, Gerald BernardinelliRequires cookie*
 Title    Crystal Structure and NQR of Two Copper (I) Complexes of 4,6-Dimethylpyrimidine-2-thione  
 Abstract    The crystal structure and 63Cu NQR spectra of two neutral hexanuclear Cu(I) complexes of 4,6-dimethylpyrimidine-2-thione, (Hdmpt); [dmptCu]6 6 CHCl3 (l) and [dmptCu]6 C2 H4 Cl2 (2), are reported. The number and relative intensities of the NQR resonances are in agreement with the results of the crystallographic study. The temperature-dependence of the resonances reveals that both compounds undergo a phase-change in the temperature range 77 K -3 0 0 K, both of which may be associated with the loss of a symmetry-element present in the high-temperature phase. The 3 5 C1 resonances of CHC13 in 1 could be observed in the low-temperature phase but the corresponding resonances for C2 H4 C12 in 2 were not detected. 
  Reference    Z. Naturforsch. 49a, 193—198 (1994); received August 30 1993 
  Published    1994 
  Keywords    6 3 Cu, 3 5 C1, Cu(I), Crystal structure 
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 Identifier    ZNA-1994-49a-0193 
 Volume    49 
38Author    Masao Hashimoto, Shuji Matsumoto, Masakazu Kunitomo, Haruo Niki, Hirotaka Odahara, Katsuji TamakiRequires cookie*
 Title    35C1 NQR Relaxation and Hydrogen Bond in Some Chloral Hemiacetals  
 Abstract    The crystal structure of chloral ethylhemiacetal has been determined at 291 K: monoclinic, space group C f -P 2 lt Z = 2, a = 854.5(1), b = 594.0(3), c = 853.3(1) pm, ß = 108.30(2)°, R = 0.0962. A sharp decrease of the spin lattice relaxation time 7i found for the 35C1 N Q R o f the CC13 groups in chloral methyl-, ethyl-and n-heptylhemiacetals is attributed to the onset of reorientation of the group over a potential barrier o f ca. 39, 37, and 32 kJ/m ol, respectively. An unusual vs. 1/T curve with a 7i minimum superimposed on the sharp decrease of 7\ due to the reorientation was observed for each of the three Cl N Q R lines of nH p-C H . This phenom enon is tentatively ascribed to a fluctuation of EFG caused by jum ping m otion o f the hydrogen atom s in the OH groups. 
  Reference    Z. Naturforsch. 49a, 279 (1994); received August 16 1993 
  Published    1994 
  Keywords    Crystal structure, Hydrogen bond, Chlorine N Q R, Spin lattice relaxation 
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 Identifier    ZNA-1994-49a-0279 
 Volume    49 
39Author    Hiroyuki Ishida, Yoshihiro Kubozono, Setsuo Kashino, Ryuichi IkedaRequires cookie*
 Title    Crystal Structure of Trimethylammonium Perchlorate in Three Solid Phases Including the Ionic Plastic Phase Obtainable above 480 K  
 Abstract    The crystal structures of (CH3)3NHC104 in three solid phases were studied by X-ray diffraction techniques. X-ray powder patterns taken at ca. 500 and 445 K revealed that the plastic phase (Phase I) attainable above 480 K crystallizes in a CsCl-type cubic structure with a = 5.845 (1) A, Z = 1, V = 199.7 (2) Ä3, and Dx = 1.327 gem -3, while Phase II, stable between 480 and 396 K, forms a tetragonal structure with a = 9.912 (4), c = 7.01 (2) Ä, Z = 4, V = 689 (3) A3, and Dx = 1.54 gem -3. The room temperature phase (Phase III) was studied by single crystal X-ray diffraction and found to form a monoclinic lattice with space group P2X , a = 5.749(1), b = 8.670(1), c = 7.5585 (9) A, ß = 102.66 (1)°, Z = 2, V = 367.6 (2) A , and Dx= 1.441 g em -3. Thermal measurements, differential thermal analysis and differential scanning calorimetry, were carried out on these solid phases, and the obtained results were compared with those observed for (CH3)3NHBF4. 
  Reference    Z. Naturforsch. 49a, 723—726 (1994); received March 12 1994 
  Published    1994 
  Keywords    Crystal structure, X-ray diffraction, Thermal measurements, Ionic plastic phase 
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 TEI-XML for    default:Reihe_A/49/ZNA-1994-49a-0723.pdf 
 Identifier    ZNA-1994-49a-0723 
 Volume    49 
40Author    JonesRequires cookie*
 Title    Polysulfonylamine  
 Abstract    , LIV [1] (12-Krone-4)lithiumdimesylamid-Acetonitril (3/2): Ein Kristall mit zwei prinzipiell unterschiedlichen Konformationen des gleichen Coronanden Polysulfonylam ines, L IV [1] (12-Crow n-4)lithium D im esylam ide-A cetonitrile (3/2): A Crystal w ith Two F undam entally D ifferent C onform ations of the Sam e C oronand A rm an d Blaschette*, K arl-H einz N agel, P e te r G. [Li(12-crown-4){N(S02CH3)2}] is obtained from equimolar amounts of lithium dimesyl­ amide and 12-crown-4 in methanol and crystallizes from acetonitrile as a 3/2 solvate. The crystallographic data of the latter at -130 °C are: monoclinic, space group P 2In, a = 1053.4(3), b = 904.3(3), c = 2791.2(8) pm, ß = 95.66(3)°, V = 2.646 nm3, Z = 6, Dx = 1.441 Mgm~3. Apart from CH3CN molecules residing in lattice cavities, the structure consists of two crystallogra-phically independent [Li(12-crown-4){N(S02CH3)2}] ion pairs A and B in the ratio 2:1. In B, the Li and N atoms lie on a crystallographic twofold axis. In both ion pairs, Li is hexa-coordinated by the four crown oxygen atoms O(C) and by one oxygen O(S) from each sul-fonyl group of the anionic ligand. The coordination geometry of Li in A closely resembles that of Cu11 in the known structure of [Cu(12-crown-4)Cl2] and can be pictured as a distorted octahedron, where two cis sites are occupied by the O(S) atoms and the remaining vertices by the four oxygens of the macrocycle, which displays a [4 8] conformation. The lithium atom, the two O(S) and two O(C) atoms are arranged in an approximately square-planar pattern with L i-O (S) 203.6 and 205.1, L i-O (C) 206.9 and 219.1 pm, trans angles of 173.7 and 174.8°, and cis angles in the range 87.1 -93.6°. The angle between the remaining two Li -O(C) bonds with distances 214.7 and 221.5 pm is only 146.5° compared with 180° in an ideal octahedron. In ion pair B, the coronand assumes a [3 3 3 3] conformation close to C4 symmetry, as observ­ ed e. g. in the known structures of [Li(12-crown-4)NCS] with a square-pyramidal 0 4N-co-ordination and [Ca(12-crown-4)(H20) 4]Cl2-4 H zO with a square-antiprismatic 0 8-geometry. The coordination polyhedron in B can be viewed as an incomplete cube in which two verti­ ces related by a face diagonal are unoccupied. Important bond lengths and angles in B are: L i-O (S) 216.8, L i-O (C) 214.0 and 228.7pm; 0 (S) -L i-0 (S) 82.0, 0 (C) -L i-0 (C) 75.7/76.3 for adjacent and 120.4/121.9° for opposite ring oxygens. 
  Reference    (Z. Naturforsch. 49b, 36—42 [1994]; eingegangen am 2. September 1993) 
  Published    1994 
  Keywords    Polysulfonylamines, (12-Crown-4)lithium Dimesylamide, Synthesis, Crystal Structure, Coronand Conformation 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-0036.pdf 
 Identifier    ZNB-1994-49b-0036 
 Volume    49 
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