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1995[X]
41Author    R. Upert Marx3, HansMichael MayerbRequires cookie*
 Title    Reindarstellung und Kristallstruktur von Lithiumnitriddibromid, Li5NBr2 Preparation and Crystal Structure of Lithium Nitride Dibromide, Li5N B r2  
 Abstract    Single phase Li5NBr2 was prepared by the reaction of Li3N and dry, O H -free LiBr under inert gas at 430 °C. In the quasi-binary system Li3_2*Ni_ vB rir, Li5NBr2 is the second most nitride rich compound after Li10N 3Br. Following unit cell indexing using laboratory X-ray powder data the previously unknown structure o f Li5NBr2 was solved from neutron powder diffraction data recorded at the flat-cone and powder diffractometer E 2 at the rebuilt reactor BER II in Berlin. The title compound crystallizes in the orthorhombic space group Immm (No. 71), a = 603.79(4), b -1181.3(1), c = 390.14(3) pm with two formula units per unit cell. The L i-N -sublattice comprises linear chains of vertex sharing Li6N-octahedra which are aligned along the short c-axis and are separated by chains o f bromine atoms. The N -B r arrangement may be regarded as an ordered A X 2 variant o f a cubic close packing involving two kinds of atoms. Lithium atoms occupy the tetrahedral holes formed by one nitrogen and three bromine atoms, as well as the N -N edges of the N 2Br2 tetrahedra. 
  Reference    Z. Naturforsch. 50b, 1353—1358 (1995); eingegangen am 16. Februar 1995 
  Published    1995 
  Keywords    Lithium Nitride Dibromide, Preparation, Crystal Structure 
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 Identifier    ZNB-1995-50b-1353 
 Volume    50 
42Author    Z. NaturforschRequires cookie*
 Title    Aminolyse von Cp2ZrCl{P(SiMe3)2} -Synthese und Molekülstruktur von Cp2ZrCl(NHPh)  
 Abstract    The reaction of Cp2ZrCl{P(SiM e3)2} with aniline yields the terminal zirconocene phenyl­ amido com plex Cp2Z rCl(N H Ph) (1) and H P(SiM e3)2. 1 was characterized spectroscopically (n.m.r., i.r.) and by X-ray structure determination (monoclinic space group P 2 {ln, a -6.589(2), b = 19.978(3), c = 13.512(2) Ä , ß = 101.09(2)° (at 200 K)). The NHPh group is planar with Z r -N 2.116(10) A. 
  Reference    Z. Naturforsch. 50b, 1359—1361 (1995); eingegangen am 24. Februar 1995 
  Published    1995 
  Keywords    Aminolysis, Zirconocene Phosphido Complex Zirconocene Phenylamido Complex, Crystal Structure 
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 Identifier    ZNB-1995-50b-1359 
 Volume    50 
43Author    CsO. Rb, H.-Jürgen Laf Reckeweg, MeyerRequires cookie*
 Title    A4[Nb6Cl12(N3)6](H20 ) 2 mit A = Rb, Cs Synthesis and Structure of the Cluster Azides: A ^N böCl^N O öK IH bO ^ with A =  
 Abstract    The new compounds A4[Nb6Cli2(N3)6](H:0)2 (A = Rb, Cs) were synthesized from In4[Nb6Cli2Cl6] by substituting six terminal Cl ligands and the In+ ions in methano-lic solution. An X-ray structure refinement was performed on single-crystal data of Rb4[Nb6Cli2(N3)6](H?0)2 (1) (space group Pi, Z = 1, a = 912.5(1) pm, b = 937.2(1) pm, c = 1062.0(1) pm, a = 96.88(2)°, ß = 101.89(1)°, 7 = 101.44(2)°) and Cs4[Nb6Cli2(N3)6](H20)2 (2) (space group PI, Z = 1, a = 920.9(5) pm, b = 947.9(7) pm, c = 1091.8(7) pm, a = 96.89(6)°,/?= 103.35(5)°, 7 = 101.60(5)°. Each of the centrosymmetric [Nb6Cli2(N3)6]4~ ions of the isotypic compounds contains six terminal azide groups at the corners of the octahedral niobium cluster (dfvj^N = 226(1) pm (1), 225(1) pm (2), bond angles Nb-N-N 120-127°). The [Nb6Cli2(N3)6]4_ ions are linked via Rb-N and Rb-Cl interactions of the Rb+ ions to form a three-dimensional structure. Crystals of the compounds react explosively on heating or mechanical pressure. Die Synthese und Struktur von Clusteraziden: 
  Reference    Z. Naturforsch. 50b, 1377—1381 (1995); eingegangen am 16. Januar 1995 
  Published    1995 
  Keywords    Niobium Cluster Azides, Synthesis, Crystal Structure 
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 Identifier    ZNB-1995-50b-1377 
 Volume    50 
44Author    Claus Feldmann, Martin JansenRequires cookie*
 Title    Darstellung und Kristallstruktur von Cs3C10 Preparation and Crystal Structure of Cs3C10  
 Abstract    The preparation and crystal structure of Cs3C10 (a = 9,442(6), b = 4,452(2), c = 16,344(10) A) is reported. In contrast to other compounds M3X O (M = alkali metal; X = halide, auride) Cs3C10 does not crystalize as an anti perovskite or a related structure, but in the a/?r/-NH4CdCl3 type of structure. 
  Reference    Z. Naturforsch. 50b, 1415—1416 (1995); eingegangen am 30. März 1995 
  Published    1995 
  Keywords    Halide, Oxide, Preparation, Single-Crystal Structure Determination 
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 Identifier    ZNB-1995-50b-1415_n 
 Volume    50 
45Author    Karl-Friedrich Tebbe3, MervatEl Essawib, Sawsan Abd, El KhalikbRequires cookie*
 Title    Untersuchungen an Polyhalogeniden, XIX [1]  
 Abstract    Bis(methyltriphenylphosphonium)oktaiodid (M ePh3P)2I8, Cäsium(18-Krone-6)triiodid [Cs(C12H 24 0 6)]I3, Iodoblei(18-Krone-6)triiodid [Pb(C12H2406I]I3 und Diiodothallium(18-Krone-6)tetraiodothallat [T1(C12H240 6)I2](T1I4) Studies of Polyhalides, XIX [1] Bis(methyltriphenylphosphonium) Octaiodide (M ePh3P)2I8, Cesium(18-crown-6) Triiodide [Cs(C12H 240 6)]I3, Iodolead(18-crown-6) Triiodide [Pb(C 12H 240 6)I]I3 and Diiodothallium(18-crown-6) Tetraiodothallate [T1(C12H 240 6)I2](T1I4) (M ePh3P)2l 8 has been prepared by the reaction of methyltriphenylphosphonium iodide with iodine in ethanol. It crystallizes in the m onoclinic space group P 2 xln with a = 985.2(2), b = 1260.0(1), c -1872.6(4) pm, ß = 91.50(2)° and Z = 4. The crystal structure has been refined to R = 0.030 for 2882 reflections. It may be described as a layerlike packing of cations and anions. The anion with point symmetry 1 consists o f two triiodide groups and a bridging iodine molecule forming a rather comm on nearly planar Z-shaped octaiodide ion I82". [Cs(18-crown-6)]I3 has been prepared by the reaction of cesium_iodide and 18-crown-6 with iodine in ethanol. It crystallizes in the triclinic space group PI with a = 921.4(1), b = 1175.4(7), c = 1178.0(4) pm, a = 112.82(4), ß = 94.24(7), y = 98.60(3)° and Z = 2. The crystal structure has been refined to R = 0.038 for 3302 reflections. The geom etry of the cation [Cs(18-crown-6)]+ and of the anion I3~ is quite normal. [Pb(18-crown-6)I]I3 has been prepared by the reaction of lead iodide and 18-crown-6 with iodine in dichloromethane. It crystallizes in the m onoclinic space group P 2 j/a7 with a = 833.6(3), b = 1721.0(6), c = 1730.6(6) pm, ß = 99.61(3)° and Z = 4. The crystal structure has been refined to R = 0.047 for 2772 reflections. It consists o f com plex cations [Pb(18-crown-6)I]+ and triiodide anions I3_ forming weakly bonded ion pairs. [Tl(18-crown-6)I2](TlI4) has been prepared by the reaction of thallium (I)iodide and 18-crown-6 with iodine in dichloromethane. It crystallizes in the m onoclinic space group P 2 xln with a = 1236.8(3), b = 1382.6(3), c = 1710.2(2) pm, ß = 90.76(1)° and Z = 4. The crystal structure has been refined to R = 0.044 for 2916 reflections. It is com posed o f com plex cations [Tl(18-crown-6)I2] + nd complex anions TII4_ with their usual and expected geometry. 
  Reference    Z. Naturforsch. 50b, 1429—1439 (1995); eingegangen am 4. Oktober 1994 
  Published    1995 
  Keywords    Triiodides, Octaiodide, Tetraiodothallate, Crown Ether Complexes, Crystal Structures 
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 Identifier    ZNB-1995-50b-1429 
 Volume    50 
46Author    Karl-Friedrich Tebbe, Taraneh FaridaRequires cookie*
 Title    Untersuchungen an Polyhalogeniden, XX [1]  
 Abstract    Darstellung und Kristallstruktur von Tetra(m ethyltriphenylphosphonium)docosaiodid (M ePh3P)4I22 Studies of Polyhalides, XX [1] Preparation and Crystal Structure of Tetra(methyltriphenylphosphonium)docosaiodide (M ePh3P)4I22 The new compound (M ePh3P)4I22 has been prepared by the reaction of Ph3MePI with iodine in a mixture of methanol and dichloromethane. It crystallizes in the triclinic space group P i with a = 1018.4(3), b = 1333.0(4), c = 2042.9(6) pm, a = 88.56(2), ß = 78.05(2), y = 76.03(2)° and Z = 1. The crystal structure has been refined to RF = 0.0487 for 5525 reflections. It may be described as a layer-like packing of cations [CH3(C6H3)3P]+ and anions I224-di­ vided in one I)22-and two I5_ groups. The central Ii22-anion with point symmetry Q consist­ ing of two L-shaped pentaiodide groups and a bridging iodine molecule is completed by two further end-on bonded pentaiodide ions with a rather short distance o f 366.7(2) pm to the weakly bonded and nearly isolated docosaiodide ion. 
  Reference    Z. Naturforsch. 50b, 1440—1444 (1995); eingegangen am 6. März 1995 
  Published    1995 
  Keywords    Methyltriphenylphosphonium Ion Polyiodide, D odecaiodide D ocosaiodide, Crystal Structure 
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 Identifier    ZNB-1995-50b-1440 
 Volume    50 
47Author    N., Silke Busche, Karsten BluhmRequires cookie*
 Title    Synthese und Kristallstruktur der ersten zinkhaltigen Pyroborate  
 Abstract    ii,5Z n 0,5(6 2 0 5) UI,d C o ^ Z n o ^ I ^ O s) Synthesis and Crystal Structure of the First Zinc Containing Pyroborates Nii.5Z n0.5(B2O 5) and Coj 5Z n0.5(B2O 5) The first zinc containing pyroborates Ni! sZ n ^ B ^ O s) (A) and 5Zn0 5(B 2O 5) (B) were prepared by using a B20 3 flux technique. Single crystals were investigated by X-ray diffrac­ tion and showed triclinic symmetry, space group C j-P l. The structures are isotypic to C o9(B 20 5) with the lattice parameters (A) « = 331.28(6), 6 = 613.87(11), c = 922.2(2), a = 104.067(11) °, ß = 90.672(13) °, y = 92.413(12) 0 and (B) 0 = 315.89(2), 6 = 612.84(6), c = 927.72(6), a = 104.103(7) °, ß = 91.020(6) °, y = 92.540(7) °, Z = 2. All metal point positions show an octahedral oxygen coordination and a partly statistical distribution o f Zn2+ and N i2+ or C o2+, respectively. Isolated nearly planar B20 5 units connect ribbons consisting o f edge sharing metal octahedra. 
  Reference    Z. Naturforsch. 50b, 1445—1449 (1995); eingegangen am 25. April 1995 
  Published    1995 
  Keywords    Zinc, Nickel, Cobalt, Pyroborate, Crystal Structure 
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 Identifier    ZNB-1995-50b-1445 
 Volume    50 
48Author    Silke Busche, Karsten BluhmRequires cookie*
 Title    Zur Synthese und Kristallstruktur von Zinkboratoxiden mit isolierten, trigonal planaren B 0 3-Baugruppen: Zn5M n(B03)20 4 und Z nF e(B 03) 0 Synthesis and Crystal Structure of Zinc Borate Oxides Containing Isolated Trigonal Planar B 0 3 Units: Z n5M n (B 0 3)20 4 and Z n F e(B 0 3) 0  
 Abstract    Single crystals of the new compounds Zn5M n (B 0 3)20 4 (A) and Z n F e (B 0 3) 0 (B) were prepared by using a B20 3 flux technique. Zn5M n (B 0 3)20 4 is isostructural with Ni5T i(B 0 3)20 4 and Z n F e (B 0 3) 0 is isotypic with the mineral warwickite. X-ray investiga­ tions on single crystals led to (A) space group D ^ -P b a m , a = 926.41(10), b = 1236.67(8), c = 304.55(3) pm, Z = 2, and (B) space group D i^ -P n m a, a = 924.62(4), b = 314.1(10), c = 935.3(2) pm, Z = 4. The structure o f Zn5M n (B 0 3)20 4 (A) contains four octahedrally coordi­ nated metal sites, one of these statistically occupied by Zn2+ and Mn4+. In the structure o f Z n F e (B 0 3) 0 the ions Zn2+ and Fe3+ occupy statistically both distorted octahedral sites. Both structures contain isolated B 0 3 units and oxygen that is not coordinated to boron. 
  Reference    Z. Naturforsch. 50b, 1450—1454 (1995); eingegangen am 25. April 1995 
  Published    1995 
  Keywords    Zinc, Manganese, Iron Borate Oxide, Crystal Structure 
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 Identifier    ZNB-1995-50b-1450 
 Volume    50 
49Author    A.Rnd Müller, Gerald Henkel, ThiolatoRequires cookie*
 Title    [Ni2(SC4H9)6]2-> ein neuartiger zweikerniger Nickel-Thiolato-Komplex mit kantenverknüpften NiS4-Tetraedern und [Ni(SC6H4SiMe3)4]2-, ein strukturchemisch verwandtes einkerniges Komplexion [Ni2(SC4H 9)6]2~, a Novel Binuclear Nickel-Thiolat Complex with NiS4 Tetrahedra Sharing Edges and [Ni(SC6H4SiMe3)4]2_, a Structurally Related M ononuclear Complex Ion  
 Abstract    Reaction of nickel(II) chloride with sodium or potassium tert-butane thiolate in acetonitrile affords the isotypical compounds [Nb(SrC4H9)6]Na2 • 4 MeCN (1) and [Ni7(SfC4H9)6]KT • 4 MeCN (2), respectively. Crystal data: 1: a = 9.859(3), b = 11.877(3), c = 19.675(5) Ä , ß = 96.11(2)°, space group P 2x/n, Z = 2:2: a = 9.854(2), b = 11.915(3), c = 20.558(5) Ä , ß = 99.62(2)°, space group P 2xln, Z = 2. The structures were refined to R = 0.0599 (1) and 0.0562 (2), respectively. Both compounds contain the complex ion [Ni2(SrC4H 9)6]2_ (3), which is not only the first example of a tetrahedral nickel complex with alkane thiolate ligands, but also the first poly-nuclear nickel complex containing tetrahedral NiS4-units sharing a comm on edge. Reaction of nickel(II) chloride and sodium (2-trim ethylsilyl)thiophenolate in acetonitrile leads to [Ni(SC6H4SiM e3)4]2~ (5) with tetrahedral stereochemistry. The m ononuclear complex ion is isolated aso [Ph4P]2[Ni(SC6H4SiM e3)4]-5M eC N (4) with a = 13.771(2), b = 14.163(2), c = 25.873(4) A , a = 77.44(1), ß = 75.13(1), y = 72.46(1)°, space group P 1 and Z = 2. The final refinement converged to R = 0.0445. 
  Reference    Z. Naturforsch. 50b, 1464—1468 (1995); eingegangen am 29. Dezem ber 1994 
  Published    1995 
  Keywords    Ligands, Nickel Complexes, Synthesis, Crystal Structure, Bioinorganic Chemistry 
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 Identifier    ZNB-1995-50b-1464 
 Volume    50 
50Author    Karl-Friedrich Tebbe, Taraneh FaridaRequires cookie*
 Title    Untersuchungen an Polyhalogeniden, XXI [1] Die Ethyltriphenylphosphonium-Polyiodide EtPI^PI,* mit n = 3, 5 und 7 Studies of Polyhalides, X X I [1] Ethyltriphenylphosphonium Poly iodides EtPh3PIn with n = 3, 5 and 7  
 Abstract    The compounds EtPh3PI3, EtPh3PI5 and EtPh3PI7 have been prepared by the stoichiometric reaction of EtPh3PI with iodine in a mixture of dichloromethane and ethanol. EtPh3PI3 cry­ stallizes in the monoclinic space group P2,/n with a = 1176.7(3) pm, b = 1202.5(3) pm, c = 1565.9(4) pm, ß = 93.22(2)° and Z = 4. The crystal structure has been refined to R f =0.043 for 3394 reflections. EtPh3PI5 crystallizes in the monoclinic space group I2/a with a = 1913.9(4) pm, b = 1239.0(2)pm, c = 2435.1(4) pm, ß = 115.84(1)° and Z -8 . The crystal structure has been refined to R f = 0.052 for 3043 reflections. EtPh3PI7 crystallizes in the orthorhombic space group Pbca with a = 1702.7(4)pm, b = 1952.5(4) pm, c = 1809.8(4) pm und Z = 8 . The crystal structure has been refined to R f = 0.053 for 3208 reflections. The structures may be described as layerlike packings of cations Ph3EtP+ and of anions If , I f and I f , respectively. The isolated triiodide ion If is slightly asymmetrical and slightly bent as expected. The pentaiodide ion If forms iodine ribbons like a rope ladder. The heptaiodide ion I f is composed of pentaiodide groups and iodine molecules connected to puckered anionic layers. 
  Reference    Z. Naturforsch. 50b, 1685—1691 (1995); eingegangen am 5. Mai 1995 
  Published    1995 
  Keywords    Ethyltriphenylphosphonium Polyiodides, Triiodide, Pentaiodide, Heptaiodide, Crystal Structure 
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 Identifier    ZNB-1995-50b-1685 
 Volume    50 
51Author    KurtO. Tto Klepp, Claudia WeithalerRequires cookie*
 Title    Die Kristallstruktur von RbCuSe4 The Crystal Structure of RbCuSe4  
 Abstract    Crystals of RbCuSe4 are orthorhombic, oP24, s.g. P 2 /2 /2 / (No. 19), Z = 4 with a = 5.541(2) A , b = 8.814(2) A , c -13.277(9) A. The crystal structure was determined from diffractometer data and refined to a conventional R of 0.019. RbCuSe4 is a pseudo-one-dim ensional com ­ pound, characterized by infinite polyanionic chains :J ;-[CuSe4]_. The atomic arrangement cor­ responds to that of « -N H 4CuS4. 
  Reference    Z. Naturforsch. 50b, 1791—1793 (1995); eingegangen am 4. Mai 1995 
  Published    1995 
  Keywords    Rubidium Tetraselenocuprate(I), Chain Structure, Crystal Structure 
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 Identifier    ZNB-1995-50b-1791 
 Volume    50 
52Author    Hk Müller-Buschbaum, St GallinatRequires cookie*
 Title    Synthese und Röntgenstrukturanalyse von KCuGd2Mo40 16 und KCuTb2Mo40 16 Synthesis and X-Ray Analysis of KCuGd2Mo4O i6 and KCuTb2Mo40 I6  
 Abstract    Single crystals of the so far unknown compounds KCuGd2M o4O t6 (I) and KCuTb2M o40 16 (II) have been prepared by flux technique. The compounds crystallize with monoclinic sym­ metry. space group C^h-C 2 /c with (I): a = 5.278(2), b = 12.666(5), c = 19.604(14) Ä; ß = 92.76(6)°; (II): a = 5.259(13), b = 12.616(3), c = 19.556(9) A, ß = 92.93(4)°, Z = 4. M olyb­ denum exhibits tetrahedral coordination. The surroundings of copper can be described by distorted tetrahedra, capped by two more distant oxygen atoms, and the rare earth ions show a square antiprism. Potassium is inside an irregular polyhedron. The relationship of the structures o f (I) and (II) is discussed with respect to the KLnMo2Os type compounds. Coulomb term calculations of the lattice energy indicate an oxidation state of copper higher than Cu1. 
  Reference    Z. Naturforsch. 50b, 1794—1798 (1995); eingegangen am 29. Mai 1995 
  Published    1995 
  Keywords    Potassium, Copper Rare Earth Molybdenum Oxide, Crystal Structure 
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 Identifier    ZNB-1995-50b-1794 
 Volume    50 
53Author    Karsten Busche, BluhmRequires cookie*
 Title    Silke  
 Abstract    The compound Cu2 Z n(B 2 0 s) 0 was prepared by using a B 2 0 3 flux technique, and single crystals were investigated by X-ray diffraction (monoclinic symmetry, space group C2 h-P 2 i/c). The structure is isotypic to Cu2 C o(B 2 0 5) 0 with lattice parameters a = 327.38(2), b = 1479.4(3), c = 915.39(13), ß = 95.794(11)°, Z = 4, but with the significant difference that zinc is penta-coordinated by oxygen. Copper exhibits a nearly square planar or a square pyramidal coordi­ nation, respectively. The structure contains isolated B2 0 ? units and oxygen which is not coordinated to boron. Zur Synthese und Kristallstruktur von Kupferzinkpyroboratoxid Cu2Zn(B20 5) 0 
  Reference    Z. Naturforsch. 50b, 1854—1858 (1995); eingegangen am 17. Mai 1995 
  Published    1995 
  Keywords    Copper, Zinc, Pyroborate, Oxide, Crystal Structure 
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 Identifier    ZNB-1995-50b-1854 
 Volume    50 
54Author    A. Franken, W. PreetzRequires cookie*
 Title    Darstellung, n B-NMR-und Schwingungsspektren  
 Abstract    von Am inohexahydro-closo-hexaborat(l-), [B6H6(NH2)]~ sowie Kristallstruktur von Cs[B6H6(NH2)]*H 20 P rep aratio n , n B N M R and V ibrational Spectra of A m in o h e x a h y d ro -c lo so -h ex a b o ra te (l-), [B6H 6(N H 2)]' , and the C rystal S tructure of Cs[B6H 6(N H 2)] • H 20 By reduction of [B6H5(N0 2)]2_ with Fe2+ in aqueous alkaline solution [B6H6(NH2)]~ is formed. The compound has been separated by extraction with dichloromethane in the presence of tetrabutylammoniumbromid and precipitated from the organic phase by adding CsCH3COO/C2H5OH. The Crystal structure of Cs[B6H6(NH2)] H20 has been determined by single crystal X-ray diffraction analysis; monoclinic space group C2 with a = 22.1075(14), b = 6.491(2), c = 5.9570(4) Ä, ß = 100.168(6)°. The UB NMR spectrum is consistent with a mono-hetero-substituted octahedral B6 cage with local C4v symmetry. The IR and Raman spectra exhibit characteristic N -H , B -H and B6 vibrations. 
  Reference    (Z. Naturforsch. 50b, 11—14 [1995]; eingegangen am 9. August 1994) 
  Published    1995 
  Keywords    Aminohexahydro-closo-hexaborate(l-), Crystal Structure, UB NMR Spectra, Vibrational Spectra 
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 Identifier    ZNB-1995-50b-0011 
 Volume    50 
55Author    Christian Drost, Carsten Jäger, Uwe Klingebiel, Christina Freire-Erdbrügger, Regine Herbst-Irm, M. Er, Artina SchäferRequires cookie*
 Title    Lithium-[N-di-terr-butylfluorsilyl-N' ,N ' -dimethyl-hydrazid] - Synthese, Kristallstruktur und Reaktivität Lithium (N-di-te/'f-butylfluorosilyl-N',N'-dimethyl)hydrazide - Synthesis, Crystal Structure and Reactivity  
 Abstract    Di-terf-butyldifluorosilane reacts with N-lithium -N',N'-dimethylhydrazine in a molar ratio 1:1 to yield the N-di-ferf-butylfluorosilyl-N',N'-dimethylhydrazine 1. The lithium derivative of 1 (2) forms a dimer with the nitrogen atoms coordinated "side-on" to the lithium atoms. The silylation with M e3SiCl gives product 3. Heating 2 in a vacuum leads to the cyclo-disilazane derivative 4. A bis(hydrazino)fluoroborane (5) is obtained in the reaction of 2 with trifluoroborane-etherate. 
  Reference    (Z. Naturforsch. 50b, 76—8 [1995]; eingegangen am 18. Juli 1994) 
  Published    1995 
  Keywords    Fluorosilylhyrazines, Lithium-Derivative, Crystal Structure, Side-on Coordination 
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 Identifier    ZNB-1995-50b-0076 
 Volume    50 
56Author    Evamarie Hey-Hawkins+, Stefan Kurz, G.Erhard BaumRequires cookie*
 Title    P-H-funktionelle Zirkonocen-Phosphido-Komplexe  
 Abstract    Synthese von Cp'2Zr{PH(2,4,6-Pr'3C6H2)}(X) (Cp = C5H4Me, X = Cl, 2,4,6-Pr'3C6H2) und Molekülstruktur von Cp'2ZrCl{PH(2,4,6-Pr/3C6H2)} P-H -Functionalized Zirconocene Phosphido Complexes -Synthesis of C p '2Zr{PH(2,4,6-Pr'3C6H 2)}(X) (Cp' = C5H 4 Me, X = Cl, 2,4,6-Pr'3C6H 2) and Molecular Structure of C p '2ZrCl{PH(2,4,6-Pr'3C6H 2)} The reaction of Cp'2ZrCl2 (Cp' = C5H4M e) with solvent-free LiPH(2,4,6-Pr'3C6H 2) yields the terminal zirconocene phosphido com plexes Cp'2ZrCl{PH(2,4,6-Pr'3C6H 2)} (1) (1:1 reac­ tion) or Cp'2Zr{PH(2,4,6-Pr'3C6H2)}2 (2) (1:2 reaction). 1 and 2 were characterized spectro­ scopically (NMR, IR, MS). An X-ray structure determination was carried out on 1 (Z r -P 2.6381(8) A, Z r-C l 2.4547(6) A , C l-Z r -P 93.55(2)°). 
  Reference    Z. Naturforsch. 50b, 239 (1995); eingegangen am 15. Septem ber 1994 
  Published    1995 
  Keywords    Zirconocene Phosphido Complexes, Lithium 2, 4, 6-Triisopropylphenylphosphide, Crystal Structure 
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 Identifier    ZNB-1995-50b-0239 
 Volume    50 
57Author    H. Szillat, Hk Müller-BuschbaumRequires cookie*
 Title    Uber das Erdalkalimetall-Lanthanoid  
 Abstract    Kupfer-Oxomolybdat (Cu0,22Mg0 ,78)BaNd2Mo4O 16 The Alkaline Earth R are E arth Copper-Oxomolybdate (C u 0 . 2 2 M g 0 . 7 8) B a N d 2 M o 4 O 1 6 Single crystals of (Cu0.22Mg0 78)B aN d2M o4O i6 have been prepared by crystallization from melts and investigated by X-ray methods. The compound crystallizes monoclinically, space group C ^ -C 1 2 /cl, Z = 4, a = 5.351(1), b = 12.891(2), c = 19.391(4) Ä, ß = 90.899(14)° and is isotypic to CuKHo2M o40 16. The crystal structure is dominated by B aO 10 and N d 0 8 poly-hedra forming a three-dimensional polyhedra network, which is filled by axially distorted (C u,M g)O fi octahedra and M o 0 4 tetrahedra. 
  Reference    Z. Naturforsch. 50b, 577 (1995); eingegangen am 4. Oktober 1994 
  Published    1995 
  Keywords    Crystal Structure, Copper, M agnesium, Barium, Neodymium, Molybdenum, Oxide 
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 Identifier    ZNB-1995-50b-0577 
 Volume    50 
58Author    Z. NaturforschRequires cookie*
 Title    Synthesis  
 Abstract    o f N itrene C om plexes w ith N -T rim ethylsilylaniline I. Characterisation and Crystal Structure o f [R e(N Ph)C l3(E t2PhP)2] and [Re(N Ph)Cl3(Ph3P)2] • 1/2CHC13 U rsula W ittern, Joachim Strähle*, U lrich A bram rra»^-mt'r-Trichlorobis(diethylphenylphosphine)phenylnitrene rhenium(V), [Re(NPh)Cl3-(Et2PhP)2], has been synthesized from [ReOCl3(Et2PhP)2] and N-trim ethylsilylaniline, while rrans-ttZfr-trichlorophenylnitrenebisCtriphenylphosphine) rhenium(V), [Re(NPh)Cl3(Ph3P)2] has been obtained via a novel route, from (Bu4N)[ReOCl4] and N-trim ethylsilylanilin. The products were studied by mass spectrometry, IR spectroscopy and X-ray diffraction. rrafls-m er-[Re(NPh)Ch(Et-'PhP)2] crystallizes in the m onoclinic space group P2i/n with a = 1498.5(3), b = 1068.6(1), c = 1784.0(4) pm and ß = 91.28(1)°, Z = 4. The rhenium atom exhibits a distorted octahedral coordination with the phosphine groups in trails positions, and the Cl ligands in a meridional arrangement. The R e = N -C moiety is linear with a bond angle o f 169,4(5)°and a R e = N bond length o f 171.8(6) pm. [ R e (N P h) C h (P h 3 P) i ] 0.5 C H C I 3 c r y s t a l l i z e s in th e t r i c l i n i c s p a c e g r o u p P i w i t h a = 1232.1 (4), b= 1431.6(5), c = 2236.6(8) pm, a = 89.19(2)°, ß = 80.50(2)°and 7 = 88.26(2)°, Z = 4. The asymmetric unit contains two symmetry independent complex m olecules o f approxima­ tely the same structure, with Cl atoms meridionally arranged and the phosphine groups in trans positions. The coordination geometry is a distorted octahedron. The almost linear R e = N -C m oieties have R e = N bond lengths o f 170.2(7) and 170.8(7) pm, respectively, and R e -N -C angles o f 173.3(6)°and 175.0(7)°. 
  Reference    Z. Naturforsch. 50b, 997 (1995); eingegangen am 15. Februar 1995 
  Published    1995 
  Keywords    Rhenium(V) C om plexes, Phenylnitrene Com plexes, Crystal Structure, Mass Spectra 
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 TEI-XML for    default:Reihe_B/50/ZNB-1995-50b-0997.pdf 
 Identifier    ZNB-1995-50b-0997 
 Volume    50 
59Author    M. Jansen, S. StrojekRequires cookie*
 Title    Darstellung und Kristallstruktur von [P(C6H5)4]C13 Preparation and Crystal Structure of [P(C6H 5)4]C13  
 Abstract    Preparation and crystal structure of [P(C6H 5)4]C13 are reported. [P(C6H 5)4]C13 crystallizes in the monoclinic space group P 2 x!c with a = 1093.4(4), b = 789.1(1), c = 2682.7(7) pm, ß = 90.39(1)°, V = 2200.27-106 pm3, and Z = 4. The geometry of the trichloride anion in the solid state is almost linear (C1-C1-C1 = 178.44(4)°) and unsymmetrical (d (C l-C l) = 226.3(1) and 230.7(1) pm). 
  Reference    Z. Naturforsch. 50b, 1171—1174 (1995); eingegangen am 13. Februar 1995 
  Published    1995 
  Keywords    Tetraphenylphosphonium Trichloride, Preparation, Crystal Structure, G eom etry of Cl3~ 
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 TEI-XML for    default:Reihe_B/50/ZNB-1995-50b-1171.pdf 
 Identifier    ZNB-1995-50b-1171 
 Volume    50 
60Author    Marcos Luján, Frank Kubel, Hans SchmidRequires 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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 TEI-XML for    default:Reihe_B/50/ZNB-1995-50b-1210.pdf 
 Identifier    ZNB-1995-50b-1210 
 Volume    50 
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