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1994 (62)
21Author    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 
22Author    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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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-0935.pdf 
 Identifier    ZNB-1994-49b-0935 
 Volume    49 
23Author    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 
24Author    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 
25Author    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 
26Author    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 
27Author    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 
28Author    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 
29Author    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 
30Author    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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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-1463.pdf 
 Identifier    ZNB-1994-49b-1463 
 Volume    49 
31Author    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 
32Author    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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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-1503.pdf 
 Identifier    ZNB-1994-49b-1503 
 Volume    49 
33Author    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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 Identifier    ZNB-1994-49b-1554 
 Volume    49 
34Author    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 
35Author    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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 Identifier    ZNB-1994-49b-0036 
 Volume    49 
36Author    Anne-Kathrin Duhme, Henry StrasdeitRequires cookie*
 Title    Ligandenmangelkomplexe des Cadmiums. Synthese und spektroskopische Charakterisierung molekularer (Pentafluorphenyl)cadmium-Thiolate und die Struktur des Cubankomplexes [{Cd(C6F5)(SBur)}4] Ligand-Deficient Complexes of Cadmium. Synthesis and Spectroscopic Characterization o f Molecular Pentafluorophenyl Cadmium Thiolates and the Structure o f the Cubane Complex [{Cd(C6F5)(SBuf)}4]  
 Abstract    In toluene, bis(pentafluorophenyl)cadmium(II) and thiols RSH (R = Bu', 2,4,6-Pr'3C6H2, 2,4,6-Bu'3C6H2) react to give soluble pentafluorophenyl cadmium thiolates [(Cd(C6F5)(SR)} J. The compounds [{Cd(C6F 5)(SBu')}4] (1)0 .5 C6H5CH3, [ {Cd(C6F5)(SC6H2Pr'3-2,4,6)} J (2)-ca. 0.25n C6H 5CH3, and [{Cd(C6F5)(SC6H2Bu'3-2,4,6)} J (3) ca. 0.25« C6H5CH3 have been prepared in 65, 59 and 78% yield, respectively. 1-0.5 C6H5CH3 crystallizes in the triclinic space group PI with a = 11,635(1)Ä, b = 11.583(1)Ä, c = 21.480(2)Ä, a = 82.12(1)°, ß = 76.26(1)°, y — 89.35(1)°, and Z = 2. 1 is a cubane-type complex with a {Cd4(/z3-SBur)4}4+ core. Each Cd atom is coordinated by three bridging thiolato ligands and one terminal C6F5 group (C d -S 2.62 A, C d -C 2.15Ä (mean values)). The central C atoms of the Bu'S" ligands of 1 show a remarkable low-field shift o f their 13C N M R resonance (12.3 ppm relative to the value of the free thiol). A characteristic spectral feature of (Cd(C6F5) } + complexes is the large value of the coupling constant 2/ (19F ,13C) o f the ipso-C atom (1, 2: 68 Hz; 3: 67 Hz). The complexes [Cd(C6F5)(SR) + H]+, [Cd(SR)2 + H]+, and [Cd2(SR)3]+ were identified in the Cl mass spectra (/50-butane) of 2 and 3. 
  Reference    (Z. Naturforsch. 49b, 119—127 [1994]; eingegangen am 17. August 1993) 
  Published    1994 
  Keywords    Cadmium Complexes, Thiolates, Crystal Structure, NMR Spectra, Mass Spectra 
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 Identifier    ZNB-1994-49b-0119 
 Volume    49 
37Author    Dietrich Mootz, Michael BornRequires cookie*
 Title    Niedere Hydrate von Aminen. Kristallstrukturen der Hemihydrate von Ethyl-und Diethylamin sowie des Hemi-und Monohydrats von 1-Butylamin [1] Lower Hydrates of Amines. Crystal Structures of the Hemihydrates of Ethyl-and Diethylamine and the Hemi-and M onohydrate of 1-Butylamine  
 Abstract    The melting diagrams of three systems alkylamine-water have been reexamined and the crystal structures of four lower hydrates determined for the first time. The hydrate EtNH2 -0.5 H20 , m.p. -72 °C, is triclinic with space^roup P 1 and Z = 4 formula units per unit cell of dimensions a = 5.104, b = 8.137, c = 9.394 Ä, a = 100.41, ß = 98.41 and y = 97.96° at -150°C. The O and N atoms are hydrogen-bonded into a two-dimensional array l[ON6/3] analogous to the layer of the Cdl2 structure type. The hydrate Et2NH • 0.5 H20 , m.p. -20 °C, is monoclinic with 12/a, Z = 8 , a -8.324, b = 15.090, c = 10.006 Ä and ß -103.34° at -100 °C. The O and N atoms are linked into a four-membered ring spiro chain ifON^] analogous to that in SiS2. The hydrate l-BuNH2 0.5H20 (m.p. -57 °C, monoclinic, P 2x/c, Z = 8,a = 14.994, b = 5.086, c = 16.15 A .,ß -103.45° at -81 °C) contains essentially the same hydrogen-bonded array as the hydrate EtNH,-0.5H20 (see above). l-BuNH2-H20 , the only monohydrate in­ vestigated besides the three hemihydrates (m.p. -60 °C, monoclinic, C 2/m, Z = 4, a = 9.68, b = 4.238, c = 15.58 A, ß = 94.9° at -81 °C), has also a two-dimensional H20/N H 2 partial structure, similar to a subset of the three-dimensional network of the adduct NH3 H20 of analogous composition. Z ur Bildung kristalliner Hydrate von einfachen Alkylaminen gibt es eine Reihe von z. T. schon recht frühen Untersuchungen mit allerdings nicht immer eindeutigen und widerspruchsfreien Ergebnissen. Die Bestimmung von Kristallstrukturen be­ schränkte sich bisher auf einige höhere Hydrate mit W assergehalten oberhalb denen von Pentahydra-ten. Solche wasserreichen Phasen wurden als Cla-thrathydrate oder Semiclathrate charakterisiert. Sie enthalten nämlich dreidimensional vernetzte W irtsstrukturen aus den W assermolekülen und in deren m ehr oder weniger gestörten polyedrischen H ohlräum en die fast immer auch noch H-brücken-aktiven (N -H — O und/oder O -H -N) Am in­ moleküle als Gastspezies [2]. Gegenstand der vorliegenden A rbeit sind nun erstmals K ristallstrukturen niederer Hydrate von * Sonderdruckanforderungen an Prof. Dr. D. Mootz. 
  Reference    Z. Naturforsch. 49b, 243—249 (1994); eingegangen am 27. Oktober 1993 
  Published    1994 
  Keywords    Amine Hydrates, Lower Hydrates, Melting Diagram, Crystal Structure, Hydrogen Bonding 
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 Identifier    ZNB-1994-49b-0243 
 Volume    49 
38Author    P. Souza, M. A. Mendiola3, A. Arquerob, V. Ferná, E. G Utiérrez-Pueblac, C. Ruiz-ValerocRequires cookie*
 Title    Copper(II) Complexes of Hydrazone Derivatives  
 Abstract    Three benzil based, macrocyclic oxygen-, nitrogen-, and sulfur-containing ligands, (3,4,10,11 -tetraphenyl-1,2,5,6,8,9,12,13-octaazacyclotetradeca-7,14-dithione-2,4,9,11 -tetraene) ethanol (L 1), 10,1 l-diethoxy-3,4,10,11-tetraphenyl-1,2,5,6,8,9,12,13-octaazacyclotetradeca-7.14-dithione-2,4-diene (L2), (3,4,10,11 -tetraphenyl-1,2,5,6,8,9,12,13-octaazacyclotetradeca-7.14-dione-2,4,9,l 1-tetraene) ethanol (L3); a cyclic ligand, 6-ethoxy-l,6-diphenyl-4-oxo-3,4,5,6-tetrahydro-2,3,5-triazine (L5) and two open chain ligands, benzilsemicarbazone (L6) and benzilbisthiosemicarbazone (L4) are reported. These ligands react with copper(II) chlor­ ide, nitrate and acetate. The complexes obtained have been characterized on the basis o f N M R , IR, electronic and mass spectral studies, conductance and analytical data. The sto-ichiometry and the spectroscopic data o f the complexes indicate that the copper ions are coor­ dinated by neutral ligands or by ligand anions formed by loss o f protons from the ligand. The molecular and crystal structure o f 6-ethoxy-l,6-diphenyl-4-oxo-3,4,5,6-tetrahydro-2,3,5-triazine (L 5) was determined by X-ray diffraction; the space group is triclinic, P 1 with a = 7.865(1), b = 14.101(6), c = 15.733(9) A, a = 69.10(3)°, ß = 75.62(2)°, y = 86.69(2)°, V = 1578(1) A 3, Z = 4. 
  Reference    Z. Naturforsch. 49b, 263—2 (1994); received June 2/October 4 1993 
  Published    1994 
  Keywords    Benzil, Hydrazones, Copper(II), M acroligands, Crystal Structure 
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 Identifier    ZNB-1994-49b-0263 
 Volume    49 
39Author    Meyer Zu Köcker, Andreas Behrendt, K. Urt Dehnicke, Dieter FenskeRequires cookie*
 Title    Phosphaniminato-Cluster des  
 Abstract    Kupfers. Synthese und Kristallstrukturen von ICu6Cl6(NPM e3)4|Cl[Me3SiNPM e3| • CH2C12 und ICu6Cl6(NPM e3)4l[Cu(Me3SiNPM e3)2lCl2 Phosphoraneim inato Clusters o f Copper. Syntheses and Crystal Structures of [Cu6Cl6(N PM e3)4]Cl[Me3SiNPM e3] • C H 2C12 and [Cu6Cl6(NPM e3)4][Cu(Me3SiNPM e3)2]Cl2 R olf The title com pounds have been prepared as black-blue crystals with metallic lustre by the reaction o f CuCl2 and CuCl, respectively, with M e3SiN P M e3 in C H 2C12 suspensions. The com ­ plexes have been characterized by cyclic voltammetry and by crystal structure determinations. [Cu6Cl6(N P M e3)4]Cl[M e3SiN P M e3] • C H 2C12: Space group P 2,2,2,, Z = 4, structure solution with 4407 unique observed reflections, R = 0.057. Lattice dimensions at -7 0 °C: a -1159.3(8), b = 2027.1(14), c = 2063.3(12) pm. The compound consists o f cluster ions [Cu6Cl6(N P M e3)4]+, in which the copper atom s form a regular octahedron. Four planes o f the octahedra are capped by //3-nitrogen atom s o f the (N P M e3)~ groups. Each o f the Cu atom s is connected with a terminal chlorine atom . Another chloride ion serves for charge com pensa­ tion; this ion occupies another Cu3 plane o f the octahedron. W ithout bonding interaction one M e3SiN P M e3 molecule and one C H 2C12 molecule are included in the lattice. [Cu6Cl6(N P M e3)4][Cu(M e3SiN P M e3)2]Cl2: Space group Pna2,, Z = 4, structure solution with 5676 unique observed reflections, R = 0.071. Lattice dimensions at -7 0 °C: a = 3117.2(21), b = 1927.4(11), c = 1002.7(8) pm. The compound consists o f cluster ions [Cu6Cl6(N P M e3)4]+, the com plex ion [Cu(M e3SiN PM e3)2]+, and chloride ions. In the cation [Cu(Me3SiN P M e3)2]+ the copper atom is linearly coordinated by the nitrogen atom s o f the phosphaneimine m olecules. 
  Reference    Z. Naturforsch. 49b, 301—3 (1994); eingegangen am 18. November 1993 
  Published    1994 
  Keywords    Phosphoraneim inato Clusters o f Copper, Synthesis, Cyclic Voltammetry, Crystal Structure 
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 Identifier    ZNB-1994-49b-0301 
 Volume    49 
40Author    Holger Szillat, Hanskarl Müller-BuschbaumRequires cookie*
 Title    Synthese und Kristallstruktur von KCuHo2Mo40 16 Synthesis and Crystal Structure of K C uH o2M o40 I6  
 Abstract    Single crystals o f K C uH o2M o40 16 have been prepared by recrystallisation from melts and investigated by X-ray diffractometer techniques. The compound crystallizes with m onoclinic symmetry, space group C 2/c, a = 521.6(1), b = 1251.3(2), c = 1953.1(2) pm, ß = 92.903(18)°, Z -4. K C uH o2M o40 16 represents a new structure type characterized by H oO s and alternate CuO6/K O 10 polyhedra chains. The connection o f these polyhedra chains to each other and by M o 0 4 tetrahedra is described and the crystal structure discussed with respect to related com ­ pounds o f the C uLnM o2Os and K L nM o20 8 types. 
  Reference    Z. Naturforsch. 49b, 350 (1994); eingegangen am 10. Dezember 1993 
  Published    1994 
  Keywords    Crystal Structure, Copper, H olm ium, M olybdenum, Potassium 
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 Identifier    ZNB-1994-49b-0350 
 Volume    49 
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