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  • 1995-1999  (325)
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  • 1996  (167)
  • 1995  (158)
  • crystal structure
  • 1
    Electronic Resource
    Electronic Resource
    Structure of 1-(2′-tosyloxyethoxy)-8-tosyloxy-9,10-anthraquinone (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 677-681 
    Details
    ISSN: 1572-8854
    Keywords: Anthraquinone ; crystal structure ; intramolecular hindrance
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The title compound crystallizes in the monoclinic space group, P21/c;a=12.938(1),b=11.041(1),c=19.285(2) Å, β=104.314(8)°,Z=4. Refinement based on 1660 unique observed reflections converged toR=0.054. The anthraquinone moiety is distorted due to intramolecular steric hindrance from the tosylate groups.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01991963
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  • 2
    Electronic Resource
    Electronic Resource
    Synthesis and crystal structure of a dinuclear organometallic phosphonium ylid complex, [(η5-C5H5(CO)C2(ε-CO)(ε-CHP(C6H5)3)+][PF – 6 ] (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 683-690 
    Details
    ISSN: 1572-8854
    Keywords: Organoiron complex ; dinuclear complex ; crystal structure ; phosphonium ylid
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The title compound crystallizes in the centrosymmetric monoclinic space group P21/n withZ=4. The cation consists of two (η5-C5h5)Fe(CO) units which are linked via a metal-metal bond (Fe(1)−Fe(2)=2.530(1) Å), a bridging carbonyl ligand (Fe(1)−C(4)=1.912(8) Å. Fe(2)−C(4)=1.940(9) Å) and a bridging phosphonium ylid ligand (Fe(1)−C(1)=1.991(6) Å, Fe(2)−C(1)=1.985(6) Å and C(1)−P(1)=1.781(6) Å).
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01991964
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  • 3
    Electronic Resource
    Electronic Resource
    Crystal and molecular structure of [(C6H5)2P(=0)(CH2CH2N(CH3)3 +][I−] (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 747-752 
    Details
    ISSN: 1572-8854
    Keywords: Phosphine oxide ; quaternary ammonium ; water-soluble phosphine ; crystal structure ; hydrogen bonding
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The title compound crystallizes in the centrosymmetric triclinic space group $$P\bar 1$$ withZ=4. The crystallographic asymmetric unit contains two independent cations; interatomic distances within these include P=O=1.47(1) and 1.47(1) Å, P−C6H5=1.78(2)–1.81(1)Å and P−CH2CH2NMe3 +=1.80(1) and 1.81(1) Å. The phosphine oxide moiety is involved in intermolecular hydrogen bonding ()...H−C, with O...H≥2.42Å) and the iodide is involved in I...H−C contacts with I...H≥3.10Å.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01664651
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  • 4
    Electronic Resource
    Electronic Resource
    Solid-state formation of an inclusion compound of cholic acid withp-toluidine (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 185-189 
    Details
    ISSN: 1572-8854
    Keywords: Solid-solid reaction ; inclusion compound ; p-toluidine ; cholic acid ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Cholic acid undergoes solid-solid reactions with some aromatic molecules to form inclusion compounds. Simple shaking of a mixture of powdered cholic acid andp-toluidine results in formation of the 1∶1 (host:guest) inclusion compound which has the same structure as that formed by conventional crystallization methods: monoclinic space groupP21 witha=13.577(4),b=8.078(2),c=14.182(6) Å, β=114.42(3)°,Z=2 andR 1=0.061 for 2680 unique reflections.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01673668
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  • 5
    Electronic Resource
    Electronic Resource
    Synthesis ofcis-[Ru{4,4′-(t-Bu)2bpy}2(PPh3)Cl+][ClO 4 − ] and the crystal structure of its disordered hemiacetonitrile, hemitoluene solvate (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 267-275 
    Details
    ISSN: 1572-8854
    Keywords: Ruthenium(II) complex ; disordered structure ; crystal structure ; solvate ; triphenylphosphine ; bipyridyl
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The complexcis-[Ru{4,4′-(t-Bu)2bpy}2(PPh3)Cl+][ClO 4 − ·0.5(toluene)·0.5(MeCN), where 4,4′-(t-Bu)2bpy=4,4′-di(t-butyl)-2,2′-bipyridyl crystallizes with an ordered racemic mixture of the chiral cations in the centrosymmetric triclinic space group $$P\bar 1$$ (No. 2). The structure was refined toR=4.42% for those 6426 reflections with 20=5–50o and |F o|〉6σ(F). Ruthenium ligand distances are Ru−Cl=2.423(2)Å, Ru−PPh3=2.346(2)Å and Ru−N=2.056(4)–2.098(4)Å. Both the Ru(II)-containing cation and the perchlorate anion are ordered, but the toluene and acetonitrile exhibit an interesting type of scrambled disorder about the inversion center atx=1,y=1/2,z=0.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01677780
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  • 6
    Electronic Resource
    Electronic Resource
    Reactions of the dirhenium(II) complexes Re2X4(dppm)2 (X= Cl, Br; dppm = Ph2PCH2PPh2) with isocyanides. Part IX. New isomeric forms of the mixed carbonyl-isocyanide dirhenium(II) Complexes Re2 Cl4(dppm)2(CO)(CNxyl) and [Re2Cl3(dppm)2(CO)(CNxyl)2]O3SCF3 The X-ray crystal structure of [(xyl NC)2ClRe(μ-dppm)2ReCl2(CO)] O3SCF3 (1996)
    Springer
    Journal of cluster science 7 (1996), S. 155-166 
    Details
    ISSN: 1572-8862
    Keywords: Rhenium ; dirhenium complexes ; rhenium-rhenium multiple bonds ; isocyanide ligands ; carbonyl ligand ; structural isomers ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract The monocarbonyl complex Re2Cl4(µ-dppm)2(CO) reacts with xylyl isocyanide in acetonitrile to afford the bioctahedral complex (CO)Cl2Re(µ-dppm)2 ReCl2(CNxyl), 2b. This is a different structural isomer from the edge-sharing bioctahedral complex Cl2Re(µ-Cl)(µ-dppm)2ReCl(CNxyl) or this same stoichiometry which A formed when acetone is be reaction solvent. The complex2b reacts with a further equivalent of xylNC in the presence of TlO3SCF3 in dichloromethane to form a red complex of composition [Re2Cl3(µ-dppm)2 (CO)(CNxyl)2]O3SCF3. 3, which has the open bioctahedral structure [(xylNC)2ClRe(µ-dppm)2ReCl2(CO)]O3SCF3. This is a third isomeric form of this dirhenium cation: the previously isolated green and yellow forms have edge-sharing bioctahedral structures. Crystal data for3 at 295 K: orthorhombic space group Pbca (No. 61) witha=22.654(5) Å,b=22.717(4) Å,c=27.324(4) A,V= 14061(7) Å3, andZ = 8. The structure was refined to R = 0.059 (R, = 0.134 ) for 14164 data. The Re-Re distance is 2.3833(8) Å.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01166054
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  • 7
    Electronic Resource
    Electronic Resource
    A hydrogen-bonded dichloromethane-perchlorate-water channel in the crystal structure ofcis-[Ru(bpy)2{PPh-(o-tolyl)2}Cl+][ClO4 −]·CH2Cl2·H2O (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 67-73 
    Details
    ISSN: 1572-8854
    Keywords: Ruthenium(II) ; bipyridyl ; phenyldi(o-tolyl)phosphine ; solvate ; hydrogen bonding ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The complexcis-[Ru(bpy)2{PPh(o-tolyl)2}Cl+][ClO4 −] crystallized from a solution in dichloromethane as the dichloromethane-water solvate. The structure was refined toR=4.5% for those 2433 reflections with |F o|〉6σ(|F o|). The octahedral Ru(II) cation is associated with metal-ligand distances as follows: Ru−Cl=2.434(3)Å, Ru-PPh(o-tol)2=2.382(2)Å, and Ru−N=2.037(7)–2.088(7)Å. The structure is stabilized by a hydrogen-bonded CH2Cl2...ClO4 −...H2O channel which incorporates adventitious water of crystallization.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF02018700
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  • 8
    Electronic Resource
    Electronic Resource
    The molecular structure of [bis-triphenylphosphine-silver(I) stearate], [((C6H5)3P)2Ag(O2C(CH2)16CH3)], solubilization of long alkyl chain silver carboxylates (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 99-105 
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    ISSN: 1572-8854
    Keywords: Silver ; stearate ; triphenylphosphine ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal and molecular structure of [bis-triphenylphosphine-silver(I) stearate], [((C6H5)3P)2Ag(O2C(CH2)16CH3)], has been determined by single crystal X-ray analysis: the space group is PT witha=12.021(4),b=13.916(5)1,c=14.678(5) Å, α=95.952(5), β=101.249(6), γ=93.259(5)°,V=2388(2) Å3, andD calc=1.293 g/cm3 forZ=2. The silver is four coordinate: the carboxylate symmetrically chelates the silver while the triphenylphosphine ligands occupy the third and fourth coordination sites. The strong bonding nature of the phosphine ligands, as indicated by the Ag−P bond lengths, 2.446(3) and 2.424(3) Å, dominates the coordination sphere of the silver and forces the initial carboxylate ligand to rearrange from bridging to chelating resulting in weaker Ag−O bonds, as indicated by the extended Ag−O bond lengths, 2.399(8) and 2.449(8) Å. Unlike the free acid, the long hydrocarbon chain is not linear, and exhibits disorder in the lattice. The structure of the title complex explains the dramatic shift in solubility properties compared to the starting phosphine free silver carboxylate.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01669724
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  • 9
    Electronic Resource
    Electronic Resource
    Crystal structure of the methanol solvate of (η5-cyclopentadienyl)[1,2-bis(diphenylphosphino)ethane] nitroruthunium(II) Ru(η5-C5H5)dppe)(NO2)·CH3OH (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 489-495 
    Details
    ISSN: 1572-8854
    Keywords: Ruthenium(II) complex ; organoruthenium compound ; bis(1,2-diphenylphosphino)ethane ligand ; ruthenium-nitro complex ; crystal structure ; cyclopentadienyl derivative ; methanol solvate
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The title complex crystallizes in the centrosymmetric monoclinic space group C2/c (No. 15) withZ=8. The structure was refined toR=4.49% for those 2745 independent reflections with 2θ=5–50o and |F σ|〉6σ(F). Ruthenium-ligand distances are as follows: Ru-P=2.284(2) and 2.286(2) Å, Ru-NO2=2.049(6) Å and Ru-C(Cp)=2.210(10)-2.246(9) Å. Bond lengths within the nitro ligand are N(1)-O(1)=1.226(10) Å and N(1)-O(2)=1.244(10) Å. The methanol of solvation is ordered but is subject to large thermal vibrational motions.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01668310
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  • 10
    Electronic Resource
    Electronic Resource
    Crystal structure and molecular dynamics simulation of tri-o-thymotide clathrates with thiophene as guest molecule (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 461-465 
    Details
    ISSN: 1572-8854
    Keywords: Molecular dynamics ; crystal structure ; TOT clathrate ; thiophene
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Tri-o-thymotide (TOT) forms a cage-type clathrate with the thiophene guest molecule in a host:guest ratio of 2∶1. This clathrate crystallizes in the trigonal system (space groupP3121). The unit cell, of dimensionsa=b=13.585(4),c=29.914(12)Å, contains 6 TOT and one thiophene molecule. The crystal structure, established by direct methods (R=0.053), indicates that the host cavity has an oblate-ellipsoid shape with a crystallographic twofold axis parallel to the largest dimension of the cage. The guest molecule within the cavity is disordered. Molecular dynamics simulations have been performed and indicate that the guest molecules have hindered molecular freedom around the shortest ellipsoid axis of the cavity, and may produce a dynamic disorder in the cage of the TOT clathrate.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01668305
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  • 11
    Electronic Resource
    Electronic Resource
    Crystal structure ofmer,trans-[Ru(NO2)(trpy)(PPr3) 2 + ][ClO 4 − ], a species with disordered PPr3 and NO2 ligands (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 543-551 
    Details
    ISSN: 1572-8854
    Keywords: Ruthenium(II) complex ; tri-n-propylphosphine ; terpyridine ; ruthenium-nitro complex ; crystal structure ; disordered ligands
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The complexmer,trans-[Ru(NO2)(trpy)(PPr3) 2 + ][ClO 4 − ]crystallizes in the centrosymmetric orthorhombic space group Pnma withZ=4. Both the ruthenium(II) cation and the perchlorate ligand lie about crystallographic mirror planes. The nitro ligand is not coplanar with the Ru(trpy) moiety and suffers from two fold disorder about its Ru−N bond such that the two sets of oxygen atoms have symmetry-related sites above or below the crystallographic mirror plane. The n-propyl groups within the PPr3 ligands suffer from disorder of their C(α) and C(β) atoms but share common C(γ) sites. Ruthenium-ligand distances are: Ru−PPr3=2.398(2)Å, Ru−NO2=2.053(7) Å, Ru−N(trpy, outer)=2.078(6) and 2.092(6) Å and Ru−N(trpy, central) =1.965(6) Å.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01668413
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  • 12
    Electronic Resource
    Electronic Resource
    Structures of 355-1355-1355-1tricarbonyl: structural evidence for the near-electroneutrality of the dialkylacetal substituent (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 355-360 
    Details
    ISSN: 1572-8854
    Keywords: Chromium ; carbonyl ; arene ; acetal ; crystal structure ; conformation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The structures of the (benzene dialkylacetal)tricarbonyl chromium complexes [η6-C6H5-CH(OR)2]Cr(CO)6 (R=Me,1; Et,2), are reported. The compounds were examined as part of a study of the conformations of the tripodal tricarbonylchromium group. For [η6-C6H5-CH(OMe)2]Cr(CO)3,1, monoclinic,P21/c (# 14),a=15.235(1) Å,b=6.5304(5) Å,c=12.702 Å, β=103.197(1)o,Z=4. For [η6-C6H5-CH(OEt)2]Cr(CO)3,2, monoclinic,P21/c (# 14),a=9.859(3) Å,b=10.547(3) Å,c=15.138(3) Å, β=108.42(2)o,Z=4. The data show that the molecules adopt the expected “three-legged piano stool” structure. The carbonyl ligands in1 adopt an eclipsed arrangement with respect to the arene ring and its substituent, while those in2 are staggered. These conformations are consistent with the notion that the acetal substituent behaves largely as an electroneutral group, or at most as a weak electronic acceptor.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01677100
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  • 13
    Electronic Resource
    Electronic Resource
    Structure of (Z)-1-p-methoxyphenyltelluro-1,4-diphenyl but-1-en-3-yne (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 389-392 
    Details
    ISSN: 1572-8854
    Keywords: p-Methoxyphenyltelluro ; x-ray diffraction ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract C23H18TeO,M r=437.97, $$P\bar 1$$ ,a=9.940(2),b=13.664(3),c=7.895(2) Å, α=80.60(1), β=69.71(2), γ=75.95(1)°,V=972.0(4) Å3,Z=2,R=0.041 for 2668 observed reflections. The Te−C bond distances are 2.109(5)Å and the C−Te−C angle is 96.0(2)°. The phenyl rings are planar to within experimental accuracy, making dihedral angles of 64.6(2), 65.3(2) and 31.1(3)°.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01665816
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  • 14
    Electronic Resource
    Electronic Resource
    Crystal structure of (diphenyl)(morpholino)phosphiniminocyclotrithiazene (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 403-406 
    Details
    ISSN: 1572-8854
    Keywords: Cyclotrithiazene ; arylaminophospine ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The title compound (C6H5)2(OC4H8N)P=N−S3N3 crystallizes in the space group $$P\bar 1$$ with unit cell parametersa=9.3900(2),b=9.4747(1),c=11.3850(3) Å, α=95.73(4), β=96.85(6), γ=104.26(2)o, and Z=2. The tricoordinated sulfur of the cyclotrithiazene ring deviates from the mean plane of other skeletal atoms by 0.683(4) Å. The angle at this atom is the smallest in the ring and is enclosed by the longest S−N bonds observed in the ring.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01665819
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  • 15
    Electronic Resource
    Electronic Resource
    Formation of copper(II) coordination polymers by a flexible double betaine: [{Cu(L)X2(H2O)} n ]·2nH2O [X=Cl, Br] and [{Cu(L)(H2O)4} n ](ClO4)2n ·2nH2O [L=−O2CCH (Me3N+)CH2CH2CH(Me3N+)CO 2 − ] (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 471-477 
    Details
    ISSN: 1572-8854
    Keywords: Copper(II) complex ; crystal structure ; coordination polymer ; betaine ; dicarboxylate ligand
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Three polymeric copper(II) complexes of a flexible double betaine, namely, [{Cu(L)Cl2(H2O)} n ]·2 n H2O (1), [{Cu(L)Br2(H2O)} n ]·2nH2O (2), and [{Cu(L)(H2O)4} n ](ClO4)2n ·2nH2O (3) [L=−O2CCH(Me3N+)CH2CH2CH(Me3N+CO2], have been prepared and characterized by singlecrystal X-ray analysis. Isomorphous complexes (1) and (2) crystallize in space groupC2/c (No. 15) witha=17.725(3),b=5.958(2),c=19.077(3) Å, β=110.70(1)o,V=1881.4(4) Å3, Z=4 anda=18.268(4),b=5.948(3),c=19.166(5) Å, β=109.08(2)o,V=1964.7(9) Å3, Z=4, respectively. Complex (3) belongs to space groupPĪ (No. 2) witha=6.203(1),b=9.293(2),c=12.035(2) Å, α=86.56(2), β=87.33(3), γ=71.23(2)o,V=655.4(2) Å3 and Z=1. The crystal structure of (1) and (2) features an infinite zigzag chain composed of an alternate arrangement of metal atoms and double betaines ligands, with each Cu(II) atom in a distorted CuX2O3 [X-Cl, Br] square-pyramidal geometry, and hydrogen bonding between adjacent chains leads to a layer structure concentrated the (200) family of planes. Complex (3) exhibits a layer structure corresponding to the (001) family of planes, in which neighboring chains constructed from the metal atoms and the double betaine ligands are cross-linked by hydrogen bonding between the aqua ligands. The Cu(II) atom is coordinated in a CuO6 octahedral geometry with Jahn-Teller distortion.
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    URL: http://dx.doi.org/10.1007/BF01668307
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  • 16
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    Electronic Resource
    Crystal structure of aquo (hydroxo) (ethylenediaminetetraacetato) sodium(I) tin(IV), NaSn(OH)(edta)(H2O) (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 503-508 
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    ISSN: 1572-8854
    Keywords: Tin(IV) sodium(I) complex ; ethylenediaminetetraacetic acid ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract NaSn(OH)(edta)(H2O) is monoclinic, space groupP21/c, witha=9.747(3)Å,b=9.121(3)Å,c=16.430(6)Å, β=98.69(4)°, Å3, andZ=4. The coordination environment of Sn(IV) is a capped octahedron. Sn−O distances range from 1.990(6)Å to 2.351(7)Å. Na(I) is five coordinated to three different edta molecules. Na−O distances range from 2.283(9)Å to 2.414(7)Å. The edta ligand presents the E, G/R conformation. The crystal structure is composed of sheets parallel to (001): inside a sheet Sn(OH)(edta) molecules are connected to each other by the Na(I) interactions.
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    URL: http://dx.doi.org/10.1007/BF01668312
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  • 17
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    Electronic Resource
    Geometry of lidocaine-like molecules. 1. Crystal structure of tocainide (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 515-518 
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    ISSN: 1572-8854
    Keywords: Antiarrhythmic agent ; crystal structure ; absolute configuration
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The title compound crystallizes in the orthorhombic space groupP212121, withZ=4,a=4.770(1)Å,b=6.620(1)Å,c=37.550(7)Å,R=0.04. The most important factors affecting conformation of the molecules are: the protonation state of the N(9) atom andortho-substitution of the benzene ring in the acetanilide system. Protonation promotes an extended form of the molecule and 2,6-substitution forces a twist of at least 60° between the benzene ring and amide group planes. The resulting separation of lipophilic (xylidine) and amine groups, being two important pharmacophores, equals about 5Å in tocainide and all other structures comprising the amino-2,6-dimethylacetanilide system.
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    URL: http://dx.doi.org/10.1007/BF01668314
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  • 18
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    Electronic Resource
    Structure of a binuclear silver(I) complex [Ph3PAg(O2CCH2Ph)]2 (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 553-557 
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    ISSN: 1572-8854
    Keywords: Silver(I) complex ; synthesis ; crystal structure ; spectroscopic properties
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The reaction of [Ph3PAgI]4 with sodium phenylacetate in MeOH and CH2Cl2 at room temperature gave rise to a binuclear silver complex with triphenylphosphine and phenylacetate mixed ligands, [Ph3PAg(O2CCH2Ph)]2. The crystal and molecular structure of the complex has been determined by single crystal X-ray diffraction analysis. The space group is $$P\bar 1$$ witha=9.198(2),b=9.516(2),c=13.842(3) Å, α=102.00(3), β=108.34(3), γ=93.58(3)°,Z=1, andDc=1.506 g cm−3. The silver atoms are each coordinated by one phosphorus atom from triphenylphosphine and two oxygen atoms from the carboxylate groups in a T-shape. The complex is further characterized by its IR,1H, and31P NMR spectra.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01668414
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  • 19
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    Electronic Resource
    Crystal structure of the hemitoluene solvate of racemiccis-bis(bipyridyl)chloro(tri-n-propylphosphine)ruthenium(II) perchlorate, a species with disordered PPr3 and toluene moieties (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 667-675 
    Details
    ISSN: 1572-8854
    Keywords: Ruthenium(II) complex ; tri-n-propylphosphine ; bipyridyl ; crystal structure ; disorder
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The complexcis-[Ru(bpy)2(PPr3)Cl+][ClO 4 − ] · 0.5 (toluene) crystallizes as a racemate in the monoclinic space group P21/n. Both the PPr3 ligand and the toluene of crystallization are subject to disorder. Ruthenium—ligand distances are: Ru−PPr3=2.348(2) Å, Ru−Cl=2.426(2) Å and Ru−N(bpy)=2.035(6)–2.112(5) Å.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01991962
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  • 20
    Electronic Resource
    Electronic Resource
    Crystal structure ofmer,trans-[Ru(NO2)(trpy) (PPh3) 2 + ][PF 6 − ]: a “problem structure” (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 853-859 
    Details
    ISSN: 1572-8854
    Keywords: Ruthenium(II) complex ; terpyridine ; triphenylphosphine ; ruthenium-nitro complex ; crystal structure ; pseudo-lattice
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The complexmer,trans-[Ru(NO2)(trpy)(PPh3) 2 + ][PF 6 − ] crystallizes in the centrosymmetric monoclinic space groupP21/n withZ=4; the ruthenium atom lies close toy=1/4 and all data withh+l=2n+1 are systematically weak. The trpy ligand is not strictly planar, but has a “dish-like” geometry. The nitro ligand is rotated from the plane of the Ru(trpy) moiety, the N3Ru/NO2 interplanar angle being 32.5o. Ruthenium-ligand distances are: Ru−PPh3=2.418(4) Å and 2.429(4) Å, Ru−NO2=2.063(12) Å, Ru−N(trpy, outer)=2.100(12) Å and 2.116(12) Å and Ru−N(trpy, central)=2.004(11) Å.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01670319
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  • 21
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    Electronic Resource
    The structure of N,N′-bis(2-hydroxyphenyl)butanediamide (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 661-665 
    Details
    ISSN: 1572-8854
    Keywords: N,N′-bis(2-hydroxyphenyl)butanediamide ; crystal structure ; hydrolysis product
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The structure of N,N′-bis(2-hydroxyphenyl)butanediamide has been determined. The molecule consists of two 2-hydroxyphenyl moieties which are attached (at the 2 position) to the two nitrogens of the butanediamide. The compound C16H16N2O4 crystallizes in the monoclinic space group P21/c witha=5.576(1),b=4.8853(6),c=25.397(6) Å and β=90.58(1)°.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01991961
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  • 22
    Electronic Resource
    Electronic Resource
    The 1∶1-adduct of chlorotriphenyltin with 2′,6′-dimethoxyflavone: a potential fungicide (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 691-694 
    Details
    ISSN: 1572-8854
    Keywords: Organotin ; crystal structure ; flavone
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The 1∶1 adduct of chlorotriphenyltin with 2′,6′-dimethoxyflavone, (C35H29O4ClSn)Mr=667.78, crystallizes in the triclinic space groupP1 with the following data:a-9.094(2),b=12.369(3),c=14.674(3) Å, α=74.78(2), β=77.00(2), γ=73.06(3)°,V=1503.8(4) Å3,Z=2, Mo-Kα, μ=9, 8 cm−1,Dc=1.475 g cm−3, F(000)=676,T=293K. The structure was solved by direct-methods and has been refined to a finalR value (l〉3σ(I)) of 0.0301. The flavone coordinates to the tin atom through the carbonyl oxygen atom. The metal center exhibits a trigonal bipyramidal configuration with the three phenyl groups in equatorial positions.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01991965
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  • 23
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    Electronic Resource
    Molecular structure and hydrogen bonding of 4-dimethylaminopyridinioacetate in its crystalline dihydrate and hydrochloride trihydrate, L·2H2O and [L2H]Cl·3H2O (L=p-Me2NC5H4N+CH2CO2 −) (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 133-139 
    Details
    ISSN: 1572-8854
    Keywords: Betaine ; 4-dimethylaminopyridinioacetate ; hydrogen bonding ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystalline dihydrate and hydrochloride trihydrate of a new betaine, namely, L·2H2O (1) and [L2H]Cl·3H2O(2) (L=p-Me2NC5H4N+CH2CO2), have been synthesized and characterized by X-ray crystallography. Molecule L in compound1 [space groupPbcn, witha=15.732(3),b=7.894(2),c=18.304(4) Å, andZ=8] possesses approximateC s symmetry. The formation of hydrogen bonds by water molecules bridging neighboring carboxy oxygen atoms leads to an infinite two-dimensional network composed of a packing of two different kinds of 12-membered rings. In compound2 [space group PT witha=7.341(2),b=9.543(2),c=17.010(4) Å, α=82.43(2)°, δ=80.34(2)°, λ=74.05(2)°, andZ=2], the carboxylate groups of a pair of betaine molecules are bridged by a proton to form a dimeric cation L2H+ with a very strong asymmetric hydrogen bond of length 2.464(7) Å. The crystal structure features a hydrogen-bonded corrugated ribbon comprising an alternate arrangement of edge-sharing centrosymmetric (H2O)4(Cl−)2 and (H2O)4 rings running parallel to thea axis.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01669730
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  • 24
    Electronic Resource
    Electronic Resource
    Crystal and molecular structure of the bidentate ligand 2,2-di(1-pyrazolyl)propane, CH3C(C3N2H3)2CH3 (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 179-183 
    Details
    ISSN: 1572-8854
    Keywords: Bidentate ligand ; crystal structure ; pyrazolyl group ; hydrogen bonding
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The title compound lies on a site of C2 symmetry, with the two planar pyrazolyl moieties oriented at 86.1° to one another. The hydrogen atoms were located and refined.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01673667
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  • 25
    Electronic Resource
    Electronic Resource
    Synthesis and structure determination of 3α-triphenylstannyl-cholest-5-ene (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 219-222 
    Details
    ISSN: 1572-8854
    Keywords: Steroid ; organometallic ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract 3α-Triphenylstannylcholest-5-ene (1) has been synthesised and its molecular structure has been determined by single crystal X-ray diffraction. Refinement in the triclinic space groupP1 witha=7.805(6),b=7.862(5),c=32.351(10)Å, α=90.87(8), β=94.77(8) and γ=101.15(4)o converged atR=0.063. One of the two crystallographically independent molecules in the unit cell has a patially disordered side chain. The bond lengths and valency angles about tin indicate some steric hindrance due to the proximity of one of the phenyl rings with the B ring of the steroid nucleus.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01673674
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  • 26
    Electronic Resource
    Electronic Resource
    Crystal and molecular structure of β-resorcylidene aminoguanidine copper(II) complex (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 841-846 
    Details
    ISSN: 1572-8854
    Keywords: Cu(II) resorcylidene aminoguanidine ; synthesis ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The tridentate Schiff base, β-resorcylidene aminoguanidine (RAG)1 was synthesized from 2,4-dihydroxybenzaldehyde and aminoguanidine and complexed with copper(II) to form a copper(II)-β-resorcylidene aminoguanidine (Cu-RAG)2 complex. X-ray diffraction analysis of compound2 (orthorhombic, Pnma,a=11.674(1);b=6.7198(7);c=17.836(2) Å) revealed a square-planar copper(II) cation with a tridentate·ligand bound through two nitrogen atoms (N1 and N3) of the aminoguanidine moiety and an oxygen (O1) of the monodeprotonated dihydroxybenzaldehyde function. The remaining coordination site was occupied by chloride and the structure was rigidly planar as demanded by the restrictions of the crystallographic space group. The unit cell contents exhibited an extended sheet-like structure constructed via hydrogen bonds both intermolecularly and involving two water molecules (O3 and O4) also restricted by the same mirror symmetry. The remaining water (O5) provided for interlayer hydrogen bonding.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01670317
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  • 27
    Electronic Resource
    Electronic Resource
    Crystal and molecular structure of di(1-pyrazolyl)methane, CH2(C3N2H3)2 (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 93-97 
    Details
    ISSN: 1572-8854
    Keywords: Pyrazolyl group ; crystal structure ; bidentate ligand ; hydrogen bonding
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The title compound consists of two planar pyrazolyl fragments oriented at 73.0° to each other and linked to a common carbon atom. All hydrogen atoms were located unambiguously and their positions were refined.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01669723
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  • 28
    Electronic Resource
    Electronic Resource
    Crystal structure ofcis-[Ru(bpy)2{PPh2(o-tol)}Cl][ClO4]·1.5(CH2Cl2), a structure containing both ordered and disordered dichloromethane molecules of crystallization (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 111-116 
    Details
    ISSN: 1572-8854
    Keywords: Ruthenium(II) complex ; bipyridyl ; diphenyl(o-tolyl)phosphine ; dichloromethane solvate ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The complexcis-[Ru(bpy)2 {PPh2(o-tol)}Cl][ClO4] crystallizes from dichloromethane as the sesqui-dichloromethane solvate. The complex crystallizes in the monoclinic space group P21/n with Z=4. The structure was refined toR=5.50% for those 2552 independent reflections with |F 0|〉6σ(|F 0|) The octahedral Ru(II) cation is associated with the following bond lengths: Ru-PPh2(o-tol)=2.360(3)Å. Ru−Cl=2.433(2)Å and Ru−N(bpy)=2.041(8)–2.095(8)Å. Both the perchlorate anion and the dichloromethane molecules of solvation exhibit large amplitudes of vibration. One dichloromethane molecule lies in a general position, the other lies about an inversion center and suffers from disorder.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01669726
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  • 29
    Electronic Resource
    Electronic Resource
    Trifluoromethyl group disorder in crystalline 2,8-bis(trifluoromethyl)-4-hydroxymethylquinoline (1996)
    Springer
    Journal of chemical crystallography 26 (1996), S. 615-619 
    Details
    ISSN: 1572-8854
    Keywords: Disordered trifluoromethyl group ; quinoline ; crystal structure ; AM1 calculation ; mefloquine
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The title compound crystallized in space groupPna21 with lattice constantsa=13.406(1),b=18.799 (4), andc=4.785(1). The molecule is essentially flat with only fluorine atoms, methylene hydrogen atoms, and the hydroxyl hydrogen atom out of the plane of the quinoline ring. Only one of the trifluoromethyl groups of the title compound is disordered following a pattern observed in other crystal structures. Quantum chemical calculations at the AM1 level are consistent with this phenomenon. Although the carbon atom of the fixed trifluoromethyl group is further from the quinoline nitrogen atom than the carbon atom of the disordered trifluoromethyl group, the fluorine atoms of the fixed trifluoromethyl group more closely approach the quinoline nitrogen atom by 0.3 Å if the C(8)−C(10) bond in the crystal structure is freely rotated.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01668622
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  • 30
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    Electronic Resource
    A double-bonded niobium(III) compound with a formamidinate core: Nb2(μ-SMe)2(μ-DTolF)2 (η2-DTolF)2.2 toluene, DToIF= di-p-tolylformamidinate (1996)
    Springer
    Journal of cluster science 7 (1996), S. 655-662 
    Details
    ISSN: 1572-8862
    Keywords: Niobium(III) ; edge-sharing bioctahedra ; di-p-tolylformamidinato ; thiomethoxide ; double-bond ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract The reaction of NaEt3BH with Nb2(μ-SMe2)3Cl6 results in the transfer of a hydride ion to dimethylthioether with concomitant production of methane. Further reaction with potassium di-p-tolylformamidinate, KDTolF, yields Nb2(μ-SMe)2(μ-DTolF)2η2-DTolF:)2.2 toluene, 1. In the latter, two thiomethoxide ions and two DTolF groups bridge the trivalent niobium atoms. Each of the other two DTolF groups chelate a metal atom to give the molecule an edge-sharing bioctahedral structure, The niobium-niobium distance of 2.655(2) A is consistent with the presence of a double bond between the metal atoms.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01165807
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  • 31
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    Electronic Resource
    Ligand displacement reactions from the coordination sphere of cobalt complexes. Part II: The displacement of ligands of [cis-Co(en)2Cl2]Cl by potassium squarate. The crystal and molecular structure of a compound with idealized formula of [cis-Co(en)2(H2O)Br]2[trans-(C2O4 2−(C2O4H−)Co-trans-(H2O)2(OH)2]Br2 (I) (1996)
    Springer
    Structural chemistry 7 (1996), S. 233-240 
    Details
    ISSN: 1572-9001
    Keywords: Cobalt complexes ; potassium squarate ; crystal structure ; molecular structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Compound (I), idealized as Br4Co3O14N8C16H41 (see text), crystallizes in the triclinic space groupP¯ 1 (No. 2) with cell constants ofa=7.4470(7),b=7.9648(4),c=15.2223(8),α=96.338(4)ℴΒ=93.504(6)ℴ,γ=112.894(6)ℴ,V=821.328 å3, and d(calc; MW=1065.97,z=1)=2.155 gm-cm−3. Data (3880 total reflections) were collected over the range 2ℴ ≤ 2θ ≤ 55ℴ and corrected for absorption (Μ=63.69 cm−1) using data from Psi scans. The unexpectedly isolated compound contains a [cis-Co(en)2Br(OH)]+ cation, while the anion contains a central Co(III) surrounded by two mondentate,trans-squarato ligands, twotrans-hydroxo, and two waters. The waters and hydroxy ligands were identified by determining, experimentally, the presence and positions of their respective hydrogens. Given the need for overall electroneutrality, one squarato ligand must be a dianion (Sq2−) and the other a monoanion (SqH−); however, since the ion bearing the squarato ligands sits at an inversion center, the hydrogen of the latter must be disordered. Refinement of the heavy atoms with anisotropic thermal parameters and fixed hydrogen positions (B's fixed at) led to the finalR(F) andR W(F) factors of 0.036 and 0.042, respectively. (I) was obtained during efforts to prepare [Co(en)2(squarate)]Br by the displacement of two chloro ligands from the coordination sphere of [cis-Co(en)2Cl2]Cl by K2 (squarate) followed by addition of NaBr. Compound (I) appears to be the first example of a coordination compound in which squarate2− and squarate H− anions are present as ligands to a transition metal ion. A search of the Cambridge file (to 1992) produced no known examples of Co(III) squarates. Thus, (I) appears to also be the first example of its kind.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF02281234
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  • 32
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    Electronic Resource
    Tryptophan-derived peptides. 1: Crystal structure and solution conformation of Boc-Gly-Trp-Ala-OtBu (1996)
    Springer
    Structural chemistry 7 (1996), S. 103-110 
    Details
    ISSN: 1572-9001
    Keywords: Protected tripeptide ; solution structure ; crystal structure ; X-ray analysis ; NMR analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The solid-state structure of Boc-Gly-Trp-Ala-OBut was determined by single-crystal X-ray diffraction analysis. The tripeptide gave crystals belonging to the orthorhombic systemP212121 and at 122.0(5) K:a=11.0663(12),b=14.107(2),c=17.275(2) Å,V=2697.0(5) Å3Z=4,R(F)=0.0259, andR w(F)=0.0695. The peptide adopts a type-Iβ-turn in the solid state with a single, rather weak, intramolecular hydrogen bond between the Boc-CO and Ala-NH groups (N⋯O 3.082(1) Å, 〈NH⋯O 167(1)°). The conformation of the Boc-Gly-Trp-Ala-OBut peptide has also been studied by1H NMR spectroscopy. The solvent and temperature dependencies of NH chemical shifts suggests that this hydrogen bond is broken and that all amide protons are solvent exposed in CDCl3 and (CD3)2SO.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF02278735
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  • 33
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    Electronic Resource
    The crystal structures and thermal shrinkage properties of aromatic polyimide fibers (1996)
    Springer
    Journal of thermal analysis and calorimetry 46 (1996), S. 719-731 
    Details
    ISSN: 1572-8943
    Keywords: aromatic polyimide fiber ; as-spun fiber ; crystallization ; crystal structure ; crystal unit cell ; draw ratio ; dry-jet wet spinning ; isotropic solution ; modulus ; self-elongation ; tensile strength ; thermal shrinkage stress ; thermal shrinkage strain ; thermomechnical analysis ; triclinic ; wide angle X-ray diffraction ; zone drawing
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Three aromatic polyimides based on 3,3′,4,4′-biphenyl-tetracarboxylic dianhydride (BPDA) and three different diamines 2,2′-bis(trifluoromethyl)-4,4′-diaminobiphenyl (PFMB), 2,2′-dimethyl-4, 4′-diaminophenyl (DMB) or 3,3′-dimethylbenzidine (OTOL) have been synthesized. These polyimides are soluble in hotp-chlorophenol,m-cresol or other phenolic solvents. Fibers have been spun from isotropic solutions using a dry-jet wet spinning method. The as-spun fibers generally exhibit low tensile properties, and can be drawn at elevated temperatures (〉380° C) up to a draw ratio of 10 times. Remarkable increases in tensile strength and modulus are achieved after drawing and annealing. The crystal structures of highly drawn fibers were determinedvia wide angle X-ray diffraction (WAXD). The crystal unit cell lattices have been determined to be monoclinic for BPDA-PFMB and triclinic for both BPDA-DMB and BPDA-OTOL. Thermomechanical analysis (TMA) was used to measure thermal shrinkage stress and strain. A selfelongation has been found in the temperature region around 450°C. This phenomenon can be explained as resulting from the structural development in the fibers as evidencedvia WAXD observations.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01983598
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  • 34
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    Electronic Resource
    Formation of various polymeric frameworks by dicarboxylate-like ligands: Synthesis and crystal structures of polymeric complexes of sodium perchlorate with flexible double betaines (1996)
    Springer
    Structural chemistry 7 (1996), S. 91-101 
    Details
    ISSN: 1572-9001
    Keywords: Betaine ; sodium perchlorate ; crystal structure ; polymeric framework
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Three crystalline complexes of sodium perchlorate with different flexible double betaines [Na 2(L1)(ClO4)(H2O) n ](ClO4) n (1), [Na 3(L2)(ClO4)3(H2O)2 n ] (2), and [Na(L 3)(CH3OH)n]-(ClO4) n ·xnH2O (x=0.25) (3) [−O2CCH2N+Me2−(CH2) n -N+Me2CH2CO2 −,n=2 L1;n=3 L2;n=4 L3] have been synthesized and characterized by single-crystal X-ray structure analysis. Complex (1) comprises tetranuclear sodium units consolidated by betaine and aqua ligands, which are bridged by half of the ClO4 − anions to form layers matching the (200) planes, the remaining uncoordinated ClO4 − anions being accommodated between adjacent layers. Complex (2) possesses a double-layer polymeric structure with the sodium atoms bridged by ligand oxygen atoms to form columns running parallel to thea axis, which are interconnected by double-betaine ligands lying parallel to theac plane. All of the ClO4 − groups and water molecules are coordinated to the metal atoms. In complex (3) the chains composed of alternating eight-membered and four-membered metallocycles are cross-linked by the betaine ligands, which lie in the (020) and (01/1) families of planes, to yield a three-dimensional network. All of the ClO4 − groups and water molcules fill the resulting infinite channels running parallel to thea axis. Two unusual carboxylate coordination modes are identified, namelyμ 3-O andhapto-3-O plushapto-2-O′ in (1) and (2), respectively.
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    URL: http://dx.doi.org/10.1007/BF02278734
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  • 35
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    Electronic Resource
    Crystal and molecular structure of organic semiconductor (ET)8[Hg4Cl12] · 2C6H6 (1996)
    Springer
    Russian chemical bulletin 45 (1996), S. 370-375 
    Details
    ISSN: 1573-9171
    Keywords: organic conductors ; bis(ethylenedithio)tetrathiafuIvalene ; mercury halides ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A new organic semiconductor, (ET)8[Hg4C112] · 2C6H6, obtained in the ET+-HgCl 3 − -PhF system has been studied by X-ray structural analysis. Radical cations of bis(ethylenedithio)tctrathiafulvalene (ET) in the organic layer of the structure are packed in stacks ofa-type. The average angle between the planes of ET cations from adjacent stacks is 50.1°. The anionic layer is formed by four-charge centrosymmetric [Hg4Cl12]4− complexes and benzene solvate molecules. A comparative crystal-chemical study of the salts obtained by the reaction in the ET+-HgX 3 − -PhY system (where X = Cl, Br, and I; Y = F, Cl, and Br) made it possible to reveal a substantial effect of the sizes of the X and Y atoms on the composition of the salts and on the structural characteristics of the layers, which are responsible for the various conductivities of these salts.
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    URL: http://dx.doi.org/10.1007/BF01433975
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  • 36
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    Tetramethyl(2-methylthioethyl)cyclopentadienyl complexes of zirconium(iv): synthesis, crystal structure, and dynamic behavior in solutions (1996)
    Springer
    Russian chemical bulletin 45 (1996), S. 940-949 
    Details
    ISSN: 1573-9171
    Keywords: substituted sulfur-containing cyclopentadienes ; cyclopentadienyl zirconium complexes ; dynamic behavior ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Chelating sulfur-containing cyclopentadienyl ligand tetramethyl(2-methylthioethyl)cyclopentadiene (1), was synthesized for the first time. Its sodium (2a) and lithium (2b) derivatives were isolated in the crystalline state. Starting from compound1 some novel ZrIV complexes were prepared: [tetramethyl(2-methylthioethyl)cyclopentadienylltriclllorozirconium (3), bis[tetramethyl(2-methylthioethyl)cyclopentadienylldichlorozirconium (4), and [pentamethylcyclopentadienyll [tetramethyl(2-methylthioethyl)cyclopentadienylldichlorozirconium (5). The crystal structures of3 and5 were determined by X-ray diffraction analysis. The dynamic behavior of complex3 in various solvents was investigated by1H and13C N MR spectroscopy. The S→Zr coordination bond was shown to exist in complex3 both in the crystalline state and in solution. No coordination of this type was found in compounds4 and5.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01431329
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    Tetramethyl(2-methoxyethyl)cyclopentadienyl complexes of zirconium(iv). Crystal structure of [η5:η1−C5(CH3)4(CH2CH2OCH3)]ZrCl3 (1996)
    Springer
    Russian chemical bulletin 45 (1996), S. 1740-1744 
    Details
    ISSN: 1573-9171
    Keywords: cyclopentadienes with oxygen-containing substituents ; cyclopentadienyl zirconium complexes ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Several novel zirconium(iv) complexes with the chelating oxygen-containing cyclopentadienyl ligand, tetramethyl(2-methoxyethyl)cyclopentadiene, have been synthesized. [η5:η1-Tetra-methyl(2-methyl)cyclopentadienyl]trichlorozirconium (2), bis[η5-tetramethyl(2-methoxyethyl)cyclopentadienyl]dichlorozirconium (3), [η5-pentamethylcyclopentadienyl][η5-tetra-methyl(2-methoxyethyl)cyclopentadienyl]dichlorozirconium (4), and [η5-tetra-methyl(2-methylthioethyl)cyclopentadienyl][η5-tetramethyl(2-methoxyethyl)-cyclopentadienyl]dichlorozirconium (5) have been prepared from the corresponding lithium cyclopentadienide (l). The crystal structure of cyclopentadienyl complex2 has been established by X-ray analysis. The coordination O→Zr bond in compound2 exists both in the crystalline state and in solutions. No coordination of this type was observed in complexes3–5. Synthesized complexes2–5 are discussed in comparison with their sulfur-containing analogs.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01431817
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  • 38
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    Computer Simulation of Crystal-liquid Interface: Application to Wettability of Solids (1996)
    Springer
    Pharmaceutical research 13 (1996), S. 1003-1007 
    Details
    ISSN: 1573-904X
    Keywords: molecular simulation ; interfacial energy ; wettability ; crystal structure ; Monte Carlo method ; potential energy calculations ; contact angle
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Purpose. This study describes the development and application of a molecular simulation technique for investigating the solid-liquid interface. It attempts to relate the molecular and crystal structure to the observed wettability of solids. Methods. Molecular simulations have been carried out for the crystal-water interface of a series of N-n-alkyl-D-gluconamide crystals using the Monte Carlo technique. The molecular system simulated consisted of a layer of water bounded by two crystal slabs. The interfacial potential energies were calculated for the crystal-water interactions and compared with experimental enthalpy values obtained from contact angle measurements. Results. The simulations clearly reveal the distinct hydrophilic and hydrophobic nature of the respective (010) and (010) faces of these compounds. The distribution of water at the interface observed in the simulations is in accord with the nature of the crystal faces. The calculated interfacial potential energies are in the right ball park, but consistently higher than the experimental values. The disparity, however, is justifiable, resulting from the highly simplified model simulated. Conclusions. Using the developed molecular simulation technique one can calculate the wettability of a solid given the crystal structure. This approach represents an important step towards the goal of engineering crystals with desired wettability characteristics.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1016094204888
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  • 39
    Electronic Resource
    Electronic Resource
    On the crystallization behavior of cold-drawn syndiotactic polypropylene (1996)
    Springer
    Colloid & polymer science 274 (1996), S. 1006-1011 
    Details
    ISSN: 1435-1536
    Keywords: Syndiotactic polypropylene ; cold stretching ; chain conformation ; crystal structure ; crystallization behavior
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract The influence of the chain conformation on the crystallization behavior of cold-drawn syndiotactic polypropylene (sPP) has been investigated. The conformational and structural changes depending on drawing conditions and thermal treatments has been observed by x-ray diffraction, infra-red spectroscopy and modulated differential scanning calorimetry. A nucleation and crystal growth model is introduced, which explains the low crystallinity of cold-drawn sPP.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00656632
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  • 40
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    Structural variation and recovery of superconductivity by Ca substitution in Y0.4Pr0.6Bs2−x Ca x Cu3 (1996)
    Springer
    Journal of superconductivity 9 (1996), S. 89-91 
    Details
    ISSN: 1572-9605
    Keywords: Y0.4Pr0.6Ba2−xCaxCu3O7−δ ; superconductivity ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Electrical Engineering, Measurement and Control Technology , Physics
    Notes: Abstract Y0.4Pr0.6Ba2−xCaxCu3O7−δ polycrystalline samples were prepared and investigated. The Ca substitution led to a structural variation toward tetragonal symmetry, possibly due to the structural modification within the Cu(1)O layer. Superconductivity and metallic conduction were recovered whenx≥0.2, giving one more evidence for the existence of the ion-size effect at the Ba site.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00728431
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  • 41
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    Topotactic solid-state polymerization of 3-aminocrotonamide by radiation (1996)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 34 (1996), S. 1087-1093 
    Details
    ISSN: 0887-624X
    Keywords: topotactic polymerization ; 3-aminocrotonamide ; radiation polymerization ; crystal structure ; condensation polymerization ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Radiation-induced solid-state polymerization of 3-aminocrotonamide (3-amino-2-butenamide) was carried out at room temperature, in open air atmosphere and under vacuum condition. The polymer obtained was white powder, soluble in methanol, but insoluble in water. The nature of polymers were investigated by IR, UV, x-ray, DP-MS, and elemental analysis to elucidate the mechanism of the polymerization. The polymer was crystalline with melting point in the range of 245-255°C. The cell parameters and space group of monomer and polymers were determined from powder x-ray diffraction patterns. The similarity of crystal structures of monomer and polymer indicated a topotactic polymerization. It was shown by spectroscopic investigations and elemental analyses that the polymerization proceeds by condensation reaction with evolution of one mole ammonia per two combined moles of monomer through a free radical mechanism. © 1996 John Wiley & Sons, Inc.
    Additional Material: 5 Ill.
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  • 42
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    The structure of the mineralomimetic cadmium cyanide-dimethyl carbonate clathrate (1996)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 26 (1996), S. 153-159 
    Details
    ISSN: 1573-1111
    Keywords: Cadmium cyanide ; crystal structure ; clathrate ; mineralomimetic chemistry ; dimethyl carbonate
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Cd(CN)2·(CH3O)2CO (1) contains a mineralomimetic framework of Cd(CN)2 analogous to the low temperature form of cristobalite. The host framework is isostructural to those of previously reported Cd(CN)2·G compounds (G = CHCl2CH2Cl2, (CH3)2CHBr3). The dimethyl carbonate molecules in the adamantane-like cage display orientation disorder associated with the location of the carbonyl oxygen atom.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01029939
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  • 43
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    Novel negatively charged cyanocuprate(I) host [Cu4(CN)7]3− built of tetrahedral Cu(I) coordination centers: Crystal structure of [{NH2(CH2CH2)2NCH2CH2NH2}2H][Cu4(CN)7] (1996)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 26 (1996), S. 119-126 
    Details
    ISSN: 1573-1111
    Keywords: Cyanocuprate(I) complex ; crystal structure ; three-dimensional framework ; bifurcated cyano group ; N-(2-aminoethyl)piperazine ; hydrogen-bond ; dimeric onium guest
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The title inclusion compound [{NH2(CH2CH2)2NCH2CH2NH2}2H][Cu4(CN)7] was obtained as single crystals from an aqueous solution containing CuCN, KCN, andN-(2-aminoethyl)piperazine. It crystallizes in the monoclinic space groupP2/n,a = 12.3829(9),b = 8.5970(9),c = 12.6633(7) Å, β = 109.984(5)°,z = 2,R = 0.035 for 2921 independent reflections. The inclusion structure is composed of the hydrogen-bonded dimeric onium guest [{NH2(CH2CH2)2NCH2CH2NH2}2H]3+ and the negatively-charged three-dimensional host [CU4(CN)7]3− in which the CN-bridged framework Cu(I) atoms are all tetrahedral. A polyacene-like one-dimensional array of hexagons cornered by Cu(I) atoms and edged by -CN- linkages is arrayed in parallel to theb axis and stacked approximately along the c axis. The Cu(I) corner shared in the one-dimensional array extends an N-coordinate CN group along the c axis to a pair of unshared Cu(I) corners for which the C end behaves as a bifurcated ligand to build up the three-dimensional host structure. The cavity is composed of two networks of the hexagons at the top and bottom and pillared by six 〉CN- groups and accommodates a dimeric guest ofN-(2-aminoethyl)piperazinium cations protonated at each 4-N with the cations being hydrogen-bonded to each other through the 2-NH2 groups sharing another H+.
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    URL: http://dx.doi.org/10.1007/BF01029936
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    Synthesis and structures of nitromethane complexes of furanotribenzo-21-crown-7 and dibenzo-21-crown-7 (1996)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 26 (1996), S. 197-207 
    Details
    ISSN: 1573-1111
    Keywords: Crown ether ; nitromethane complex ; coordination isomers ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Single crystal X-ray diffraction analyses of two nitromethane complexes of furanotribenzo-21-crown-7 (1 and2) and the nitromethane complex of dibenzo-2l-crown-7 (3) are reported. The two nitromethane complexes1 and2 are polymorphic in that the macrocyclic ring adopts the ‘dentist's chair’ conformation in both structures, with a single nitromethane molecule coordinating to either the lower, concave (1) or upper, convex (2) face of the crown ether. Complex3 adopts an entirely different conformation with a coplanar arrangement of the crown ether oxygen atoms binding a single nitromethane molecule.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01053538
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  • 45
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    An unexpected structural principle for crystalline MgBr2·OEt2: Chains of trigonal bipyramids (1996)
    Weinheim : Wiley-Blackwell
    Chemistry - A European Journal 2 (1996), S. 1112-1114 
    Details
    ISSN: 0947-6539
    Keywords: coordination ; crystal structure ; halogen compounds ; magnesium compounds ; structure elucidation ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: MgBr2·OEt2 (1), which is commercially available and has been examined by different methods in the past, was obtained in crystalline form as a by-product of the reaction of amine-stabilised A1C1 solution with mesitylene magnesium bromide. The following unexpected structure was obtained by X-ray techniques: five-coordinate magnesium centres form trigonal bipyramids, which are connected by two common bromine atoms into chains. Structural details and especially the relationship with solid MgBr2, MgBr2·(OEt2)2 and MgI2·(OEt2)2 (2) are discussed in order to illuminate the unusual bonding in 1.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/chem.1460020910
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    Se2NBr3, Se2NCl5, Se2NCl-6: New Nitride Halides of Selenium(III) and Selenium(IV) (1996)
    Weinheim : Wiley-Blackwell
    Chemistry - A European Journal 2 (1996), S. 1373-1378 
    Details
    ISSN: 0947-6539
    Keywords: ab initio calculations ; crystal structure ; halogen compounds ; nitrides ; selenium compounds ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Se2NBr3, a planar molecule shaped liked dividers, was formed by the reaction of SeBr4 with N(SiMe3)3, which reduced the selenium to the trivalent state. Under the same conditions, Se2NCl5 was obtained by the reaction of SeCl4 with N(SiMe3)3, retaining the tetravalent state of selenium. The molecule is formed by two edge-sharing pseudotrigonal bipyramids with selenium as their central atoms. Se2NCl5 reacts with PPh4Cl to form the Se2NCl-6 ion by the addition of a Cl- ion to only one of the two selenium atoms, resulting in pseudooctahedral coordination of this atom. Ab initio calculations for all the compounds reported confirm the experimentally determined structures.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/chem.19960021108
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  • 47
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    13C CP/MAS NMR studies of morphological changes in polypropylene: 2. The double melting endotherm of spunbonded fabrics (1996)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part B: Polymer Physics 34 (1996), S. 2085-2098 
    Details
    ISSN: 0887-6266
    Keywords: polypropylene ; CP/MAS NMR ; spunbonded fabrics ; crystal structure ; melting ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The double melting endotherm of spunbonded isotactic polypropylene (iPP) fabrics was investigated by monitoring changes in the solid-state NMR spectrum that result from thermal annealing. The DSC melting thermogram was found to change from a double to a single endotherm at anneal temperatures ≥156°C, with a concomitant increase in percent crystallinity. All of the carbon resonances in the CP/MAS NMR spectrum of the purely crystalline phase of iPP were found to be composed of multiple peaks with relative intensities that depend on anneal temperature. By monitoring the changes in the distribution of intensity among the various peaks of a given resonance, a transition temperature of 156°C was identified. Arguments are presented that this redistribution of intensity within a given carbon resonance characterizes the transformation from the α1 to the α2 monoclinic crystal form. The exothermicity associated with this transformation is responsible for the observation of a double melting endotherm by DSC. The splitting patterns observed in the NMR spectrum are discussed in terms of interlayer distances between layers of isochiral helices and the density of exposed methyls at the contact faces of these interlayers. © 1996 John Wiley & Sons, Inc.
    Additional Material: 15 Ill.
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  • 48
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    Electronic Resource
    The “Peroxo Perrhenic Acid” H4Re2O13: An Oxygen-Rich Metal Peroxide and Oxidation CatalystMultiple Bonds between Transition Metals and Main-Group Elements, Part 149. Part 148: W. A. Herrmann, F. E. Kühn, C. C. Romão, J. Organomet. Chem. 1995, 495, 209-213.Dedicated to Professor Herbert Roesky on the occasion of his 60th birthday (1996)
    Weinheim : Wiley-Blackwell
    Chemistry - A European Journal 2 (1996), S. 168-173 
    Details
    ISSN: 0947-6539
    Keywords: catalysis ; crystal structure ; oxidations ; rhenium peroxo complexes ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The rhenium oxides Re2O7 and ReO3 react with hydrogen peroxide solutions yielding peroxo complexes that efficiently catalyze the oxidation of olefins, aromatics, and certain organometallic compounds. In contrast, related oxides of molybdenum (MoO3) and vanadium (V2O5) do not activate H2O2 under comparable conditions. The active rhenium peroxo complex was isolated from the system Re2O7/H2O2: the crystalline red-orange, explosive compound of formula H4Re2O13 is the most oxygen rich rhenium compound isolated to date. Its structure resembles a “peroxo perrhenic acid”. The binuclear compound could be isolated in the form of a diglyme adduct, structurally defined as two corner-sharing pentagonal bipyramids with apical oxo and aquo ligands; the equatorial positions are occupied by the bridging oxygen and by n2-peroxo groups (two [O2]2- ligands per rhenium). In contrast to the known complex [CH3ReO(O2)2].H2O, the new peroxo species [O{ReO(O2)2.H2O}2] decomposes hydrolytically during the catalytic cycle and can thus not compete in terms of catalytic activity in oxidation reactions involving H2O2. Hydrolysis yields “perrhenic acid” Re2O7.2H2O, the diglyme adduct of which compound was also characterized by means of an X-ray diffraction analysis.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/chem.19960020208
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  • 49
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    Zintl Anions as Starting Compounds for the Synthesis of Polynuclear Transition Metal ComplexesDedicated to Professor Kurt Dehnicke on the occasion of his 65th birthday (1996)
    Weinheim : Wiley-Blackwell
    Chemistry - A European Journal 2 (1996), S. 238-244 
    Details
    ISSN: 0947-6539
    Keywords: crystal structure ; density functional calculations ; polyarsenido complexes ; polyphosphido complexes ; Zintl anions ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The Zintl anion P3-7 reacts with complexes of transition metal halides to form multinuclear metal phosphorus clusters. Reaction of Li3P7·3 DME with [FeCp(CO)2Br] or [NiCl2(PBu3)2] leads to the formation of [P7{FeCp(CO)2}3] (1) and [{Ni(PBu3)2}4P14] (2), respectively. X-ray structure determinations show that in 1 the P7 cage of Li3P7 remains intact but in 2 a P14 framework is formed by linkage of two norbornadiene-like P7 units. The P14 skeleton coordinates to four Ni(PBu3)2 groups. LiCp* and CoCl2 react with P7(SiMe3)3 to give [(Cp*Co)3-(P2)3] (3) with three Cp*Co groups bridged by P2 units. Reaction of FeCl2 and LiCp* with P7(SiMe3)3 yields [(Cp*Fe)3P6][FeCl3(thf)] (4) or [(Cp*Fe)3{n3-P3)Fe}P6] (5), depending on the reaction conditions. In 4 the structure of the Fe3P6 core of the [(Cp*Fe)3P6]+ cation is comparable to closo-B9H92-, while in 5 the Fe4P6 core does not obey the Wade rules. The unusual Co-As cluster [Co6As12(PEt2Ph)6] (6), prepared from K, As, and [CoCl2(PEt2-Ph)2], can be described as a Co6As6 heteroicosahedron linked to two Co3As3 octahedra by common Co3 faces. A theoretical treatment within the density functional approximation reproduces the experimental structures of 2 and 6 and allows an interpretation of molecular electronic structures. In 2 one finds P-P double bonds that are delocalized to some extent into vacant Ni AOs. For the cage compound 6 the Co 3 d AOs participate in cage bonding and 38 electrons can be assigned to cage bonds; this is in accord with the (2N + 2) rule for 18-atom cages but not with the usual electron counting rules.
    Additional Material: 8 Ill.
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    URL: http://dx.doi.org/10.1002/chem.19960020217
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  • 50
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    Dimensional reduction in II-VI materials: A2Cd3Q4 (A = K, Q = S, Se, Te; A = Rb, Q = S, Se), novel ternary low-dimensional cadmium chalcogenides produced by incorporation of A2Q in CdQ (1996)
    Weinheim : Wiley-Blackwell
    Chemistry - A European Journal 2 (1996), S. 656-666 
    Details
    ISSN: 0947-6539
    Keywords: cadmium compounds ; chalcogen compounds ; crystal structure ; dimensionality ; photoluminescence ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The synthesis of the isomorphous, layered chalcogenides K2Cd3S4 (I), Rb2Cd3S4 (II), K2Cd3Se4 (III), Rb2Cd3Se4 (IV), and K2Cd3Te4 (V) in molten A2Qx fluxes in reported (A = K, Rb; Q = S, Se, Te; x = 2 to 3). The compounds form as (Cd3Q4)n2n- layers interspersed with A + cations; the layers are composed of Cd3Q2-4 units shaped as truncated cubes. The compounds have room-temperature band gaps of 2.75, 2.92, 2.36, 2.37, and 2.26 eV for I, II, III, IV, and V, respectively, and also display strong photoluminescence. The thermal analysis data for all compounds are reported. The properties of these compounds are compared with those of the three-dimensional compounds CdS, CdSe, and CdTe, as well as those of the nanometer-sized CdQ clusters. A conceptual context is presented to connect all these different types of compounds.
    Additional Material: 15 Ill.
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    URL: http://dx.doi.org/10.1002/chem.1460020607
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    Synthesis, crystal structure, electronic structure, and properties of Hf2In5, a metallic hafnide with one-dimensional Hf-Hf and two-dimensional in-in bonding (1996)
    Weinheim : Wiley-Blackwell
    Chemistry - A European Journal 2 (1996), S. 800-804 
    Details
    ISSN: 0947-6539
    Keywords: crystal structure ; electronic structure ; hafnium compounds ; indium compounds ; metallic conductivity ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Hf2In5 - previously reported with the tentative composition “Hf3In4” - was prepared from the elements in a tantalum tube at 970 K. The X-ray diffractional characterization by means of single-crystal refinement reveals the presence of a tetragonal structure (a = 1024.71 (9), c = 305.66 (3) pm, P4/mbm, Z = 2) of Mn2Hg5 type. Hf2In5 is Pauli-paramagnetic and a good metallic conductor. Quasi-relativistic semiempirical and scalar-relativistic ab initio band structure calculations reveal Hf2In5 to be a hafnide, composed of a two-dimensional indium network threaded by infinite hafnium chains. The amount of In-In bonding scales counterintuitively with the interatomic distances.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/chem.1460020709
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    Conformational studies of chiral vinylogous sulfonamidopeptides (1996)
    Weinheim : Wiley-Blackwell
    Chemistry - A European Journal 2 (1996), S. 644-655 
    Details
    ISSN: 0947-6539
    Keywords: conformation ; crystal structure ; molecular modeling ; NMR spectroscopy ; sulfonamido-pseudopeptides ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The conformational preferences of chiral vinylogous aminosulfonic acids (vs-amino acids) and of the corresponding oligomers (vs-peptides) were investigated by a combination of X-ray crystallography, variable-temperature (VT) 1H NMR spectroscopy, FT-IR spectroscopy, and NOE experiments. The major source of conformational freedom in the monomers is the rotation around the C—C bond connecting the double bond with the allylic stereocenter (N—C*—C=C). The allylic conformational perferences can be altered in the oligomers by the formation of secondary structures enforced by hydrogen bonding. Twelve-membered-ring hydrogen bonding is detected in the crystal structure of vs-dipeptide 9, while fourteen-membered-ring bydrogen bonding is the most common folding pattern for the oligomers in chloroform solution. The experimental results are complemented by computer modeling: suitable force-field (FF) parameters for the unsaturated sulfonamide group nwere develiped from ab initio calculations. A Goodman-Still systematic pseudo-Monte-Carlo search was used for the conformational search. The conformers were minimized in chloroform with the GB/SA model. The calculations correctly predicted both the size of the hydrogen-bonded ring and its relative importance, in agreement with the experimental data in solution.
    Additional Material: 16 Ill.
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    URL: http://dx.doi.org/10.1002/chem.1460020606
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    Crystal structure and conformational disorder of poly(hexamethylene terephthalate) (1996)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part B: Polymer Physics 34 (1996), S. 83-92 
    Details
    ISSN: 0887-6266
    Keywords: poly(hexamethylene terephthalate) ; x-ray diffraction ; polymorphism ; conformation ; crystal structure ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Packing polymorphism and conformational disorder of poly(hexamethylene terephthalate) were analyzed by x-ray diffraction technique. The measurements were performed in the temperature range from 20 to 135°C. At high temperature, several unassignable reflections were found to disappear, and all reflections were satisfactorily indexed by single-chain unit cell. The crystal structures of β form (135°C) and β form (20°C) were similarly triclinic. The β′ unit cell assumed the double b-axis dimension, and the centrosymmetric conformations of the two chains adjacent along the b-axis differed in the orientation of the phenylene rings. At the elevated temperature (β form), the chains were indistinguishable by x-ray diffraction owing to the ring-flipping motion. The β and β′ structures were different in the local conformational disorder around the terephthaloyl groups. Conformational polymorphism of homologous poly(oligomethylene terephthalate)s was considered to originate from the difference in bulkiness of the aromatic and aliphatic residues. © 1996 John Wiley & Sons, Inc.
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    Poly(terephthalic anhydride) single crystals: Morphology and crystal structure (1996)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part B: Polymer Physics 34 (1996), S. 2843-2851 
    Details
    ISSN: 0887-6266
    Keywords: poly(terephthalic anhydride) ; crystal structure ; single crystals ; morphology ; confined thin film melt polymerization ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Single crystals of poly(terephthalic anhydride) (PTA) have been grown using the confined thin film melt polymerization technique. Thin lamellae (ca. 50 Å) are found for low polymerization temperatures, with thick crystals forming for polymerization at 200°C. Shearing of the material shortly after the initiation of polymerization at 200°C yielded single crystal domains composed of fibrillar texture material; these samples gave [010] zone ED patterns complementing the [001] zone patterns from the unsheared CTFMP samples. A monoclinic, single chain, two repeat unit, unit cell (Pc11) is proposed based on four different electron diffraction zone patterns: a = 6.01 Å, b = 3.945 Å, c = 14.11 Å, α = 106.9°. Simulations, using the Cerius2 program, of the corresponding molecular conformation, packing and electron diffraction (ED) patterns were performed; the ED simulations are in good agreement with the observed patterns. An R-factor of 0.23 is obtained based on a comparison of calculated and observed structure factors for the 39 independent ED reflections observed on the different zone patterns. © 1996 John Wiley & Sons, Inc.
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    A Modified Cyclodextrin with a Fully Encapsulated Dansyl Group: Self-Inclusion in the Solid State and in Solution (1996)
    Weinheim : Wiley-Blackwell
    Chemistry - A European Journal 2 (1996), S. 373-381 
    Details
    ISSN: 0947-6539
    Keywords: crystal structure ; cyclodextrins ; dansyl derivatives ; fluorescent sensors ; self-inclusion ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A monofunctionalized β-cyclodextrin containing a dansyl moiety, 6- deoxy- 6 - N - ( N′- (5- dimethylamino - 1 - naphthalenesulfonyl)diaminoethane) - β-cyclodextrin (CD-en-DNS, 2), was synthesized and its crystal structure determined. It was shown that the dansyl group is fully encapsulated within the cyclodextrin cavity, with the dimethylamino and sulfonyl groups emerging from opposite sides. The shape of the cavity is considerably flattened, since O(4)-O(4) distances parallel to the naphtalene ring were found to be longer than the others. The conformation of the diaminoethane linker was found to be determined by the inclusion of the dansyl group and by a hydrogen bond between the sulfonamide NH and one of the O(6)-H groups on the cyclodextrin rim. The self-inclusion features of the aromatic moiety were found to be consistent with the solution data: 1H NMR ROESY spectra suggested that the orientation of the dansyl moiety observed in the solid state was retained in aqueous solution; the circular dichroism spectrum was consistent with an axial complexation model. Fluorescence spectra showed that the inclusion of the dansyl group in the cyclodextrin cavity considerably increases the quantum yield: time-resolved fluorescence experiments showed the presence of a long-lifetime component (16.1 ns), which was attributed to the included fluorophore. The ability of 2 to act as a fluorescence sensor was evaluated by the addition of several guests of different shape: fluorescence intensity was lowered, especially upon addition of adamantanecarboxylic acid. All the data obtained were consistent with the model of the in-out movement of the dansyl group from the self-included conformation observed in the solid state to a position more exposed to the bulk solvent. Copper(II) was shown to enhance the difference in the fluorescence of 2 in the presence of guests by additional static quenching.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/chem.19960020404
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    Cesium Fluoride-Bromine Intercalation Compounds (1996)
    Weinheim : Wiley-Blackwell
    Chemistry - A European Journal 2 (1996), S. 1303-1307 
    Details
    ISSN: 0947-6539
    Keywords: bromine compounds ; cesium compounds ; crystal structure ; fluorides ; intercalation compounds ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: CsF reacts with Br2 to form the two intercalation compounds CsF·Br2 and 2CsF·Br2. The former consists of layers of CsF squares separated by layers of Br2 molecules oriented perpendicular to the CsF layers. 2CsF·Br2 is a second-stage compound, composed of two layers of CsF followed by one layer of bromine molecules. Iodine cannot replace bromine; instead, it reacts with CsF to form Cs2I8, and probably CsIF6 between 0° and 120 °C. Chlorine does not react at all with CsF. Bromine reacts with RbF only superficially, and after a long time some RbBr3 is observed; RbF and I2 give RbI3.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/chem.19960021018
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  • 57
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    310-Helices, Helix Screw Sense and Screw Sense Reversal in the Dehydro-peptide Boc-Val-ΔPhe-Gly-ΔPhe-Val-OMe (1996)
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Peptide Science 2 (1996), S. 47-58 
    Details
    ISSN: 1075-2617
    Keywords: Dehydro-peptides 310-helix ; helix reversal ; crystal structure ; circular dichroism ; Chemistry ; Biochemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The pentapeptide Boc-Val-ΔPhe-Gly-ΔPhe-Val-OMe, containing two dehydro-phenylalanine (ΔPhe) residues, has been synthesized and its structure investigated. In the crystalline state, the molecule adopts a right-handed 310-helical conformation stabilized by two intramolecular hydrogen bonds between CO of Val1 and NH of ΔPhe4, and between CO of ΔPhe2 and NH of Val5, respectively. NMR measurements are consistent with the presence of 310-helical structures also in acetonitrile and dimethylsulphoxide solution: the distances between backbone protons estimated from NOE connectivities are in overall agreement with those observed in the solid state; the chemical shifts of the amide protons show the smaller temperature coefficients for the NHs that in solid state are involved in intramolecular hydrogen bonds. The CD spectra in acetonitrile, chloroform, methanol and dimethylsulphoxide display exciton couplets of bands corresponding to the ΔPhe electronic transition at 280nm; the sign of the bands is consistent with the presence of helical structures having a prevalent left-handed screw sense. Addition of 1,1,1,3,3,3-hexafluoro- propan-2-ol gives rise to the gradual appearance of a couplet of opposite sign, suggesting the helix reversal from left-handed sense to right-handed sense. The conformational behaviour is discussed on the basis of the specific sequence of the peptide.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/psc.47
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    Folded Structures in Protonated Reduced Dipeptides (1996)
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Peptide Science 2 (1996), S. 381-391 
    Details
    ISSN: 1075-2617
    Keywords: conformational analysis ; crystal structure ; folded structures ; pseudopeptides ; reduced peptides ; Chemistry ; Biochemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reduced dipeptides with the general formula RCO-Xaa- rXbb-N+HR′R′′ (rXbb, reduced analogue of residue Xbb: NH-Cα HR1 -Cr H2) are shown to adopt a folded conformation in solution and in the solid state. The protonated reduced amide bond is an active proton donor capable of interacting with a peptide carbonyl to give a strong hydrogen bond topologically equivalent to the i+2 or i+3⇒ i interaction. The resulting conformation is similar to the γ- or β-turn structure found in peptides and proteins.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/psc.78
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  • 59
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    Preparation and crystal structure of the Copper Silicon Polyphosphide Cu4SiP8In memoriam Professor Wilhelm Klemm (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 53-56 
    Details
    ISSN: 0044-2313
    Keywords: Copper silicon polyphosphide Cu4SiP8 ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Darstellung und Kristallstruktur des Kupfer-Silicium-Polyphosphids Cu4SiP8Die neue Verbindung Cu4SiP8 wurde durch eine Festkörperreaktion aus den Elementen hergestellt. Sie kristallisiert mit einem neuen Strukturtyp, der aus Röntgen-Einkristalldiffraktometerdaten bestimmt worden ist: I41/a, a = 1 218,6(2) pm, c = 573,2(2) pm, Z = 8, R = 0,023 für 970 Strukturfaktoren und 31 variable Parameter. Tetraedrische SiP4-Gruppen sind über zusätzliche Phosphoratome zu einem dreidimensional-unendlichen Silicium-Phosphor-Netzwerk verknüpft, das Cu2-Paare mit oktaedrischer Phosphorumgebung umschließt, wie das von der nahe verwandten Struktur von CuP2 her bekannt ist. Die Verbindung kann mit Hilfe von Oxidationszahlen durch die Formel (Cu+1)4Si+4(P0)4(P-2)4 beschrieben werden, im Einklang mit dem Zintl-Klemm-Konzept.
    Notes: The new compound Cu4SiP8 was prepared by solid state reaction of the elemental components. It crystallizes with a new structure type, which was determined from single-crystal X-ray diffractometer data: I41/a, a = 1 218.6(2) pm, c = 573.2(2) pm, Z = 8, R = 0.023 for 970 structure factors and 31 variable parameters. Tetrahedral SiP4 groups are linked via additional phosphorus atoms to a three-dimensionally infinite silicon phosphorus network, accommodating Cu2 pairs with octahedral phosphorus coordination as is known for the closely related structure of CuP2. Using oxidation numbers the compound may be rationalized by the formula (Cu+1)4Si+4(P0)4(P-2)4 in agreement with the Zintl-Klemm concept.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19966220109
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    Neue arsinidenverbrückte Mehrkern-Clusterkomplexe des Ag und Au. Die Kristallstrukturen von [Ag14(AsPh)6Cl2(PR3)8], (PR3 = PEt3, PMenPr2, PnPr3), [M4(As4Ph4)2(PR3)4], (M = Ag, PR3 = PEt3, PnPr3; M = Au, PR3 = PnPr3), [Au10(AsPh)4(PhAsSiMe3)2(PnPr3)6]In memoriam Professor Wilhelm Klemm (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 45-52 
    Details
    ISSN: 0044-2313
    Keywords: Arsinidene-bridged silver clusters ; arsinidene-bridged gold clusters ; multinuclear complexes of silver and gold ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Arsinidene-bridged Multinuclear Cluster Complexes of Ag and Au. The Crystal Structures of [Ag14(AsPh)6Cl2(PR3)8], (PR3 = PEt3, PMenPr2, PnPr3), [M4(As4Ph4)2(PR3)4], (M = Ag, PR3 = PEt3, PnPr3; M = Au, PR3 = PnPr3), [Au10(AsPh)4(PhAsSiMe3)2(PnPr3)6]The reaction of AgCl with PhAs(SiMe3)2 in presence of tertiary phosphines (PR3) leads to arsinidene-bridged silver clusters with the composition [Ag14(AsPh)6Cl2(PR3)8], (PR3 = PEt3 1, PMenPr2 2, PnPr3 3). Further it is possible to obtain the multinuclear complexes [Ag4(As4Ph4)2(PR3)4], (PR3 = PEt3 4, PMenPr2 5). In analogy to that [PMe3AuCl] reacts with PhAs(SiMe3)2 and PnPr3 to form the compound [Au4(As4Ph4)2(PnPr3)4] 6, which is isostructurell to 4 and 5. The gold cluster [Au10(AsPh)4(PhAsSiMe3)2(PnPr3)6] 7 was obtained from the same solution. The structures were characterized by X-ray single crystal structure analysis.(Crystallographic data see “Inhaltsübersicht”)
    Notes: Bei der Reaktion von AgCl mit PhAs(SiMe3)2 bilden sich in Gegenwart der tertiären Phosphane PEt3, PMenPr2 und PnPr3 die Silbercluster der Zusammensetzung [Ag14(AsPh)6Cl2(PR3)8] (PR3 = PEt3 1, PMenPr2 2, PnPr3 3). Ferner konnten die Mehrkernkomplexe [Ag4(As4Ph4)2(PR3)4] (PR3 = PEt3 4, PMenPr2 5) isoliert werden. Bei analogen Umsetzungen von [PMe3AuCl] mit PhAs(SiMe3)2 und von PnPr3 bildet sich neben dem zu 4 und 5 isostrukturellen Goldkomplex [Au4(As4Ph4)2(PnPr3)4] 6 ein Goldcluster der Zusammensetzung [Au10(AsPh)4(PhAsSiMe3)2(PnPr3)6] 7. Die Strukturen von 1-7 konnten durch Kristallstrukturanalysen aufgeklärt werden.(1: Raumgruppe Pccn, a = 2 239,3(5) pm, b = 2 230,0(5) pm, c = 2 291,6(6) pm; 2: Raumgruppe P21/n, a = 1 703,1(9) pm, b = 2 241,0(20) pm, c = 1 730,8(14) pm, β = 98,79(4)°; 3: Raumgruppe P21/n, a = 1 741,8(3) pm, b = 2 260,0(9) pm, c = 1 867,5(5) pm, β = 94,63(2)°; 4: Raumgruppe P1, a = 1 535,2(4) pm, b = 1 599,3(3) pm, c = 1 644,5(5) pm, α = 90,90(2)°, β = 93,54(2)°, γ = 89,98(2)°; 5: Raumgruppe P1, a = 1 336,0(5) pm, b = 1 371,0(7) pm, c = 1 477,0(4) pm, α = 117,03(3)°, β = 93,93(2)°, γ = 103,82(3)°; 6: Raumgruppe P21/n, a = 1 305,9(2) pm, b = 2 227,1(3) pm, c = 1 619,6(4) pm, β = 108,38(2)°; 7: Raumgruppe 12, a = 1 948,5(3) pm, b = 1 638,9(5) pm, c = 2 148,7(4) pm, β = 94,93(1)°.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19966220108
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    Die Kristallstrukturen von α- und β-K3OClIn memoriam Professor Wilhelm Klemm (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 153-156 
    Details
    ISSN: 0044-2313
    Keywords: Tripotassium oxide chloride ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structures of α- and β-K3OClThe orange coloured compound K3OCl has been prepared. It exists in a low temperature modification (α-K3OCl) and a high temperature modification (β-K3OCl). The transition temperature is 364 ± 5 K. The crystal structures were determined by x-ray diffraction. α-K3OCl crystallizes at room temperature in the orthorhombic space group Pbnm (Z = 4) with the cell parameters a = b = 723.9(2) pm and c = 1 027.7(2) pm in the anti-GdFeO3-structure type. The high temperature modification β-K3OCl crystallizes (Z = 1) in the cubic space group Pm3m in the β-Ag3SI-structure type with a = 516.2(2) pm (T = 393 K).
    Notes: Die orangefarbene Verbindung K3OCl wurde dargestellt. Sie tritt in einer Tieftemperaturmodifikation (α-K3OCl) und in einer Hochtemperaturmodifikation (β-K3OCl) auf. Die Umwandlungstemperatur beträgt 364 ± 5 K. Die Kristallstrukturen wurden durch Röntgenstrukturanalyse aufgeklärt. α-K3OCl kristallisiert bei Raumtemperatur in der orthorhombischen Raumgruppe Pbnm (Z = 4) mit den Gitterkonstanten a = b = 723,9(2) pm und c = 1 027,7(2) pm im anti-GdFeO3-Strukturtyp. Die Hochtemperaturmodifikation, β-K3OCl, kristallisiert mit Z = 1 in der kubischen Raumgruppe Pm3m im β-Ag3SI-Strukturtyp mit a = 516,2(2) pm (T = 393 K).
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19966220121
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    Reindarstellung, Kristallzüchtung und Kristallstrukturbestimmung von IodtrioxidIn memoriam Professor Wilhelm Klemm (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 167-172 
    Details
    ISSN: 0044-2313
    Keywords: Iodine trioxide ; crystal structure ; Raman ; IR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Crystal Growth, and Crystal Structure Determination of Iodine TrioxideFor the first time, pure and single crystalline iodine trioxide has been obtained and its identity proven by a crystal structure determination, unambigously. It forms at slow decomposition of orthoperiodic acid in concentrated sulfuric acid at 70°C during 3-6 weeks. The crystal structure (triclinic, P1; a = 500.6(2), b = 674.1(3), c = 679.5(3) pm, α = 97.31(3), β = 96.43(3), γ = 105.36(3)°; 1754 independent reflections, R = 0.064) contains one I4O12 molecule per unit cell. The oxide can be regarded as a mixed anhydride formed by condensation of two molecules H5IO6 and HIO3, each. The axial atoms in an I2O10 doubleoctahedron are bridged by two IO groups. The pointsymmetry is C2h. The molecules are connected via short intermolecular oxygen iodine bridges to form twodimensional infinite layers. The crystal structure thus represents an intermediate between molecular and polymeric.
    Notes: Erstmals wurde Jodtrioxid in reiner und einkristalliner Form erhalten und seine Identität durch Röntgenstrukturanalyse eindeutig belegt. Es bildet sich bei langsamer Zersetzung von Orthoperiodsäure in konzentrierter Schwefelsäure bei 70°C im Verlaufe von 3-6 Wochen. In der Kristallstruktur (triklin, P1; a = 500,6(2), b = 674,1(3), c = 679,5(3) pm, α = 97,31(3), β = 96,43(3), γ = 105,36(3)°; 1754 unabhängige Reflexe, R = 0,064) liegt pro Elementarzelle ein I4O12-Molekül vor, das als gemischtes Anhydrid aus je zwei Molekülen H5IO6 und HIO3 aufgefaßt werden kann. Die axialen O-Atome in einem I2O10-Doppeloktaeder werden von IO-Gruppen verbrückt. Die Punktsymmetrie ist C2h. Die Moleküle werden über relativ kurze intermolekulare Sauerstoff-Iod-Brücken untereinander zu zweidimensional unendlichen Schichten verknüpft; die Kristallstruktur weist also eine hybride Natur zwischen Molekülkristall und kollektivem Festkörper auf.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19966220124
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    Strukturchemische und impedanzspektroskopische Untersuchungen an Mg2+-stabilisierten Na+/Pr3+-β″-Al2O3-KristallenIn memoriam Professor Wilhelm Klemm (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 191-196 
    Details
    ISSN: 0044-2313
    Keywords: Na-β″-alumina ; lanthanide ion exchange ; crystal structure ; impedance spectroscopy ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Structural Chemistry and Impedance Spectroscopy of Mg2+ stabilized Na+/Pr3+-β″-AluminasThe structure with the ionic distribution in the conduction planes of a Pr3+-exchanged Mg2+ stabilized Na+-β″-alumina crystal, composition determined by electron microprobe analysis to Na1.19Pr0.13Mg0.49Al10.49O17 (degree of exchange ξ = 25%, related to Na+ content), has been investigated by single crystal X-ray diffraction methods at room temperature (R3m, Z = 3, a = 561.8(2) pm, c = 3 361.5(11) pm). Pr3+ is slightly shifted in the ab-plane from the centrosymmetric 9 d (mO) into a 18 h site. Na+ occupies 18 h as well as 6 c (BR) positions. Ionic conductivity data of Mg2+ stabilized Na+/Pr3+-β″-Al2O3 crystals with varying degree of exchange determined by impedance spectroscopy are given in an Arrhenius diagram. With growing Pr3+ content the conductivity σ decreases with increasing activation energy.
    Notes: Die Struktur mit der Ionenverteilung in den Leitungsschichten eines Pr3+-ausgetauschten Mg2+-stabilisierten Na+-β″-Al2O3-Kristalls, analytisch durch Mikrosondemessungen bestimmte Zusammensetzung Na1,19Pr0,13Mg0,49Al10,49O17 (Austauschgrad ξ = 25%, bezogen auf Na+-Gehalt), wurde bei Raumtemperatur anhand röntgenographischer Einkristalldaten bestimmt (R3m, Z = 3, a = 561,8(2) pm, c = 3 361,5(11) pm). Pr3+ ist innerhalb der ab-Ebene geringfügig von der zentrosymmetrischen 9 d (mO) Lage in eine 18 h-Position ausgelenkt. Na+ besetzt sowohl die Punktlage 18 h als auch 6 c (BR). Impedanzspektroskopisch ermittelte Leitfähigkeitsdaten werden in Form eines Arrhenius-Diagramms für Mg2+-stabilisierte Na+/Pr3+-β″-Al2O3-Kristalle unterschiedlichen Austauschgrades vorgestellt. Mit zunehmendem Pr3+-Einbau fällt die Ionenleitfähigkeit σ, bei gleichzeitigem Anstieg der Aktivierungsenergie, ab.
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    URL: http://dx.doi.org/10.1002/zaac.19966220128
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    Syntheses and X-Ray Crystal Structures of 2-Aminoindenes and AminocymantrenesProfessor Gerhard Thiele zum 60. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 225-230 
    Details
    ISSN: 0044-2313
    Keywords: Aminoindene ; cymantrene ; zinc complex ; crystal structure ; manganese ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesen und Kristallstrukturen von 2-Aminoindenen und AminocymantrenenSubstituierte 2-Aminoindene werden in nahezu quantitativer Ausbeute bei der Reaktion von Aminen wie Methylpiperazin, Trimethylethylendiamin, 1,4-Diazacycloheptan und N,N′-Dimethylethylendiamin mit 2-Indanon gebildet. Diese 2-Aminoindene können deprotoniert und mit BrMn(CO)3(py)2 in 55-70% Ausbeute zu den entsprechenden Aminoindenyl-Cymantren-Derivaten umgesetzt werden. Die Einkristallstrukturanalysen von 2-(Methylpiperazin)indenylcymantren 5 (P1, a = 12.667(3) Å, b = 16.630(3) Å, c = 17.382(3) Å, α = 72.70(3)°, β = 74.59(3)°, γ = 88.66(3)°, V = 3364.1(12) Å3, Z = 8, R1(2σ(I)) = 4.02%, wR2(2σ(I)) = 10.30%) und die HClO4-Adduktes von 2-(Trimethylethylendiamin)indenyl-cymantren 6 (Cc, a = 23.722(5) Å, b = 6.9080 Å, c = 13.264 Å, β = 111.77(3)°, V = 2018.6(7) Å3, Z = 4, R1(2σ(I)) = 2.94%, wR2(2σ(I)) = 7.90%) wurden bestimmt. In beiden Komplexen weist das am Indenyl-Stickstoff gebundene Kohlenstoffatom deutlich längere Bindungen zum Mangan auf [223.5(3) - 225.8(3) pm] als die vier anderen Kohlenstoffatome [213.3(3) - 219.1(3) pm]. Die kurzen Indenyl-Stickstoff-Abstände von 136.2(4) und 137.8(4) pm belegen den substantiellen Mehrfachbindungscharakter dieser Bindung. Die Komplexierung von Zn2+ durch die Stickstoffatome in 6 hat deutliche Verschiebungen der CO-Valenzschwingungen zur Folge.
    Notes: Substituted 2-aminoindenes have been synthesized in almost quantitative yields by reactions of amines such as methylpiperazine, trimethylethylenediamine, 1,4-diaza-cycloheptane and N,N′-dimethylethylenediamine with 2-indanone. The 2-aminoindenes can be deprotonated and reacted with BrMn(CO)3(Py)2 to produce the respective aminoindenyl-cymantrenes in yields between 55-70%. The X-ray crystal structures of 2-(methylpiperazine)indenyl-cymantrene 5 (P1, a = 12.667(3) Å, b = 16.630(3) Å, c = 17.382(3) Å, α = 72.70(3)°, β = 74.59(3)°, γ = 88.66(3)°, V = 3364.1(12) Å 3, Z = 8, R1(2σ(I)) = 4.02%, wR2(2σ(I)) = 10.30%) and the HClO4 adduct of 2-(trimethylethylenediamine)-indenyl-cymantrene 6 (Cc, a = 23.722(5) Å, b = 6.9080 Å, c = 13.264 Å, β = 111.77(3)°, V = 2018.6(7) Å 3, Z = 4, R1(2σ(I)) = 2.94%, wR2(2σ(I)) = 7.90%) were determined. In both complexes the indenyl-carbon bonded to nitrogen displays significantly longer bonds to manganese [223.5(3)-225.8(3) pm] than the other four carbon atoms [213.3(3)-219.1(3) pm]. The short indenyl-nitrogen bonds of 136.2(4) and 137.8(4) pm are indicative of a substantial multiple bond character. The complexation of Zn2+ by the nitrogen atoms of 6 results in significant shifts of the CO stretching frequencies.
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    Li2PtH2, Darstellung und StrukturProfessor John D. Corbett zum 70. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 462-464 
    Details
    ISSN: 0044-2313
    Keywords: Metal hydrides ; platinum ; crystal structure ; neutron diffraction ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Li2PtH2, Synthesis and StructureThe synthesis of Li2PtH2 succeeded in decomposing Li5Pt2H9 at 220°C in an argon atmosphere. X-ray investigations on a powdered sample and elastic neutron diffraction experiments on the deuterated compound led to the complete structure. Li2PtH2 crystallizes in the space group Immm with Z = 2. The structure is characterized by [PtH2]2- -dumb-bells which are hitherto unknown in platinum compounds. The arrangement of the [PtH2]2- -anions and of the lithium cations shows a close relationship to the hydride Li2PdH2 which crystallizes tetragonal I-centred.
    Notes: Die Darstellung von Li2PtH2 gelang aus Li5Pt2H9 durch eine Abbaureaktion bei 220°C in einer Argonatmosphäre. Röntgenographische Untersuchungen an pulverförmigen Proben und elastische Neutronenbeugungsexperimente an der deuterierten Verbindung führten zur vollständigen Strukturaufklärung. Li2PtH2 kristallisiert in der Raumgruppe Immm mit Z = 2. Die Anordnung der in Platinverbindungen bisher unbekannten linearen [PtH2]2- -Baueinheiten und der Lithiumionen zeigt eine nahe Verwandtschaft zum tetragonal kristallisierenden Hydrid Li2PdH2.
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    On Mixed-Valence Dinuclear PtII, PtIII Nucleobase Complexes Derived from cis-Diamineplatinum(II): Effect of steric bulk of amine ligands on the Pt-oxidation stateProfessor Gerhard Thiele zum 60. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 267-274 
    Details
    ISSN: 0044-2313
    Keywords: Mixed-valence platinum complexes ; nucleobase complexes ; 1-methyluracil ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Über gemischtvalente, zweikernige PtII, PtIII-Nukleobase-Komplexe des cis-Diaminplatin(II): Einfluß des Raumbedarfs der AminligandenEine Reihe verwandter Zweikernkomplexe des PtII der Zusammensetzung cis-[a2PtL2Pta2′]2+ mit a,a′ = NH3 oder CH3NH2 und L = 1-Methyluracilat-N3,O4 (1-MeU) oder 1-Methylthyminat-N3,O4 (1-MeT) in Kopf-Kopf-Anordnung wird beschrieben und ihr Lösungsverhalten gegenüber Oxidation mittels CeIV studiert. Die Kristallstrukturanalyse eines repräsentativen Vertreters, cis-[(CH3NH2)2Pt(1-MeU)2Pt(CH3NH2)2](ClO4)2 · 0.5 H2O (1b), wird beschrieben: Monoklines System, Raumgruppe P21/c, a = 11.907(7) Å, b = 19.087(14) Å, c = 12.525(7) Å, β = 90.49(4)°, Z = 4. Oxidation dieser Diplatin(II)-Verbindungen ([Pt2.0]2) mittels CeIV in wäßriger Lösung zu den entsprechenden Diplatin(III)-Spezies ([Pt3.0]2) erfolgt entweder über gemischtvalente vierkernige [Pt2.25]4 oder zweikernige [Pt2.5]2 Zwischenstufen, je nach Natur der a′-Liganden: Für a′ = NH3 wird blaugrünes [Pt2.25]4 gebildet, wohingegen mit a′ = CH3NH2, violettes [Pt2.5]2 auftritt. Dieser Unterschied läßt sich auf den unterschiedlichen Raumbedarf von NH3- und CH3NH2-Liganden in trans-Position zu den O(4)-Gruppen der verbrückenden Nukleobasen zurückführen und damit auf das Vermögen von Diplatin-Komplexen, über die O(4)2Pt a′2-Ebenen zu stapeln.
    Notes: A series of closely related dinuclear (head-head) PtII complexes of general composition cis-[a2PtL2Pta′2]2+ with a,a′ = NH3 or CH3NH2 and L = 1-methyluracilate-N3,O4 (1-MeU) or 1-methylthyminate-N3,O4 (1-MeT) has been prepared and the solution behavior toward CeIV oxidation studied. The X-ray crystal structure of a representative example cis-[(CH3NH2)2Pt(1-MeU)2Pt(CH3NH2)2](ClO4)2 · 0.5 H2O (1b), has been determined: Monoclinic, space group P21/c, a = 11.907(7) Å, b = 19.087(14) Å, c = 12.525(7) Å, β = 90.49(4)°, Z = 4. Oxidation of these diplatinum(II) complexes ([Pt2.0]2) with CeIV in aqueous solution to the corresponding diplatinum(III) species ([Pt3.0]2) proceeds via tetranuclear [Pt2.25]4 or dinuclear [Pt2.5]2 mixed-valence state compounds, depending on the nature of the a′ ligands: with a′ = NH3, blue green [Pt2.25]4 forms, whereas with a′ = CH3NH2, purple [Pt2.5]2 represents the intermediate. This difference is interpreted in terms of differences in bulk between NH3 and CH3NH2 ligands trans to the O(4) positions of the bridging nucleobases which influence the ability of dinuclear species to associate via the O(4)2 Pt a2′ faces.
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    Trigonal-planare CuX3-Gruppen in Cu2Mo6X14, X = Cl, Br, IProfessor Herbert Jacobs zum 60. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 663-669 
    Details
    ISSN: 0044-2313
    Keywords: Dicopper(I)-octa-μ3-halogeno-hexahalogeno-octahedro-hexamolybdate(II) ; crystal structure ; Mo6X14-group ; trigonal planar CuX3-group ; ionic conduction ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Trigonal Planar CuX3-Groups in Cu2Mo6X14, X = Cl, Br, ICu2Mo6Cl14 (I), Cu2Mo6Br14 (II) and Cu2Mo6I14 (III) were synthesized by thermal treatment of corresponding mixtures of copper(I) and molybdenum(II) halides. The crystal structures were determined by single crystal X-ray analyses. I and II show isotypism, cubic, Pn3 (no. 201, sec. setting), Z = 4, I: a = 12.772(3) Å, II: a = 13.350(2) Å. III shows a new structural type, orthorhombic, Pbca (No. 61), Z = 4, a = 16.058(3) Å, b = 10.643(2) Å, c = 16.963(3) Å. Trigonal planar CuX3 units were found in I—III. Structural behaviour relations are discussed, especially with regard to ionic conductivity.
    Notes: Cu2Mo6Cl14 (I), Cu2Mo6Br14 (II) und Cu2Mo6I14 (III) wurden durch thermische Behandlung der Gemenge der binären Halogenide CuX und Mo6X12 im molaren Verhältnis 2:1 in einkristalliner Form erhalten. Röntgenographische Strukturbestimmung wurde an Einkristallen durchgeführt. I und II zeigen Isotypie, Pn3 (Nr. 201, sec. setting) Z = 4, I: a = 12,772(3) Å, II: a = 13,350(2) Å. III weist eigenen Strukturtyp auf: Pbca (Nr. 61), Z = 4, a = 16,058(3) Å, b = 10,643(2) Å, c = 16,963(3) Å. In I—III liegen trigonal planare CuX3-Gruppen vor. Bindungsverhältnisse und Meßergebnisse der Ionenleitfähigkeit werden diskutiert.
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    URL: http://dx.doi.org/10.1002/zaac.19966220415
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    Hydrogensulfate mit fehlgeordneten Wasserstoffatomen - Synthese und Struktur von Li[H(HSO4)2](H2SO4)2 sowie Verfeinerung der Struktur von α-NaHSO4Professor Gerhard Thiele zum 60. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 337-342 
    Details
    ISSN: 0044-2313
    Keywords: Hydrogen sulfate of sodium and lithium ; synthesis ; crystal structure ; disordered hydrogen atoms ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Hydrogen Sulfates with Disordered Hydrogen Atoms - Synthesis and Structure of Li[H(HSO4)2](H2SO4)2 and Refinement of the Structure of α-NaHSO4The structure of Li[H(HSO4)2](H2SO4)2 has been determined for the first time whereas the structure of α-NaHSO4 has been refined, so that direct determination of the hydrogen positions was possible. Both compounds crystallize triclinic in the space group P1 with the lattice constants a = 6.708(2), b = 6.995(1), c = 7.114(1) Å, α = 75.53(1), β = 84.09(2) and γ = 87.57(2)° (Z = 4) for α-NaHSO4 and a = 4.915(1), b = 7.313(1), c = 8.346(2) Å, α = 82.42(3), β = 86.10(3) and γ = 80.93(3)° (Z = 1) for Li[H(HSO4)2](H2SO4)2. In both compounds there are disordered hydrogen positions.In the structure of α-NaHSO4 there are two crystallographically different HSO4- tetrahedra and two different coordinated Na atoms. The system of hydrogen bonds can be described by chains in [0-11] direction. The disordering of the H atoms reduces the differences between the S—O and S—OH distances (1.45 and 1.50 Å) while in the ordered HSO4 unit “regular” bond lengths are observed (1.45 und 1,57 Å).In the structure of Li[H(HSO4)2](H2SO4)2 there are two crystallographically different SO4-tetrahedra. The first one belongs to the [H(HSO4)2]- unit while the second one represents H2SO4 molecules. The H atom which is located nearby the symmetry centre and connects two HSO4 units by a short O…O distance of 2.44 Å. Li is located on a symmetry centre and is slightly distorted octahedrally coordinated by oxygen atoms of six different SO4 tetrahedra. The system of hydrogen bonds can be regarded as consisting of double layers parallel to the xy-plane.
    Notes: Von Li[H(HSO4)2](H2SO4)2 konnte die Struktur erstmals bestimmt und für α-NaHSO4 so verfeinert werden, daß die direkte Bestimmung der Wasserstoffpositionen möglich wurde. Beide Verbindungen kristallisieren in der triklinen Raumgruppe P1 mit den Gitterkonstanten a = 6,708(2), b = 6,995(1), c = 7,114(1) Å, α = 75,53(1), β = 84,09(2) und γ = 87,57(2)° (Z = 4) für α-NaHSO4 sowie a = 4,915(1), b = 7,313(1), c = 8,346(2) Å, α = 82,42(3), β = 86,10(3) und γ = 80,93(3)° (Z = 1) für Li[H(HSO4)2](H2SO4)2. Beiden Verbindungen ist gemeinsam, daß fehlgeordnete Wasserstoffpositionen vorliegen.In der Struktur von α-NaHSO4 liegen zwei kristallographisch unterschiedliche HSO4--Tetraeder und zwei verschieden koordinierte Na-Atome vor. Das Wasserstoffbrückensystem läßt sich durch Ketten mit Seitenabzweigungen beschreiben. Die Fehlordnung der H-Atome einer HSO4-Gruppe nivelliert die Unterschiede zwischen den S—O- und S—OH-Abständen (1,45 und 1,50 Å), während in der geordneten HSO4-Gruppe die üblicherweise vorliegenden Bindungslängen gefunden werden (1,45 und 1,57 Å).In der Struktur des Li[H(HSO4)2](H2SO4)2 treten zwei kristallographisch unterschiedliche SO4-Tetraeder auf. Dabei gehört eines zu der [H(HSO4)2]--Einheit während das zweite das H2SO4-Molekül darstellt. Das in der Nähe eines Symmetriezentrums liegende H-Atom verbindet zwei HSO4-Gruppen mit einem kurzen O…O-Abstand von 2,44 Å. Li liegt in einem Symmetriezentrum und wird durch Sauerstoff von sechs verschiedenen SO4-Tetraedern schwach verzerrt oktaedrisch koordiniert. Das System der Wasserstoffbindungen läßt sich als Doppelschicht beschreiben.
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    CuClS0.94Te1.06 und CuBrS0.92Te1.08, zwei neue Kupfer(I)-chalkogenhalogenide mit neutralen ∞1[STe]-Schrauben (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 853-857 
    Details
    ISSN: 0044-2313
    Keywords: Copper(I) sulfur tellurium halides ; chalcogen ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: CuClS0.94Te1.06 and CuBrS0.92Te1.08, Two New Copper(I) Chalcogen Halides Containing Neutral ∞1[STe] ScrewsCuClS0.94Te1.06 and CuBrS0.92Te1.08 are two new, isotypic compounds of general composition CuXYY′ (X = halide, Y, Y′ = chalcogen) with a mixed chalcogen substructure. They crystallize in the monoclinic system, space group P21/n (No. 14), a = 7.878(2), b = 4.727(1), c = 10.759(2) Å, β = 103.97(2)°, V = 388.8(2) Å3 (CuClS0.94Te1.06) and a = 8.043(3), b = 4.746(2), c = 11.240(4) Å, β = 103.46(3)°, V = 417.3(3) Å3 (CuBrS0.92Te1.08), both with Z = 4. The crystal structures are dominated by ordered ∞1[STe±0]-screws. From a crystal chemical point of view the sulfur and tellurium atoms are significantly different. The melting points are 341 °C (CuClS0.94Te1.06) and 336 °C (CuBrS0.92Te1.08). The compounds CuXYY′ (X = Cl, Br, I; Y, Y′ = S, Se, Te) are compared and discussed.
    Notes: Mit CuClS0.94Te1.06 und CuBrS0.92Te1.08 wurden zwei neue, isotype Verbindungen der Zusammensetzung CuXYY′ (X = Halogenid, Y, Y′ = Chalkogen) mit gemischtem Chalkogenteilgitter erhalten. Sie kristallisieren monoklin, RG P21/n (Nr. 14) mit a = 7,878(2), b = 4,727(1) und c = 10,759(2) Å, β = 103,97(2)°, V = 388,8(2) Å3 (CuClS0.94Te1.06) bzw. a = 8,043(3), b = 4,746(2) und c = 11,240(4) Å, β = 103,46(3)°, V = 417,3(3) Å3 (CuBrS0.92Te1.08), jeweils mit Z = 4. Strukturbestimmendes Merkmal sind die geordneten ∞1[STe±0]-Schrauben. Kristallchemisch sind die Schwefel- und Telluratome deutlich unterschiedlich. Die Schmelzpunkte liegen bei 341 °C (CuClS0.94Te1.06) bzw. 336 °C (CuBrS0.92Te1.08). Die Strukturen von CuXYY′ (X = Cl, Br, I; Y, Y′ = S, Se, Te) werden verglichen und diskutiert.
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    Ba4[WN4]Cl2: The first nitridotungstate(VI) chloride (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 885-888 
    Details
    ISSN: 0044-2313
    Keywords: Barium tetra nitridotungstate(VI) dichloride ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ba4[WN4]Cl2: Das erste Nitridowolframat(VI)-chloridDurch Umsetzung von Ba(NH2)2 mit W in einer KCl-Schmelze bei 850°C unter strömendem Stickstoff wurden transparente gelbe Kristalle von Ba4[WN4]Cl2 gezüchtet. Die Verbindung kristallisiert monoklin in P21/m und Z = 2 mit den Zellparametern a = 8,447(4) Å, b = 6,143(2) Å, c = 10,727(6) Å und β = 99,04(4)°. Die Kristallstruktur enthält isolierte Ionen [WN4]6- und Cl-. Es ist das erste bisher beschriebene Nitridowolframat(VI)-chlorid.
    Notes: Transparent yellow crystals of Ba4[WN4]Cl2 were grown at 850°C by the reaction of Ba(NH2)2 with W in a KCl melt under flowing nitrogen. The compound crystallizes monoclinic in P21/m and Z = 2 with the cell parameters a = 8.447(4) Å, b = 6.143(2) Å, c = 10.727(6) Å and β = 99.04(4)°. The crystal structure contains isolated anions [WN4]6- and Cl-. It is the first nitridotungstate(VI) chloride reported so far.
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    Cs5[Na{W4N10}]: The first framework nitridotungstate(VI)Professor Wolfgang Jeitschko zum 60. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 881-884 
    Details
    ISSN: 0044-2313
    Keywords: Penta caesium sodium nitrido tetra tungstate(VI) ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Cs5[Na{W4N10}]: Das erste Nitridowolframat(VI) mit GerüststrukturCs5[Na{W4N10}] wurde aus einem Gemenge von NaNH2, CsNH2 und Wolframpulver (Molverhältnis 1 : 10 : 4) bei 700°C in Autoklaven dargestellt. Nach beendeter Reaktion ist das Nitrid in einer Alkalimetallmatrix eingebettet. Dunkelrote Kristalle werden durch Auswaschen des Alkalimetalls mit flüssigem Ammoniak bei Raumtemperatur isoliert. Die Struktur von Cs5[Na{W4N10}] wurde über Röntgeneinkristalldaten bestimmt: I41 (Nr. 80), Z = 4, a = 13,926(3) Å, c = 8,723(3) Å, Z(Fo2) ≥ 3σ(Fo2) = 1535, Z(Variable) = 63, R/Rw = 0,040/0,052.An feuchter Luft hydrolysiert die Verbindung schnell zu Oxowolframat und Ammoniak. Sie enthält ein Tetraedergerüst ∞3[WNN3/21.5-]. Natrium ist von vier terminalen Stickstoffliganden umgeben. Einschließlich des Natriums ergibt sich eine Anordnung vom β-Cristobalittyp ∞3[Na{W4N10}5-]. Dieses enthält Caesium in allen Lücken, sogenannten Friauf-Polyedern, die durch zwölf Stickstoffliganden gebildet werden.
    Notes: Cs5[Na{W4N10}] was prepared from a mixture of NaNH2, CsNH2 and tungsten powder (molar ration 1 : 10 : 4) at 700°C in autoclaves. After the reaction is finished the nitride is embedded in an alkali metal matrix. Dark red crystals were isolated by washing out the alkali metal with liquid ammonia at room temperature. The structure of Cs5[Na{W4N10}] was solved by X-ray single crystal data: I41 (No. 80), Z = 4, a = 13.926(3) Å, c = 8.723(3) Å, Z(Fo2) ≥ 3σ(Fo2) = 1535, Z(Variables) = 63, R/Rw = 0.040/0.052.The compound is highly sensitive against moisture giving oxotungstates and ammonia. It contains a framework of tetrahedra ∞3[WNN3/21.5-]. Sodium shares four terminal nitrogen ligands. Including sodium a distorted, β-cristobalite type arrangement ∞3[Na{W4N10}5-] results. It contains caesium in all interstices formed by twelve nitrogen ligands in so-called Friauf polyhedra.
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    Darstellung und Eigenschaften von Diphthalocyaninaten des Bismuts, [Bi(Pc)2]k (k = 1-, 0, 1+); Kristallstruktur von gemischtvalentem [Bi(Pc)2] · CH2Cl2 (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 873-880 
    Details
    ISSN: 0044-2313
    Keywords: Diphthalocyaninates ; bismuth(III) compounds ; crystal structure ; electrochemistry ; optical spectra ; vibrational spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Properties of Diphthalocyaninates of Bismuth, [Bi(Pc)2]k (k = 1-, 0, 1+); Crystal Structure of mixed-valent [Bi(Pc)2] · CH2Cl2Blue di(phthalocyaninato(2-))bismuthate(III), [Bi(Pc2-)2]-, is obtained by the reaction of BiO(NO3) with molten 1,2-dicyanobenzene in the presence of potassium methylate and isolated as tetra-n-butylammonium (nBu4N)+ and bis(triphenylphosphine)iminium (PNP)+ salt. Green mixed-valent [Bi(Pc)2] · CH2Cl2 is prepared by anodic oxidation of [Bi(Pc2-)2]-. It crystallizes in the orthorhombic γ modification (Pnma; a = 28.176(5), b = 22.913(3), c = 7.925(1) Å, Z = 4). The BiIII ion is eightfold coordinated by the Niso atoms of the slightly distorted Pc ligands in a square antiprismatic manner. The average Bi—Niso bond distance is 2.467 Å. The complex is paramagnetic (μeff = 1.84 μB). Oxidation of [Bi(Pc2-)2]- with bromine yields purple, diamagnetic [Bi(Pc-)2]Brx (1.5 ≤ x ≤ 2.5). The redox properties are investigated electrochemically. UV-Vis-NIR, MIR/FIR and resonance Raman spectra of the new bismuth(III) complexes are discussed and compared with those of diphthalocyaninates of the lanthanides.
    Notes: Blaues Di(phthalocyaninato(2-))bismutat(III), [Bi(Pc2-)2]-, wird aus BiO(NO3) mit geschmolzenem Phthalodinitril bei Anwesenheit von Kaliummethylat dargestellt und als Tetra-n-butylammonium(nBu4N)+ - und Bis(triphenylphosphin)-iminium(PNP)+-Salz isoliert. Grünes gemischtvalentes [Bi(Pc)2] · CH2Cl2 wird durch anodische Oxydation von [Bi(Pc2-)2]- synthetisiert. Dieses kristallisiert in der orthorhombischen γ-Modifikation (Pnma; a = 28,176(5) Å, b = 22,913(3) Å, c = 7,925(1) Å, Z = 4). Das BiIII-Ion ist von den acht Stickstoff-Atomen der Isoindol-Einheiten (Niso) der beiden wenig verzerrten Pc-Liganden quadratisch-antiprismatisch koordiniert. Der mittlere Bi—Niso-Abstand beträgt 2,467 Å. Die Verbindung ist paramagnetisch (μeff = 1,84 μB). Mit Brom reagiert [Bi(Pc2-)2]- zu rot-violettem, diamagnetischem [Bi(Pc-)2]Brx (1,5 ≤ x ≤ 2,5). Das Redox-Verhalten wird elektrochemisch untersucht. Die UV-Vis-NIR-, FIR/MIR- und Resonanz-Raman-Spektren der drei neuen Bismut-Komplexe werden diskutiert und mit denen der Diphthalocyaninate der Lanthanide verglichen.
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    Zur Kenntnis von Na4Br(NH2)3: Ein Amidbromid im System NaNH2/NaBr (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 895-897 
    Details
    ISSN: 0044-2313
    Keywords: Sodium triamide bromide ; synthesis ; single-crystals ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Na4Br(NH2)3: An Amide Bromide in the System NaNH2/NaBrThe pseudobinary system NaNH2/NaBr was investigated by X-ray methods. The crystal structure of Na4Br(NH2)3 was solved by single crystal data: Pnnm, Z = 4, a = 6.579(2) Å, b = 12.755(4) Å, c = 8.776(2) Å Z(Fo) with (Fo)2 ≥ 3σ = (Fo)2 = 503, Z(parameter) = 39, R/Rw = 0.082/0.106.It is a new type of structure, built up by a three-dimensional network of ∞3[Na4(NH2)3+] containing the bromide ions.
    Notes: Das pseudobinäre System NaNH2/NaBr wurde röntgenographisch untersucht und die Struktur von Na4Br(NH2)3 über Einkristalldaten aufgeklärt: Pnnm, Z = 4, a = 6,579(2) Å, b = 12,755(4) Å, c = 8,776(2) Å, Z(Fo) mit (Fo)2 ≥ 3σ(Fo)2 = 503, Z(Parameter) = 39, R/Rw = 0,082/0,106.Es liegt ein eigener Strukturtyp vor, der aus einem dreidimensionalen Netzwerk von ∞3[Na4(NH2)3+] aufgebaut ist, das Br- enthält.
    Additional Material: 4 Ill.
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    Das prismatische Te62+-Ion in der Struktur von Te6(NbOCl4)2Professor Hans Georg von Schnering zum 65. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 823-828 
    Details
    ISSN: 0044-2313
    Keywords: Tellurium ; niobium oxytrihalides ; hexatellurium(2+) ; tetrachlorooxoniobate (1-) ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Prismatic Te62+ Ion in the Structure of Te6(NbOCl4)2Te6(NbOCl4)2 is obtained from Te, TeCl4 and NbOCl3 at 200°C. It crystallizes triclinic, space group P1 (a = 915,5(4) pm, b = 1655,3(6) pm, c = 3134,4(9) pm, α = 42,62(2)°, β = 117,12(6)°, γ = 138,24(8)°). The crystal structure analysis shows, that the structure is built of one-dimensional polymeric ∞1[NbOCl4-] chains in which the monomers are linked via linear O—Nb—O-bridges and from discrete Te62+ polycations that are also arranged in strands, but without significant interactions. The structure is closley related but not isotypic to the previously reported tungsten containing analogue Te6(WOCl4)2 (monoclinic, P21/c). A comparison of the two structures shows that rotations of the cationic strands relative to the anionic strands lead to different cation-anion interactions.
    Notes: Te6(NbOCl4)2 wird aus Te, TeCl4 und NbOCl3 bei 200°C erhalten. Es kristallisiert triklin, P1, a = 915,5(4) pm, b = 1655,3(6) pm, c = 3134,4(9) pm, α = 42,62(2)°, β = 117,12(6)°, γ = 138,24(8)°. Die Kristallstrukturanalyse zeigt, daß die Struktur aus eindimensional-polymeren, über O-Atome verknüpften ∞1[NbOCl4-]-Strängen und aus diskreten, strangartig angeordneten Te62+-Polykationen aufgebaut ist. Die Struktur ist eng verwandt, aber nicht isotyp mit derjenigen der analogen wolframhaltigen Verbindung Te6(WOCl4)2 (monoklin, P21/c). Ein Strukturvergleich zeigt, daß Verdrehungen der Kationenstränge relativ zu den Anionensträngen zu unterschiedlichen Kation-Anionwechselwirkungen führen.
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    URL: http://dx.doi.org/10.1002/zaac.19966220513
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    Magnesiumphthalocyanine: Darstellung und Eigenschaften von Halogenophthalocyaninatomagnesat, [Mg(X)Pc2-]- (X = F, Cl, Br); Kristallstruktur von Bis(triphenylphosphin)iminiumchloro(phthalocyaninato)magnesat-Aceton-Solvat (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1085-1090 
    Details
    ISSN: 0044-2313
    Keywords: Magnesium compound ; phthalocyanine complex ; crystal structure ; vibrational spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Magnesium Phthalocyanines: Synthesis and Properties of Halophthalocyaninatomagnesate, [Mg(X)Pc2-]- (X = F, Cl, Br); Crystal Structure of Bis(triphenylphosphine)iminiumchloro-(phthalocyaninato)magnesate Acetone SolvateMagnesium phthalocyanine reacts with excess tetra(n-butyl)ammonium- or bis(triphenylphosphine)iminiumhalide ((nBu4N)X or (PNP)X; X = F, Cl, Br) yielding halophthalocyaninatomagnesate ([Mg(X)Pc2-]-; X = F, Cl, Br), which crystallizes in part as a scarcely soluble (nBu4N) or (PNP) complex-salt. Single-crystal X-ray diffraction analysis of b(PNP)[Mg(Cl)Pc2-] · CH3COCH3 reveals that the Mg atom has a tetragonal pyramidal coordination geometry with the Mg atom displaced out of the center (Ct) of the inner nitrogen atoms (Niso) of the nonplanar Pc ligand toward the Cl atom (d(Mg—Ct) = 0.572(3) Å; d(Mg—Cl) = 2.367(2) Å). The average Mg—Niso distance is 2.058 Å. Pairs of partially overlapping anions are present. The cation adopts a bent conformation (b(PNP)+: d(P1—N(K)) = 1.568(3) Å; d(P2—N(K)) = 1.587(3) Å; ∡(P1—N(K)—P2) = 141.3(2)°). Electrochemical and spectroscopic properties are discussed.
    Notes: Magnesiumphthalocyanin reagiert mit überschüssigem Tetra(n-butyl)ammonium- oder Bis(triphenylphosphin)iminiumhalogenid ((nBu4N)X oder (PNP)X; X = F, Cl, Br) zu Halogenophthalocyaninatomagnesat ([Mg(X)Pc2-]-; X = F, Cl, Br), welches teilweise als wenig lösliches (nBu4N)- oder (PNP)-Komplexsalz kristallisiert. Die Kristallstrukturanalyse von b(PNP)[Mg(Cl)Pc2-] · CH3COCH3 bestätigt die tetragonal-pyramidale Koordinationsgeometrie des Mg-Atoms, wobei dieses aus dem Zentrum (Ct) der inneren vier Stickstoffatome (Niso) des nicht-planaren Pc-Liganden in Richtung des Cl Atoms verschoben ist (d(Mg—Ct) = 0,572(3) Å; d(Mg—Cl) = 2,367(2) Å). Der mittlere Mg—Niso-Bindungsabstand beträgt 2,058 Å. Im festen Zustand bilden je zwei Anionen partiell überlappende Dimere. Das Kation liegt in gewinkelter Konformation vor (b(PNP)+: d(P1—N(K)) = 1,568(3) Å; d(P2—N(K)) = 1,587(3) Å; ∡(P1—N(K)—P2) = 141,3(2)°). Elektrochemische und spektroskopische Eigenschaften werden diskutiert.
    Additional Material: 6 Ill.
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    Darstellung und Kristallstruktur von Rb2Ni3Se4Professor Herbert Jacobs zum 60. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 627-629 
    Details
    ISSN: 0044-2313
    Keywords: Ternary metal selenides ; crystal structure ; MAPLE ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Crystal Structure of Rb2Ni3Se4The compound Rb2Ni3Se4 was synthesized by heating a mixture of rubidium carbonate, nickel and selenium at 850°C in an atmosphere of hydrogen. The compound has a golden lustre and crystallizes with the K2Pd3S4-type structure; a = 10.555(3) Å, b = 27.588(6) Å, c = 6.031(6) Å, Z = 8, Fddd (No. 70).The structure can be described as a stacking of layers of the composition Rb2Ni3Se4 with a stacking sequence abcd. The electrostatic part of lattice energy (MAPLE) will be discussed for compounds of the compositions A2M3X4 (A K, Rb, Cs; M Ni, Pd, Pt and X S, Se).
    Notes: Die Darstellung von Rb2Ni3Se4 gelang durch Umsetzung von Rubidiumcarbonat, Nickel und Selen in einem Wasserstoffstrom bei 850°C. Die goldfarbig glänzende Verbindung kristallisiert im K2Pd3S4-Typ; a = 10,555(3) Å, b = 27,588(6) Å, c = 6,031(6) Å, Z = 8, Fddd (Nr. 70).Die Struktur läßt sich als Stapelung von Schichten der Zusammensetzung Rb2Ni3Se4 mit der Stapelfolge abcd beschreiben. Der elektrostatische Anteil der Gitterenergie (MAPLE) wird für Verbindungen des Typs A2M3X4 (mit A K, Rb, Cs; M Ni, Pd, Pt und X S, Se) diskutiert.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19966220409
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    Verbindungen in den Systemen Kalium(Rubidium)/Gold/Antimon: K3Au3Sb2, Rb3Au3Sb2 und K1,74Rb0,26RbAu3Sb2Professor Herbert Jacobs zum 60. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 635-639 
    Details
    ISSN: 0044-2313
    Keywords: Alkali metal gold antimon ; synthesis ; single-crystals ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Compounds in the Systems Potassium(Rubidium)/Gold/Antimony: K3Au3Sb2, Rb3Au3Sb2, and K1,74Rb0,26RbAu3Sb2Brittle, silver coloured single crystals of K3Au3Sb2, Rb3Au3Sb2 and K1,74Rb0,26RbAu3Sb2 were obtainded by reaction of the alkali metal azides (KN3, RbN3) with gold and antimon powder at 550°C. The structures of the isotypic compounds (R3m, Z = 3) were determined by X-ray single-crystal diffractometer data: K3Au3Sb2, a = 6,198(2) Å, c = 21,520(5) Å, R/Rw (w = 1) = 0,046/0,058, Z(F02) ≥ 3σ(F02) = 175, Z(Var.) = 14; Rb3Au3Sb2, a = 6,443(3), c = 21,69(2), R/Rw (w = 1) = 0,059/0,082, Z(F02) ≥ 3σ(F02) = 258, Z(Var.) = 14; K1,74Rb0,26RbAu3Sb2, a = 6,288(2) Å, c = 21,617(5) Å, R/Rw (w = 1) = 0,049/0,069, Z(F02) ≥ 3σ(F02) = 390, Z(Var) = 14. The compounds crystallize with the K3Cu3P2-structure type. The Au—Sb partial structures consist of ∞2[AuSb2/3] layers with linear Sb—Au—Sb dumb-bells and SbAu3 pyramids. The layers are separated by two crystallographically independent alkali metal atoms along [001].
    Notes: Spröde, silberfarbene Einkristalle von K3Au3Sb2, Rb3Au3Sb2 und K1,74Rb0,26RbAu3Sb2 wurden durch Reaktion der Alkalimetallazide (KN3, RbN3) mit Gold- und Antimonpulver bei 550°C erhalten. Die Strukturen der isotypen Verbindungen (R3m, Z = 3) wurden aus Einkristall-Röntgen-Diffraktometerdaten bestimmt: K3Au3Sb2, a = 6,198(2) Å, c = 21,520(5) Å, R/Rw (w = 1) = 0,046/0,058, Z(F02) ≥ 3σ(F02) = 175, Z(Var.) = 14; Rb3Au3Sb2, a = 6,443(3), c = 21,69(2), R/Rw (w = 1) = 0,059/0,082, Z(F02) ≥ 3σ(F02) = 258, Z(Var.) = 14; K1,74Rb0,26RbAu3Sb2, a = 6,288(2) Å, c = 21,617(5) Å, R/Rw (w = 1) = 0,049/0,069, Z(F02) ≥ 3σ(F02) = 390, Z(Var) = 14. Die Verbindungen kristallisieren im K3Cu3P2-Typ. Die Au—Sb-Teilstruktur besteht aus ∞2[AuSb2/3]-Schichten mit linearen Sb—Au—Sb-Hanteln und SbAu3-Pyramiden. Die Schichten werden längs [001] durch zwei kristallographisch unterschiedliche Alkalimetallatome separiert.
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    URL: http://dx.doi.org/10.1002/zaac.19966220411
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    Pb2PdX6 (X = Cl, Br) - Verbindungen mit gestreckten [PdX6]-OktaedernProfessor Hanskarl Müller-Buschbaum zum 65. Geburtstage gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1231-1235 
    Details
    ISSN: 0044-2313
    Keywords: Dilead(II)-hexahalogenopalladate(II) ; crystal structure ; strongly elongated PdX6 octahedra ; DTA, IR/RAMAN, 207Pb MAS NMR ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Pb2PdX6 (X = Cl, Br) - Compounds with Elongated [PdX6] OctahedraIn contradiction to published data new compounds in the systems PbX2 - PdX2 (X = Cl, Br) with the formula Pb2PdCl6 (I) and Pb2PdBr6 (II) were found. These were synthesized by thermal treatment of the corresponding mixtures of PbX2 and PdX2 (X = Cl, Br). X-ray single crystal structure analysis shows isotypism of I and II, monoclinic, P21/c (No. 14), Z = 2, I: a = 9.037(2) Å, b = 6.224(1) Å, c = 8.162(1) Å, β = 90.31(7)β, II: a = 9.512(7) Å, b = 6.584(8) Å, c = 8.383(3) Å, β = 90.07(5)º. Strongly elongated PdX6 octahedra are found in the crystal structure. Additional characterisation of the compounds was done by DTA, IR/RAMAN spectra and 207Pb MAS NMR investigations. Remarcable low field shifts were found for 207Pb.
    Notes: Entgegen Literaturangaben wurden in den Systemen PbX2 - PdX2 (X = Cl, Br) die neuen Verbindungen Pb2PdCl6(I) und Pb2PdBr6(II) aufgefunden. Sie wurden durch thermische Behandlung der binären Halogenide PbX2 und PdX2 im molaren Verhältnis 2:1 dargestellt (Einkristalle). Die Kristallstrukturen wurden mit Einkristallröntgenuntersuchungen ermittelt. I und II sind isotyp, monoklin, P21/c (Nr. 14), Z = 2, I: a = 9,037(2) Å, b = 6,224(1) Å, c = 8,162(1) Å, β = 90,31(7)º, II: a = 9,512(7) Å, b = 6,584(8) Å, c = 8,383(3) Å, β = 90,07(5)º. In Pb2PdX6 werden stark gestreckte PdX6-Oktaeder beobachtet. Die Verbindungen wurden außerdem mittels DTA, IR/RAMAN-Spektren und 207Pb-MAS-NMR-Untersuchungen charakterisiert. Für 207Pb wurde eine bemerkenswerte Tieffeldverschiebung beobachtet.
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    URL: http://dx.doi.org/10.1002/zaac.19966220721
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    Zum System Zn/Mo/O. I. Phasenbestand und Eigenschaften der ternären Zinkmolybdate; Struktur von Zn3Mo2O9 (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1274-1280 
    Details
    ISSN: 0044-2313
    Keywords: Phase investigation ; phase diagram ; crystal structure ; differential thermo analysis ; zinc molybdate ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the System Zn/Mo/O. I. Phases and Properties of Ternary Zinc Molybdates; Crystal Structure of Zn3Mo2O9Several ternary compounds are known in the Zn/Mo/O-system. The phases ZnMoO4, Zn2Mo3O8 and Zn3Mo2O9 are stable at 900°C. The coexistence ranges are shown in the ternary phase diagram. The structure of Zn3Mo2O9 has been determined by single crystal X-ray diffraction. The compound crystallizes in the monoclinic space group P21/m (a = 7,757(1) Å, b = 7,132(1) Å, c = 8,370(2) Å, β = 117,40(1)º, Z = 2).
    Notes: Im System Zn/Mo/O sind mehrere ternäre Phasen bekannt. Bei 900°C sind die Phasen ZnMoO4, Zn2Mo3O8 und Zn3Mo2O9 stabil. Die Koexistenzgebiete sind am ternären Phasendiagramm dargestellt. Die Strukturbestimmung von Zn3Mo2O9 erfolgte mit Röntgenbeugung an Einkristallen. Die Verbindung kristallisiert in der monoklinen Raumgruppe P21/m (a = 7,757(1) Å, b = 7,132(1) Å, c = 8,370(2) Å, β = 117,40(1)º, Z = 2).
    Additional Material: 8 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19966220728
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    Nitrido-Sodalithe. III [1]. Synthese, Struktur und Eigenschaften von Zn8[P12N24]X2 mit X = O, S, Se, TeHerrn Professor Max Herberhold zum 60. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1281-1286 
    Details
    ISSN: 0044-2313
    Keywords: P—N-Sodalites ; crystal structure ; UV-Vis spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Nitrido-Sodalites. III. Synthesis, Crystal Structure, and Properties of Zn8[P12N24]X2 with X = O, S, Se, TeThe P—N-sodalites Zn8[P12N24]X2 with X = O, S, Se, Te are obtained by the reaction of HPN2 with the corresponding zinc chalcogenide ZnX at 750°C. They crystallize in a filled up variant of Zn7[P12N24]Cl2 and are isotypic to Zn8[B12O24]O2 (I43m, a = 823 to 830 pm, Z = 1). The P—N-sodalites contain in the center of their β-cages XZn46+ units which can be described as sections of II/VI-semiconductors. The UV/Vis-spectra of the compounds show in comparison with binary bulk zinc chalcogenides a blue shift of the absorption edge according to the size quantization effect.
    Notes: Die P—N-Sodalithe Zn8[P12N24]X2 mit X = O, S, Se, Te wurden durch Umsetzung von HPN2 mit dem jeweiligen Zinkchalkogenid ZnX bei 750°C dargestellt. Sie kristallisieren in einer aufgefüllten Variante von Zn7[P12N24]Cl2 und somit isotyp zu Zn8[B12O24]O2 (I43m, a = 823 bis 830 pm, Z = 1) Die P—N-Sodalithe enthalten im Zentrum ihrer β-Käfige XZn46+-Einheiten, die als kleinstmögliche Ausschnitte aus den Strukturen von II/VI-Halbleitern angesehen werden können. Die UV/Vis-Spektren der Verbindungen zeigen im Vergleich mit makrokristallinen binären Zinkchalkogeniden gemäß dem Größenquantisierungseffekt eine Blauverschiebung der Absorptionskante.
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    Darstellung und Charakterisierung von RbLiSe im Rahmen einer Struktursystematik für ternäre Interalkalimetallchalkogenide vom Formeltyp ABXProfessor Hanskarl Müller-Buschbaum zum 65. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1311-1313 
    Details
    ISSN: 0044-2313
    Keywords: Inter alkali metal chalcogenides ; rubidium lithium selenide ; X-ray ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Crystal Structure of RbLiSeRbLiSe is in the system Rb2Se/Li2Se the only ternary phase without mixed crystals of the binary compounds. The single crystal X-ray investigation of this yellow hygroscopic compound leads to the tetragonal space group P4/nmm (Z = 2) with the lattice constants a = 461.6(1) and c = 748.2(3) pm. Its crystal structure confirms a simple rule of expected structure types for inter alkali metal chalcogenides of the general formula ABX.
    Notes: Im System Rb2Se/Li2Se wurde RbLiSe als einzige Phase gefunden. Mischkristallbildung konnte nicht beobachtet werden. Die gelbe, sehr hygroskopische Verbindung kristallisiert nach Einkristalluntersuchungen tetragonal in der Raumgruppe P4/nmm (Z = 2) mit den Gitterkonstanten a = 461,6(1) und c = 748,2(3) pm. Als Vertreter des anti-PbFCl-Strukturtyps befolgt RbLiSe eine von uns empirisch ermittelte „Regel“ zur Struktursystematik der ternären Interalkalimetallchalkogenide des Formeltyps ABX.
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    URL: http://dx.doi.org/10.1002/zaac.19966220806
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    Preparation, crystal structure, and magnetic properties of β-Li3TiF6 = Li2[4]Li7[6](TiF6)(TiF6)2 - a double fluoride?Professor Hans Georg von Schnering zum 65. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1329-1334 
    Details
    ISSN: 0044-2313
    Keywords: β-Li3TiF6 ; crystal structure ; band structure ; Jahn Teller effect ; magnetism ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Darstellung, Kristallstruktur und magnetische Eigenschaften von β-Li3TiF6 = Li2[4]Li7[6](TiF6)(TiF6)2 - ein Doppelfluorid?Purpurfarbene Einkristalle von β-Li3TiF6 wurden durch Erhitzen eines Gemenges von LiF und TiF3 (3 : 1) bei 820°C unter Argon erhalten. β-Li3TiF6 kristallisiert in C2/c mit a = 14.452(2) Å, b = 8.798(1) Å, c = 10.113(1) Å und β = 96.30(1)º. Die Struktur ist isotyp mit β-Li3VF6 und enthält isolierte gestauchte TiF6-Oktaeder (dTi-F = 1.91-2.01 Å). Die magnetischen Eigenschaften von β-Li3TiF6 untersucht und diskutiert. Die Bindungsverhältnisse werden anhand von Bandstruktur Rechnungen und Berechnungen des Madelunganteils der Gitterenergie, MAPLE, diskutiert.
    Notes: Purple colored single crystals of the β-modification of Li3TiF6 have been prepared by heating an appropriate mixture of LiF and TiF3 at 820°C under an argon atmosphere. β-Li3TiF6 crystallizes in C2/c with a = 14.452(2) Å, b = 8.798(1) Å, c = 10.113(1) Å and β = 96.30(1)º. The structure is isotypic to β-Li3VF6 and contains isolated compressed TiF6 octahedra (dTi-F = 1.91-2.01 Å). Magnetic properties of β-Li3TiF6 were studied and discussed. Band structure calculations and calculations of the Madelung part of the lattice energy, MAPLE, were performed to discuss the chemical bonding.
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    URL: http://dx.doi.org/10.1002/zaac.19966220810
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    Synthese, Kristallstrukturen und Eigenschaften von Lanthanoid(III)-Komplexen mit 7-Oxa-bicyclo[2.2.1]heptan-2,3-dicarbonsäureProfessor Hans Georg von Schnering zum 65. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1335-1341 
    Details
    ISSN: 0044-2313
    Keywords: Lanthanoid(III) carboxylate complexes ; synthesis ; crystal structure ; IR spectra ; thermal decomposition ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Crystal Structures, and Properties of Lanthanoid(III) Complexes with 7-Oxa-bicyclo[2.2.1]heptane-2,3-dicarboxylic AcidThe synthesis of coordination compounds [ML(HL)(H2O)] with M = La3+, Ce3+, Pr3+, Nd3+ and H2L = 7-oxa-bicyclo[2.2.1]heptane-2-exo,3-cis-dicarboxylic acid (1) has been described. Results of IR spectroscopy and thermal decomposition are given. As a result of X-ray analyses, the four investigated lanthanoid(III) complexes are isotypic. Their stereochemistry approximates to the tri-capped trigonal prism with nine O atoms coordinating the metal atom. The bicyclic ligand acts as a tridentate chelating monoanion HL- as well as a pentadentate dianion L2- with both chelating and bridging function. One coordination place at the metal atom is occupied by a water molecule.
    Notes: Die Synthese der Koordinationsverbindungen [ML(HL)(H2O)] mit M = La3+, Ce3+, Pr3+ und Nd3+ und H2L = 7-Oxa-bicyclo[2.2.1]heptan-2-exo,3-cis-dicarbonsäure (1) wird beschrieben. Ergebnisse der IR-Spektroskopie und thermoanalytischer Untersuchungen werden mitgeteilt. Nach den Ergebnissen von Röntgenkristallstrukturanalysen sind die vier untersuchten Lanthanoid(III)-Komplexe isotyp. In ihnen ist das Metallatom in dreifach überkappter trigonal-prismatischer Koordination von neun O-Atomen als nächsten Nachbarn umgeben. Dabei tritt der bicyclische Ligand einmal als dreizähniges Monoanion HL- und zum anderen als fünfzähniges Dianion L2- mit Brückenfunktion auf. Die neunte Koordinationsstelle wird von einem Wassermolekül besetzt.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19966220811
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    HfNixP - Intercalation of Ni into the Three-Dimensional Compound HfP (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1342-1348 
    Details
    ISSN: 0044-2313
    Keywords: Hafnium nickel phosphide, HfNixP ; metal-rich phosphide ; intercalation ; crystal structure ; electronic structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: HfNixP - Einlagerung von Nickel in die dreidimensionale Verbindung HfPDie neue Verbindung HfNixP (x = 0.426(1); Kristallstruktur: P63/mmc, a = 3.737(1) Å, c = 12.666(2) Å, V = 153.21(7) Å3) wurde durch Aufschmelzen von HfP und Nickel im Lichtbogen und anschließendem Tempern Bei 1400°C hergestellt. Formal kann man die Struktur von HfNixP als gefüllte HfP-Struktur beschreiben, wobei die Nickelatome die Zentren der trigonalen Prismen des Hf-Teilgitters besetzen. Dadurch, daß die benachbarten trigonalen Hf6-Prismen von P-Atomen zentriert sind, sind alle drei Rechtecksflächen des trigonalen Hf6Ni-Prismas von je einem P-Atom überdacht. Von einem anderen Blickwinkel aus betrachtet, besteht die Struktur von HfNixP aus alternierenden Schichten von Hf-Atomen, die gemäß der Stapelfolge AABB gepackt sind. Zwischen den ekliptisch übereinanderliegenden Hf-Schichten befinden sich eine P- und die Ni-Lage, während ein zweites P-Atom zwischen den A- und B-Schichten von sechs Hf-Atomen oktaedrisch umgeben ist. Nach Berechnungen der Zustands-dichte (Extended-Hückel-Näherung) sollte HfNixP metallisch leitfähig sein; aufgrund der bindenden Hf—Hf-Wechselwirkungen in allen drei Raumrichtungen sind dreidimensionale metallische Eigenschaften anzunehmen.
    Notes: The new compound HfNixP (x = 0.426(1), crystal structure: P63/mmc, a = 3.737(1) Å, c = 12.666(2) Å, V = 153.21(7) Å3) has been prepared by arc-melting of HfP with nickel and subsequent annealing at 1400°C. Its crystal structure can be considered as a filled HfP structure, with the Ni atoms inserted into the trigonal prismatic voids of the Hf sublattice. Since the neighboring trigonal Hf6 prisms are centered by P atoms, each of the three rectangular faces of the Hf6Ni prism is capped with one P atom. Altogether, the structure of HfNixP consists of alternating layers of Hf atoms with the packing sequence AABB. One P and the Ni position are situated between the eclipsed Hf layers, whereas the other P site between the A and B layers is surrounded by six Hf atoms in a staggered arrangement. The calculated density of states (Extended Hückel approximation) points to metallic conductivity; threedimensional metallic behavior is assumed because of the Hf-Hf bonding interactions along all three directions.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19966220812
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  • 85
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    Über grünes Bis-(2-Iminoisopropyl-thiophenolato)-nickel(II) und weitere, ähnliche NiII-KomplexeProfessor Herbert Schumann zum 60. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1765-1772 
    Details
    ISSN: 0044-2313
    Keywords: Nickel ; Schiff base complexes ; synthesis ; crystal structure ; hydrogenase ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Green Bis-(2-iminoisopropyl-thiophenolato)nickel(II) and other Similar NiII ComplexesThe compounds [NiII(iitp)2] 1 (iitp = 2-iminoisopropyl-thiophenolate), [Ni2II(imptp)2] · 2 CH3OH 2, a dinuclear compound with an Ni—Ni distance of 276 pm, and [PPh4] · [NiII(imptp)(SCN)] 3 (imptp = 2-(2-iminopentane-4-on)-thiophenolate) have been prepared by the reaction of nickel(II)-acetate-tetrahydrate with 2-iminoisopropyl-thiophenole and 2-(2-iminopentane-4-on)-thiophenole in methanol, respectively. They have been characterized by single-crystal X-ray structure analysis and other physical methods. The redox behaviour of 1-3 has been studied in detail (chemically as well as by cyclovoltammetry and ESR spectroscopy). Particularly interesting are the electronic properties of 1 and its reduction with NaBH4 and the following reaction of the product with O2. The complexes are model compounds for some Ni-containing enzymes. For details of the crystal structure determination see “Inhaltsübersicht”.
    Notes: Die Verbindungen [NiII(iitp)2] 1 (iitp = 2-Iminoisopropyl-thiophenolat), [Ni2II(imptp)2] · 2 CH3OH 2, eine Zweikernverbindung mit einem Ni—Ni-Abstand von 276 pm und [PPh4][NiII(imptp)(SCN)] 3 (imptp = 2-(2-Iminopentan-4-on)-thiophenolat) wurden durch Umsetzung von Nickel(II)-acetat-tetrahydrat mit 2-Iminoisopropyl-thiophenol bzw. 2-(2-Iminopentan-4-on)-thiophenol in Methanol dargestellt und durch Einkristallstrukturanalyse und andere physikalische Methoden charakterisiert. Das Redoxverhalten der Verbindungen 1-3 wurde mittels elektrochemischer, chemischer und spektroskopischer Methoden untersucht. Bemerkenswert sind die elektronischen Eigenschaften der grünen Verbindung 1, sowie ihre Reduktion mit NaBH4 und die darauffolgende Umsetzung des Reaktionsproduktes mit O2. Die Verbindungen besitzen Modellcharakter für einige Ni-haltige Enzyme.1: C2/c, a = 1298,3(2); b = 695,7(1); c = 1958,7(3) pm; β = 103,92(1)°; V = 1717,4(5) · 106 pm3; R = 0,035 für 1230 unabhängige Reflexe (Fo 〉 4σ(Fo)), Z = 4.2: P1, a = 947,9(2); b = 1229,5(3); c = 1254,7(3) pm; α = 67,28(2), β = 74,63(2), γ = 81,18(2)°; V = 1298,4(5) · 106 pm3; R = 0,082 für 3655 unabhängige Reflexe (Fo 〉 4σ(Fo)), Z = 2.3: P21, a = 1119,3(2); b = 2389,7(4); c = 1245,8(2) pm; β = 102,52(1)°; V = 3253,0(9) · 106 pm3; R = 0,051 für 4218 unabhängige Reflexe (Fo 〉 4σ(Fo)), Z = 4.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19966221022
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  • 86
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    Syntheses and Crystal Structures of Ca3Fe2(SeO3)6 and Sr3Fe2(SeO3)6 (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1788-1792 
    Details
    ISSN: 0044-2313
    Keywords: M3Fe2(SeO3)6 (M = Ca, Sr) ; crystal structure ; crystal chemistry ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesen und Kristallstrukturen von Ca3Fe2(SeO3)6 und Sr3Fe2(SeO3)6Die neuen Verbindungen M3Fe2(SeO3)6 (M = Ca, Sr) wurden als kristalline Niederschläge aus wäßrigen Lösungen der jeweiligen Ionen erhalten, die in Teflon-beschichteten Behältern für mehrere Tage auf eine Temperatur von 227(2)°C erhitzt wurden.Die kristallographischen Daten sind: Raumgruppe R3c, a = 8,531(2), 8,802(2) Å; c = 38,89(1), 39,00(1) Å; V = 2451,1, 2616,7 Å3, Z = 6. Die Kristallstrukturen wurden aus Einkristallröntgenbeugungsdaten bestimmt und zu R-Werten von R1 = 0,021, 0,023; wR2 = 0,038, 0,039 verfeinert. Die Gerüststruktur besteht aus zwei Arten von FeO6 Oktaedern sowie aus MO8 Gruppen und SeO3 trigonalen Pyramiden, die über gemeinsame Ecken und Kanten verbunden sind.
    Notes: The new compounds M3Fe2(SeO3)6 (M = Ca, Sr) were obtained as crystalline precipitates from aqueous solutions of the respective ions, kept in Teflon-coated vessels at a temperature of 227(2)°C for several days.The crystal data are: space group R3c, a = 8.531(2), 8.802(2) Å; c = 38.89(1), 39.00(1) Å; V = 2451.1, 2616.7 Å3, Z = 6. The crystal structures have been refined by single-crystal X-ray diffraction methods to R1 = 0.021, 0.023; wR2 = 0.038, 0.039. The framework structure is built up by two types of FeO6 octahedra as well as by MO8 groups and SeO3 trigonal pyramids by corner- and edge-linkage of the polyhedra.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19966221025
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    Tetramethyldisilan-1,2-diyl-verbrückte Dicyclopentadienyl-und Diindenylmetalldichloride der 4. Gruppe - Kristallstruktur von (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1806-1810 
    Details
    ISSN: 0044-2313
    Keywords: Metallocene dichlorides, bridged cyclopentadienyl and indenyl compounds ; crystal structure ; 1H ; 13C ; 29Si n.m.r., and MS spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Tetramethyldisilane-1,2-diyl bridged Dicyclopentadienyl and Diindenyl Metal Dichlorides of the Group 4 Metals - Crystal Structure of Dicyclopentadienyl and diindenyl metal dichlorides of the type Cp′—SiMe2SiMe2—Cp′MCl2 (Cp′ = C5H4, M = Ti (1), Zr (2), Hf (3); Cp′ = C9H7, M = Zr (4), Hf (5)) were synthesized and characterized by means of their 1H, 13C, 29Si-n.m.r., MS, and IR spectra. The crystal structure of 2 was determined.
    Notes: Dicyclopentadienyl- und Diindenylmetalldichloride des Typs Cp′—Me2Si—Me2Si—Cp′MCl2(Cp′ = C5H4; M = Ti(1), Zr (2), Hf (3); Cp′ = C9H7; M = Zr (4), Hf (5)) wurden synthetisiert und mittels ihrer 1H-, 13C- und 29Si-NMR-Spektren sowie MS- und IR-Spektren charakterisiert. Die Kristallstruktur von 2 wurde ermittelt.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19966221028
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    Die Kristallstruktur des synthetischen Stützits, Ag5-xTe3Professor Hans Georg von Schnering zum 65. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1823-1832 
    Details
    ISSN: 0044-2313
    Keywords: Silver telluride ; stuetzite ; crystal structure ; tetrahedrally close-packed ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of Synthetic Stuetzite, Ag5-xTe3The crystal structure of Ag5-xTe3 was determined by single crystal X-ray structure analysis. The structure is of hexagonal symmetry (P 62m, Nr. 189) with a = 13.456(9) Å and c = 16.917(9) Å. The compound consists of highly mobile silver cations distributed in a tellurium framework forming Frank-Kasper polyhedra. Tellurium exists as Te2- as well as Te22--dumbbells and forms three types of tetrahedral sites. A description of the distribution of silver on the tetrahedral voids is given resulting in a suggestion of possible diffusion paths. Finally the homogenity region of Ag5-xTe3 is derived from the structure.
    Notes: Die Kristallstruktur von Ag5-x Te3 wurde durch Einkristall-Röntgenstrukturanalyse ermittelt. Die Struktur besitzt hexagonale Symmetrie (P62m, Nr. 189) mit a = 13,456(9) Å und c = 16,917(9) Å. Die Verbindung besteht aus beweglichen Silberkationen, die in einem Tellur-Gerüst von Frank-Kasper-Polyedern verteilt sind. Tellur liegt als Te2- und als Te22--Hantel vor und bildet drei verschiedene Arten von Tetraederlücken. Die Verteilung des Silbers auf die Tetraederlücken wird beschrieben. Daraus resultieren Vorschläge für mögliche Diffusionspfade. Schließlich wird der Homogenitätsbereich von Ag5-xTe3 aus der Struktur hergeleitet.
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    URL: http://dx.doi.org/10.1002/zaac.19966221105
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    Preparation and crystal structure of barium caesium undecaphosphide-ammonia (1/11) BaCsP11 · 11 NH3Dedicated to Professor Hans-Georg von Schnering on the Occasion of his 65th Birthday (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1833-1838 
    Details
    ISSN: 0044-2313
    Keywords: Barium caesium undecaphosphide-ammonia (1/11), BaCsP11 · 11 NH3 ; barium nonaammine complex ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Darstellung und Kristallstruktur von Barium-Caesium-Undecaphosphid-Ammoniak (1/11) BaCsP11 · 11 NH3Die neue Verbindung BaCsP11 · 11 NH3 wurde in flüssigem Ammoniak ausgehend von Cs3P11 und einem mit Ba2+ -Ionen beladenen Ionenaustauschmaterial hergestellt. BaCsP11 · 11 NH3 bildet gelbe Kristalle, die sich ab 246 K unter Verlust des Kristallammoniaks zersetzen. Die Kristallstruktur wurde mit Hilfe von Röntgen-Einkristalldiffraktometerdaten bestimmt: P21/a, a = 1599.9(2) pm, b = 1793.9(3) pm, c = 1998.1(7) pm, β = 93.02(4)°, Z = 8, wR2 = 0.118 (R1 = 0.047) für 8969 Strukturfaktoren und 631 variable Parameter. Die Kationen Cs+ sind durch Undecaphosphatrishomocuban-Anionen P113- so koordiniert, daß eindimensional-unendliche Stränge ∞1[CsP11]2- vorliegen, die voneinander durch Ba(NH3)n2+ -Kationen (n = 8 und 9) getrennt sind. Es wird nur ein direkter Ba—P-Kontakt beobachtet.
    Notes: The new compound BaCsP11 · 11 NH3 was prepared in liquid ammonia, using Cs3P11 and a cation exchange resin loaded with Ba2+ cations as starting materials. BaCsP11 · 11 NH3 forms yellow crystals which decompose at 246 K under loss of the ammonia of crystallisation. The crystal structure was determined from single-crystal X-ray diffractometer data: P21/a, a = 1599.9(2) pm, b = 1793.9(3) pm, c = 1998.1(7) pm, β = 93.02(4)°, Z = 8, wR2 = 0.118 (R1 = 0.047) for 8969 structure factors and 631 variable parameters. The Cs+ cations are co-ordinated by undecaphosphatrishomocubane anions P113- in such a way that one-dimensionally infinite chains ∞1[CsP11]2- result which are separated by Ba(NH3)n2+ (n = 8 and 9). Only one Ba—P contact is observed.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19966221106
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    Beiträge zum thermischen Verhalten und zur Kristallchemie von wasserfreien Phosphaten. XV. Darstellung, Kristallstruktur und Eigenschaften von Kupfer(II)-ultraphosphat CuP4O11 (≙ Cu2P8O22)Professor Wolfgang Jeitschko zum 60. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1839-1846 
    Details
    ISSN: 0044-2313
    Keywords: Chemical vapour transport ; ultraphosphate ; CuP4O11 ; crystal structure ; electronic spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Crystal Structure, and Properties of Copper(II) Ultraphosphate CuP4O11CuP4O11 was synthesised from Cu2P4O12 and P4O10 (500°C, sealed silica ampoules) using iodine and a few mg of CuP2 or phosphorus as mineraliser. Chemical transport reactions in a temperature gradient 600 → 500°C led to the formation of well developed, colourless, transparent crystals with edge-lengths up to 5 mm (deposition rate m ≍ 2 mg/h).The crystal structure of copper(II) ultraphosphate (C1; Z = 8; a = 13.084(3) Å, b = 13.024(2) Å, c = 10.533(2) Å, α = 89.28(2)°, β = 118.42(2)°, γ = 90.30(2)°) has been determined and refined from X-ray data obtained from a pseudo-merohedrally twinned crystal (twin element two-fold rotation axis // b; volume ratio: 17/3; 3063 independent reflections with 2θ ≤ 53.4°; 291 variables; conventional residual (based on F) R1 = 0.038, wR2 = 0.101 (based on F2), GooF = 1.10).The crystal structure of CuP4O11 is built from four crystallographically independent ten-membered polyphosphate rings of very similar conformation. These rings are linked to form two-dimensional nets parallel (-2 0 1) planes. There is a close topological relationship between these nets and those formed in polyphosphides CdP4 and CuP2. Copper on two crystallographic sites (Cu2P8O22) is coordinated by oxygen thus forming elongated [CuO6] octahedra (deq(Cu—O) ≍ 1.96 Å; dax(Cu—O) ≍ 2.34 Å).The crystal g-tensor of CuP4O11 has been determined from powder samples to g1 = 2.09, g2 = 2.24, g3 = 2.36. These values are in good agreement with molecular g-values from calculations within the framework of the angular overlap model on the two independent CuO6 octahedra (Cu2+(1): gx = 2.09, gy = 2.10, gz = 2.52; Cu2+(2): gx = 2.08, gy = 2.11, gz = 2.52) assuming exchange coupling. The observed broad absorption band (7000 cm-1 to 13000 cm-1) from powder reflectance measurements (4000-28000 cm-1) and the bulk magnetic susceptibility of μexp = 1.99 μB is also reproduced nicely by this calculations.
    Notes: Die Synthese von CuP4O11 gelingt aus Cu2P4O12 und P4O10. In direkt anschließenden chemischen Transportexperimenten (600 → 500°C, Zusatz von Iod und wenigen mg CuP2 oder Phosphor als Transportmittel) werden wohlausgebildete, farblos-transparente Kristalle mit Kantenlängen bis 4 mm erhalten (Transportrate ca. 2 mg/h).Anhand von Röntgenbeugungsdaten eines pseudomeroedrisch nach (010) verzwillingten Kristalls konnte die Kristallstruktur von Kupfer(II)-ultraphosphat (C1; Z = 8; a = 13,084(3) Å, b = 13,024(2) Å, c = 40,533(2) Å, α = 89,28(2)°, β = 118,42(2)°, γ = 90,30(2)°, Gitterkonstanten aus Guinier-Aufnahmen) bestimmt und verfeinert werden (Volumenverhältnis 17/3; 3063 symmetrieunabhängige Reflexe mit 2θ ≤ 53,4° und F02 ≥ 4σ(F02); 291 freie Parameter; konventioneller R-Wert R1 = 0,038, wR2 = 0,101, GooF = 1,10).Die Kristallstruktur enthält vier kristallographisch unterschiedliche zehngliedrige Polyphosphatringe ähnlicher Konformation, die zu zweidimensionalen Netzen parallel zu (-2 0 1) verknüpft sind. Kupfer ist auf zwei kristallographischen Lagen (Cu2P8O22) gestreckt-oktaedrisch von Sauerstoff koordiniert (deq(Cu—O) ≍ (1,96 Å; dax(Cu—O) ≍ (2,34 Å).Die Hauptachsen des g-Tensors für CuP4O11 wurden an pulverförmigen Proben bestimmt zu g1 = 2,09, g2 = 2,24 und g3 = 2,36. Diese Werte stehen bei Annahme einer Austauschkopplung in sehr guter Übereinstimmung mit molekularen g-Tensoren für die beiden unabhängigen CuO6-Oktaeder (Cu2+(1): gx = 2,09, gy = 2,10, gz = 2,52; Cu2+(2): gx = 2,08, gy = 2,11, gz = 2,52) wie sie aus Berechnungen im Rahmen des „angular overlap model“ für CuP4O11 abgeleitet werden. Diese Betrachtungen geben auch das beobachtete Remissionsspektrum (4000-28000 cm-1) mit einer breiten Bande zwischen 7000 cm-1 und 13000 cm-1 sowie die magnetische Suszeptibilität μexp = 1,99 μB gut wieder.
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    URL: http://dx.doi.org/10.1002/zaac.19966221107
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    Nitridsulfidchloride der Lanthanide: II. Der Formeltyp M6N3S4Cl (M = La—Nd)Professor Gerhard Thiele zum 60. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 275-282 
    Details
    ISSN: 0044-2313
    Keywords: Lanthanides ; nitride sulfide chlorides ; M6N3S4Cl ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Nitride Sulfide Chlorides of the Lanthanides. II. The Composition M6N3S4Cl (M = La—Nd)The oxidation of the “light” lanthanides (M = La—Nd) with sulfur and NaN3 in the presence of the chlorides MCl3 yields chlorine-poor nitride sulfide chlorides with the composition M6N3S4Cl when appropriate molar ratios of the reactants are used. Additional NaCl as a flux secures complete and fast reactions (7 d) at 850°C in evacuated silica vessels as well as single-crystalline products (red-brown needles).The crystal structure was determined from X-ray single crystal data for the limiting representatives La6N3S4Cl (orthorhombic, Pnma (no. 62), Z = 4, a = 1159.7(4), b = 410.95(7), c = 2756.8(9)pm, R = 0.030, Rw = 0.027) and Nd6N3S4Cl (a = 1137.1(3), b = 399.34(6), c = 2687.6(9)pm, R = 0.034, Rw = 0.033). Guinier powder data revealed the cerium and praseodymium analogues to be isotypic.The crystal structure exhibits two different chains of connected [NM4] tetrahedra which are commensurate in translation. Six crystallographically different M3+ are present, two of them (M1 and M2) build up the chain ∞1[(N1)(M1)3/3k · (M2)1/1t]3+ together with (N1)3- by cis-edge connection of tetrahedra. The four remainders (M3—M6) arrange as pairs [N2M6] of edge-shared [NM4] tetrahedra with (N2)3- and (N3)3- which are further connected via four vertices to form the ∞1[(M5)2/2e(N-2){(M3)(1+1)/(1+1)(M4)(1+1)/(1+1))}e(N3)(M6)2∞2v]6+ double chain. Bundled along [010] like a closest packing of rods, both types of chains are held together by five crystallographically different but by X-ray diffraction indistinguishable anions S2- (S1—S4) and Cl- adjusting the charge balance in a molar ratio of 4:1.
    Notes: Die Oxidation der „leichten“ Lanthanide (M = La—Nd) mit Schwefel und NaN3 in Gegenwart der Chloride MCl3 liefert aus Gemengen mit entsprechenden molaren Verhältnissen der Edukte chlorarme Nitridsulfidchloride der Zusammensetzung M6N3S4Cl. Der Zusatz von NaCl als Flußmittel gewährleistet vollständige und schnelle Umsetzungen (7 d) bei 850°C in evakuierten Quarzglasampullen sowie einkristalline Produkte (rotbraune Nadeln).Die Kristallstruktur wurde anhand röntgenographischer Einkristalldaten für die Randvertreter La6N3S4Cl (orthorhombisch, Pnma (Nr. 62), Z = 4; a = 1159,7(4); b = 410,95(7); c = 2756,8(9) pm; R = 0,030; Rw = 0,02(7) und Nd6N3S4Cl (a = 1137,1(3); b = 399,34(6); c = 2687,6(9) pm; R = 0,034; Rw = 0,033) bestimmt. Guinier-Pulveraufnahmen wiesen zudem die Isotypie der Cer-und der Praseodym-Verbindung aus.In der Kristallstruktur liegen zwei unterschiedliche, translationskommensurable Stränge aus verknüpften Tetraedern [NM4] vor. Von den sechs kristallographisch unabhängigen M3+ bilden zwei (M1 und M2) mit (N1)3- durch cis-Kanten-verknüpfung der Tetraeder die Kette ∞1[(N1)(M1)3/3k(M2)1/1t]3+. Die übrigen vier (M3—M6) treten mit (N2)3- und (N3)3- zunächst zu Tetraederdoppeln [N2M6] aus zwei [NM4]-Einheiten mit gemeinsamer Kante zusammen. Diese Dimere sind zusätzlich über vier gemeinsame Ecken zur Doppelkette ∞1[(M5)2/2e · (N2){(M3)(1+1)/(1+1)(M4)(1+1)/(1+1)}k(N3)(M6)2/2e]6+ verbunden. Längs [010] nach Art einer dichtesten Stabpackung gebündelt, wird der Zusammenhalt der Stränge durch fünf kristallographisch unterschiedliche, röntgenographisch jedoch nicht unterscheidbare Anionen S2- (S1—S4) und Cl- besorgt, die im molaren Verhältnis von 4:1 auch den Ladungsausgleich regeln.
    Additional Material: 5 Ill.
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    Die Kristallstrukturen von Tl2AgI3 und NaAgI2 · 3 H2OProfessor Gerhard Thiele zum 60. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 308-312 
    Details
    ISSN: 0044-2313
    Keywords: Iodoargentates ; crystal structure ; dithallium triiodoargentate ; sodium diiodoargentate trihydrate ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure Investigations of Tl2AgI3 und NaAgI2 · 3 H2OTl2AgI3 was synthesized by the reaction of TlI with AgI in aqueous HI (25%) in a pressure vessel. The compound crystallizes in the rhombohedral space group R3; a = 1044,3(2); c = 1993,5(3)pm; Z = 9. The crystal structure contains trinuclear anions [Ag3I8]5- and [ITl6]5+ octahedra. The anions are composed of two AgI4-tetrahedra which are connected to an AgI6 octahedron via common faces.Single crystals of NaAgI2 · 3 H2O were formed by reaction of NaI with AgI in aqueous solution. The compound crystallizes in the orthorhombic space group Pbca with lattice parameters a = 711,2(2); b = 939,8(3); c = 2462,2(4) pm; Z = 8. The crystal structure is built up by polymeric layers ∞2[AgI3/3I½1/2-] of corner sharing AgI4 tetrahedra (GaOCl type) and ∞1[Na(H2O)4/2(H2O)I½1/2+] octahedra chains.
    Notes: Tl2AgI3 wurde durch Umsetzung von TlI mit AgI in wäßriger HI (25%) in einem Aufschlußautoklaven kristallin erhalten. Es kristallisiert in der rhomboedrischen Raumgruppe R3; a = 1044,3(2); c = 1993,5(3) pm; Z = 9. Die Kristallstruktur ist aus dreikernigen Anionen [Ag3I8]5- und [ITl6]5+-Oktaedern aufgebaut. Die Anionen bestehen aus zwei AgI4-Tetraedern, die über gemeinsame Flächen an ein AgI6-Oktaeder gebunden sind.Die Verbindung NaAgI2 · 3 H2O wurde aus wäßriger Lösung durch Umsetzung von NaI mit AgI einkristallin gewonnen. Die orthorhombische Raumgruppe Pbca hat die Zellparameter a = 711,2(2); b = 939,8(3); c = 2462,2(4) pm; Z = 8. Die Kristallstruktur ist durch polymere Schichten ∞2[AgI3/3I½1/2-] aus eckenverknüpften AgI4-Tetraedern (GaOCl-Typ) und ∞1[Na(H2O)4/2(H2O)I1/2+]-Oktaederketten gekennzeichnet.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19966220217
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    Die ersten oligomeren Anionen bei Fluoro-Litho-Metallaten mit Oktaeder-Sandwich-Motiv: Cs4K{[F3MIIIF3]Li[F3MIIIF3]}, MIII = Ga, Fe [1]Professor Gerhard Thiele zum 60. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 297-307 
    Details
    ISSN: 0044-2313
    Keywords: Cs4K{Li[Ga2F12]} ; Cs4K{Li[Fe2F12]} ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The First Oligomeric Anions of Fluoro-Litho Metallates with Octahedra Sandwich Motive: Cs4K{[F3MIIIF3]Li[F3MIIIF3]}, MIII = Ga, FeColourless single crystals of Cs4K{Li[Ga2F12]} (A) and Cs4K{Li[Fe2F12]} (B) have been obtained by solid state reaction from intimate mixtures of the corresponding binary fluorides (Pt-tube, 750°C, 40 d). The trigonal unit cells with (A) a = 631,3(1)pm; c = 3059,9(6)pm and (B) a = 635,0(1)pm; c = 3089,2(7)pm, respectively (Z = 3, Guinier-Simon data, Cu-Kα1), are confirmed by single crystal investigations. The compounds crystalize isostructural in the space group R3m (No. 166). The structures were determined using four-circle diffractometer data (Siemens AED 2) with (A) R = 2.95%, 3627 Io and (B) R = 1.86%, 4179 Io, respectively (SHELX-76), and are characterized by triplets of facesharing octahedra parallel [00.1] with the cation-sequence MIII—Li—MIII, six of which are connected by [KF6]-octahedra via common corners and each triplet is surrounded by six different [KF6]-octahedra. The structure is completed by Cs+ filling the cavities. The Madelung Part of Lattice Energy (MAPLE), Mean Fictive Ionic Radii (MEFIR) and Effective Coordination Numbers (ECoN) are calculated and compared. The classification as lithometallate could be verified by a new MAPLE concept. The Charge Distribution (CHARDI) was calculated and compared with the results according to ‘bond length-bond strength’.
    Notes: Durch Festkörperreaktionen wurden aus innigen Gemengen der entsprechenden binären Fluoride erstmals Fluoro-Litho-Metallate des neuen Typs Cs4K{Li[Ga2F12]} (A) und Cs4K{Li[Fe2F12]} (B) in Form farbloser Einkristalle dargestellt (Pt-Rohr, 750°C, 40 d). Einkristalluntersuchungen belegen die trigonalen Elementarzellen mit (A) a = 631,3(1)pm und c = 3059,9(6)pm bzw. (B) a = 635,0(1)pm und c = 3089,2(7)pm (Z = 3, Guinier-Simon-Daten, Cu-Kα1). Die Verbindungen kristallisieren isotyp in der Raumgruppe R3m (Nr. 166). Die Strukturbestimmungen erfolgten mittels Vierkreisdiffraktometerdaten (Siemens AED 2) mit (A) R = 2,95%, 3627 Io bzw. (B) R = 1,86%, 4179 Io (SHELX-76). Charakteristisch für die Struktur sind Oktaedertripel längs [00.1] (Kationenfolge MIII—Li—MIII), von denen jeweils sechs über gemeinsame Ecken von den Einzeloktaedern [KF6] dreidimensional verknüpft werden und umgekehrt. Die ‚Hohlräume‘ dieses Strukturteils sind durch Cs+ aufgefüllt. Der Madelung-Anteil der Gitterenergie (MAPLE), Mittlere Fiktive Ionenradien (MEFIR) sowie Effektive Koordinationszahlen (ECoN) wurden berechnet und verglichen. Die Einordnung der Verbindungen als Litho-Metallate wird mit Hilfe eines neuen MAPLE-Konzeptes überprüft und begründet. Die Ladungsverteilung wurde nach dem CHARDI-Konzept berechnet und mit den Werten nach ‚bond length-bond strength‘ verglichen.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19966220216
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  • 94
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    Pseudoelementverbindungen. VII [1]. Kristall- und Molekülstruktur von Tris(ethylendiamin)nickel(II)-bis(2-methyl-4-chlorphenoxycyanamidoacetat)Professor Heinrich Kriegsmann zum 70. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 361-366 
    Details
    ISSN: 0044-2313
    Keywords: Cyanamidocarboxylate complexes ; IR ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Pseudoelement Compounds VII. [1] Crystal and Molecular Structure of Tris(ethylenediamine)nickel(II)-bis(2-methyl-4-chlorophenoxy-cyanamidoacetate)Surprisingly, in the presence of ethylenediamine 2-methyl-4-chlorphenoxy-cyanamidoactetate reacts with nickel(II) and copper(II) ions preferentially under formation of complexes of the type [M(en)3]X2. The IR spectra and the X-ray diffraction investigations corresponding to [Ni(en)3][2-Me-ClC6H3OCH2C(O)NCN]2 show that two cyanamidocarboxylate ions [RC(O)NCN]- are bonded to the complex cation through, in each case, two N—H … O=C hydrogen bonds between NH protons of ethylenediamine ligands and the carbonyl oxygen atoms. Additionally, in the crystal weak N—H … N≡C bridges were found between the nitrile nitrogen atoms of the anions and NH protons of neighbouring complex cations.
    Notes: 2-Methyl-4-chlorphenoxy-cyanamidoacetat bildet zu unserer Überraschung mit Nickel(II)- und Kupfer(II)-Ionen in Gegenwart von Ethylendiamin bevorzugt Komplexe der Zusammensetzung [M(en)3]X2. IR-spektroskopische Messungen und die Kristallstruktrukturuntersuchung an [Ni(en)3][2-Me-4-ClC6H3OCH2C(O)NCN]2 zeigen, daß zwei Cyanamidocarboxylat-Anionen [RC(O)NCN]- über jeweils zwei N—H … O=C-Wasserstoffbrückenbindungen zwischen N—H-Protonen der Ethylendiamin-Liganden und den Carbonyl-Sauerstoffatomen an ein komplexes Kation [Ni(en)3]2+ gebunden sind. Im Kristall liegen außerdem noch schwache N—H … N≡C-Brücken zwischen Nitril-N-Atomen der Anionen und NH-Protonen benachbarter komplexer Kationen vor.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19966220226
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  • 95
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    Synthesis, Crystal Structure, and High Temperature Behavior of Zr3N4 (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 367-372 
    Details
    ISSN: 0044-2313
    Keywords: Zirconium nitride ; synthesis ; crystal structure ; high temperature behavior ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthese, Kristallstruktur und Hochtemperaturverhalten von Zr3N4Durch Ammonolyse von ZrCl4 konnte ein rotbraunes Zirconiumnitrid dargestellt werden. Die chemische Analyse ergab eine Zusammensetzung von Zr3N4. Mit Pulvermethoden ist es für das Zr3N4 nicht möglich, zwischen den Raumgruppen Pnam und Pna21 zu unterscheiden. Die Gitterkonstanten ergaben sich zu: a = 972,94(5) pm, b = 1031,75(6) pm, c = 328,10(1) pm (Z = 4). Zur Verfeinerung der Kristallstruktur dienten Pulver-Röntgenbeugungsdaten. Das Hochtemperaturverhalten wurde mittels in situ XRD-Methoden untersucht. Zr3N4 zersetzt sich bei Temperaturen oberhalb von 800°C in ZrN und Stickstoff.
    Notes: A red-brown zirconium nitride was prepared by ammonolysis of ZrCl4. Chemical analysis leads to a composition of Zr3N4. It is not possible to distinguish between the space groups Pnam and Pna21 in the case of Zr3N4 using powder methods. The lattice constants are: a = 972.94(5) pm, b = 1081.75(6) pm, c = 328.10(1) pm (Z = 4). X-ray powder diffraction data were used for structure refinement. The high temperature behavior was investigated with in situ XRD methods. Zr3N4 decomposes into ZrN and nitrogen gas at temperatures above 800°C.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19966220227
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  • 96
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    Über die Halogenaminierung von Diseleniden. Synthese und Struktur des achtgliedrigen Ring-Kations [Me2SN2SeMe]2++Professor Rolf Appel zum 75. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 745-750 
    Details
    ISSN: 0044-2313
    Keywords: Selenium-nitrogen compounds ; diselenides ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Haloamination of Diselenides. Synthesis and Structure of the Eight-membered Ring Cation [Me2SN2SeMe]2++N-halogen compounds of benzamidine and S,S-dimethylsulfone diimides react with diselenides by Se—Se-bond cleavage yielding different types of selenium-nitrogen compounds. With N-bromo-benzamidine the diazene derivatives RSeN(Ph)CN=NC(Ph)NSeR 2a, b (a: R = Me; b: R = Ph) are formed. In the reaction of N,N′-Dichloro-S,S-dimethylsulfone diimide, Me2S(NCl)2, with diselenides cyclic hetero-selenonium salts [(Me2SN2SeR)Cl]2 (4a, b) are obtained. The structure of the eight membered ring compound 4a was determined by x-ray crystallography (space group P1, Z = 1) and compared with that of the isotypic sulfonium salt [(Me2SN2SMe)Br]2 (3a).
    Notes: N-Halogenverbindungen des Benzamidins und des S,S-Dimethylsulfodiimids reagieren mit Diseleniden unter Se—Se-Bindungsspaltung zu verschiedenartigen Selen-Stickstoffverbindungen. Mit N-Brom-benzamidin entstehen Diazen-Derivate RSeN(Ph)CN=NC(Ph)NSeR 2a, b(a: R = Me; b: R = Ph). N,N′-Dichlor-S,S-dimethylsulfodiimid, Me2S(NCl)2, reagiert mit Diseleniden unter Bildung cyclischer Heteroselenonium-Salze [(Me2SN2SeR)Cl]2 (4a, b). Die Struktur der achtgliedrigen Ringverbindung 4a wurde durch Röntgenstrukturanalyse bestimmt (Raumgruppe P1, Z = 1) und mit der des isotypen Sulfoniumsalzes [(Me2SN2SMe)Br]2 (3a) verglichen.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19966220431
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  • 97
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    Meso- und Rac-Decaisopropylstannocen: Stereoisomerie bedingt durch parallele Anordnung zweier Pentaisopropylcyclopentadienyl-Liganden in Schaufelrad-KonformationProfessor Herbert Schumann zum 60. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 751-755 
    Details
    ISSN: 0044-2313
    Keywords: Decaisopropylstannocene ; crystal structure ; CPMAS 119Sn NMR ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Meso- and Rac-Decaisopropylstannocene: Stereoisomerism Caused by Parallel Arrangement of Two Pentaisopropylcyclopentadienyl Ligands in Paddlewheel ConformationDecaisopropylstannocene 1 is the first Decaisopropylmetallocene, where X-ray diffraction data could be successfully refined and the third example of a group 14 Metallocene with a symmetric sandwich structure. Due to the directionality of the isopropyl substituents 1 occurs as a mixture of diastereomers in the crystalline state as well as in solution. The stereoisomers exhibit the expected signals in solution (1H and 13C NMR) and in the crystal (CPMAS 119Sn NMR).
    Notes: Decaisopropylstannocen 1 ist das erste Decaisopropylmetallocen, dessen Röntgendiffraktometer-Datensatz erfolgreich verfeinert werden konnte und das dritte Beispiel eines Metallocens der Gruppe 14 mit einer symmetrischen Sandwichstruktur. Aufgrund der Direktionalität der Isopropylsubstituenten beider Ringliganden liegt 1 im Kristall und in Lösung als Diastereomerengemisch vor. Die Stereoisomeren zeigen die erwarteten Signale in Lösung (1H- und 13C-NMR) und im Kristall (CPMAS- 119Sn-NMR).
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19966220432
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  • 98
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    Zur Chemie des Dimesityleisens. VIII. Lösungsverhalten von Tetramesityldieisen und die Kristallstruktur eines Dimethoxyethan-Addukts (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 756-758 
    Details
    ISSN: 0044-2313
    Keywords: Dimesityliron ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Chemistry of Dimesityl Iron. VIII Solution Behaviour of Tetramesityldiiron and Crystal Structure of Dimesityl(dimethoxyethane)ironThe dimer dimesityliron yields in polar solvents solvated monomers. The adduct with dimethoxyethane was isolated and characterized by X-ray structure determination.
    Notes: Während Dimesityleisen in unpolaren Lösungsmitteln dimer vorliegt, spaltet es in stärker polaren Lösungsmitteln in solvatisierte Monomere auf. Mit Dimethoxyethan wurde ein Addukt isoliert und strukturell charakterisiert.
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    URL: http://dx.doi.org/10.1002/zaac.19966220433
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  • 99
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    Li2CrO4 · 2H2O: Ungewöhnliche Wasserstoffbrückenbindung und Koordination der O-Liganden des Anions CrO42- (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 721-723 
    Details
    ISSN: 0044-2313
    Keywords: Lithium chromate dihydrate ; single-crystals ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Li2CrO4 · 2H2O: Unusual Hydrogen Bridge Bonding and Coordination for Oxygen of the Anions CrO42-The crystal structure of Li2CrO4 · 2H2O was solved including the positions of hydrogen by X-ray methods. Li2CrO4 · 2H2O: P212121, Z = 4, a = 5.503(1) Å, b = 7.733(2) Å, c = 11.987(2) Å, Z(Fo) with (Fo)2 ≥ 3σ(Fo)2 = 2284, Z (parameter) = 99, R/Rw = 0.025/0.029 LiCrO4 · 2H2O contains a locally bordered hydrogen bridge bonding system between water molecules as donors and two O of CrO42- as acceptors. This system connects anions in the direction [010]. It is noticeable that oxygen ligands of the anion CrO42- have strongly differing coordination.
    Notes: Die Kristallstruktur von Li2CrO4 · 2 H2O wurde einschließlich der Wasserstofflagen röntgenographisch ermittelt: Li2CrO4 · 2 H2O: P212121, Z = 4, a = 5,503(1) Å, b = 7,733(2) Å, c = 11,987(2) Å, Z(Fo) mit (Fo)2 ≥ 3σ(Fo)2 = 2284, Z (Parameter) = 99, R/Rw = 0,025/0,029 Li2CrO4 · 2H2O enthält lokal begrenzte Wasserstoffbrückenbindungssysteme zwischen Wassermolekülen als Donatoren und zwei O von CrO42- als Akzeptoren. Sie verknüpfen Anionen in Richtung [010]. Auffallend ist die sehr unterschiedliche Koordination der O-Liganden des Anions CrO42-.
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    URL: http://dx.doi.org/10.1002/zaac.19966220426
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  • 100
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    Thioureato-verbrückte zweikernige Komplexe der Lanthanoide Darstellung und Struktur von [{PhC(NPh)NC(S)NEt2}{Et2NC(S)NH}LnBr(thf)]2 (Ln = Gd, Sm)Professor Kurt Dehnicke zum 65. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 734-738 
    Details
    ISSN: 0044-2313
    Keywords: GdIII ; SmIII ; binuclear complex ; thioureato-ligand ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Thioureato Brigded Binuclear Complexes of the Lanthanides Synthesis and Crystal Structure of [{PhC(NPh)NC(S)NEt2}{Et2NC(S)NH}LnBr(thf)]2 (Ln = Gd, Sm)The reaction of potassium-N-(diethylaminothiocarbonyl)-N′-phenyl-benzamidinat with LnBr3 (Ln = Gd, Sm) leads to the formation of the binuclear complexes [{PhC(NPh)NC(S)NEt2}{Et2NC(S)N}LnBr(thf)]2} (Ln = Gd 1, Sm 2). The two bridging thiureatoligands are probably built during the reaction of potassium with the starting ligand. Coordination by one N-(diethylaminothiocarbonyl)-N′-phenylbenzamidinato-ligand, one Br-ion and one THF-ligand leads to square antiprismatic coordination of the lanthanoids. The structures of both compounds were characterized by X-ray analysis (1: P1 (Nr.2), Z = 1, a = 12,006(4) Å, b = 12,245(4) Å, c = 13,612(3) Å, α = 70,55(3)°, β = 68,21(3)°, γ = 81,31(3)° 2: P1 (Nr.2), Z = 1, a = 11,803(3) Å, b = 12,344(5) Å, c = 12,797(8) Å, α = 103,07(5)°, β = 101,76(3)°, γ = 114,13(3)°)
    Notes: Bei der Reaktion von Kalium-N-(diethylaminothiocarbonyl)-N′-phenyl-benzamidinat mit LnBr3 (Ln = Gd, Sm) bilden sich die zweikernigen Komplexe [{PhC(NPh)NC(S)NEt2}{Et2NC(S)N}LnBr(thf)]2} (Ln = Gd 1, Sm 2). Die Lanthanoidionen werden durch zwei Thioureatoeinheiten verbrückt, die sich vermutlich schon bei der Metallierung des Liganden bilden. Durch zusätzliche Koordination eines N-(Diethylaminothiocarbonyl)-N′-phenyl-benzamidinato-Liganden sowie eines THF-Moleküls und eines Brom-Atoms erhält jedes Lanthanoidion eine quadratisch antiprismatische Koordination.Der Aufbau dieser Verbindungen konnte durch Kristallstrukturuntersuchungen geklärt werden (1: P1 (Nr.2), Z = 1, a = 12,006(4) Å, b = 12,245(4) Å, c = 13,612(3) Å, α = 70,55(3)°, β = 68,21(3)°, γ = 81,31(3)° 2: P1 (Nr.2), Z = 1, a = 11,803(3) Å, b = 12,344(5) Å, c = 12,797(8) Å, α = 103,07(5)°, β = 101,76(3)°, γ = 114,13(3)°)
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19966220429
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