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'Synthesis' in keywords Facet   Publication Year 2000  [X]
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1Author    A. N. Ägele3, E. A. Nokhinab, J. Sitarb, H.-JM. Eyer3, A. LachgarbRequires cookie*
 Title    Synthesis and Crystal Structures of ATi[Nb6Cli8] Compounds (A = K, Rb, Cs, In, Tl)  
 Abstract    New quaternary niobium cluster chlorides corresponding to the general formula ATi[Nb6Clis] (A = K, Rb, Cs, In, Tl) have been synthesized in sealed quartz tubes at 720 °C, starting from stoichiometric amounts of NbCls, niobium metal, TiCb, and AC1 (A = K, Rb, Cs), or In or Tl metals. The structures of RbTi[Nb6Clis] and CsTifNböClis] were determined using single­ crystal X-ray diffraction. RbTifNböClis] crystallizes in the rhombohedral crystal system, space group R3 (no. 148), Z = 3, with lattice parameters: a = 9.163(4), c = 25.014(14) A (hexagonal setting). The structure refinement converged to R] = 0.044 and wRi = 0.058 for all data. In this structure, discrete [NböClig]4-cluster units are linked by Rb+ and Ti3+ cations, located in a 12-coordinated anticubeoctahedral and octahedral chloride coordination environment, respectively. In contrast, CsTifNböClis] crystallizes in the trigonal crystal system, space group P31c (no. 163), Z = 2. The lattice parameters were determined to be a -9.1075(6), c = 17.0017(8) A. The structure refinement gives the reliability factors Ri = 0.029 and wRa = 0.063 for all data. The structure is built up of discrete octahedral [N bödis]4-cluster units, linked by Cs+ and Ti3+ cations which are located in a distorted hexagonal antiprismatic and octahedral chloride coordination environment, respectively. The structures of the compounds ATifNböClis] (A = K, In, Tl) were found to be isotypic with RbTi[NböCli8], and their unit cell parameters were refined using X-ray powder diffraction analysis. In tro d u ctio n 
  Reference    Z. Naturforsch. 55b, 139—144 (2000); received September 13 1999 
  Published    2000 
  Keywords    Niobium, Titanium, Cluster, Chlorides, Synthesis 
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 TEI-XML for    default:Reihe_B/55/ZNB-2000-55b-0139.pdf 
 Identifier    ZNB-2000-55b-0139 
 Volume    55 
2Author    C. Bender, D. W. Ulff-M, H. Older, F. Vogt, M. M. Ritschl, EiselRequires cookie*
 Title    Synthese und Kristallstruktur des Bromdifluormethyl-triphenyl- phosphoniumbromids, [(C6H5)3 PCF2Br]+ Br" Synthesis and Crystal Structure o f B rom odifluorom ethyl-triphenylphosphonium Brom ide, [(C6H5)3PC F2Br]+ Br~  
 Abstract    Difluorobromomethyl-triphenylphosphonium bromide [(C6H5)3PCF2Br]+ Br-(1) has been prepared by the reaction of triphenylphosphine with dibromodifluoro-methane in acetonitrile or methylene chloride. The colorless crystals are monoclinic, space group P 2,/n, Z=4, a = 1067.1(2), b = 1488,5(2), c = 1178,2(2) pm, ß = 95,67(3)°. The lattice contains Br~ anions and [(C6H5)3PCF2Br]+ cations with a Br-Br distance of 322,33(11) pm.. For the title compound the results of AM 1, PM 3 ,and MNDO calculations are in good agreement with corresponding values determined by the X-ray analysis only in the case of PM 3. The yellow-red [(C6H5)3PCF2Br]+ Br3~ (2) has been obtained by treating 1 with equimolar quantities of elemental bromine in methylene chloride solution. E inleitung 
  Reference    Z. Naturforsch. 55b, 167—170 (2000); eingegangen am 28. Oktober 1999 
  Published    2000 
  Keywords    Bromodifluoromethyl-triphenylphosphonium Bromide, Synthesis, Crystal Structure 
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 TEI-XML for    default:Reihe_B/55/ZNB-2000-55b-0167.pdf 
 Identifier    ZNB-2000-55b-0167 
 Volume    55