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'Crystal Structure' in keywords Facet   section ZfN Section B:Volume 046  [X]
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1991 (24)
1Author    SylviaM. Agull, Bernhard Neumüller, K. Urt DehnickeRequires cookie*
 Title    Synthese und Kristallstrukturen der Polyselenido-Mercurate (PPh4)2|H g(Se4)2| und |Cs(18-Krone-6)|2|H g2(Se4)3l Syntheses and Crystal Structures of the Polyselenido M ercurates (PPh4)2[Hg(Se4)2] and [Cs(18-Crown-6)]2[Hg2(Se4)3]  
 Abstract    (PPh4)2[Hg(Se4)J has been prepared by the reaction o f (PPh4)2[Sn(Se4)3] with H g(C H 3COO)2 in dimethylformamide (D M F) solution. [Cs(18-crown-6)]2[Hg2(Se4)3] has been prepared by the reaction o f a lithium polyselenide solution in D M F with H g(C H 3COO)2 in the presence o f CsBr and 18-crown-6. Both com pounds are obtained as dark red crystals and characterized by X-ray structure determinations. (PPh4) 2[H g(Se4) 2]: Space group P 2,/c, Z = 4, 3021 observed unique reflexions, R = 0.082. Lattice dim ensions at 20 °C: a = 1046.0(3), b = 2129.4(2), c = 2213.1(3) pm,/? = 97.62(2)°. The com pound consists o f PPh4+ ions and anions [Hg(Se4)2]2", in which the mercury atom is a spi-rocenter o f puckered HgSe4 rings. [ Cs(18-crown-6) J2[H g2(Se4)3J: Space group la, Z = 4, 2859 observed unique reflexions, R = 0.074. Lattice dimensions at 20 °C: a = 2018(1), b = 1097.0(2), c = 2317.1(5) pm, ß = 99.40(3)°. The compound forms an ion triple which originates from Cs-Se contacts o f 382 to 390 pm with the [Hg2(Se4)3]2~ ion. The latter can be described as a [FlgtSe^JJ2-ion, which has contacts with a HgSe4 fragment. 
  Reference    Z. Naturforsch. 46b, 985—9 (1991); eingegangen am 12. Dezember 1990 
  Published    1991 
  Keywords    Polyselenido Mercurates, Synthesis, Crystal Structure 
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 Identifier    ZNB-1991-46b-0985 
 Volume    46 
2Author    Bernhard NeumüllerRequires cookie*
 Title    Darstellung und Kristallstruktur von [(Me3Si)2CH(7-Pr)InCll2 Synthesis and Crystal Structure o f [(Me3Si)2CH(/-Pr)InCl]2  
 Abstract    The title com pound 1 has been prepared by the reaction o f z-PrlnCl, with LiC H (SiM e3)2 in diethylether at -3 0 °C. The colorless substance 1 was characterized by N M R , IR, and RE spectroscopy, as well as by mass spectrometry. 1 is dimer in solution and the solid state and crystallizes in the space group P 2 ,/c with the cell parameters a = 1206.4(3) pm, b = 905.7(2) pm, c = 1591.2(5) pm, and ß = 101.18(2)°. The unit cell contains two centrosymmetri-cal dimeric molecules. 
  Reference    Z. Naturforsch. 46b, 1539—1543 (1991); eingegangen am 12. April 1991 
  Published    1991 
  Keywords    Diorganoindiumchloride, Synthesis, Crystal Structure 
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 Identifier    ZNB-1991-46b-1539 
 Volume    46 
3Author    Klaus-Jürgen Range, Franz Rau, Ulrich KlementRequires cookie*
 Title    Hochdrucksynthese und Strukturverfeinerung von S r V 0 3, Sr2V 0 4 und Sr3V20 7 High-Pressure Synthesis and Structure Refinement of S rV 03, Sr2V 0 4, and Sr3V20 7  
 Abstract    Single crystals o f S rV 0 3, Sr2V 0 4 and Sr3V20 7 have been obtained by high-pressure reactions in a m odified belt-type apparatus. The crystal structures, refined from diffractometer data, are as follows; S rV 03, perovskite type. Pm 3m, a = 3.8408(3) A, R = 0.017, /?w = 0.018, com posi­ tion from occupancy refinement o f oxygen positions SrV O ,93(2); Sr2V 0 4, K 2N iF 4 type, I 4/m m m , a = 3.837(1), c = 12.569(1) Ä, R = 0.014, R w = 0.017; Sr3V ,0 7, Sr3T i,0 7 type, I 4/m m m , a = 3.839(1), c = 20.262(2) Ä, R = 0.020, R w = 0.029. 
  Reference    Z. Naturforsch. 46b, 1315—1318 (1991); eingegangen am 10. Mai 1991 
  Published    1991 
  Keywords    Strontium Vanadium(IV) Oxides, High-Pressure Synthesis, Crystal Structure 
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 Identifier    ZNB-1991-46b-1315 
 Volume    46 
4Author    Jürgen Silberzahn, Hans Pritzkow, HansPeter LatschaRequires cookie*
 Title    Synthese und Kristallstruktur eines l(A5),4(A5)-Diphosphaazulens sowie dreier 1 -Phospha-1,6a-dihy dropentalene Synthesis and Crystal Structure o f a l(/l5),4(^5)-Diphosphaazulene and of Three 1 -Phospha-1,6a-dihydropentalenes  
 Abstract    The reaction o f acetylene-bis(phosphonous-bisdimethylamide) (1) with tetraphenyl-cyclo-pentadienone (2) yields a 1-phospha-1,6a-dihydropentalene (4), which can be sulfurized with CS2 to give the 1-thio-compound 5, and oxidized with H 20 2 to give the 1-oxo-compound 6. With dim ethyl-acetylenedicarboxylate (7) an amazingly stable l (/ 5),4(A5)-diphosphapen-talene (8) is generated, which reacts further with 7 to yield a l(/.5),4 (/5)-diphosphaazulene (9). The preparation o f the new molecules 4, 5, 6, 9 and the crystal structures o f 5 and 9 are reported. 
  Reference    Z. Naturforsch. 46b, 197—201 (1991); eingegangen am 15. Juni 1990 
  Published    1991 
  Keywords    Phosphororganic Azulene and Dihydropentalenes, Synthesis, Crystal Structure 
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 Identifier    ZNB-1991-46b-0197 
 Volume    46 
5Author    Frank Weller, Irene Pauls, K. Urt Dehnicke, Gerd BeckerRequires cookie*
 Title    Die  
 Abstract    Reaktionen von Wolframhexachlorid mit überschüssigem 2,2-Dimethylpropylidinphosphan; die Kristallstrukturen von WC15P2(C5H9)3, WC14P5(C5H 9)s und |C3(C4H9)3| +|WC1S(C4H9C -C C 4H9)|-The Reactions of Tungsten Hexachloride with Excess 2,2-Dimethylpropylidynephosphane; the Crystal Structures of WC15P2(C5H9)3, WC14P5(C5H 9)5, and [C3(C4H9)3]+[WC15(C4H9C = C C 4H 9)]- The reaction of tungsten hexachloride with excess 2,2-dimethylpropylidynephosphane, C4H9-C = P , leads to the tungsten phosphaalkyne clusters WC15P2(C5H9)3 and WC14P5(C5H9)5, as well as to the tris(/'-butyl)cyclopropenium pentachloro tungsten alkyne complex [C3(C4H9)3]+[WC15(C4H9C=CC4H9)]-. All complexes were characterized by X-ray structure determinations. WC15P2(C5H9)3: Space group P 2,/«, Z = 8, 4653 observed unique reflexions, R = 0.033. Lat­ tice dimensions at 20 C: a = 1577.8(2), b = 1661.3(1), c = 1869.8(2) pm, ß = 110.64(1)°. The compound has a molecular structure, in which the tungsten atom is surrounded by three chlo­ rine atoms, three carbon atoms with W -C distances of 182, 230, and 231 pm. and by one phosphorus atom with W -P = 246 pm. WC14P5(C5H9)5: Space group P2,/c, Z = 4, 3517 observed unique reflexions, R = 0.043. Lat­ tice dimensions at 20 °C: a = 1770.0(2), b = 1032.9(2), c = 1876.0(3) pm, ß = 102.86(1)°. The complex has a molecular structure, in which the tungsten atom is surrounded by two chlorine atoms, two carbon atoms with W -C distances of 189 and 215 pm, as well as by four phospho­ rus atoms with W -P distances of 242, 250, 264, and 268 pm. [C3(C4H9)3]*[WC15(C4H9C=CC4H9)] : Space group P2l/c', Z = 4, 3284 observed unique re­ flexions, R = 0.052. Lattice dimensions at 20 °C: a = 941.5(3), b = 1762.2(6), c = 1903.5(7) pm, ß = 92.27(3)°. The compound consists of tris(/-butyl)cyclopropenium ions, and anions [WC15(C4H9C=CC4H9)]_, in which the bis(r-butyl)alkyne ligand is coordinated side-on, corre­ sponding to a cyclopropene type structure with W -C distances of 198 pm. 
  Reference    Z. Naturforsch. 46b, 519—529 (1991); eingegangen am 8. November 1990 
  Published    1991 
  Keywords    Phosphaalkyne Clusters of Tungsten, Syntheses, Crystal Structure 
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 Identifier    ZNB-1991-46b-0519 
 Volume    46 
6Author    Dirk Adam, Bernhard Herrschaft, Hans HartlRequires cookie*
 Title    Synthese und Strukturuntersuchungen von Iodocupraten(I) XIV. Iodocuprate(I) mit /f-(7-gebundenen Kationen [1] Synthesis and Structure Investigations of Iodocuprates(I) XIV. Iodocuprates(I) with «-er-Bonded Cations [1]  
 Abstract    Reactions o f Cul with N-methylpyrazinium iodide, (pyr)I, N-methyl-4,4'-bipyridinium iodide, (bp 4)1 and N-methyl-2,2'-bipyridinium iodide, (bp 2)1, in organic solvents led to three novel types o f copper(I) complexes o f stoichiometries (pyr)Cu2I3, (bp4)C u3I4 and (bp2)C u2I3. In all o f them the cations are n-a-bonded to copper(I) through donation o f their unshared electron pairs. (pyr)Cu2I3 crystallizes with an ionic structure (trigonal, R 3 c , hexagonal axes a -3053(2), c = 671.9(3) pm, Z = 18). Polymeric cations i[((pyr)C uI3/3)3]3+ and anions i[C u I4/2]-form parallel rod packings. The structure m otif o f the cations can be described as a columnar part o f the ß-Cu\ structure in which the copper and iodine atom s are also arranged to Cu3I3 rings. The crystal structure o f (bp4)C u3I4 (triclinic, P I, a = 938.8(2), b = 980.0(4), c = 1070.1(3) pm, a = 73.56(3), ß = 75.79(2), y = 89.50(3)°, Z = 2) is built up by uncharged chains i[(C uI4/3)(CuI3 3I1/2)((bp4)C uI2/3I1;2)]. The trinuclear units (bp4)C u3I4 are connected via com ­ mon iodide edges. The copper halide connection m otif o f the polymeric com pound has some features in com m on with the "stair" and "cube" structures o f adducts o f Cul with unidentate, neutral P-, As-or N-bases. The com pound (bp2)C u2I3 (m onoclinic, P 2 ,/«, a = 1054.0(2), b = 1034.8(3), c = 1512.6(3) pm, ß = 108.10(2)°, Z = 2) has a structure, in which two edge-sharing (C ul4,2)-tetra-hedra and two approximately planar (C u l2/2(bp2))-units form tetranuclear molecules (bp2)2Cu4I6. These are linked to chains with a "stair" m otif by intermolecular Cu • • • I contacts. 
  Reference    Z. Naturforsch. 46b, 738—7 (1991); eingegangen am 16. N ovem ber 1990 
  Published    1991 
  Keywords    Iodocuprates(I), Cationic Ligands, Crystal Structure 
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 Identifier    ZNB-1991-46b-0738 
 Volume    46 
7Author    K.-J Range, U. Klement, G. Döll, E. Bucher, J. R. BaumannRequires cookie*
 Title    The Crystal Structure of MnIn2Se4, a Ternary Layered Semiconductor  
 Abstract    Single crystals o f M nIn2Se4 have been grown by the chemical vapour phase transport technique using A1C13 as the transporting agent. The struc­ ture was refined to R = 0.064, Rn = 0.059 for 609 reflections. MnIn-,Se4 (R 3 m , hexagonal axes 
  Reference    Z. Naturforsch. 46b, 1122—1124 (1991); received February 21 1991 
  Published    1991 
  Keywords    M anganese Diindium Tetraselenide, Layered Semiconductor, Crystal Structure 
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 Identifier    ZNB-1991-46b-1122_n 
 Volume    46 
8Author    Rüdiger Staffel, Ulrich Müller, Andreas Ahle, K. Urt DehnickeRequires cookie*
 Title    Die Kristallstruktur von [Na(12-Krone-4)2+l2Se82 * (Se6, Se7) The Crystal Structure o f [Na(12-Crown-4)2+]2Se82 -(Se6, Se7)  
 Abstract    The title com pound was prepared from sodium polyselenide and 12-crown-4 in D M F solution in the presence o f cerium(IlI)chloride in the form o f black needles. The crystal structure determination by X-ray diffraction shows a partially disordered structure, in which the anionic units Se82-■ Se7 and Se82- • Se6 are present in the ratio 0.72/0.28. These units are as­ sociated to layers parallel to (1 0 0); the layers alternate with pseudohexagonal layers o f [N a(12-crown-4)2]+ ions. Space group P i, Z = 2, 3903 observed unique reflections, R = 0.114, w R = 0.084. Lattice dim ensions at -6 5 °C: a = 1247.9(3), b = 1367.8(8), c = 1660(1) pm, a = 94.65(5), ß = 98.94(3), y = 91.10(3)°. 
  Reference    Z. Naturforsch. 46b, 1287—1292 (1991); eingegangen am 8. April 1991 
  Published    1991 
  Keywords    Octaselenide, Cycloheptaselenium, Cyclohexaselenium, Synthesis, Crystal Structure 
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 Identifier    ZNB-1991-46b-1287 
 Volume    46 
9Author    Stefan Vogler, W. Erner Massa, Kurt DehnickeRequires cookie*
 Title    Über die Reaktion von Wolframhexachlorid mit Se4N 2; Kristallstruktur von PPh4|W Cl5(NSeCl)| On the Reaction of Tungsten Hexachloride with Se4N 2; Crystal Structure of PPh4[WCl5(NSeCl)]  
 Abstract    The reaction of tungsten hexachloride with Se4N2 leads to [WCl4(NSeCl)]2, which reacts with pyridine to form [WCl4(NSeCl)Py], and with tetraphenylphosphonium chloride to form PPh4[WCl5(NSeCl)]. which was characterized by an X-ray structure determination. Space group P 2j, Z = 2, 1657 observed unique reflections, R = 0.074, wR = 0.061. Lattice dimen­ sions at -8 0 C: a = 710.7(1), b = 2217.9(4), c = 953.6(2) pm; ß = 111.93(3) . The [WC15(NScC1)] ion possesses an almost linear WNSe group with bond lengths WN = 188 pm, corresponding to a double bond, and NSe = 200 pm. 
  Reference    Z. Naturforsch. 46b, 1625—1628 (1991); eingegangen am 29. Mai 1991 
  Published    1991 
  Keywords    Chloroselenonitrene Complexes of Tungsten, Synthesis, Crystal Structure 
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 Identifier    ZNB-1991-46b-1625 
 Volume    46 
10Author    Ulrich Bierbach, Wolfgang Saak, Detlev Haase, Siegfried PohlRequires cookie*
 Title    Neutrale und kationische Eisen-Schwefel-Komplexe und -Cluster  
 Abstract    Synthese und Kristallstrukturen von [Fe(SR)2L2l * PhMe und [Fe4S4(SR)2 L2| sowie zur Bildung von [Fe(SR)L3]+, [FeL4]2+, [Fe4S4(SR)L3| + und [Fe4S4L4|2+ (R = 2,4,6-/-Pr3C6H 2; L = SC (N M e2)2) Neutral and Cationic Iron-Sulfur Complexes and Clusters Syntheses and Crystal Structures of [Fe(SR)2 L2] • PhM e and [Fe4S4(SR)2 L2], and on the Form ation of [Fe(SR)L3]+, [FeL4]2+. [Fe4S4(SR)L3]+ and [Fe4S4 L4]2+ (R = 2,4,6-/-Pr3C6H 2; L = SC(NM e2)2) The reaction of [FeLL,] (1; L = SC(NMe,),) with KSR (R = 2,4,6-/-Pr3C6H-,) yields [Fe(SR)2L2] • PhMe (2). 
  Reference    Z. Naturforsch. 46b, 1629—1634 (1991); eingegangen am 13. Juni 1991 
  Published    1991 
  Keywords    Iron Sulfur Complexes and Clusters, Synthesis, Crystal Structure 
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 Identifier    ZNB-1991-46b-1629 
 Volume    46 
11Author    Dietrich Mootz, Klemens BartmRequires cookie*
 Title    Zur Kristallchemie von Supersäuren: Bildung und Struktur der tiefschmelzenden Addukte SbF5 * CF3S 0 3H und SbF5 * 7 HF [ 1 ] Crystal Chemistry o f Superaeids: Form ation and Structure of the Low-Melting Adducts SbF5 * C F 3 S 0 3H and S bF s-7 H F [l]  
 Abstract    The melting diagram of the superacid system SbFs-C F 3SO,H as well as of SbF5-H F has 
  Reference    Z. Naturforsch. 46b, 1659—1663 (1991); eingegangen am 15. Mai 1991 
  Published    1991 
  Keywords    Superaeids, Melting Diagrams, Crystal Structure, Fluoronium Ion 
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 Identifier    ZNB-1991-46b-1659 
 Volume    46 
12Author    Z. NaturforschRequires cookie*
 Title    Oxidative Addition von Tetramethyldiphosphan und -arsan an C p '-S iM e2-Cp'-überbrückte Molybdän-und Wolframcarbonyl-Komplexe*  
 Abstract    O xidative A d d itio n o f T etram ethyldiphosphane and -arsane to Binuclear C p '-S iM e 2 -C p '-B rid g e d M olybdenum and T ungsten C arbonyl Com plexes** W alter A b riel+,a, G e rh a rd B aum +b, H eike B urdorf*5 und Jürgen Heck*-C a AW H chem consult, Thermal reaction o f M e2Si[Cp'M(CO)3]2 (M = M o, W; Cp' = C5H 4) with tetramethyldi­ phosphane and -diarsane gives oxidative coupling products with bridging EM e2-groups (E = P, As). With E = P discrete binuclear com pounds are obtained, which on further thermolysis afford new species o f the general formula {M e2Si(Cp'M)2(CO)3(J w-PMe2)2} (5). X -R ay struc­ ture determ ination o f 5a (M = M o) and N M R data show a PM P-heteroallylic system which is bound to the second metal. In the case o f M = W a second com pound with a mixed hydrido and dim ethylphosphido bridge can be isolated, which shows fluxionality in solution. However, the oxidative additions with tetramethyldiarsane lead to insoluble products which are assumed to be polymeric with C p '-S iM e2-C p ' as well as A sM e2 bridges linking the metal centers. 
  Reference    Z. Naturforsch. 46b, 841—8 (1991); eingegangen am 28. N ovem ber 1990 
  Published    1991 
  Keywords    Oxidative A ddition, Tetramethyldiphosphane, Tetramethyldiarsane, Crystal Structure, Fluxional Behaviour 
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 Identifier    ZNB-1991-46b-0841 
 Volume    46 
13Author    Dieter Fenske, Sylvia Magull, K. Urt DehnickeRequires cookie*
 Title    Synthese und Kristallstruktur von |Rb(18-Krone-6)|2IZn(Se4)(Se6)l Synthesis and Crystal Structure o f [Rb(18-Crown-6)]2[Zn(Se4)(Se6)]  
 Abstract    [Rb(18-crown-6)]-,[Zn(Se4)(Se6)] has been prepared by the reaction o f a lithium polyselenide solution in D M F with zinc acetate in the presence o f rubidium iodide and 18-crown-6. It forms dark red crystals, which were characterized by FIR spectroscopy as well as by an X-ray struc­ ture determination. Space group C 2/c, Z = 4, 3012 observed unique reflections, R = 0.073. Lattice dim ensions at —50 °C: a = 1963.1(14), b = 1125.9(9), c = 2060.3(16) pm,/? = 90.05(3) . The com pound has a com plex ionic structure, in which the zinc atom o f the anion [Zn(Se4)(Se6)]2" is coordinated tetrahedrally by four selenium atoms o f a Se42~ and a Se62~ unit in five and seven membered rings, respectively. The complex cations [Rb(18-crown-6)]+ have Rb • ■ • Se contacts o f 360.7 and 372.0 pm with selenium atoms o f the ZnSe4-ring. 
  Reference    Z. Naturforsch. 46b, 1011—1014 (1991); eingegangen am 6. Februar 1991 
  Published    1991 
  Keywords    Polyselenide Complex o f Zinc, Synthesis, IR Spectrum, Crystal Structure 
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 Identifier    ZNB-1991-46b-1011 
 Volume    46 
14Author    J. Skowronek, W. Preetz, S. M. JessenRequires cookie*
 Title    Darstellung, Schwingungsspektren und Normalkoordinatenanalyse der Acetatochloroditechnetate(III)  
 Abstract    , cis-T ^ C ^ C C F ^ C ^ I^ (L = axiale Donorbase) sowie Kristallstruktur von a s-T c2(0 2CCH3)2Cl4((CH3)2NC0CH3)2 Preparation, Vibrational Spectra and Norm al C oordinate Analysis o f Acetatochloroditechnetates(III), c« -T c2(0 2C CH 3)2C14L2 (L = Axial Donorbase) and the Crystal Structure of ds-Tc2(0 2C CH 3)2Cl4((CFI3)2N C 0C FI3)2 Tc2(0 2C C H 3),C l4(H 20)2 has been prepared by reaction o f [Tc2C18]2" with acetic anhydride and fluoroboric acid. By treatment with the donor bases L = N ,N-dim ethylform am ide (D M F), N ,N-dim ethylacetam ide (D M A A), dimethylsulfoxide (D M SO), triphenylphosphin-oxide (TPO) and pyridine (Py), the green adducts Tc2(0 2CCH3)2Cl4L2 are formed. The structure o f T c,(O .C C H 3),C l4(D M A A), was determined by X-ray diffraction; space group C 2/c with a = 29.604(4), b = 10.895(2), c = 14.404(2) Ä, ß = 97.87(2)°, Z = 8, /?w = 2.7% . The T c -T c distance is 2.1835(7) Ä , the bridging acetate groups are in c/s-positions. The IR and Raman spectra have been recorded at 80 K and assigned according to point group C-,v, supported by a normal coordinate analysis o f Tc2(0 2C C H 3)2C14(D M A A)2 based on a general valence force field. The stretching interaction constant fd(TcTc) is determined to 3.38 m dyn/Ä. With in­ creasing donor strength o f the axial ligands, the intense Raman vibration v(TcTc), showing up to three overtones, is lowered from 311 to 282 cm *1. The <5-<5* transitions o f all adducts are observed at 6 4 8 -6 5 2 nm. 
  Reference    Z. Naturforsch. 46b, 1305—1314 (1991); eingegangen am 4. März 1991 
  Published    1991 
  Keywords    Diacetatotetrachloroditechnetate(III) Adducts, Synthesis, Crystal Structure, Vibrational Spectra, Normal Coordinate Analysis 
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 Identifier    ZNB-1991-46b-1305 
 Volume    46 
15Author    R.Alf Fuchs, Peter KlüfersRequires cookie*
 Title    Heteronukleare Komplexverbindungen mit M etall-M etall-Bindungen, V [1]  
 Abstract    Umsetzungen mit [(NH3)2CuCo(CO)4l: Synthese und Struktur von |(PPh3)2CuCo(CO)4|, [Cu{P(OM e)3}4][Cu{Co(CO)4}2] und (Ph3P)2N |C u{C o(C O)4}2] H eteronuclear C o-ordination Com pounds with M e ta l-Metal-Bonds, V [1] Reactions with [(NH3)2CuCo(CO)4]: Synthesis and Structure of [(PPh3)2CuCo(CO)4], [Cu{ P(OM e)3}4][Cu{Co(CO)4}2] and (Ph3P)2N[Cu{Co(CO)4}2] The heteronuclear carbonyl complex [(NH3)2CuCo(CO)4] 1 reacts with the phosphane li­ gands PPh3, PEt3 and P(OMe)3. A dinuclear complex, [(PPh3)2CuCo(CO)4] 2, is formed with PPh3, while trinuclear anionic [Cu{Co(CO)4}2]~ species are formed with the other phosphane ligands. The crystal structure of 2 (C u-C o = 255.2(2) pm) and the structures of two com­ pounds with trinuclear anions, [Cu{P(OMe)3}4][Cu{Co(CO)4}^] 3 (C u-C o = 232.64(8) and 233.10(8) pm) and PPN[Cu{Co(CO)4}2] 6 (C u-C o = 238.1(l)"and 234.3(1) pm), have been determined by X-ray crystallography. The angle Cax-C o -C eq of tetracarbonyl cobalt com­ pounds (i.e. the deviation from tetrahedral geometry) depends on the charge of the Co(CO)4 fragment, as calculated with the electronegativity equalization scheme of Bratsch (J. Chem. Ed. 61, 588 (1984)). 
  Reference    Z. Naturforsch. 46b, 507—518 (1991); eingegangen am 18. September 1990 
  Published    1991 
  Keywords    Cobalt Carbonyl Complexes, Bi-and Trinuclear Copper Cobalt Compounds, Phosphorus Ligands, Crystal Structure, Electronegativity Equalization 
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 Identifier    ZNB-1991-46b-0507 
 Volume    46 
16Author    Pilar Souza, Luisa Sanz, Vicente Fernández, Agueda Arquero, Enrique Gutierrez, AngelesM. OngeRequires cookie*
 Title    Complexes of Zn, Cd and Hg Halides with S and N Polydentate Schiff-Base. Metal Template Effect in the Synthesis o f Analogous Oxygenated Base. Crystal Structure of [Zn(btsc)2Cl2l and [Cd(btsc)2Br2] M ontegancedo s/n, E-28660-Boadilla del M onte (Madrid), Spain  
 Abstract    Zinc, cadmiun and mercury dihalide react with 4-acetylpyridinthiosemicarbazone (4-aptsc) to give complexes with 1:1 and 2:1 ligand/m etal stoichiom etric ratios. These metals are effec­ tive templates for the Schiff-base condensation o f 4-acetylpyridine with semicarbazide to give the complexes [M (4-apsc)XJ and [M (4-apsc)2X 2] where M = Zn, Cd or Hg and X = Cl, Br or I. These com pounds were characterized by elemental analyses, conductivities measurements, IR and l3C, 'H N M R spectra. The zinc chloride and bromide com plexes o f benzalthiosem icarbazone (btsc) have been pre­ pared and characterized by X-ray measurements. The com pounds Zn(btsc)2Cl2 and Cd(btsc)2Br2 are isostructural and crystallize in the space group P 2j/«. The crystal structure o f the chlorine derivative has been resolved by single-crystal X-ray diffraction. The zinc centre is in a slightly distorted tetrahedral environment. There are intra and intermolecular hydrogen bonds. 
  Reference    Z. Naturforsch. 46b, 767 (1991); received June 27/O ctob er 22 1990 
  Published    1991 
  Keywords    4-Acetylpyridinthiosemicarbazone, 4-Acetylpyridinsemicarbazone, Benzalthiosemicarbazone, II-b-Metal Complexes, Crystal Structure, X -Ray 
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 Identifier    ZNB-1991-46b-0767 
 Volume    46 
17Author    J. Thesing, J. Baurmeister, W. Preetz, D. Thiery, H. G. Von SchneringRequires cookie*
 Title    Kristallstrukturen  
 Abstract    von [P(C6H 5)4 l2 lB6Cl6](CH3CN) 2 und |P(C 6H 5)4]2 lB6Br6](CH3CN) 2 sowie Schwingungsspektren und Normalkoordinatenanalyse der isotopomeren c/osö-Hexahalogenohexaborate |"B",#B6-Ä I 2' , X = Cl, Br; n = 0 -6 Crystal Structures o f [P(C6H 5)4]2[B6C16](C H ,C N)2 and [P(C6H s)4]2[B6Br6](CH3CN)2, Vibrational Spectra and Norm al C oordinate Analysis of Isotopomeric cVavo-Hexahalogenohexaborates [n B"10B6_/?X6]2", X = Cl, Br; n = 0 -6 The crystal structures o f (TPP)2[B6C16](CH3CN)2 and (TPP)2[B6Br6](CH3CN)2 were deter­ mined from single crystal X-ray diffraction analyses at 147 K. They are triclinic, space group P I, and contain nearly regular octahedral anions with bond lengths d (B -B) 1.716, d (B -C l) 1.818 for [B6C16]2" and d (B -B) 1.684, d (B -B r) 1.993 A for [B6Br6]2~. Using these molecular data, norm al coordinate analyses for the ten isotopomers [n Bnl0B6_nX6]2", n = 0 -6 , X = Cl, Br, including the pairs of geometric isomers for n = 2, 3, 4 have been performed, based on a general valence force field. W ith a set of 8 force constants for Cs2[B6Br6] (e.g. fd(BB) = 1.39, fd(BBr) = 3.18 mdyn/Ä) and 10 for Cs2[B6Cl6] (e.g. fd(BB) = 1.30, fd(BCl) = 4.01 mdyn/Ä) the calculated frequencies are in good agreement with observed IR (10 K) and Raman bands (80 K) in natural abundance as well as for "B-and l0B-enriched derivatives. For the series [B6X6]2", X = Cl, Br, I the correlation of decreasing bond lengths d(B -B) and increasing force constants fd(BB) along with vibrational coupling between the B6 cage and the substituent sphere is discussed. 
  Reference    Z. Naturforsch. 46b, 800—808 (1991); eingegangen am 6. Dezember 1990 
  Published    1991 
  Keywords    H exachlorohexaborate(2-), H exabrom ohexaborate(2-), Crystal Structure, Normal Coordinate Analysis, Isotopomers 
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 Identifier    ZNB-1991-46b-0800 
 Volume    46 
18Author    Bernt Krebs, Stefan Bonmann, Klemens ErpensteinRequires cookie*
 Title    Synthese, Struktur und Eigenschaften der Hexabromoteilur(I V)-und Tridekabromotritellur(IV)säure-Hydrate. Kristallstrukturen der Oxonium-Salze |H 90 4]2ITeBr6l und IH904l[Te3Br13] Synthesis, Structure and Properties of Hexabromotellurous and Tridecabrom otritellurous Acid Hydrates. Crystal Structures of the Oxonium Salts [H90 4 ]2[TeBr6] and [H90 4 ][Te3 Br13]  
 Abstract    From solutions o f TeBr4 in concentrated aqueous HBr red needles o f the crystalline hexa­ bromotellurous acid with the stoichiometric com position H,TeBr6 -8H -,0 (1) were isolated (space group P 2 Jn, a = 7.662(5), b = 9.796(6), c = 11.987(8) A, ß = 91 ,35'(4)° at 259 K). If the H B r: TeBr4 concentration ratio in the system TeBr4/H B r/H 20 was kept low, a novel acid with formal com position H T ejB r^ ^ H iO (2) could be prepared (space group Cm, a = 13.501(5), b = 15.453(6), c = 9.153(3) A, ß = 138.11(2) at 140 K). The X-ray structural analysis o f 1 shows the acid to contain, besides regular octahedral [TeBrJ2-ions (T e-B r: 2 .6 7 1 (4)-2.716(4) Ä), [H90 4]+ hydroxonium ions (O -O : 2 .48 (3)-2 .6 2 (3) Ä). The [H90 4]+ units are linked through a hydrogen bond system (O -O : 2 .8 0 (3)-2 .9 7 (4) Ä) to form a three-dimen­ sional network. The formula has to be written as [H90 4]2[TeBr6 ]. 2 is the first acid in this class with a trinuclear anion. Its structural formula is [H90 4][Te3 Br13]. A s a fragment o f the Te4 Br16 cube the anion consists o f three edge-sharing octahedra with a central triply bridging Br; The mean bond distances are 2.515 Ä for terminal T e -B r , 2.944 Ä for T e -^ 2Br and 3.077 Ä for T e -/ / 3 Br. The 0 -0 distances in the isolated [H90 4]+ hydroxonium ions are 2 .4 5 (3)-2.57(2) A. Raman spectra o f both acids are reported. 
  Reference    Z. Naturforsch. 46b, 919 (1991); eingegangen am 16. N ovem ber 1990 
  Published    1991 
  Keywords    H exabrom otellurous Acid, Tridecabromotritellurous Acid, Chalcogen Halogen C om pounds, Crystal Structure, Hydroxonium Compounds 
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 Identifier    ZNB-1991-46b-0919 
 Volume    46 
19Author    Fluoro, Petra Neumann, K. Urt Dehnicke, Dieter Fenske, G.Erhard BaumRequires cookie*
 Title    Fluoro-, Chloro-und Bromo-Wolfram(VI)-Alkinkomplexe. Die Kristallstrukturen von [K(18-Krone-6)l[WF5( P h -C = C -H ) | * CH3CN und | WCl4( P h -C = C -S e -/ i -C 4H 9)(C H 3CN)|  
 Abstract    -, Chloro-, and Bromo-Tungsten(VI) Alkyne Complexes. The Crystal Structures of [K(18-Crown-6)][WF5(P h ~ C = C -H)] • C H 3CN and [WCl4(P h -C = C -S e -w -C 4 H9)(CH 3CN)] Several tungsten alkyne complexes o f the type [WC14(R -C = C -H) ] 2 and [WC14(R -C = C -R') ] 2 have been prepared by reactions o f WC16 with the alkynes in the presence o f C2C14. Treat­ ing with BrSiMe3 leads to corresponding bromo com plexes, whereas reactions o f N aF and KF, respectively, in acetonitrile solution in the presence o f crown ethers yield the fluoro complexes [N a(l 5-crown-5)][WFs(R -C = C -R ') ] and [K(18-crown-6)][W F5(R -C = C -R ') ] , respectively. All complexes were characterized by IR and l3C N M R spectroscopy. The crystal structures o f [K(18-crown-6)][W F5(P h -C = C -H) ] C H 3CN and [WCl4(P h -C = C -S e -« -C 4 H9)(C H 3C N)] have been determined by X-ray methods. [K(18-crown-6)][W F5(P h -C = C -H ] C H 3 CN: Space group P 2,, Z = 2, 8555 observed unique reflections, R = 0.034. Lattice dim ensions at -7 0 °C: a = 1199.4(3), b = 893.4(2), c = 1351.8(3) pm, ß = 109.73(3)°. The com pound forms ion pairs via three K -F contacts with bond lengths o f 262.0, 282.7, and 293.3 pm; the potassium ion is thus nine-fold coordinated by the six oxygen atoms o f the crown ether molecule and by three fluoride ligands. The alkyne ligand is bonded side on to the tungsten atom o f the [W F5(P h -C = C —H)] unit with WC bond lengths o f 202.4 and 202.6 pm, respectively. [WCl4(P h -C = C -S e -t t -C 4 H9)(C H 3C N)]: Space group P 2 Ja, Z = 4, 4595 observed unique reflections, R = 0.058. Lattice dim ensions at -7 0 °C: a = 1030.3(5), b = 1596.3(9), c = 1170.9(7) pm, ß = 104.28(3)°. The com pound has a molecular structure, in which the tungsten atom is seven-fold coordinated by four chloride ligands, by the two alkyne carbon atom s (WC bond lengths 200 and 203 pm), and in trans position to the latter by the nitrogen atom o f the acetonitrile molecule with a W -N bond length o f 226 pm. 
  Reference    Z. Naturforsch. 46b, 999—1010 (1991); eingegangen am 4. Februar 1991 
  Published    1991 
  Keywords    Tungsten Alkyne Complexes, Synthesis, IR Spectra, 13C N M R Spectra, Crystal Structure 
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 Identifier    ZNB-1991-46b-0999 
 Volume    46 
20Author    EnriqueG. Utiérrez-PueblaRequires cookie*
 Title      
  Reference    Z. Naturforsch. 46b, 1113 (1991); eingegangen am 9. Januar 1991 
  Published    1991 
  Keywords    Hexachlorodicuprates, Tetrachlorocuprates, 3-D iethylam ino-5-phenyl-1, 2, 4-dithiazolium Salts, Synthesis, Crystal Structure 
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 Volume    46 
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