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1Author    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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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-1499.pdf 
 Identifier    ZNB-1994-49b-1499 
 Volume    49 
2Author    IrisM. Müller, WilliamS. SheldrickRequires cookie*
 Title    CuX (X = Br, I) Oligomers and Polymerie Chains in Tetramethylcyclotetra- arsoxane-Bridged Networks [Cu/iX/Jcjc/o-CCH^AsO)^] (n = 4, 6, 8)  
 Abstract    Open lamellar structures 2 [Cu-jLjcyc/o-tCH iA sO ^}?] (1) and 2 [{CuX(CuX • C H 3CN)2}{c>'c/o-(CH3 AsO)4}] [X = Br (2), X = 1 (3)] may be prepared by self-assembly from CuX and methylcycloarsoxane (CH3AsO)" in acetonitrile solution at 100-130 °C. W hereas 1 contains CU4I4 oligomers consisting of three fused (C ul)2 rings, 2 and 3 exhibit infinite J. [CuX] single chains. An acceleration in the rate of heating between 20 
  Reference    Z. Naturforsch. 52b, 951—957 (1997); received June 6 1997 
  Published    1997 
  Keywords    Copper(I) Halides, Macrocyclic Ligands, Methylcycloarsoxane, Layered Compounds 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0951.pdf 
 Identifier    ZNB-1997-52b-0951 
 Volume    52 
3Author    Takahiro Ueda, Katsuyuki Shimizu, Hiroshi Ohki, Tsutomu OkudaRequires cookie*
 Title    C CP/MAS NMR Study of Motion and Local Structure of Phenethyl- ammonium Ion in [C 6 H 5 CH 2 CH 2 NH 3 ] 2 PbX 4 (X = Cl, Br, I)  
 Abstract    Ionic motion and local structure of phenethylammonium ion (C 6 H 5 CH-,CH 2 NH 3 +) in a series of phenethylammonium lead(II) halides, [C 6 H 5 CH 2 CH 2 NH 3 ] 2 PbX 4 (X = Cl, Br, I) were studied by means of 13 C cross polarization/magic angle sample spinning (CP/MAS) NMR technique. Among the three salts, remarkable differences in the spectra were observed in the signals corresponding to the phenyl carbons. The peaks from C2, C3, C5, and C6 in the phenyl group were split into three for the chloride and into two for the bromide, although in the iodide those were observed as a single peak. Coalescence of those peaks, as well as line broadening were observed on heating. This indicated that peak split brings about disorder of the orientation in the phenyl group around the C1-C4 axis, suggesting to have three and two orientations for the chloride and the bromide, respectively. Above room temperature the phenyl group undergoes chemical exchange among these orientations, and at higher temperature, reorientation with a large amplitude takes place around its axis. The apparent activation energies of the reorientation of the phenyl group for the chloride and bromide were estimated from the temperature dependence of the linewidth of the resonance peaks to be about 24 kJ mol -1 , 25 kJ mol -1 , respectively, which is similar to in the iodide (25.0 kJ mol -1). Ab initio molecular orbital energy calculation was carried out to evaluate the potential barrier of the internal rotation of the phenyl group in a free phenethylammonium ion. The intramolecular interaction was evaluated to be 13.9 kJ mol -1 from the calculation, and the intermolecular interaction results to be 10 kJmol -1 . 
  Reference    Z. Naturforsch. 53a, 983—988 (1998); received April 30 1998 
  Published    1998 
  Keywords    13 C CP/MAS NMR, Layered compound, Disorder, Reorientation, Activation energy 
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 TEI-XML for    default:Reihe_A/53/ZNA-1998-53a-0983.pdf 
 Identifier    ZNA-1998-53a-0983 
 Volume    53