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  • Articles: DFG German National Licenses  (158)
  • 1995-1999  (158)
  • 1985-1989
  • 1995  (158)
  • crystal structure  (158)
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  • Articles: DFG German National Licenses  (158)
Material
Years
  • 1995-1999  (158)
  • 1985-1989
Year
Keywords
  • 1
    Electronic Resource
    Electronic Resource
    α-Iminohydroxylamine-α-aminonitrone tautomerism: a 1∶1 mixture of two tautomeric forms in crystals of N-(4,5-dihydro-1H-imidazol-2-yl)-N-phenyl-hydroxylamine (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 813-821 
    Details
    ISSN: 1572-8854
    Keywords: Tautomerism ; hydrogen bonding ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Crystals consisting of two distinct chemical entities, tautomers of each other, in exact 1∶1 ratio, have been obtained and their structure determined by X-ray analysis. The crystals of C9H11N3·C9H11N3 are monoclinic,P21/c,a=15.674(3),b=17.085(3),c=13.758(3)Å, β=90.78(2)°,Z=8. There are two hydroxylamine and two aminonitrone molecules in the asymmetric unit. Hydrogen bonds connect those molecules into chiral layers. Layers of opposite chirality alternate andthe crystal is centrosymmetric as a whole. Within those layers chains of tautomers joined by very strong O−H... O and strong N−H... N bonds can be recognized. Proton transfer along those chains with simultaneous rearrangement of π-bonds within the molecules would result in interconversion of tautomers and would affect chirality of the layer.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01671076
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  • 2
    Electronic Resource
    Electronic Resource
    Dialkylimidazolium-sodium chloroaluminate ternary salt system: phase diagram and crystal structure (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 57-62 
    Details
    ISSN: 1572-8854
    Keywords: phase diagram ; buffered chloroaluminate ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The phase diagram of the buffered neutral aluminum chloride + 1-ethyl-3-methyl-1H-imidazolium chloride + sodium chloride (AlCl3-EMIC-NaCl) ternary melt system can be represented by a binary phase diagram composed of (EMI)AlCl4 and NaAlCl4. In the binary phase diagram, the salts are liquid at, or near, room temperature for a wide range of compositions. At the 1∶1 composition, the congruently melting compound (EMI)(Na)(AlCl4)2 with m.p.=36.7°C is formed. Crystals of this mixed organic-inorganic salt were grown for single crystal x-ray diffraction analysis. The compound crystalizes in the space group $$P\bar 1$$ with lattice parametersa=10.321(1) Å,b=10.895(3) Å,c=9.284(4) Å, α=98.31(2)°, β=100.83(4)°, γ=101.95(3)°. Data collected at −120°C gave final residuals ofR=0.037 andR w=0.045 using 2713 observed reflections. The packing diagram reveals Na+ ion zig-zag chains running along thea-axis with each Na+ surrounded by four AlCl 4 − units, reminiscent of NaAlCl4. The AlCl 4 − ions form a distorted square planar coordination sphere around Na+ at an average Na−Al distance of 3.76(4) Å. Using a sodium ionic radius of 1.16 Å, a new AlCl 4 − ionic radius of 2.60 Å is calculated. This radius is 0.21 Å shorter than the reported thermodynamic radius.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01667037
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  • 3
    Electronic Resource
    Electronic Resource
    Antifungal copyrine alkaloids: crystal structure of 3-methylsampangine (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 223-226 
    Details
    ISSN: 1572-8854
    Keywords: Antifungal alkaloids ; 3-methylsampangine ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract 3-Methylsampangine, C16H10N2O, crystallizes in the monoclinic space group P21/c witha=7.260(3),b=10.697(5),c=15.342(6) Å, and β=102.69(4). All nonhydrogen atoms of this potent antifungal agent are planar to within 0.082 Å. The title compound exhibits potentin vitro antifungal activity againstC. neoformans, C. albicans andA. fumigatus.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01665173
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  • 4
    Electronic Resource
    Electronic Resource
    Crystal structure of decacalcium tetrapotassium hexakis (pyrophosphate) nonahydrate (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 219-222 
    Details
    ISSN: 1572-8854
    Keywords: Calcium phosphate ; calcium pyrophosphate ; calcium potassium pyrophosphate ; crystal structure ; layer-type structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal structure of Ca10K4(P2O7)6·9H2O has been determined by single crystal X-ray diffraction. Crystals are hexagonal, space group P63cm witha=11.761(1),c=9.770(1) Å, andZ=1. The structure was refined toR=0.028 andR w=0.037 for 468 reflections withI≥3σ(I). The structure consists of a compact assembly of Ca and P2O7 ions arranged in layers perpendicular to thec-axis in a hexagonal array with relatively large open channels along thec-axis. The K ions and the water molecules are located in these open channels and are disordered.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01665172
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  • 5
    Electronic Resource
    Electronic Resource
    Unusual occurrence of photooxidation of a cage diol (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 295-298 
    Details
    ISSN: 1572-8854
    Keywords: Cage-diol ; crystal structure ; photooxidation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract An unusual photooxidation was noted upon photolytic cage closure of a substituted tricyclo[6.2.1.02.7]undecane-exo, exo-diol. The resultant compound, which may be regarded as a mono-reduced pentacyclo[5.4.0.02,6.03,10.05,9]undecane-8,11-dione, was characterizedvia X-ray crystallography. This species could be reduced to the tricyclo[6.2.1.02,7]undecane-endo, exo-diol under conditions previously shown to be inert for the parent dione.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01796053
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  • 6
    Electronic Resource
    Electronic Resource
    Crystal and molecular structure of 6,7-benzo-3,4 (1,4-dimethoxy-2,3-naphtho)-1,5-dioxosuberane (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 379-382 
    Details
    ISSN: 1572-8854
    Keywords: Benzonaphthodioxosuberane ; crystal structure ; radermachol
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal and molecular structure of the title compound (2) C21H16O4 has been determined by an X-ray analysis, by direct methods from diffractometer data and refined by full-matrix least squares. The compound (2) crystallizes in the space group P21/a, with cell parameters:a=36.432(5),b=5.512(3),c=8.269(5) Å, β=108.0(3)°,z=4,D c =1.397 g/cm−3,R=7.8 for 1136 observed reflections. The conformation of the tetracyclic ring system shows a folding of two planar parts of the carbon skeleton about an axis passing thorough C8 and C16 of the seven membered ring C.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01665273
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  • 7
    Electronic Resource
    Electronic Resource
    Synthesis and structural characterization of [Au2Pd14(μ3-CO)7(μ2-CO)2(PMe3)11](PF6)2—An icosahedrally-based high nuclearity mixed metal cluster (1995)
    Springer
    Journal of cluster science 6 (1995), S. 71-91 
    Details
    ISSN: 1572-8862
    Keywords: Palladium ; gold ; cluster ; phosphine ; 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 [Au2Pd14(μ3-CO)7(μ2-CO)2(PMe3)11](PF6)2 has been synthesized from [Pd8(CO)8(PMe3)7] and AuCl(PCy3) in the presence of TIPF6. It has been characterised on the basis of mass spectrometry, infrared and NMR spectroscopy, and a single crystal X-ray diffraction study. The structure is based on a palladium-centered Au2Pd11 icosahedron which shares an edge with a Pd5 trigonal bipyramid.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01175837
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  • 8
    Electronic Resource
    Electronic Resource
    The synthesis and reactivity of the heptanuclear dianion [Os7(CO)20]2− including the synthesis and structural characterizations of the compounds [Os7(CO)20(AuPEt)3 2] and [Os8(CO)20(η6-C6H6] (1995)
    Springer
    Journal of cluster science 6 (1995), S. 163-173 
    Details
    ISSN: 1572-8862
    Keywords: Cluster carbonyl ; osmium ; gold ; arene ; 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 Reduction of the heptaosmium cluster [Os7(CO)21] With [Et4N][NH4) gives the cluster dianion [Os7(CO)20]2−,1, in high yield. The reaction of the dianion with [AuPR 3Cl] (R=Et or Ph) in the presence of TlPF6 forms [Os7((CO)20(AuPR 3)2] [R=Et (2a);R = Ph(2b)] in 80% yield, while the corresponding reaction with (Os(C6H6)(CH3CN)3]2+ gives [Os8(CO)20 (η 6-C6H6)] (3) in reasonable yield (ca. 30%). The dianion,1, and the clusters2 and3 have been fully characterized by bout spectroscopic and crystallographic methods. The crystal structure of the [Ph4P]+ salt of1 shows that the metals in the anion adopt a capped octahedral geometry, with all twenty carbonyl ligands in terminal sites. The metal core geometry in2a is best described as a tricapped octahedron, and is based on the structure of the dianion1 with two adjacent octahedral faces capped by the Au atoms of the two AuPEt3 groups. In a similar fashion, the geometry of3 is related to that of1 with the addition of an Os(C6H6) unit capped to a triangular face, to give a bicapped octahedral framework.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01175843
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  • 9
    Electronic Resource
    Electronic Resource
    Synthesis and characterization of the undecaosmium carbido carbonyl cluster: Crystal and molecular structures of [N(PPh3)2][Os11C(CO)27(μ-Cl)] (1995)
    Springer
    Journal of cluster science 6 (1995), S. 343-346 
    Details
    ISSN: 1572-8862
    Keywords: Undecaosmium carbido cluster ; µ-bridged chlorol preparation ; 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 A chloro-derivative of undecaosmium carbido cluster [Os11C(CO)27(µ-Cl)]-1 anion has been prepared and fully characterized by spectroscopic and crystallographic methods. The structure1 is an important intermediate for the conversion of [Os11C(CO)27]2 2 dianion to [OS10C(CO)24]2-3 dianion.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01169700
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  • 10
    Electronic Resource
    Electronic Resource
    Synthesis, chemical, and electrochemical characterization of the [Ag13{μ3-Fe(CO)4}] n− (n = 3, 4, 5) cluster anions: X-Ray structural determination of [N(PPh3)2]3 [Ag12(μ12-Ag){μ3Fe(CO)4}8]1 (1995)
    Springer
    Journal of cluster science 6 (1995), S. 107-123 
    Details
    ISSN: 1572-8862
    Keywords: Silver ; iron ; carbonyl ; cluster ; 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 oxidation of the [Fe(CO)4]2− dianion with Ag+ salts occurs through a particularinner-sphere mechanism, which involves an intermediate cascade of silver clusters stabilized by Fe(CO)4 ligands. The last detectable Ag-Fe cluster of the sequence is the [Ag13{μ-Fe(CO)4}8]3− trianion, which has been selectively obtained by using ca. 1.7 equivalents of Ag+ per mole of [Fe(CO)4]2−. The [Ag13{μ-Fe(CO)4}8]3−- trianion has been isolated in a crystalline state with several quaternary cations, and has been characterized by X-ray diffraction studies of its bis(triphenylphosphine)iminium salt. [N(PPh3)2]3 [Ag13{μ 3-Fe(CO)4}8]·2(CH3)2CO, monoclinic, space group P21 (No.4),a = 16.284(2) Å,b =18.767(5) Å,c = 25.905(4) Å,β = 90.46(1)°,V = 7916(3) Å3,Z = 2,R = 0.0324. The molecular structure of the anion consists of a centered cuboctahedron of silver atoms with the triangular faces capped by Fe(CO)4 units. Chemical reduction of ( Ag13{μ 3-Fe(CO)4}8]3− affords the corresponding [Ag13{μ 3-Fe(CO)4)8]4−, which in turn gives [Ag13{μ 3-Fe(CO)4)8]5− and [Ag6{μ 3-Fe(CO)4}4]– upon further reduction. Electrochemical investigations confirm the reversibility of the [Ag13{μ 3-Fe(CO)4}8]3−/4− redox change. Furthermore, in spite of some electrode poisoning effects, evidence of the existence of the [Ag13{μ 3-Fe(CO)4}8]5− pentaanion was obtained. The yet structurally uncharacterized [Ag6{μ 3-Fe(CO)4)4]2− dianion is quantitatively obtained by reaction of [Fe(CO)4]2− with ca. 1.5 equivalents of Ag+ or by addition of one equivalent of Ag+ to solutions of the [Ag5{Fe(CO)4}4]3− trianion. All attempts to isolate its quaternary salts as crystalline materials failed owing to formation of amorphous insoluble precipitates. The above series ofμ 3-Fe(CO)4 octa-capped cuboctahedral Ag13 clusters can be envisioned as the Ag+ . Ag and Ag− cryptates of the [Ag12{μ}3-Fe(CO)4}8]4− cryptand. respectively.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01175839
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  • 11
    Electronic Resource
    Electronic Resource
    The synthesis and structural characterization of Os3(CO)8[Si(OMe)3][μ-PMe2(C6H4](μ-H)2: An unusual unsaturated triosmium cluster complex (1995)
    Springer
    Journal of cluster science 6 (1995), S. 437-447 
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    ISSN: 1572-8862
    Keywords: Osmium ; unsaturated cluster ; ortho-metallation ; siloxyl ligand ; 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 Os3(CO)10(NCMe)[Si(OMe)3](μ-H),1, with PMe2Ph yielded the new complex Os3(CO)10(PMe2Ph)[Si(OMe)3](μ-H),2 by substitution of the MeCn ligand with the phosphine ligand. When heated to 125°C compound2 was decarbonylated and transformed into the new unsaturated cluster complex Os3(CO)8[μ-PMe2(C6H4)][Si(OMe)3](μ-H)2,3 in 54% yield. Compound3 was characterized by a single crystal X-ray diffraction analysis, osmium bonds. The phenyl ring of the phosphine ligand has undergoneortho-metallation by a neighboring metal atom. A terminally coordinated Si(OMe)3 ligand is coordinated to the third osmium atom. The cluster is unsaturated by the amount of 2 electrons, and there is an open coordination site on the siloxyl substituted osmium atom that is partially filled by a weak interaction with one of the π-bonds of theortho-metalled phenyl ring. Complex3 reacts with CO at 1 atm to reform compound2 in 85% yield in 5 h at 40°C. Crystal Data: for3: space group = P21/n,a = 9.911(2) Å,b = 18.451(6) Å,c = 14.872(2) Å,β = 95.64(2)°,Z = 4, 1994 reflections,R = 0.028.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01165472
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  • 12
    Electronic Resource
    Electronic Resource
    Doubly-bridged binuclear complexes of oxomolybdenum(V) and oxotungsten(V) containing sexadentate ligands (1995)
    Springer
    Journal of cluster science 6 (1995), S. 549-566 
    Details
    ISSN: 1572-8862
    Keywords: Molybdenum ; tungsten ; di-μ-oxo bridge ; sexadentate ligands ; asymmetric distortion ; stereoselectivity ; 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 Binuclear oxomolybdenum(V) and oxotungsten(V) complexes of the type, [M 2(O)2(μ-X)(μ-X 1)]”, where M=Mo, W;X.X 1=O, S; L=edta, pdta (n=2-), tpen, tppn (n=2+) (edta4– =ethylenediaminetetraacetate(4–), pdta=R- orR,S-propylenediaminetetraacetate(4–), tpen=N,N,N 1,N1-tetrakis(2-pyridyhnethyl)-ethylenediamine, and tppn=R- orR,S-N,N,N 1,N1-tetrakis(2-pyridylmethyl)-propylenediami ne) are reviewed with respect to their preparation, structure, spectroscopic properties, reactivities, and in particular asymmetric distortion around the bicyclo [4.1.1 ] type core and stereoselectivity related to this distortion,
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01165773
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  • 13
    Electronic Resource
    Electronic Resource
    Comparison of the crystal structure and molecular models of N,N-diisobutyl-2-(octylphenylphosphinyl)acetamide (CMPO) (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 43-49 
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    ISSN: 1572-8854
    Keywords: Molecular mechanics ; molecular dynamics ; MNDO ; CMPO ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal structure of N,N-diisobutyl-2-(octylphenylphosphinyl)acetamide, or CMPO was recently determined. The compound crystallizes in the space group P21/c witha=13.446(6),b=22.280(7),c=17.217(7) Å, β=92.07(4)°, andD calc=1.05 g/cm3 forZ=8 @20°C). Molecular mechanics, molecular dynamics, and MNDO calculations were also performed on CMPO utilizing the SYBYL1 suite of programs. The results from these calculations are compared to the crystal structure and to similar calculations performed on CMPO using ALCHEMY2,3. In general, the results from the calculations agree fairly well with the parameters from the crystal structure.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01666193
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  • 14
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    Electronic Resource
    Mercury(II) complex with terpyridine: structure of the 2∶1 solvate of [Hg(terpy)2](CF3SO3)2 with acetone (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 453-458 
    Details
    ISSN: 1572-8854
    Keywords: Mercury(II) terpyridine complex ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract [Hg(terpy)2](CF3SO3)2·0.5(CH3)2CO crystallizes in the triclinic $$P\bar 1$$ space group witha=14.631(6),b=15.258(4),c=18.785(7) Å, α=69.66(2), β=70.72(1), γ=88.55(1)°. The crystal structure consists of two independent [Hg(terpy)2]2+ cations, four trifluoromethanesulfonate anions and an acetone molecule in the asymmetric unit. Each mercury atom is coordinated by two tridentate terpyridine ligands forming an irregular six-coordination polyhedron. The Hg−N bond lengths range from 2.27(2) to 2.53(2) Å.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01665700
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  • 15
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    Crystal structures of twoN-substituted 2-thioxo-1,3-dithiole-4-carboxamides (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 463-467 
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    ISSN: 1572-8854
    Keywords: 1,3-dithiole-4-carboxamides ; resonance effect ; short intramolecular S...O contact ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The two closely related compoundsN,N-dimethyl 5-(methylthio)-2-thioxo-1,3-dithiole-4-carboxamide1 andN-(p-methoxy-phenyl)-N-methyl 5-(methylthio)-2-thioxo-1,3-dithiole-4-carboxamide2 have been characterized by X-ray crystal structure determination. Crystal data for1: triclinic, $$P\bar 1$$ ,a=6.767(1),b=12.594(2),c=6.648(1) Å, α=101.38(1), β=93.37(2), γ=79.62(1)°,V=546.2 Å3,Z=2. Crystal data for2: monoclinic, Cc,a=19.836(4),b=6.057(1),c=15.860(3) Å, β=127.61(3)°,V=1509.5Å3,Z=4. The molecular structures of1 and2 show remarkable differences concerning the conformational behavior. These differences are related to the nature of the substituents at the nitrogen atom. The presence of an aromatic system in2 leads to an almost planar arrangement of the α-oxoketene dithioacetal moiety. This effect is accompanied by a short intramolecular S...O contact of 2.648(2) Å. In the absence of an aromatic system, as is the case for compound1, neither a resonance effect along the α-oxoketene dithioacetal fragment nor a short S...O distance is observed.
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    URL: http://dx.doi.org/10.1007/BF01665702
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  • 16
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    Electronic Resource
    The crystal structure of a heterobimetallic crown ether complex: [Na(dibenzo-18-crown-6)][FeCl4] (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 579-582 
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    ISSN: 1572-8854
    Keywords: Dibenzo-18-crown-6 ; hetero bimetallic ; crown ether ; crystal structure ; ferric chloride
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Slow evaporation of a solution of ferric chloride and dibenzo-18-crown-6 in 3∶1 CH3CN∶CH3OH produced single crystals of the title complex. This heterobimetallic crown ether complex, [Na(dibenzo-18-crown-6)][FeCl4], crystallizes in the monoclinic space group P2t/n with cell parameters (at 22°C)a=14.608(6),b=10.466(9),c=17.276(9)Å, β=91.47(6)°, andD calc=1.46 g cm−3 for Z=4. The structure consists of discrete ions with the shortest Na ... Cl distance a lengthy contact of 3.56(1)Å. The average Na...O separation is 2.69(3)Å. The [FeCl4]− anion exhibits a distorted tetrahedral geometry with an average Fe−Cl bond length of 2.16(2)Å.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01667027
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  • 17
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    Electronic Resource
    Nucleophilic additions of primary and secondary amines to pentacyclo[5.4.0.02,6.03,10.05,9]undecane-8,11-dione (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 633-640 
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    ISSN: 1572-8854
    Keywords: Amines ; crystal structure ; pentacycloundecane-8,11-dione
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The crystal structures of three compounds formedvia nucleophilic attack of a heterocyclic secondary amine on PCU-8,11-dione, with the concomitant intramolecular attack of one keto oxygen on the carbon of the other ketone, are presented. In all three compounds, the bridging oxygen contains substantial p-character, and the bonds to the “attacking” nitrogen are significantly shorter than would be expected.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01665969
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  • 18
    Electronic Resource
    Electronic Resource
    X-ray structure of sesterterpene, 16β-acetoxy-24-methyl-12,24-dioxoscalaran-25-al (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 765-768 
    Details
    ISSN: 1572-8854
    Keywords: Sesterterpene ; scalaran ; crystal structure ; marine compound
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The molecular geometry of a tetracyclic sesterterpene has been determined by X-ray diffraction. The conformation of the aldehyde group as observed in the crystal structure supports the rationalization for the absence of aldehyde proton coupling in the nmr spectra of the compound. Crystal data: C28H42O5, M.W.=458.6; orthorhombic, P212121;a=10.797(2),b=29.270(9),c=8.033(1)Å,V=2538.7Å3,Dx=1.199 g cm−3;R=0.045 for 2287 observed reflections.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01670333
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  • 19
    Electronic Resource
    Electronic Resource
    Synthesis of a chiral calixarene: 5,11,17,23-tetra (tert-butyl)-25,27-bis[((+)-camphor-10-sulfonyl)-oxy]-calix[4]arene-26,28-diol: crystal and molecular structure of its (1∶2) complex with toluene (1995)
    Springer
    Journal of chemical crystallography 25 (1995), S. 401-406 
    Details
    ISSN: 1572-8854
    Keywords: Calixarene ; complex ; crystal structure ; chirality
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The title compound was obtained by treatment ofp-tert-butylcalix[4]arene with (+) camphorsulfonyl chloride in triethylamine and toluene. A (1∶2) complex with toluene has been found. Its structure has been determined by X-ray crystallography. Crystals are triclinic with space group P1,a=16.426(3),b=18.553(3),c=13.661(2) Å, α=94.78(2), β=110.76(2), γ=72.83(2)°,V=3720(2) Å3,d c =1.127 g/cm3 Z=2. Refinement based on 10495 observed reflections led to a finalR value of 0.100. The two independent molecules of calixarene in the asymmetric unit are in the cone conformation and the calixarene cavities are empty. The guest molecule occupies the interhost space. The norborane skelton of (+) camphorsulfonyl group is the same as ones found in literature. Only van der Waals interactions exist between the host and the guest molecules.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01665277
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  • 20
    Electronic Resource
    Electronic Resource
    Synthesis and structure of a seven electron triangular cluster complex [Mo3S4Cl3(dppe)2(PEt3] (1995)
    Springer
    Journal of cluster science 6 (1995), S. 523-532 
    Details
    ISSN: 1572-8862
    Keywords: Molybdenum ; reduction ; seven-electron triangular cluster ; bridging sulfide ; 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 triangular six-electron cluster complex [Mo3S4Cl4(PEt3) x (thf)5] produced by the excision reaction of Mo3S7Cl4 with triethypholsphine is reduced by magnesium at − 20°C. Subsequent addition of dppe (=1,2-his(diphenylphosphino)ethane) to the reduced species affords a seven-electron triangular cluster complex [Mo3S4Cl3(dppe)2(PEt3)]. The complex crystallizes in the space groupCm witha=17.170(6),b-19.878(6),c = 13.289(5)β = 121.73(2)°,V = 3858(2) A3, andZ = 2. The structure shows an almost equilateral triangle of three molybdenum atoms capped by a Sulfur atom and bridged by three sulfur atoms. The Mo Mo distances, ranging from 2.804(1) to 2.809(1) A are elongated ca. 0.04 A as compared with lose of a six-electron cluster complex with drape ligands. Two molybdenum atoms have a chlorine and a dppe ligands, and the other molybdenum atom bas a chlorine and a triethylphosphine ligands. The UV-Vis spectrum has a characteristic broad hand centered at 1410 n m, which is not observed for six-electron clusters. The ESR spectrum indicates the presence of an unpaired electron consistent with the formulation of the compound as a seven-electron cluster.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01165771
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  • 21
    Electronic Resource
    Electronic Resource
    Linear and Nonlinear Optical Properties Of Racemic (±)2-(α-Methylbenzylamino)-5-Nitropyridine Single Crystals (1995)
    Springer
    Optical review 2 (1995), S. 128-131 
    Details
    ISSN: 1349-9432
    Keywords: organic crystal ; racemic form ; second-harmonic generation ; refractive index ; nonlinear optical coefficient ; crystal structure ; oriented-gas model
    Source: Springer Online Journal Archives 1860-2000
    Topics: Physics
    Notes: Abstract Linear and nonlinear optical properties of racemic (±)2-(α-methylbenzylamino)-5-nitropyridine ((±)MBANP) single crystals have been comprehensively investigated and compared with those of the enantiomorph (–)2-(α-methylbenzylamino)-5-nitropyridine ((–)MBANP) crystals. (±)MBANP crystal exhibits very high chemical and physical stability, but relatively small nonlinear optical coefficients (d31 = 6.8 pm/V, d32 = 4.7 pm/V, d33 = 0.84 pm/V). A comparison between the nonlinear optical coefficients of (±)MBANP and (–)MBANP demonstrates the validity of the oriented-gas model in molecular crystals that neglects all the contributions from intermolecular interaction.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/s10043-995-0128-5
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  • 22
    Electronic Resource
    Electronic Resource
    The synthesis and X-Ray crystallographic analysis of a stable norbornadienone: 17-Oxo-7,16-methano-7,16-diphenylcyclopenta[d,e]tribenzo[a,h,j]anthracene (1995)
    Springer
    Structural chemistry 6 (1995), S. 167-173 
    Details
    ISSN: 1572-9001
    Keywords: MM3 ; PM3 ; MMX ; crystal structure ; norbonadienone ; distorted compound
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The reaction of 4,5-didehydroacenaphthene with phencyclone yields the title compound, a stable dibenzo-fused norbornadienone (8). The X-ray structure of8 is presented and compared with the structure predicted from a MM3, PM3, and a MMX calculation. Thermal decomposition of 8 produces, 7,16-diphenylcyclopenta[d,e]tribenzo[a,h,j]anthracene (9), a hydrocarbon that is computed to have a significantly twisted polycyclic aromatic skeleton with 19 kcal/mole of strain energy.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF02286444
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  • 23
    Electronic Resource
    Electronic Resource
    Molecular Structure of 5-Methylchrysene-7,8-dihydro-7,8-trans-(e, e)-diol (1995)
    Springer
    Structural chemistry 6 (1995), S. 57-63 
    Details
    ISSN: 1572-9001
    Keywords: Hydrogen bonding ; carcinogen ; polycyclic aromatic hydrocarbon derivative ; dihydrodiol ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal structure of the weak carcinogen 5-methylchrysene-7,8-dihydro-7,8-trans-(e,e)-diol is reported. This molecule contains a distorted bay region as a result of the presence of the 5-methyl group as found in 5-methylchrysene and 5,6- and 5, 12-dimethylchrysene. One torsion angle in this bay region is 20
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF02263528
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  • 24
    Electronic Resource
    Electronic Resource
    Synthesis and structure of 13- and 26-membered crown ethers, derivatives of resorcinol (1995)
    Springer
    Russian chemical bulletin 44 (1995), S. 2353-2360 
    Details
    ISSN: 1573-9171
    Keywords: resorcinol-based crown ethers ; crystal structure ; intramolecular nonbonded C-H...O contacts
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract 13- and 26-Membered crown ethers have been synthesized based on resorcinol and 1,8-dichloro-3,6-dioxaoctane. The products with substituents in the benzene ring have been prepared by alkylation of 13-membered crown ether. Complexing properties of the macrocycles have been studied with the use of ion-selective membrane electrodes. The structures of 13- and 26-membered crown ethers have been established by X-ray structural analysis.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00713607
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  • 25
    Electronic Resource
    Electronic Resource
    Oxidation of 1-hydrazino-3,3-dimethyl-3,4-dihydroisoquinoline. X-ray, spectroscopic, and quantum-chemical study of the structure of 3,3-dimethyl-3,4-dihydroisocarbostyryl azine (1995)
    Springer
    Russian chemical bulletin 44 (1995), S. 2364-2370 
    Details
    ISSN: 1573-9171
    Keywords: dihydroisoquinoline derivatives ; crystal structure ; electronic, IR, and1H NMR spectra ; quantum-chemical calculation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract 3,3-Dimethyl-3,4-dihydroisocarbostyryl azine (2) has been synthesized by oxidation of l-hydrazino-3,3-dimethyl-3,4-dihydroisoquinoline (1). The crystal and molecular structures of compound 2 were determined. It has been established that in the solid state, compound2 exists as an azine tautomer. The IR, electronic, and NMR spectral data indicate that in solution the tautomeric form of2 does not change. A possible mechanism of the oxidation of1 to2 is suggested.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00713609
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  • 26
    Electronic Resource
    Electronic Resource
    Crystal Structure of 2-Debenzoyl, 2-Acetoxy Paclitaxel (Taxol®): Conformation of the Paclitaxel Side-Chain (1995)
    Springer
    Pharmaceutical research 12 (1995), S. 337-341 
    Details
    ISSN: 1573-904X
    Keywords: 2-debenzoyl, 2-acetoxy paclitaxel ; docetaxel ; paclitaxel side-chain ; crystal structure ; solid state conformation ; intramolecular hydrogen bonding ; intermolecular hydrogen bonding
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Crystals of the C2-acetate analog of paclitaxel, grown from a mixture of isopropyl alcohol and methanol, belong to the space group P2l with a = 9.058(3), b = 18.306(5), c = 15.043(1) Å, β = 97.09(1)°, Z = 2, V = 2475.1(9)Å3, D calc = 1.269 gcm−3 and µ = 0.75 cm−1. The structure was determined by direct methods and refined to R(F) = 0.054 and wR(F) = 0.057 for 605 variables and 3496 observed reflections. The paclitaxel side chain possesses a conformation similar to that observed in the crystal structure of docetaxel (Taxotere®). A three dimensional network of hydrogen bonds is formed through solvent molecules and stabilizes the crystal lattice.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1016236014766
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  • 27
    Electronic Resource
    Electronic Resource
    Structure ofp-tetrakis-(4-nitrophenylazo)calix[4]-arene-4-picoline (1∶4) complex (1995)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 22 (1995), S. 33-40 
    Details
    ISSN: 1573-1111
    Keywords: Calixarene-dye ; crystal structure ; inclusion compound
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The structure of thep-tetrakis-(4-nitrophenylazo)calix[4]arene-4-picoline (1∶4) complex has been determined by X-ray crystallography. Crystals are monoclinic, space groupC2/c,a=24.9097) Å,b=8.425(6) Å,c=33.81(1) Å, β=101.13(2)°,D c =1.330 g/cm3,Z=4, finalR value =0.067. The cone conformation adopted by this azocalixarene is disturbed by the positions of the picoline molecules. Two of them are inside the macorocycle cavity and the two others are outside.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00706496
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  • 28
    Electronic Resource
    Electronic Resource
    New synthesis and complexing properties ofp-tert-butyldihomooxacalix[4]arene. Structure of its 1∶2 complex with tetrahydrofuran (1995)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 22 (1995), S. 119-130 
    Details
    ISSN: 1573-1111
    Keywords: Calixarene ; complexation ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A new method is described for the synthesis of isolatedp-tert-butyldihomooxacalix[4]arene (CALO) with a 24% yield. The ability of CALO to form complexes in the solid state with small neutral molecules has been studied; the potential guests were common solvents bearing various chemical functions. The powder obtained after evaporation of the solvent has been characterized by the X-ray powder diffraction technique. Analysis of the patterns shows the non-complexation of linear alkanes and alcohols, but formation of complexes when the guest is cyclic or when it bears an amine or a ketone function. As illustration of the possible arrangement of molecules in complexes, the structure of the 1:2 complex with tetrahydrofuran (THF) is presented: the crystals are monoclinic, space groupP21/c,a=9.459(2) Å,b=17.286(2) Å,c=30.469(6) Å, β=92.52(2)o,V=4977(2) Å3,Z=4,D c=1.099 Mg m−3, λ=1.54178 Å, μ=5.6 cm−1,R=0.086 for 3590 reflections withF〉4σ (F); one of the THF molecules is inside the cavity of the macrocycle, while the other, in the interhost space, exhibits disorder. In the CALO molecule, three out of the fourtert-butyl groups are disordered which may induce the disorder of the THF molecule.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00707687
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  • 29
    Electronic Resource
    Electronic Resource
    Inclusion compounds of (±) gossypol. Structure of the gossypol-n-valeric acid (1/2) coordinato-clathrate (1995)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 22 (1995), S. 187-201 
    Details
    ISSN: 1573-1111
    Keywords: Inclusion compounds ; gossypol ; crystal structure ; hydrogen bonds
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal structure of the inclusion compound of gossypol withn-valeric acid as a guest molecule has been determined by X-ray structure analysis. The crystals of C30H30O8·(C5H10O2)2, are triclinic, space group $$P\bar 1$$ ,a=6.912(2),b=14.506(3),c=19.387(4) Å, α=78.85(2)°, β=83.92(3)°, γ=86.78(3)°V=1895(1) Å3,Z=2,D x=1.267 g cm−3, μ (CuK α)=0.768 mm−1,T=292 K. The structure has been solved by direct methods on intensity data collected for a twinned crystal and refined to the finalR value of 0.062 for 1606 observed reflections and 470 refined parameters. Gossypol-n-valeric acid (1/2) coordinato-clathrate is not isostructural with any of the previously investigated gossypol inclusion compounds but shows some structural similarities to gossypol-acetic acid (1/1). The host and one of the carboxylic acid molecules are connected via hydrogen bonds into molecular assemblies of a column type which are further bonded to centrosymmetric dimers of the secondn-valeric acid molecule. In effect, host and guest molecules are assembled into layer-type H-bonded aggregates. Structural features common to gossypol-n-valeric acid (1/2) and other earlier reported gossypol inclusion compounds are discussed.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00707082
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  • 30
    Electronic Resource
    Electronic Resource
    Lattice dynamics of (Ba/K)BiO3 (1995)
    Springer
    Journal of superconductivity 8 (1995), S. 595-598 
    Details
    ISSN: 1572-9605
    Keywords: (Ba/K)BiO3 ; lattice dynamics ; electron phonon coupling ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Electrical Engineering, Measurement and Control Technology , Physics
    Notes: Abstract The Lattice dynamics of Ba.6K.4BiO3 was investigated by inelastic neutron scattering on a superconducting single crystal (T c =26 K (midpoint)). At low frequencies the dispersion curves are very similar to those observed in BaPb.75Bi.25O3. Differences were found in the bond bending vibrations of the BiO6 octahedra which indicate that the binding in the K-doped compound is more ionic. Rather anomalous features were observed in the high frequency Bi-O bond stretching vibrations which resemble those observed in the high T c cuprates La1.85Sr.15CuO4 and YBa2Cu3O7. The observed frequency shifts are interpreted as the consequence from a strong electron phonon coupling. The data are compared to the results obtained on non superconducting Ba.98K.02BiO3.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00727434
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  • 31
    Electronic Resource
    Electronic Resource
    Binding geometry of α-helices that recognize DNA (1995)
    New York, NY : Wiley-Blackwell
    Proteins: Structure, Function, and Genetics 23 (1995), S. 525-535 
    Details
    ISSN: 0887-3585
    Keywords: DNA-protein interaction ; crystal structure ; transcription factor ; gene regulation ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Medicine
    Notes: Many transcription factors have an α-helix that binds to DNA bases in a specific fashion. The DNA-binding geometry of these recognition helices varies substantially. We define a set of parameters to describe the binding geometry of recognition helices and analyze specific stereochemical elements that determine particular geometries. Because the convex surface of the helix must fit into the concave surface of the DNA major groove, the number of degrees of freedom of the recognition helix is reduced from a possible six to a single angle, which we call α. The chemically interacting DNA bases and amino acid residues must lie along a common line and have the same spacing along it. This pairing of base positions with residue positions seems to restrict the binding geometry further to a set of discrete values for α. © 1995 Wiley-Liss, Inc.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/prot.340230407
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  • 32
    Electronic Resource
    Electronic Resource
    Effect of Humidity-Dependent Changes in Crystal Structure on the Solid-State Fluorescence Properties of a New HMG-CoA Reductase Inhibitor (1995)
    Springer
    Pharmaceutical research 12 (1995), S. 556-559 
    Details
    ISSN: 1573-904X
    Keywords: HMG-CoA reductase inhibitor ; SQ-33600 ; crystal structure ; hydrates ; solid-state fluorescence
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract It has been shown previously that the disodium salt of a new HMG-CoA reductase inhibitor (SQ-33600) is capable of existing as a number of hydrate species [1]. Three crystalline solid hydrates and one liquid crystalline phase have been identified, each having a definite stability over a defined range of humidity. These forms have been found to exhibit varying fluorescence properties in their respective solid states, with differences in bandshapes and intensities being noted for each. These spectral variations have been correlated with the known pseudopolymorphism of the compound.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1016206130213
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  • 33
    Electronic Resource
    Electronic Resource
    The 7.25-hydrate oftert-butylamine. A semi-clathrate and complex variant of the cubic 12 Å structure type (1995)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 22 (1995), S. 145-154 
    Details
    ISSN: 1573-1111
    Keywords: tert-Butylamine 7.25 H2O ; amine hydrate ; semi-clathrate ; clathrate hydrate ; hydrate ; hydrogen bonding ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Of the various hydrates oftert-butylamine, the title compound has been identified as the second-highest, melting incongruently at −19°C. Its crystal structure (orthorhombic, space groupPca21,Z=32 formula units per unit cell,a=24.80,b=16.440,c=25.29 Å) and the exact composition have been determined from X-ray diffraction at −150°C. The hydrate is a rather complex semi-clathrate, with the amine molecules not merely encaged, but also hydrogen-bonded, in a three-dimensional water host structure, which in turn is not fully four-connected. Nevertheless, it bears a clear relationship to the basic and genuine clathrate-hydrate cubic 12 Å type.
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    URL: http://dx.doi.org/10.1007/BF00707689
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  • 34
    Electronic Resource
    Electronic Resource
    Crystal structure of supramolecular complexes formed by 18-crown-6 andcis-anti-cis-dicyclohexano-18-crown-6 (host) with 3,4-diaminofurazane (guest) (1995)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 23 (1995), S. 181-193 
    Details
    ISSN: 1573-1111
    Keywords: 18-crown-6 ; diaminofurazane ; crystal structure ; host-guest complexes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract An X-ray—diffraction study is reported for two molecular complexes containing 3,4-diamino-1,2,5-oxadiazole as guest (G) with 18-crown-6 (18-C-6) andcis-anti-cis-dicyclohexano-18-crown-6 (DCH-6B) as host. Both complexes are of the polymeric-chain structure with the guest molecule bridging two crown neighbours. ComplexI: [18-C-6*G*H2O], 1∶1∶1, monoclinic,P21/n,a=8.171(1),b=15.042(2),c=16.209(6) Å, β=101.15(2)°, finalR-factor 0.068. ComplexII: [DCH-6B*G], 1∶1, monoclinicC2/c,a=21.212(4),b=9.380(2),c=13.049(3) Å, β=108.61(3)°, finalR 0.047.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00709576
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  • 35
    Electronic Resource
    Electronic Resource
    TheO, O′-dibenzoyl derivative of (R, R)-tartaric acid as a host compound for simple organic ethers (1995)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 22 (1995), S. 211-219 
    Details
    ISSN: 1573-1111
    Keywords: (R, R)-Tartaric acid derivatives ; host-guest compounds ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract TheO, O′-dibenzoyl derivative of (R, R)-tartaric acid shows a good inclusion ability for diethyl and di-n-propol ethers. The two crystalline inclusion compounds have 1:1 stoichiometry and reveal isomorphous structures. Hydrogen bonded host molecules form chains running along thez axis of the unit cell and guest molecules join to these chains by short O−H...O hydrogen bonds. Hydrogen bonding in the crystals is characterized by a C(7)D first-order network. The ether molecules are in a fully extended conformation. They are accommodated in channel-like voids running along thex axis. Atomic displacement parameters are significantly larger for diethyl ether than for the di-n-propyl ether molecule reflecting less dense packing for this inclusion compound.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00707084
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  • 36
    Electronic Resource
    Electronic Resource
    Crystal and molecular structures of binuclear caesium complexes with 1,3-calix[4]-bis-crown-6 and 1,3-calix[4]-bis-benzo-crown-6 (1995)
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 23 (1995), S. 305-312 
    Details
    ISSN: 1573-1111
    Keywords: Bridged calix[4]arene ; caesium complex ; ditopic receptor ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal structures of two binuclear complexes between caesium and 1,3-calix[4]-bis-crowns have been determined. Cs2 Bis-benzoC6(NO3)2. 3CHCl3 (1) in whichBis-benzoC6 is 1,3-calix[4]-bis-benzo-crown-6, crystallizes in the orthorhombic system: space groupPca2 1 a=19.513(10),b=15.382(5),c=23.708(9) Å,V=7116(5) Å3,Z=4. Refinement led to a final conventionalR value of 0.065 for 2321 reflections. The structure of (1) is analogous to those already reported withBis-C6, (in whichBis-C6 is, 1,3-calix[4]-bis-crown-6) and NO 3 − as a counter-ion. Cs2 Bis-C6(NCS)2 (2) crystallizes in the monoclinic system: space, groupC2 a=36.57(2),b=11.47(1),c=13.65(1) Å, β=109.03(5)°.,V=5415(6) Å3,Z=4. Refinement led to a final conventionalR value of 0.063 for 2227 reflections. Compound (2) is made of dimers bridged by a disordered NCS− ion. The crown ether chain conformations are discussed.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00707934
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  • 37
    Electronic Resource
    Electronic Resource
    Absolute configurations and conformations of the opioid agonist and antagonist enantiomers of picenadol (1995)
    New York, NY [u.a.] : Wiley-Blackwell
    Chirality 7 (1995), S. 518-525 
    Details
    ISSN: 0899-0042
    Keywords: crystal structure ; molecular mechanics ; MM2-87 ; opioid ligand model ; Chemistry ; Organic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The absolute configurations of the enantiomers of the opiod picenadol [cis-1,3-dimethyl-4-propyl-4-propyl-4-(3-hydroxyphenyl)piperidine; cis-3-methyl, 4-propyl] have been determined by an X-ray crystallographic study of the chloride salt of the (+)-enantiomer. The agonist (+)-enantiomer and the antagonist (-)-enantiomer were found to have the 3R, 4R and 3S, 4S absolute configurations, respectively. The conformational properties of the enantiomers were also examined with MM2-87 calculations. There was good agreement between the computed global minimum and the crystallographic structure with the phenyl ring approximately bisecting the piperidine ring by both methods. This orientation of the phenyl ring differs from that of related opioids such as the phenylmorphans, prodines, meperidine, and ketobemidone in which the phenyl ring tends to eclipse one edge of the piperidine ring. Because the phenyl ring bisects the piperidine ring in picenadol, there is little difference in the three-dimensional orientations of the phenyl rings of the two enantiomers when one superimposes the piperidine rings. The agonist (+)-enantiomer is ambiguous with respect to an opioid ligand model, which suggests that agonist activity requires a specific range of dihedral angles for the phenyl ring. While the global minimum of the agonist is not consistent with the model, a second conformer that is only 1.2 kcal/mol above the global minimum is consistent. An alternative explanation is that agonist or antagonist activity is solely due to the presence of the 3-methyl group on the different edges of the piperidine ring. MM2-87 calculations were also performed on the opioid agonist des-3-methyl analog of picenadol and the closely related trans-1,3,4-trimethyl-4-(3-hydroxyphenyl)piperidines (trans-3-methyl, 4-methyl) in which both enantiomers are opioid antagonists. The conformational properties of these compounds are consistent with the ligand model. © 1995 Wiley-Liss, Inc.
    Additional Material: 9 Ill.
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    URL: http://dx.doi.org/10.1002/chir.530070705
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  • 38
    Electronic Resource
    Electronic Resource
    In3Ti2Br9: Jahn-Teller Unstable Indium(I) and Antiferromagnetically Coupled Titanium(III) Atoms (1995)
    Weinheim : Wiley-Blackwell
    Chemistry - A European Journal 1 (1995), S. 118-123 
    Details
    ISSN: 0947-6539
    Keywords: antiferromagnetic exchange ; crystal structure ; indium compounds ; Jahn-Teller distortion ; titanium compounds ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Dark green crystals of In3Ti2Br9 have been synthesized from elemental Ti and molten InBr3 at 450°C. The X-ray diffractional characterization by means of single-crystal and powder Rietveld refinement reveals a hexagonal crystal structure (a = 738.2(2), c = 1813.9(3) pm; P63/mmc, Z = 2) of Cs3Cr2Cl9 type, containing Ti2Br3-9 dimers and univalent indium cations. Self-consistent, semiempirical band structure calculations show the structural distortions of the two monovalent indium cations to arise from a second-order Jahn-Teller instability. The new compound's magnetic susceptibility and microscopic antiferromagnetic exchange are analyzed by using a Bleaney-Bowers ansatz.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/chem.19950010205
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  • 39
    Electronic Resource
    Electronic Resource
    Phase Relationships in the N2O3/N2O4 System and Crystal Structures of N2O3 (1995)
    Weinheim : Wiley-Blackwell
    Chemistry - A European Journal 1 (1995), S. 389-393 
    Details
    ISSN: 0947-6539
    Keywords: crystal structure ; differential thermal analysis ; nitrogen oxides ; phase transitions ; twinning ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Mixtures of N2O3 and N2O4 have been prepared from measured volumes of NO and O2. Phase relationships in the system N2O3/N2O4, which depend on the composition of the samples and on the temperature, were studied by the Guinier technique and differential thermal analysis. Single crystals of phases A and B of N2O3 were grown in situ on a diffractometer and studied at temperatures between -107 and -170°C by X-ray diffraction. The structure analysis of A-N2O3 (tetragonal, space group I41/a, T = -170°C, a = 1625.57 (16), c = 880.49(13) pm, Z = 32, R1 = 0.051 for 1030 unique reflections) is hampered by twinning and additional disorder of one of two crystallographically independent molecules. B-N2O3 is nicely ordered with one molecule in the asymmetric unit (orthorhombic, space group P212121, T = -160°C, a = 506.86(4), b = 647.96(5), c = 863.26(6) pm, Z = 4, R1 = 0.023 for 1352 unique reflections). The most interesting features of the N2O3 molecule are its planarity and the extraordinarily long N—N bond (189.0(1) pm).
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/chem.19950010610
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  • 40
    Electronic Resource
    Electronic Resource
    Reactions of the “Naked” Fluoride Ion: Syntheses and Structures of SeF62- and BrF6- (1995)
    Weinheim : Wiley-Blackwell
    Chemistry - A European Journal 1 (1995), S. 261-265 
    Details
    ISSN: 0947-6539
    Keywords: crystal structure ; fluorides ; hexafluorobromate(V) ; hexafluoroselenate(IV) ; naked fluoride ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 1,1,3,3,5,5-Hexamethylpiperidinium fluoride (pip+F-) and 1,2-dimethylpropyltrimethylammonium fluoride have been prepared. They dissolve in fluorohydrocarbons (CH2F2, CF3-CHF-CF3, CHF3) even at very low temperatures. The nature of these solutions is indicated by the crystal structure of the adduct pip+F-·4CH2F2, which shows (C)H…F bridging. The high fluoride activity is exemplified by the previously unknown reaction between SeF5- and F- to yield SeF62-. The salt pip+BrF6- is obtained by a metathesis reaction of Cs+BrF6- with pip+F-. The distortion of the SeF62- structure from octahedral symmetry is intermediate between IF6- (strongly distorted) and BrF6- (octahedral). The electron-pair repulsion model is checked against these results.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/chem.19950010410
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  • 41
    Electronic Resource
    Electronic Resource
    Metal-Mediated Synthesis of Multidomain Ligands - A New Strategy for Metallosupramolecular Chemistry (1995)
    Weinheim : Wiley-Blackwell
    Chemistry - A European Journal 1 (1995), S. 360-367 
    Details
    ISSN: 0947-6539
    Keywords: crystal structure ; polynuclear ; complexes ; ruthenium compounds ; supramolecular chemistry ; terpyridines ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The bridging ligand bis{4′-(2,2′:6′,2″-terpyridinyl)}ether (1) can be prepared in 69% yield from the reaction of 4′-chloro-2,2′:6′,2″-terpyridine (3) with 2,2′:6′,2″-terpyridin-4′(1′H)-one (2) in Me2NCHO in the presence of KOH. More conveniently, complexes of 1 can be prepared in situ by the reaction of 2 with a ruthenium(II) complex of 3 in the presence of K2CO3. This methodology has been developed for the synthesis of a range of mono-, di-, tri- and hexanuclear complexes with a variety of Xtpy (Xtpy = 4′-substituted 2,2′:6′,2″-terpyridine) terminator ligands. The molecular structure of 1 (a = 9.623(2), b = 11.241(1), c = 11.828(1) Å; space group P1; α = 93.064(9), β = 107.072(14), γ = 99.088(14)°; Z = 2, R = 0.0450, Rw = 0.0577) has been determined. The generality of the methodology may ultimately be limited by the sensitivity of the ether-linkage in 1 to attack by nucleophiles.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/chem.19950010606
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  • 42
    Electronic Resource
    Electronic Resource
    Molecular structure and conformational analysis of chirai (−)-3-(4-bromobenzylidene)-1-isopropyl-2-methoxy-4-methylcyclohexene (1995)
    Springer
    Russian chemical bulletin 44 (1995), S. 2331-2336 
    Details
    ISSN: 1573-9171
    Keywords: molecular structure ; conformational analysis ; crystal structure ; X-ray structural analysis ; molecular mechanics ; (−)-3-(4-bromobenzylidene)-l-isopropyl-2-methoxy-4-methylcyclohexene
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract (−)-3-(4-Bromobenzylidene)-1-isopropyl-2-methoxy-4-methylcyclohexene, capable of inducing spiral supramolecular ordering when introduced to nematic and some smectic mesophases, has been studied by an X-ray structural analysis. The crystals are orthorhombic; at 20 °Ca = 6.055(1),b = 13.282(3),c=20.734(4) Å,V=1668(1) Å3,d calc = 1.380 g cm−3, space groupP2 12121 Z=4. The cyclohexene ring has a conformation intermediate between a sofa and a half-chair. The methyl and methoxyl groups are in asyn orientation with respect to the mean plane of the cycle. The angle between the plane of the aryl substituent and the exocyclic double bond is 33°. The observed distortions of bond angles at unsaturated carbon atoms are typical of derivatives of benzylidenecyclohexene. Molecular mechanics calculations demonstrated that the conformation observed in the crystalline state is not the most favorable, and this conformation is stabilized through intermolecular interactions upon stacking in crystals. It was shown that the relative orientation of the methyl and methoxyl groups as well as the orientation of the aryl substituent substantially affect the conformation of the cyclohexene ring.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00713603
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  • 43
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    Electronic Resource
    Chiral β-hydroxycarbonyl compounds based on (−)-menthone: structure and behavior in liquid crystalline systems (1995)
    Springer
    Russian chemical bulletin 44 (1995), S. 1200-1209 
    Details
    ISSN: 1573-9171
    Keywords: stereoisomeric 2-(1′-biphenyl-4-yl-1′-hydroxy)methyl-p-menthan-3-ones ; molecular structure ; X-ray structural analysis ; crystal structure ; conformational analysis ; molecular mechanics ; hydrogen bond ; induced cholesteric liquid crystals ; twisting power
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract It has been established by X-ray structural analysis that 2-(1′-biphenyl-4-yl-1′-hydroxy)methyl-p-menthan-3-one, one of the products of the reaction of (−)-menthone triisopropyloxytitanium enolate with 4-phenylbenzaldehyde, has a 1R,2S,4S,1′S configuration. In crystals, this β-hydroxyketone adopts a chair conformation with equatorial methyl and isopropyl groups and an axial 2-(1′-biphenyl-4-yl-1′-hydroxy)methyl substituent. Unlike the stereoisomeric compound with the 1R,2S,4S,1′S configuration, the exocyclic fragment of which has an intramolecular 〉C=O...H-O- hydrogen bond in crystals and solutions, in the crystals of the 1R,2S,4S,1′S ketol under study, molecules are linked by a network of cooperative -O-H...O-H...O-H... hydrogen bonds. Based on the results of molecular mechanics calculations and experimental data of1H NMR and IR spectroscopy, conformations of molecules of this compound, which are in equilibrium in solution, have been characterized. Based on data on spatial structures of stereoisomeric β-hydroxyketones and the character of H-bonds formed by these compounds, the characteristic features of the effect of these chiral alloying additives on the supramolecular structure and macroscopic properties of liquid crystalline systems have been interpreted.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00700889
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  • 44
    Electronic Resource
    Electronic Resource
    Elastic modulus of the crystalline regions of cellulose triesters (1995)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part B: Polymer Physics 33 (1995), S. 611-618 
    Details
    ISSN: 0887-6266
    Keywords: elastic modulus ; crystalline regions ; cellulose triester ; crystal structure ; mechanical property ; hydrogen bond ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Elastic moduli of the crystalline regions of cellulose triesters in the direction both parallel El and perpendicular Et to the chain axis are measured by x-ray diffraction. El values for cellulose triesters are as follows: cellulose triacetate (CTA), 33.2 GPa; cellulose tripropionate (CTP), 21.6 GPa; cellulose tributyrate (CTB), 17.6 GPa; cellulose trivalerate (CTV), 17.9 Gpa. These are very small compared with that of cellulose I (134 GPa) and resemble each other despite the fact that the skeletal structure of CTP (32 helix) is much different from those of other cellulose triesters (2-fold helix). The small El values for cellulose triesters can be explained by both the large cross-sectional area of one molecule in the crystal lattice and the lack in intramolecular hydrogen bonds. Et values for cellulose triesters are as follows: CTA (310), 2.8 GPa; CTP (110), 1.4 GPa; (020), 2.1 GPa; (120), 2.2 GPa; CTB (110), 1.1 GPa. These are one of the smallest Et values already reported, and decrease with increasing the length of the side chain. Intermolecular interaction is considered to decrease with the length of acyl groups. The large Et value in the b direction of CTP reflects the dense packing of the chains in the crystal lattice. © 1995 John Wiley & Sons, Inc.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/polb.1995.090330411
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  • 45
    Electronic Resource
    Electronic Resource
    Elastic modulus of the crystalline regions of cellulose polymorphs (1995)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part B: Polymer Physics 33 (1995), S. 1647-1651 
    Details
    ISSN: 0887-6266
    Keywords: elastic modulus ; crystalline regions ; cellulose ; crystal structure ; mechanical property ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The elastic modulus El of the crystalline regions of cellulose polymorphs in the direction parallel to the chain axis was measured by x-ray diffraction. The El values of cellulose I, II, IIII, IIIII, and IVI were 138, 88, 87, 58, 75 GPa, respectively. This indicates that the skeletons of these polymorphs are completely different from each other in the mechanical point of view. The crystal transition induces a skeletal contraction accompanied by a change in intramolecular hydrogen bonds, which is considered to result in a drastic change in the El value of the cellulose polymorphs. © 1995 John Wiley & Sons, Inc.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/polb.1995.090331110
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  • 46
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    Electronic Resource
    Crystal structure of the poly(ethylene oxide)-p-nitrophenol molecular complexPresented at ‘MacroAkron '94, 35th IUPAC Symposium on Macromolecules’, Akron, Ohio, 11-15 July 1994. (1995)
    New York, NY [u.a.] : Wiley-Blackwell
    Polymer International 36 (1995), S. 117-125 
    Details
    ISSN: 0959-8103
    Keywords: poly(ethylene oxide) ; p-nitrophenol ; molecular complexes ; crystal structure ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: A crystalline complex of poly(ethylene oxide) (PEO) and p-nitrophenol (PNP) was studied by differential scanning calorimetry, X-ray diffraction, and FTIR spectroscopy, The phase diagram of this system is characterized by a peritectic reaction, and reveals the formation of a new crystal form different from those of PEO, and PNP. The triclinic unit cell of the complex was determined from the X-ray diffraction patterns of differently oriented samples obtained by mechanical deformations or spherulitic crystallizations. Finally, the molecular packing and the conformation adopted by the PEO chains were determined by FTIR spectroscopy. Polarization measurements have shown that the aromatic rings are very nearly normal to the c parameter (chain axis) and that the 1-4 axes of PNP molecules are parallel to the a* reciprocal parameter (spherulitic growth direction). Finally, a new (t2 gt2 gt3) conformation is proposed for the PEO chains on the basis of a normal mode analysis and the calculation of the intramolecular energy.
    Additional Material: 11 Ill.
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    URL: http://dx.doi.org/10.1002/pi.1995.210360202
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  • 47
    Electronic Resource
    Electronic Resource
    Ein neues Oxophosphat (IV/III)-Anion - Darstellung und Kristallstruktur von Na6P4O10 · 2 H2O (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 7-13 
    Details
    ISSN: 0044-2313
    Keywords: Sodium phosphate ; oxophosphate (IV/III) ; crystal structure ; 31P-NMR ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A New Oxophosphate (IV/III) Anion - Preparation and Crystal Structure of Na6P4O10 · 2 H2OA new oxophosphate anion, P4O106-, was obtained by cleavage and simultaneous oxidation of the cyclo-hexaphosphate(III) anion in a solution of aqueous ammonia and ethanol. With sodium it forms a salt with the composition Na6P4O10 · 2 H2O. The crystal structure has been determined by single crystal X-ray diffraction (3 745 diffractometer data), the cell constants were obtained from X-ray powder data, space group P1; a = 6.004(1), b = 6.173(2), c = 11.496(2) Å, α = 99.26(2)°, β = 95.92(2)°, γ = 117.63(2)°, Z = 1, R = 0.044. The backbone of the anion is formed by phosphorus atoms directly bonded to each other. The coordination of each phosphorus atom is completed to four by oxygene. The resulting oxidation numbers are +III for the inner phosphorus atoms and +IV for the terminal phosphorus atoms. The site symmetry of the anion is approximately C2h. Based on a 31P-NMR spectra of a solution the coupling constants of the AA ‘BB’ system were determined.
    Notes: Ein neues Oxophosphation, P4O106-, wurde durch oxidative Ringspaltung an cyclo-Hexaphosphaten(III) in ammoniakalisch/ethanolischer Lösung erhalten und die Struktur von Na6P4O10 · 2 H2O [Vierkreisdiffraktometerdaten (3 745 unabhängige Strukturfaktoren)] gelöst. Raumgruppe P1; a = 6,004(1); b = 6,173(2); c = 11,496(2) Å; α = 99,26(2)° β = 95,92(2)°; γ = 117,63(2)°; Z = 1; R = 0,044. Das „Rückgrat“ des kettenförmigen Anions sind vier verbundene Phosphoratome, deren Koordination mit Sauerstoff auf vier aufgefüllt wird. Dem entspricht die Oxidationsstufe +III für die inneren bzw. +IV für die terminalen Phosphoratome. Für das komplexe Anion ist die Punktsymmetrie C2h näherungsweise erfüllt. Aus 31P-NMR-Daten in Lösung wurden die vier Kopplungskonstanten des AA ‘BB’-Systems durch Spektrensimulation ermittelt.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956210104
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  • 48
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    Eine ‚Reduktive Austausch-Reaktion‘: Einkristalle von Rb2[MnO4] aus Li[MnO4]Professor Hans-Uwe Schuster in memoriam (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 177-180 
    Details
    ISSN: 0044-2313
    Keywords: Oxomanganate(VI), Rb2[MnO4] ; preparation ; crystal structure ; MAPLE calculation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A ‘Reductive Exchange Reaction’: Single Crystals of Rb2[MnO4] from Li[MnO4]By heating of well ground mixtures of the oxides RbO0.9 and Li[MnO4] (Rb:Mn = 1.5:1; Ag-tubes; 660°C, 56 d) dark-green, orthorhombic single-crystals of Rb2[MnO4] were obtained. The structural determination revealed the isotype to K2[MnO4]; a β-K2SO4-typ. Thus, for the first time by a pure solid-state-chemical way, via a reductive, complete alkali-metal exchange, single crystals of an oxomanganate(VI) of the alkali metals were prepared.The Madelung Part of the Lattice Energy, MAPLE, and the charge distribution were calculated.
    Notes: Durch Tempern inniger Gemenge der Oxide RbO0,9 und Li[MnO4] (Rb:Mn = 1,5:1; Ag-Zylinder; 660°C, 56 d) wurden dunkelgrüne, orthorhombische Einkristalle von Rb2[MnO4] erhalten. Die Einkristallstrukturbestimmung belegt die Isotypie zu K2[MnO4]; es liegt der β-K2SO4-Typ vor. Somit konnten erstmals auf rein festkörperchemischem Weg, über einen reduktiven, vollständigen Alkalimetall-Austausch, Einkristalle eines Oxomanganates(VI) der Alkalimetalle dargestellt werden.Der Madelung-Anteil der Gitterenergie, MAPLE, sowie die Ladungsverteilung wurden berechnet.
    Additional Material: 6 Tab.
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    URL: http://dx.doi.org/10.1002/zaac.19956210202
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    Untersuchungen an Polyhalogeniden. XVII. Darstellung und Kristallstruktur von Urotropiniumtriiodid, UrHI3 (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 225-228 
    Details
    ISSN: 0044-2313
    Keywords: Polyiodide ; triiodide ; urotropinium triiodide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Studies on Polyhalides. 17. Preparation and Crystal Structure of Urotropinium Triiodide, UrHI3Urotropinium triiodide C6H13N4I3 is formed by the reaction of equimolar amounts of urotropinium iodide and iodine in tBuOH as red-brown cube-like crystals melting at 402 K under decomposition. The compound crystallizes monoclinically in the space group P21/c with a = 952.0(3) pm, b = 1 160.2(6) pm, c = 1 149.9(4) pm, β = 92.22(3)° and Z = 4. The till now not described crystal structure (R = 0.027 for 1 860 observed reflexes) contains urotropinium ions UrH+ and slightly distorted triiodide ions I3-(d(I - I) = 292.3(1), 294.1(1) pm, ϕ(I - I - I) = 178.27(2)°) which are linked to ion pairs by a rather short contact (d(I … I) = 389.0(1) pm, ϕ(I - I … I) = 149.12(2)°).
    Notes: Urotropiniumtriiodid C6H13N4I3 fällt bei der Umsetzung äquimolarer Mengen Urotropiniumiodid und Iod aus tBuOH in rotbraunen würfelähnlichen Kristallen an, die bei 402 K unter Zersetzung schmelzen. Die Substanz kristallisiert in der monoklinen Raumgruppe P21/c mit a = 952,0(3) pm, b = 1 160,2(6) pm, c = 1 149,9(4) pm, β = 92,22(3)° und Z = 4. Die bisher nicht beschriebene Kristallstruktur (R = 0,027 für 1 860 beobachtete Reflexe) enthält Urotropiniumionen UrH+ und geringfügig verzerrte Triiodidionen I3-(d(I - I) = 292,3(1), 294,1(1) pm, ϕ(I - I - I) = 178,27(2)°), die über einen kurzen Kontakt Ionenpaare bilden (d(I … I) = 389,0(1) pm, ϕ(I - I … I) = 149,12(2)°).
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956210211
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  • 50
    Electronic Resource
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    The Cobalticinium Cation [CoIII(η5-C5H5)2]+: A metal-organic complex as a novel template for the synthesis of clathrasils (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 311-322 
    Details
    ISSN: 0044-2313
    Keywords: Cobalticinium cation ; template effect ; clathrasils ; crystal structure ; penta-coordinated silicon ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Das Cobaltocenium-Kation [CoIII(η5-C5H5)2]+: Ein metallorganischer Komplex als neuartiges Templat für die Synthese von ClathrasilenDas Cobaltocenium-Kation [CoIII(η5-C5H5)2]+ ≡ Cocp2+ ist der erste metallorganische Komplex, der bei der Synthese von mikroporösen Feststoffen nachweislich als strukturdirigierendes Templat wirkt. Bei der hydrothermalen Behandlung des Synthesesystems SiO2—NH4F—Cocp2PF6—H2O bei 420-470 K kristallisieren drei verschiedene Clathrasil-Gerüststrukturen: Nonasil (NON), Octadecasil (AST) und Dodecasil 1H (DOH). Aus den Infrarot-, optischen und Röntgenabsorptions(XANES, EXAFS)-Spektren folgt, daß das Cobaltocenium-Kation unzersetzt in das kristallisierende Silicat-Gerüst eingebaut wird, was seine Rolle als Templat bestätigt. Thermoanalytische Untersuchungen zeigen, daß im Silicat-Gerüst eingeschlossenes Cocp2+ eine viel höhere thermische Stabilität besitzt als in einfachen Salzen.Vom Cobaltocenium-Nonasil wurde eine Röntgen-Einkristall-Strukturbestimmung bei 220 K durchgeführt: [Cocp2F]4 · 88 SiO2, orthorhombisch, Raumgruppe Pccn (No. 56), a = 22,125(2) Å, b = 13,612(3) Å, c = 14,889(2) Å, Z = 1. Jeder große [58612]-Käfig des Nonasil-Gerüsts ist mit einem Cocp2+-Kation in staggered-Konformation besetzt, das keine Orientierungs- oder Rotations-Fehlordnung aufweist, sondern aufgrund sterischer Hinderung und durch schwache C—H … O(Wirt)-Wechselwirkungen fixiert ist. Die Fluorid-Anionen kompensieren die positive Ladung des Cocp2+ und befinden sich in der Hälfte der kleinen [4158]-Käfige vor den Vierring-Fenstern. Sie koordinieren zu den benachbarten Gerüstatomen Si1 (d(Si1—F): 1,836(6) Å) und bewirken dadurch eine Verzerrung der tetraedrischen Sauerstoff-Umgebung zu einer nahezu idealen, trigonal-bipyramidalen Penta-Koordination von Si1.
    Notes: The cobalticinium cation [CoIII(η5-C5H5)2]+ ≡ Cocp2+ is the first metal-organic complex that acts as a structure-directing template in the hydrothermal synthesis of microporous solids. Three different clathrasil framework structures - nonasil (NON), octadecasil (AST) and dodecasil 1H (DOH) - crystallize during hydrothermal treatment from the synthesis system SiO2—NH4F—Cocp2PF6—H2O at 420-470 K. From infrared, optical and x-ray absorption (XANES, EXAFS) spectroscopic measurements, it is evident that the cobalticinium cation remains unchanged upon incorporation into the crystallizing silica framework proving its role as a template. Thermal analysis demonstrates that Cocp2+ entrapped in silica frameworks possesses a much higher thermal stability than the cation in simple salts.An X-ray single-crystal structure determination of cobalticinium nonasil was performed at 220 K: [Cocp2F]4 · 88 SiO2, orthorhombic, space group Pccn, a = 22.125(2) Å, b = 13.612(3) Å, c = 14.889(2) Å, Z = 1. Each of the large [58612]-cages of the nonasil structure is occupied by a Cocp2+ cation in staggered conformation which does not show any orientational or rotational disorder but is fixed due to steric confinement and weak C—H … O(host) interactions. Fluoride anions that compensate the charge of the Cocp2+ cations reside in half of the small [4158] cages in front of the four-membered rings. They coordinate to the neighbouring framework atom Si1 (d(Si1—F): 1.836(6) Å), causing a distortion of the tetrahedral oxygen environment to a nearly ideal trigonal-bipyramidal penta-coordination of Si1.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956210218
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    Structural Studies on some Iodoantimonate and Iodobismuthate Anions (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 47-56 
    Details
    ISSN: 0044-2313
    Keywords: Iodoantimonate anion ; iodobismuthate anion ; complex compounds ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Strukturuntersuchungen an einigen Iodoantimonat- und Iodobismutat-AnionenDie Reaktion zwischen BiI3 und zwei Äquivalenten dmpu (dmpu = N,N′-Dimethylpropylharnstoff) in THF oder Toluol ergibt dunkelrote Kristalle von [Bi(dmpu)6] · [Bi3I12]. Nach röntgenographischer Charakterisierung besteht die Verbindung aus oktaedrischen [Bi(dmpu)6]3+-Kationen und [Bi3I12]3--Anionen, beide mit der Symmetrie 3. Die analoge Reaktion mit SbI3 ergibt orange Kristalle von [C5NH6]2[H(dmpu)2][Sb2I9], wahrscheinlich ein Hydrolyseprodukt. Die röntgenographische Charakterisierung ergab flächenverknüpfte dioktaedrische [Sb2I9]3--Anionen mit zwei Pyridinium und einem [H(dmpu)2]+-Kation.[CH2=C(C6H4-4-NO2)CH2NMe3]I und ein Äquivalent SbI3 ergibt den orangen, kristallinen Komplex [CH2=C(C6H4-4-NO2)CH2NMe3]3[Sb2I9] mit flächenverknüpften dioktaedrischen [Sb2I9]3--Anionen.[CH2=C(C6H4-4-NO2)CH2NMe3]I und vier Äquivalente BiI3 ergeben [CH2=C(C6H4-4-NO2)CH2NMe3]3[Bi3I12] mit dem zum [Bi(dmpu)6][Bi3I12] analogen Anion.[CH3(CH2)2COS(CH2)2NMe3]I mit vier Äquivalenten SbI3 ergeben orange Kristalle von [CH3(CH2)2COS(CH2)2NMe3]4 · [Sb8I28], die nach Röntgenstrukturuntersuchungen einen neuen Strukturtyp von [E8X28]4--Anionen (E = As, Sb, Bi; X = Halogen) darstellen.
    Notes: The reaction between BiI3 and two equivalents of dmpu (dmpu = N,N′-dimethylpropylene urea) in thf (tetrahydrofuran) or toluene affords dark red crystals of the complex [Bi(dmpu)6][Bi3I12] which was characterised by X-ray crystallography and consists of octahedral [Bi(dmpu)6]3+ cations and [Bi3I12]3- anions both with 3 symmetry. An analogous reaction between SbI3 and dmpu afforded orange crystals of what is probably a hydrolysis product, [C5NH6]2[H(dmpu)2][Sb2I9], which was also characterised by X-ray crystallography and contains a face-shared bioctahedral [Sb2I9]3- anion with two pyridinium cations and a hydrogen bonded [H(dmpu)2]+ cation. [CH2=C(C6H4-4-NO2)CH2NMe3]I and one equivalent of SbI3 afforded the orange crystalline complex [CH2=C(C6H4-4-NO2)CH2NMe3]3[Sb2I9] an X-ray crystallographic study of which revealed a face-shared bioctahedral [Sb2I9]3- anion similar to that present in [C5NH6]2[H(dmpu)2][Sb2I9]. Four equivalents of BiI3 and [CH2=C(C6H4-4-NO2)CH2NMe3]I afforded the complex [CH2=C(C6H4-4-NO2)CH2NMe3]3[Bi3I12], the [Bi3I12]3- anion being essentially identical to that encountered in [Bi(dmpu)6][Bi3I12]. [CH3(CH2)2COS(CH2)2NMe3]I and four equivalents of SbI3 yielded orange crystals of the complex [CH3(CH2)2COS(CH2)2NMe3]4[Sb8I28] which was also characterised by X-ray crystallography and shown to contain a new structural type of [E8X28]4- anion (E = As, Sb, Bi; X = halide).
    Additional Material: 9 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956210110
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    Strukturen aus AlB2- und CeMg2Si2-analogen Einheiten. Die Verbindungen Eu3Pd4As4, Ca4Pd5P5 und Ca5Pd6P6 (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 57-62 
    Details
    ISSN: 0044-2313
    Keywords: ternary palladium pnictides ; europium ; calcium ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Structures with AlB2- and CeMg2Si2-Type Units. The Compounds Eu3Pd4As4, Ca4Pd5P5, and Ca5Pd6P6The new compounds Eu3Pd4As4, Ca4Pd5P5, and Ca5Pd6P6 (space groups and lattice constants see „Inhaltsübersicht“) have been prepared by heating mixtures of the elements. Their structures were determined by means of single-crystal X-ray methods and contain exclusively units, which are characteristic for the AlB2- and CeMg2Si2-type. The non-metal atoms are isolated from each other or connected to pairs; the ratio between these two kinds can be interpreted by ionic splittings of the formulas.
    Notes: Eu3Pd4As4 (Pmmm; a = 4,205(2) Å, b = 4,308(1) Å, c = 12,640(7) Å; Z = 1), Ca4Pd5P5 (Cmcm; a = 4,094(1) Å, b = 31,061(4) Å, c = 8,168(1) Å; Z = 4) und Ca5Pd6P6 (Pmma; a = 8,172(2) Å, b = 4,088(1) Å, c = 19,077(6) Å; Z = 2) wurden durch Erhitzen der jeweiligen Elemente dargestellt. Die mit Röntgen-Einkristallmethoden bestimmten Kristallstrukturen setzen sich ausschließlich aus AlB2- und CeMg2Si2-analogen Einheiten zusammen. Die Nichtmetallatome sind teils voneinander isoliert und teils zu Hanteln miteinander verknüpft; das jeweilige Verhältnis läßt sich mit Hilfe einer ionischen Formelaufspaltung interpretieren.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956210111
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  • 53
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    Darstellung und Kristallstruktur von Cobalt(II)-Hexaoxodiphosphat(P—P)(4-)-dodecahydrat, Co2P2O6 · 12 H2O (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 149-152 
    Details
    ISSN: 0044-2313
    Keywords: Hexaoxodiphosphate(IV) hydrate of cobalt ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of Cobalt(II)-hexaoxodiphosphate(P—P)(4-)-dodecahydrate, Co2P2O6 · 12 H2OCo2P2O6 · 12H2O was obtained by cleavage and simultaneous oxidation of cyclo-hexaphosphate(III) in a solution of ethanol and aqueous ammonia. The crystal structure has been determined (1 898 independent diffractometer data): space group Pbam (No. 55), a = 6.710(2), b = 12.196(2), c = 10.073(3) Å, V = 825.3(1) Å3, Z = 2, R = 0.060. The P2O64- anions show site symmetry C2h and are connected to form chains via cobalt. Two cobalt ions together with two sets of four water molecules and two oxygen atoms of P2O64- form pairs of edge connected octahedra. The common edges are formed by the oxygen atoms of the P2O6 groups.
    Notes: Co2P2O6 · 12 H2O entsteht bei oxidativer Ringspaltung an cyclo-Hexaphosphaten(III) in ammoniakalisch ethanolischer Lösung. Die Kristallstruktur wurde auf der Basis von Vierkreisdiffraktometerdaten (4018 gemessene Reflexe) gelöst (1 898 unabhängige Reflexe): Raumgruppe Pbam (No. 55); a = 6,710(2), b = 12,196(2), c = 10,073(3) Å, V = 825,3(1) Å3; Z = 2; R = 0,060. Die Anionen P2O64- mit der Lagesymmetrie C2h sind über Cobalt zu Ketten verknüpft. Je zwei Cobaltionen bilden mit je vier Wassermolekülen und zwei terminalen Sauerstoffatomen des P2O64- verzerrte, kantenverknüpfte Oktaederpaare aus. Deren gemeinsame Kanten werden durch Sauerstoffatome der P2O6-Gruppen gebildet.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956210127
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  • 54
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    Ein neuer Strukturtyp bei Kupfer-Lanthanoid-Oxowolframaten: CuDy5(WO4)8Professor Hans-Uwe Schuster in memoriam (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 181-185 
    Details
    ISSN: 0044-2313
    Keywords: Copper lanthanoide oxotungstate ; CuDy5(WO4)8 ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A New Structure Type of Copper Lanthanoide Oxotungstates: CuDy5(WO4)8Single crystals of the hitherto unknown compound CuDy5(WO4)8 were prepared in closed copper tubes and investigated by X-ray technique. It shows monoclinic symmetry, space group C2h6 - C2/c, a = 19.118, b = 5.612, c = 11.518 Å, β = 111.32°, Z = 2. The crystal structure is characterized by [W4O18] groups which are connected to layers. Dy3+ shows one sided capped trigonal prisms and Cu+/Dy3+ with statistical distribution an octahedral oxygen surrounding.
    Notes: Die bisher unbekannte Verbindung CuDy5(WO4)8 wurde einkristallin in geschlossenen Kupferrohren dargestellt und röntgenographisch untersucht. Sie kristallisiert mit monokliner Symmetrie, Raumgruppe C2h6 - C2/c mit a = 19,118; b = 5,612; c = 11,518 Å; β = 111,32°; Z = 2. Die Kristallstruktur zeichnet sich durch [W4O18]-Baugruppen aus, die zu Schichten verknüpft sind. Dy3+ zeigt einfach überkappt trigonal prismatische, die in statistischer Verteilung vorliegenden Cu+/Dy3+-Ionen eine oktaedrische Sauerstoffumgebung.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956210203
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  • 55
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    Ba8Cu16P30 - eine neue ternäre Variante des Clathrat I-StrukturtypsProfessor Hans-Uwe Schuster in memoriam (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 191-196 
    Details
    ISSN: 0044-2313
    Keywords: Ternary phosphide ; copper ; barium ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ba8Cu16P30 - a New Ternary Variant of the Clathrate I Type StructureBa8Cu16P30 (a = 14.117(1) Å, b = 10.093(1) Å, c = 28.022(2) Å) was prepared by heating a mixture of the elements (800°C; excess of Ba and P; removal of the by-products by acetic acid/H2O2). The compound crystallizes orthorhombically (Pbcn; Z = 4) in a new superstructure of the cubic clathrate I type structure with an ordered distribution of the atoms. The structure is characterized by a three-dimensional framework of CuP4 tetrahedra with cavities in the form of pentagonal dodecahedra and tetrakaidecahedra, which are occupied by the Ba atoms. The compound shows semiconduction, therefore the composition should be Ba8Cu15.5P30.5.
    Notes: Ba8Cu16P30 (a = 14,117(1) Å, b = 10,093(1) Å, c = 28,022(2) Å) wurde durch Erhitzen eines entsprechenden Elementgemenges auf ca. 800°C erhalten (Ba- und P-Überschuß; Entfernen der Nebenprodukte mit Eisessig/H2O2). Die Verbindung kristallisiert orthorhombisch (Pbcn; Z = 4) in einer neuen Überstruktur des kubischen Clathrat I-Strukturtyps mit einer geordneten Atomverteilung und wird durch ein dreidimensionales Gerüst aus CuP4-Tetraedern geprägt. Diese sind über gemeinsame Ecken so miteinander verknüpft, daß Käfige in Form von Pentagondodekaedern und Tetrakaidekaedern entstehen, die für diesen Strukturtyp charakteristisch und hier mit Ba-Atomen belegt sind. Die Verbindung ist ein Halbleiter, deren Zusammensetzung aufgrund der Ladungsbilanz Ba8Cu15,5P30,5 sein sollte.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956210205
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  • 56
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    Ga8Ir4B - ein Gallium-Iridiumborid mit isolierten, annähernd quadratisch planaren Ir4B-Gruppen in einer vom CaF2-Typ abgeleiteten StrukturProfessor Hans-Uwe Schuster in memoriam (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 197-200 
    Details
    ISSN: 0044-2313
    Keywords: Gallium iridium boride ; crystal structure ; preparation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ga8Ir4B - a Gallium Iridium Boride with isolated, nearly square planar Ir4B Groups in a Structure derived from the CaF2 TypeThe new compound Ga8Ir4B (tetragonal, I41/acd, a = 853.69(2) pm, c = 2 105.69(6) pm, Z = 8, 614 reflections, 31 parameters, R = 0.034) was prepared by reaction of the elements at 1 100°C. The structure is derived from the CaF2 type. It contains isolated Ir4B groups with boron in an unusual, nearly square planar coordination.
    Notes: Die neue Verbindung Ga8Ir4B (tetragonal, I41/acd, a = 853,69(2) pm, c = 2105,69(6) pm, Z = 8, 614 Reflexe, 31 Parameter, R = 0,034) wurde durch Reaktion der Elemente bei 1 100°C dargestellt. Die Struktur läßt sich vom CaF2-Typ ableiten. Sie enthält isolierte Ir4B-Gruppen mit Bor in einer ungewöhnlichen, nahezu quadratisch planaren Koordination.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956210206
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    Phosphido- und arsenido-verbrückte Zweikernkomplexe: Synthese und Struktur von (η5-C5H4R)2Zr{μ-P(SiMe3)2}2M(CO)4 (R = Me, M = Cr; R = H, M = Mo) sowie die Synthese von (η5-C5H5)2Zr{μ-As(SiMe3)2}2Cr(CO)4 (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 771-778 
    Details
    ISSN: 0044-2313
    Keywords: Phosphido-bridged dinuclear complexes ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Phosphido- and Arsenido-bridged Dinuclear Complexes. Synthesis and Molecular Structure of (η5-C5H4R)2Zr{μ-P(SiMe3)2}2M(CO)4 (R = Me, M = Cr; R = H, M = Mo) and Synthesis of (η5-C5H5)2Zr{μ-As(SiMe3)2}2Cr(CO)4The reaction of (η5-C5H4R)2Zr{E(SiMe3)2}2 with M(CO)4(NBD) (NBD = norbornadiene) yields the dinuclear phosphido- or arsenido-bridged complexes (η5-C5H4R)2Zr{μ-E(SiMe3)2}2M(CO)4 (R = Me, E = P, M = Cr (1); R = H, E = P, M = Mo (2); R = H, E = As, M = Cr (3)). No formation of dinuclear complexes was observed in the reaction of (η5-C5H4Me)2Zr{P(SiMe3)2}2 with Ni(PEt3)4, Ni(CO)2(PPh3)2 or with NiCl2(PPh3)2 in the presence of Mg. Complexes 1-3 were characterised spectroscopically (i. r., n. m. r., m. s.), and X-ray structure investigations were carried out on 1 and 2. The central four-membered ZrP2M ring is slightly puckered (dihedral angle between planes ZrP2/CrP2 14.7°, ZrP2/MoP2 14.2°). The Zr—P bond lengths are equivalent (1: Zr—P1 2.654(4), Zr—P2 2.657(4) Å; 2: Zr—P1 2.6711(9), Zr—P2 2.6585(7) Å), as are the M—P bond lengths (M = Cr (1): Cr—P1 2.513(4), Cr—P2 2.502(4) Å; M = Mo (2): Mo—P1 2.6263(7), Mo—P2 2.6311(10) Å). The long Zr ··· M distances of 3.414 Å (M = Cr (1)) and 3.461 Å (M = Mo (2)) indicate the absence of a metal-metal bond.
    Notes: Die Reaktion von (η5-C5H4R)2Zr{E(SiMe3)2}2 mit M(CO)4(NBD) (NBD = Norbornadien) liefert die phosphido- oder arsenido-verbrückten Zweikernkomplexe (η5-C5H4R)2Zr{μ-E(SiMe3)2}2M(CO)4 (R = Me, E = P, M = Cr (1); R = H, E = P, M = Mo (2); R = H, E = As, M = Cr (3)). Hingegen führen die Umsetzungen von (η5-C5H4Me)2Zr{P-(SiMe3)2}2 mit Ni(PEt3)4, Ni(CO)2(PPh3)2 oder mit NiCl2(PPh3)2 in Gegenwart von Mg nicht zu entsprechenden Zweikernkomplexen. Die Verbindungen 1-3 wurden spektroskopisch charakterisiert (IR, NMR, MS), 1 und 2 zusätzlich durch eine Röntgenstrukturanalyse. Der zentrale Vierring ZrP2M ist leicht gewellt (Diederwinkel zwischen den Ebenen ZrP2/CrP2 14,7°, ZrP2/MoP2 14,2°). Die Zr—P- oder M—P-Bindungslängen sind nahezu gleich (1: Zr—P1 2,654(4), Zr—P2 2,657(4) Å, Cr—P1 2,513(4), Cr—P2 2,502(4) Å; 2: Zr—P1 2,6711(9), Zr—P2 2,6585(7) Å; Mo—P1 2,6263(7), Mo—P2 2,6311(10) Å). Der lange Zr ··· M-Abstand von 3,414 Å (M = Cr (1)) und 3,461 Å (M = Mo (2)) weist auf das Fehlen einer Metall-Metall-Bindung hin.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956210514
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    CuTb[B5O10]: Das erste „Metaborat“ mit einem ∞1[B5O10]5- -Anion (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 567-570 
    Details
    ISSN: 0044-2313
    Keywords: Copper terbium borate ; synthesis ; crystal structure ; X-ray-diffraction ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: CuTb[B5O10]: The first “Metaborate” with a ∞1[B5O10]5- AnionSingle crystals of the new compound CuTb[B5O10] were obtained by a B2O3 flux-technique. They crystallize in a so far unknown structure. X-ray investigations on single crystals led to the space group C2v21-I ba2 (Nr. 45); a = 6.294(1) Å; b = 8.406(8) Å; c = 12.733(2) Å; Z = 4. The structure contains ∞1[B5O10]5- chains isolated from each other. These chains include twelf membered rings of boron and oxygen. Each ring consists of two tetrahedral BO4 and two planar B2O5 groups and is connected with the next one via the BO4 units. Tb3+ is eightfold- and Cu2+ elongated octahedraly coordinated by oxygen.
    Notes: Aus einer B2O3-Schmelze entstanden hellbraune, transparente Einkristalle von CuTb[B5O10] mit völlig neuartigem Kristallstrukturtyp. Röntgenographische Untersuchungen an Einkristallen ergaben die Raumgruppe C2v21-Iba2 (Nr. 45); a = 6,294(1) Å; b = 8,406(8) Å; c = 12,733(2) Å; Z = 4. Die Struktur weist voneinander isolierte ∞1[B5O10]5--Ketten auf. Diese Ketten enthalten Bor-Sauerstoff-Zwölfringe, die jeweils aus zwei tetraedrischen BO4- und zwei planaren B2O5-Baugruppen gebildet werden. Die Verknüpfung der Ringe untereinander geschieht über die BO4-Baugruppe. Tb3+ ist achtfach und Cu2+ elongiert oktaedrisch von Sauerstoff umgeben.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956210413
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  • 59
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    Zur Kristallstruktur von Cu2M(BO3)O2 (M = Fe3+, Ga3+) (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 571-575 
    Details
    ISSN: 0044-2313
    Keywords: Copper ; iron ; gallium ; borate ; oxide ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of Cu2M(BO3)O2 (M = Fe3+, Ga3+)Single Crystals of the compounds Cu2M(BO3)O2 (M = Fe3+ (I), Ga3+ (II)) were obtained by a B2O3 flux-technique. They crystallize in a monoclinic distorted variant of a Ludwigite structure with a partly ordered metal distribution. X-ray investigations on single crystals led to the space group C2h5-P21/c (No. 14); I: a = 3.108(1); b = 12.003(1); c = 9.459(3) Å; b̃ = 96.66(3)°; Z = 4 and II: a = 3.1146(2); b = 11.921(3); c = 9.477(2) Å; b̃ = 97.91(2)°; Z = 4. All metal-sites are distorted octahedraly coordinated by oxygen-ions. The structure contains isolated planar BO3-units and oxygen which is not coordinated to boron.
    Notes: Aus einer B2O3-Schmelze gelang die Synthese von Einkristallen der Substanzen Cu2M(BO3)O2 (M = Fe3+ (I), Ga3+ (II)), die isotyp zueinander sind und in einer monoklin verzerrten Strukturvariante eines Ludwigites mit teilweise geordneter Metallverteilung kristallisieren. Röntgenographische Untersuchungen an Einkristallen ergeben die Raumgruppe C2h5-P 21/c (Nr. 14) mit I: a = 3,108(1); b = 12,003(1); c = 9,459(3) Å; b̃ = 96,66(3)°; Z = 4 und II: a = 3,1146(2); b = 11,921(3); c = 9,477(2) Å; b̃ = 97,91(2)°; Z = 4. Die Metallkationen sind verzerrt oktaedrisch von Sauerstoffionen koordiniert. Die Struktur weist sowohl isolierte, planare BO3-Baugruppen als auch nicht an Bor gebundenen Sauerstoff auf.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956210414
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    Synthese und Strukturbestimmung von (tBuP)4Sn(CH3)2 und (CH3)2Sn[(tBu)P—P(tBu)]2Sn(CH3)2 (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1358-1364 
    Details
    ISSN: 0044-2313
    Keywords: Phosphorus tin heterocycles ; syntheses ; crystal structure ; NMR ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure Analysis of (tBuP)4Sn(CH3)2 and (CH3)2Sn[(tBu)P—P(tBu)]2Sn(CH3)2The diphosphides K2[(tBu)P—(tBuP)2—P(tBu)] 7 or K2[(tBu)P—P(tBu)] 8 react with (CH3)2SnCl2 in a molar ratio of 1 : 1 to form the binary 5-membered ring system P4Sn 4 a and the 6-membered ring system Sn(P2)2Sn 5 a respectively. When (CH3)2SnCl2, however, is treated with 8 in a molar ratio of 2 : 1 the 4-membered ring system P3Sn 2 a is formed which includes the fragmentation of the intermediate K2[(CH3)2Sn ((tBu)P—P(tBu))2] 9. 4 a and 5 a could be obtained in a pure form and characterized NMR spectroscopically and by X-ray structure analyses; 2 a was identified only NMR spectroscopically.
    Notes: Die Diphosphide K2[(tBu)P—(tBuP)2—P(tBu)] 7 bzw. K2[(tBu)P—P(tBu)] 8 reagieren mit (CH3)2SnCl2 im Molverhältnis 1 : 1 zu dem binären Fünfringsystem P4Sn 4 a bzw. dem Sechsringsystem Sn(P2)2Sn 5 a. Wird jedoch (CH3)2SnCl2 mit zwei Äquivalenten 8 umgesetzt, so erhält man nach einer Fragmentierung des Intermediats K2[(CH3)2Sn ((tBu)P—P(tBu))2] 9 das binäre Vierringsystem P3Sn 2 a. 4 a und 5 a konnten in reiner Form isoliert, NMR-spektroskopisch und durch Röntgenstrukturanalysen charakterisiert werden; 2 a konnte bisher nur NMR-spektroskopisch identifiziert werden.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956210814
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    Zur Kristallstruktur von LiPdGaF6, RbPdAlF6 und K1,06Pd0,95Fe1,05F6 (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1385-1394 
    Details
    ISSN: 0044-2313
    Keywords: Palladium ; quaternary fluorides ; LiPdGaF6 ; RbPdAlF6 ; K1.06Pd0.95Fe1.05F6 ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of LiPdGaF6, RbPdAlF6 and K1.06Pd0.95Fe1.05F6Single crystals of LiPdGaF6 (blue; trigonal, P31c-D3d2 (No. 163), a = 505.72(2), c = 923.7(2) pm; LiCaAlF6-Type [1]), RbPdAlF6 (violet; orthorhombic, Pnma-D2h16 (No. 62), a = 729.0(1), b = 711.1(1), c = 1006.5(2) pm; CsAgFeF6-Type [2]) and K1.06Pd0.95Fe1.05F6 (greenish-blue; tetragonal, P42/mbc-D4h13 (No. 135), a = 1 279.07(7), c = 800.2(1) pm; K1,08MnFeF6-Type [3]; four cycle diffractometer data, Siemens AED2) are obtained by heating the binary fluorides in sealed Pd-tubes under dry argon [solid state reaction, T ≈ 650, t ≈ 19 d (39 d, 24 d)].
    Notes: Durch Umsetzung von äquimolaren Gemengen der binären Fluoride im verschweißten Pd-Rohr unter Schutzgas [Ar, Festkörperreaktion, T = 650°C, t = 19 d (39 d, 24 d)] erhält man Einkristalle von LiPdGaF6 (blau, trigonal, P31c-D3d2 (No. 163), a = 505,72(2), c = 923,7(2) pm, LiCaAlF6-Typ [1]), RbPdAlF6 (violett, orthorhombisch, Pnma-D2h16 (No. 62), a = 729,0(1), b = 711,1(1), c = 1006,5(2) pm, CsAgFeF6-Typ [2]) sowie K1,06Pd0,95Fe1,05F6 (blau-grün, tetragonal, P42/mbc-D4h13 (No. 135), a = 1279,07(7), c = 800,2(1) pm; K1,08MnFeF6-Typ [3]; jeweils Vierkreisdiffraktometerdaten).
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956210818
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    Nitrido-silicate. II [1]. Hochtemperatur-Synthesen und Kristallstrukturen von Sr2Si5N8 und Ba2Si5N8 (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1380-1384 
    Details
    ISSN: 0044-2313
    Keywords: silicon nitrides ; nitrido-silicates ; strontium ; barium ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Nitrido-Silicates. II. High Temperature Syntheses and Crystal Structures of Sr2Si5N8 and Ba2Si5N8Pure Sr2Si5N8 and Ba2Si5N8 were obtained by reaction of silicon diimide with metallic strontium and barium, respectively. The reactions have been carried out under nitrogen atmosphere in a specially developed high-frequency furnace at temperatures between 1 550 and 1 650°C. Sr2Si5N8 (Pmn21, a = 571.0(2), b = 682.2(2), c = 934.1(2) pm, Z = 2, R = 0.037, wR = 0.021) and Ba2Si5N8 (Pmn21, a = 578.3(2), b = 695.9(2), c = 939.1(2) pm, Z = 2, R = 0.022, wR = 0.018) are isotypic and contain M2+ ions as well as a three-dimensional covalent network structure of corner-sharing SiN4 tetrahedra. Two sorts of N occur with molar ratio 1 : 1 which are bonded to two and three Si, respectively. Predominantly, the N which are bonded to two Si belong to the coordination spheres of the M2+ ions.
    Notes: Sr2Si5N8 und Ba2Si5N8 werden phasenrein durch Umsetzung von Siliciumdiimid mit den jeweiligen Metallen Strontium bzw. Barium unter Stickstoffatmosphäre in einem speziellen Hochfrequenzofen bei 1 550 bis 1 650°C synthetisiert. Sr2Si5N8 (Pmn21, a = 571,0(2), b = 682,2(2), c = 934,1(2) pm, Z = 2, R = 0,037, wR = 0,021) und Ba2Si5N8 (Pmn21, a = 578,3(2), b = 695,9(2), c = 939,1(2) pm, Z = 2, R = 0,022, wR = 0,018) kristallisieren isotyp und sind aus M2+-Ionen (M = Sr bzw. Ba) sowie einer kovalenten dreidimensionalen Raumnetzstruktur eckenverknüpfter SiN4-Tetraeder aufgebaut. Je 4 N sind an zwei bzw. drei Si gebunden. Die an je zwei Si gebundenen N leisten den dominierenden koordinativen Beitrag für die M2+-Ionen.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956210817
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    Thermisches Verhalten und Kristallstruktur von YAl3Cl12 (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1414-1420 
    Details
    ISSN: 0044-2313
    Keywords: Yttrium chloroaluminate ; crystal structure ; solution calorimetry ; thermodynamic data ; phase diagram ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Thermal Behaviour and Crystal Structure of YAl3Cl12We determined the thermodynamic data of YAl3Cl12 ΔHYOAl3Cl12,298 = -739.9 ± 3 kcal/mol and SYOAl3Cl12,298 = 136.1 ± 4 cal/K · mol by total pressure measurements and ΔHYOAl3Cl12,298 = -739.1 ± 1.6 kcal/mol by solution calorimetry. Using DTA-investigations we established the phase diagram in the system AlCl3-YCl3. The crystal structure was refined on the basis of single crystal data (P31 12; Z = 3; a = 1 046.8(2); c = 1 562.3(3) pm).
    Notes: Mit phasenreinem YAl3Cl12 werden Zersetzungsdruckmessungen im Membrannullmanometer und lösungskalorimetrische Messungen zur Bestimmung der thermodynamischen Daten der Verbindung durchgeführt, wobei wir aus den Druckmessungen ΔHYOAl3Cl12,298 = -739,9 ± 3 kcal/mol und SYOAl3Cl12,298 = 136,1 ± 4 cal/K · mol ermitteln und lösungskalorimetrisch ΔHYOAl3Cl12,298 = -739,1 ± 1,6 kcal/mol herleiten. DTA-Untersuchungen dienten der Aufstellung eines Phasendiagrammes im System YCl3—AlCl3.Anhand der Einkristalldaten wurde die Struktur verfeinert (P3112; Z = 3; a = 1 046,8(2); c = 1 562,3(3) pm).
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956210822
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    Einfache Trithio- und Perthiocarbonatokomplexe mit interessanter Koordinationschemie: [E(CS3)2]2- (E = Sn, Zn, Cd), [E(CS3)3]3- (E = As, Sb, Bi, Co), {Cu(CS3)-}∞ und [Zn(CS4)2]2-Professor Hubert Schmidbaur zum 60. Geburtstag gewidmet (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1160-1170 
    Details
    ISSN: 0044-2313
    Keywords: zinc, cadmium, tin, arsenic, antimony, bismuth, cobalt, copper, trithio complexes, perthio complexes, perthiodicarbonate ; synthesis ; crystal structure ; IR spectroscopy ; Raman spectroscopy ; 113Cd and 59Co NMR spectroscopy ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Simple Trithio- and Perthiocarbonato Complexes with Interesting Bond Properties: [E(CS3)2]2- (E = Sn, Zn, Cd), [E(CS3)3]3- (E = As, Sb, Bi, Co), {Cu(CS3)-}∞ and [Zn(CS4)2]2-By reactions of potassium trithiocarbonate (1) with solutions of zinc(II)- acetylacetonate, cadmium(II)-chloride, tin(II)-chloride, arsenic(III)-sulfide (suspension), antimony(III)-chloride, bismuth(III)-chloride and copper(II)-chloride in dimethyl sulfoxide, as well as of trisodium hexanitrito cobaltate(III) in water, and the precipitation of the complexes with an aqueous solution of tetraphenylphosphonium chloride the compounds (PPh4)2[Zn(CS3)2] (2), (PPh4)2[Cd(CS3)2] (3), (PPh4)2[Sn(CS3)2] (4), (PPh4)3[As(CS3)3] (5), (PPh4)3[Sb(CS3)3] (6), (PPh4)3[Bi(CS3)3] (7), (PPh4)3[Co(CS3)3] (8) and (PPh4)Cu(CS3) (9) have been isolated. (PPh4)2[Zn(CS4)2] · CH3NO2 (10) has been prepared by heating a solution of 2 in nitromethane to 60--70°C in presence of air. The reaction of 1 in dimethyl sulfoxide with an aqueous tetraphenylphosphonium chloride solution in presence of oxygen leads to (PPh4)2[C2S6] (11). The compounds have been characterized by spectroscopical studies (IR, Raman, UV/Vis, 113Cd/59Co-NMR), magnetic susceptibility measurements, powder diffractometry, elemental analyses and single crystal X-ray structure analysis (4-7, 10 and 11). The difficult growing of single crystals has been reported in detail. For crystal data see Inhaltsübersicht.
    Notes: Durch Reaktion von Lösungen von Zink(II)-acetylacetonat, Cadmium(II)-chlorid, Zinn(II)-chlorid, Arsen(III)-sulfid (Suspension), Antimon(III)- chlorid, Bismut(III)-chlorid und Kupfer(II)-chlorid in Dimethylsulfoxid - bzw. von Trinatriumhexanitritocobaltat(III) in Wasser - mit Kaliumtrithiocarbonat (1) sowie anschließender Fällung der Komplexe mit wäßriger Tetraphenylphosphoniumchlorid-Lösung wurden die Verbindungen (PPh4)2[Zn(CS3)2] (2), (PPh4)2[Cd(CS3)2] (3), (PPh4)2[Sn(CS3)2] (4), (PPh4)3[As(CS3)3] (5), (PPh4)3[Sb(CS3)3] (6), (PPh4)3[Bi(CS3)3] (7), (PPh4)3[Co(CS3)3] (8) und (PPh4)Cu(CS3) (9) isoliert. (PPh4)2[Zn(CS4)2] · CH3NO2 (10) ließ sich aus einer Lösung von 2 in Nitromethan, die in Gegenwart von Luftsauerstoff auf 60-70°C erwärmt wurde, isolieren. Bei Umsetzung von 1 in Dimethylsulfoxid mit einer wäßrigen Tetraphenylphosphoniumchlorid-Lösung in Gegenwart von Sauerstoff bildete sich (PPh4)2[C2S6] (11). Die Verbindungen wurden durch spektroskopische Methoden (IR, Raman, UV/VIS sowie 113Cd- und 59Co-NMR), Messung der magnetischen Suszeptibilität, Pulverdiffraktometrie, Elementaranalysen und Einkristall-Röntgenstrukturanalyse (4-7, 10 und 11) charakterisiert. Die schwierige Züchtung von Einkristallen wird im Detail beschrieben. 4:P1, a = 969,1(2), b = 1 335,3(3), c = 3 749,9(7) pm, α = 84,54(3)°, β = 80,88(3)°, γ= 74,90(3)°, V = 4 618(2)×106 pm3, Z = 4, R = 0,082 für 7 635 unabhängige Reflexe (Fo 〉 4σ(Fo));5:C2/c, a = 2 236,6(4), b = 1 441,0(3), c = 4 267,7(9) pm, β = 98,59(3)°, V = 13 600(15)×106 pm3, Z = 8, R = 0,130 für 3 807 unabhängige Reflexe (Fo 〉 4σ(Fo));6:P21, a = 1 555,0(9), b = 1 437,1(5), c = 1 587,6(9) pm, β = 90,30(5)°, V = 3 547(3)×106pm3, Z = 2;7:P21, a = 1 559,6(4), b = 1 425,2(4), c = 1 585,1(4) pm, β = 90,05(2)°, V = 3 523(2)×106 pm3, Z = 2, R = 0,088 für 4 206 unabhängige Reflexe (Fo 〉 4σ(Fo));10:C2/c, a = 1 049,1(4), b = 2 023,9(9), c = 2 474,7(9) pm, β = 99,93(3)°, V = 5 176(3)×106 pm3, Z = 4, R = 0,079 für 2 172 unabhängige Reflexe (Fo 〉 4σ(Fo));11:P21/c, a = 1 673,0(5), b = 1 430,8(5), c = 1 859,1(5) pm, β = 94,12(2)°, V = 4 439(2)×106 pm3, Z = 4, R = 0,086 für 4 014 unabhängige Reflexe (Fo 〉 4σ(Fo)).
    Additional Material: 7 Ill.
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    Na7I2(OH)5: Ein Hydroxidiodid im System NaOH/NaI (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1189-1192 
    Details
    ISSN: 0044-2313
    Keywords: Sodium hydroxide iodide ; synthesis ; single-crystals ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Na7I2(OH)5: A Hydroxide Iodide in the System NaOH/NaIThe pseudobinary system NaOH/NaI is investigated by X-ray methods. The crystal structure of the compound Na7I2(OH)5 was solved by single crystal data:Na7I2(OH)5: P4/nmm, Z = 2, a = 7.748(2) Å, c = 10.260(3) Å, Z(Fo) = 443 with (Fo)2 ≥ 3σ(Fo)2, Z(parameter) = 28, R/Rw = 0.044/0.059Na7I2(OH)5 crystallizes in a new type of structure which contains puckered layers of ∞2[Na7(OH)52+] connected via iodide ions.
    Notes: Das pseudobinäre System NaOH/NaI wurde röntgenographisch untersucht und die Struktur einer Verbindung, Na7I2(OH)5, mittels Röntgenstrukturanalyse an Einkristallen aufgeklärt:Na7I2(OH)5: P4/nmm, Z = 2, a = 7,748(2) Å, c = 10,260(3) Å, Z(Fo) = 443 mit (Fo)2 ≥ 3σ(Fo)2, Z(Parameter) = 28, R/Rw = 0,044/0,059.Die Verbindung kristallisiert in einem eigenen Strukturtyp, der gewellte Schichten von ∞2[Na7(OH)52+] enthält, die über I- verknüpft sind.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956210713
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    Na5Br(OH)4: Darstellung und Kristallstruktur einer Verbindung im System NaOH/NaBr (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1185-1188 
    Details
    ISSN: 0044-2313
    Keywords: Sodium bromide hydroxide ; synthesis ; single-crystals ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Na5Br(OH)4: Synthesis and Structure of a Compound in the System NaOH/NaBrThe pseudobinary system NaOH/NaBr is investigated by X-ray methods. The structure of the compound Na5Br(OH)4 was solved by single crystal data:Na5Br(OH)4: Pnma, Z = 8, a = 11.846(2) Å, b = 18.782(4) Å, c = 6.431(1) Å, Z(Fo) = 1 202 with (Fo)2 ≥ 3σ(Fo)2, Z(parameter) = 100, R/Rw = 0.030/0.035The compound crystallizes in a new type of structure. Pairs of octahedra around O by 5 Na and 1 H to [Na5(OH)]2 are orientated in such a way to one another that two ions OH- form a parallelogram hinting to unusual bent hydrogen bridge bonding.
    Notes: Das pseudobinäre System NaOH/NaBr wurde röntgenographisch untersucht und die Struktur von Na5Br(OH)4 mittels Röntgenstrukturanalyse an Einkristallen aufgeklärt:Na5Br(OH)4: Pnma, Z = 8, a = 11,846(2) Å, b = 18,782(4) Å, c = 6,431(1) Å, Z(Fo) = 1 202 mit (Fo)2 ≥ 3σ(Fo)2, Z(Parameter) = 100, R/Rw = 0,030/0,035.Auffällig an dem neuen Strukturtyp ist eine paarweise Anordnung von Oktaedern um O durch 5 Na und 1 H zu [Na5(OH)]2. Je zwei OH- sind so zueinander orientiert, daß auf ungewöhnlich gewinkelte H-Brücken auf zwei gegenüberliegenden Seiten eines Parallelogramms zu schließen ist.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956210712
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    K2Br(OH) und Rb2Br(OH): Zwei neue ternäre Alkalimetallhalogenidhydroxide mit ausgeprägter Strukturverwandtschaft zu KOH bzw. RbOH (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1193-1196 
    Details
    ISSN: 0044-2313
    Keywords: Potassium bromide hydroxide ; Rubidium bromide hydroxide ; synthesis ; single-crystals ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: K2Br(OH) and Rb2Br(OH): Two New Ternary Alkali Metal Halide Hydroxides with a Pronounced Structural Relationship to KOH resp. RbOHTwo isotypic compounds K2Br(OH) and Rb2Br(OH) were prepared in the systems KOH/KBr and RbOH/RbBr. Their structures were determined by single crystal X-ray methods:K2Br(OH): P21/m, Z = 2, a = 6.724(1) Å, b = 4.272(4) Å, c = 8.442(2) Å, β = 108.14(2)°, Z(Fo) = 651 with (Fo)2 ≥ 3σ(Fo)2, Z(parameter) = 28, R/Rw = 0.041/0.047Rb2Br(OH): P21/m, Z = 2, a = 6.918(3) Å, b = 4.483(2) Å, c = 8.850(5) Å, β = 108.08(6)°, Z(Fo) = 326 mit (Fo)2 ≥ 3σ(Fo)2, Z(parameter) = 27, R/Rw = 0.074/0.082.The compounds are built up by chains of ∞1[M2(OH)+] connected via Br-. The structure of the chains as well as their orientation to one another show a pronounced relationship to the structures of the room temperature modifications of the isotypic binary hydroxides KOH and RbOH.
    Notes: In den pseudobinären Systemen KOH/KBr und RbOH/RbBr konnten die beiden isotypen Verbindungen K2Br(OH) und Rb2Br(OH) dargestellt werden. Ihre Struktur wurde mittels Röntgenstrukturanalyse an Einkristallen aufgeklärt:K2Br(OH): P21/m, Z = 2, a = 6,724(1) Å, b = 4,272(4) Å, c = 8,442(2) Å, β = 108,14(2)°, Z(Fo) = 651 mit (Fo)2 ≥ 3σ(Fo)2, Z(Parameter) = 28, R/Rw = 0,041/0,047.Rb2Br(OH): P21/m, Z = 2, a = 6,918(3) Å, b = 4,483(2) Å, c = 8,850(5) Å, β = 108,08(6)°, Z(Fo) = 326 mit (Fo)2 ≥ 3σ(Fo)2, Z(Parameter) = 27, R/Rw = 0,074/0,082.Die Verbindungen sind aus isolierten Strängen von ∞1[M2(OH)+] aufgebaut, die durch Br- verknüpft werden. Sowohl der Aufbau der einzelnen Stränge als auch ihre Orientierung zueinander zeigen eine deutliche Verwandtschaft zum Aufbau der Raumtemperaturform der ebenfalls isotypen binären Hydroxide KOH und RbOH.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956210714
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    Reaktion von Chlornitrat mit CF3I: Isolierung von Trifluormethylchloriodnitrat CF3I(Cl)ONO2 und Kristallstruktur von Trifluormethylioddinitrat CF3I(ONO2)2 (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1552-1557 
    Details
    ISSN: 0044-2313
    Keywords: Chlorine Nitrate ; Trifluormethylchloroiodinenitrate ; Trifluormethyliodinedinitrate ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reaction of Chlorine Nitrate with CF3I: Isolation of Trifluormethylchloroiodinenitrate CF3I(Cl)ONO2 and the Crystal Structure of Trifluormethyliodinedinitrate CF3I(ONO2)2CF3I reacts with ClONO2 to Iodine(III)-compounds. After an addition CF3I(Cl)ONO2 is isolated and characterized by vibrational spectra. With surplus ClONO2 it is formed CF3I(ONO2)2.CF3I(ONO2)2 crystallizes monoclinic in the space group P21/c with the cell parameters a = 1 024.3(6) pm, b = 873.5(6) pm, c = 873.4(6) pm and Z = 4.We measered following bonding distances: I—O: 207.3(3) and 220.8(2) pm, I—C: 221.1(4) pm and N—O: from 119.1(4) to 141.5(3) pm.Through an intermolecular I ··· O-contact the central iodine becomes a distorted plane geometry.
    Notes: CF3I reagiert mit ClONO2 in einer oxidativen Additionsreaktion zu Iod(III)-Verbindungen. Das Additionsprodukt CF3I(Cl)ONO2 wird isoliert und schwingungsspektroskopisch charaktersiert. Mit überschüssigem ClONO2 bildet sich CF3I(ONO2)2.CF3I(ONO2)2 kristallisiert monoklin in der Raumgruppe P21/c mit a = 1 024,3(6) pm, b = 873,5(6) pm, c = 873,4(6) pm und Z = 4.Es werden folgende Bindungslängen gemessen: I—O: 207,3(3) bzw. 220,8(2) pm, I—C: 221,2(4) pm und N—O: 119,1(4) bis 141,5(3) pm.Durch einen intermolekularen I ··· O-Kontakt erlangt das zentrale Iodatom eine verzerrt-planare Umgebung.
    Additional Material: 3 Ill.
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    Synthese und Kristallstrukturbestimmung von Dimethyldi-(N-Methylimidazolium)siliciumbromid (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 101-104 
    Details
    ISSN: 0044-2313
    Keywords: Dimethyldi(N-Methylimidazolium)silicon bromide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure Determination of Dimethyldi-(N-Methylimidazolium)silicon BromideThe reaction of dibromodimethylsilane with n-methylimidazole (NMI) leads to a 1:2 compound stable at room temperature. The reaction was carried out at room temperature and colorless, moisture sensitive crystals were obtained by sublimation. The addition compound crystallizes in the orthorhombic space group Pcam (No. 57) with lattice constants a = 1 110 96(8) pm, b = 1 142.3(2) pm and c = 1 238.9(3) pm. For 1 317 independent reflections, measured at 21°C, the structure could be refined to R = 0.040 and Rw = 0.041.
    Notes: Die Reaktion von Dibromdimethylsilan mit N-Methylimidazol (NMI) führt zu einer bei Raumtemperatur stabilen 1:2-Verbindung. Die Umsetzung wurde bei Raumtemperatur durchgeführt, und durch Sublimation ließen sich farblose, feuchtigkeitsempfindliche Einkristalle der Verbindung erhalten. Die Additionsverbindung kristallisiert in der orthorhombischen Raumgruppe Pcam (Nr. 57) mit den Gitterkonstanten a = 1 110,96(8) pm, b = 1 142,3(2) pm und c = 1 238,9(3) pm. Unter Verwendung von 1 317 symmetrieunabhängigen Reflexen konnte die Struktur, gemessen bei 21°C, bis auf R = 0,040 und Rw = 0,041 verfeinert werden.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956210118
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  • 70
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    Synthese, Struktur und Phasenumwandlung von Se4(MoOCl4)2 (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 131-136 
    Details
    ISSN: 0044-2313
    Keywords: Tetraselenium(2+) bis(tetrachlorooxomolybdate)-(2-) ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Crystal Structure, and Phase Transition of Se4(MoOCl4)2Dark green, very air sensitive crystals of Se4(MoOCl4)2 are formed from selenium and MoOCl4 at 190°C in a sealed, evacuated glass ampoule in quantitative yield. The structure is built of nearly square planar Se42+ ions and centrosymmetric dimeric MoOCl4- ions which are linked by bridging Cl atoms. At -21°C Se4(MoOCl4)2 undergoes a reversible solid state phase transition of first order. Structure determinations at -70°C and 23°C show that during the phase transition the structures of the ions remain unchanged, while the orientations of the ions with respect to each other change in such a way that in the low temperature form the Se42+ ions obtain a higher coordination number by Cl and O atoms of neighboring MoOCl4- ions.
    Notes: Bei 190°C entstehen aus Selen und MoOCl4 in einer evakuierten, zugeschmolzenen Glasampulle in quantitativer Ausbeute dunkelgrüne, sehr hydrolyseempfindliche Kristalle von Se4(MoOCl4)2. Die Struktur ist aus nahezu quadratisch planaren Se42+-Ionen und aus zentrosymmetrischen, über verbrückende Chloratome dimerisierten (MoOCl4-)2-Ionen aufgebaut. Bei -21°C durchläuft Se4(MoOCl4)2 eine reversible, diskontinuierliche Phasenumwandlung nach der 1. Ordnung. Strukturbestimmungen bei -70°C und bei 23°C zeigen, daß beim Phasenübergang die Strukturen der Ionen erhalten bleiben, sich jedoch die Orientierungen der Ionen zueinander in der Weise ändern, daß in der Tieftemperaturform die Se42+-Ionen eine höhere Koordination durch O- und Cl-Atome benachbarter MoOCl4--Ionen erhalten.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956210124
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  • 71
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    Kristallstruktur und Phasenumwandlungen von As(CH3)4I (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 143-148 
    Details
    ISSN: 0044-2313
    Keywords: Tetramethylarsoniumiodide ; crystal structure ; phase transitions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure and Phase Transitions of As(CH3)4IThe crystal structure of α-As(CH3)4I at room temperature was determined using single crystal data: cubic, space group Pa3, a = 1 198.0(2) pm. Therefore α-As(CH3)4I displays a novel crystal structure, which is not comparable to known AB-Typ structures with respect to the arrangement of anions and the baricenters of the complex cations. Differential thermal analysis showed three phase transitions at 103, 175 and 215°C. The lattice parameters of the high temperature phases (temperature dependent Guinier measurements) are: β-As(CH3)4I (tetragonal): a = 845.2(2) pm, c = 615.0(2) pm; γ-As(CH3)4I (hexagonal): a = 737.7(2) pm, c = 1 082.2(3) pm; and to δ-As(CH3)4I (hexagonal): a = 705.8(2) pm, c = 1 147(1) pm. β-and γ-As[(CH3)]4I are isotypic to N(CH3)4Cl and As(CH3)4Br, respectively.
    Notes: Die Struktur von α-As(CH3)4I wurde an Einkristallen bei Raumtemperatur bestimmt: kubisch, RG: Pa3, a = 1 198,0(2) pm. Danach hat α-As(CH3)4I eine neuartige Kristallstruktur, die sich bezüglich der Anordnung von Anionen und Schwerpunkten der komplexen Kationen auf keinen bekannten AB-Typ zurückführen läßt. Mittels DTA wurden drei Phasenumwandlungen bei 103, 175 und 215°C gefunden. Die Gitterkonstanten der Hochtemperaturphasen (Heizguinier-aufnahmen) betragen für β-As(CH3)4I (tetragonal): a = 845,2(2) pm, c = 615,0(2) pm; für γ-As(CH3)4I (hexagonal): a = 737,7(2) pm, c = 1 082,2(3) pm; und für γ-As(CH3)4I (hexagonal): a = 705,8(2) pm, c = 1 147(1) pm. β- und γ-As(CH3)4I sind isotyp zu N(CH3)4Cl bzw. As(CH3)4Br.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956210126
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  • 72
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    Deprotonierte Dithiocarbaminsäureester als Thiolat-S-Donor-Liganden. Strukturen von Ph(H)NC(S)SMe, Co(PhNC(S)SMe)3 und Cu6(PhNC(S)SMe)6 (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 72-76 
    Details
    ISSN: 0044-2313
    Keywords: Dithiocarbamate complexes of cobalt and copper ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Deprotonated Dithiocarbamic Acid Esters as Thiolate S-Donor Ligands. Structures of Ph(H)NC(S)SMe, Co(PhNC(S)SMe)3, and Cu6(PhNC(S)SMe)6The reaction of N-phenyl-S-methyldithiocarbamate, PhN(H)C(=S)SMe, (1) with cobalt(II) and copper(II) salts yields the monomeric compound CoIII(PhNC(S)SMe)3 (2) and the hexameric compound Cu6I(PhNC(S)SMe)6 (3). These complexes contain the negatively charged imino-thiolate ligand PhN=C(—S)SMe, which has been formed by deprotonation of 1. The crystal structures of 1-3 have been determined. 1 forms centrosymmetrical dimers through N—H … S bridge bonds, the conformation in the solid state and in solution is Z,E′. CoIII shows in 2 a trigonal-antiprismatic coordination, with the ligands acting as N,S-chelates. 3 contains an octahedral Cu6-core with Cu … Cu-distances ranging from 276.3(5) to 305.7(4) pm. Each copper center is trigonally coordinated to one nitrogen and two sulfur atoms of three different ligands.Crystal data: 1, triclinic, space group P1, a = 590.5(6), b = 869.0(1), c = 968.5(9) pm, α = 67.29(8), β = 78.44(8), γ = 81.64(9)°, Z = 2, 1 775 reflections, R(Rw) = 0.0317(0.032). 2, orthorhombic, space group Pbca, a = 978.0(2), b = 1 842.9(4), c = 3 059.7(6) pm, Z = 8, 1 129 reflections, R(Rw) = 0.0997(0.0886). 3, monoclinic, space group P21/c, a = 1 363.1(3), b = 1 342.8(3), c = 1 671.9(3) pm, β = 103.48°, Z = 2, 1 374 reflections, R(Rw) = 0.0708(0.0617).
    Notes: Die Reaktion von N-Phenyl-S-methyl-dithiocarbaminsäureester, PhN(H)C(=S)SMe (1) mit Cobalt- und Kupfersalzen ergibt monomeres CoIII(PhNC(S)SMe)3 (2) und hexameres Cu6I(PhNC(S)SMe)6 (3). 2 und 3 enthalten den aus 1 durch Deprotonierung entstandenen anionischen Liganden PhN=C(—S)SMe. Die Kristallstrukturen von 1-3 wurden ermittelt. 1 bildet über N—H … S-Brückenbindungen zentrosymmetrische Dimere und liegt im festen Zustand und auch in Lösung als Z,E′-Konformer vor. Die Koordinationssphäre von 2 ist trigonal-antiprismatisch; die Liganden sind als N,S-Chelat gebunden, mit facialer Anordnung gleichartiger Donorzentren. 3 enthält als Kern eine verzerrt oktaedrische Cu6-Einheit mit Cu … Cu-Abständen von 276,3(5) bis 305,7(4) pm. Jedes Kupferatom ist von zwei Schwefelatomen und einem Stickstoffatom dreier verschiedener Liganden koordiniert. Die Schwefelatome haben verbrückende Funktion.Kristalldaten: 1, triklin, Raumgruppe P1, a = 590,5(6), b = 869,0(1), c = 968,5(9) pm, α = 67,29(8), β = 78,44(8), γ = 81,64(9)°, Z = 2, 1 775 Reflexe, R(Rw) = 0,0317(0,032). 2, orthorhombisch, Raumgruppe Pbca, a = 978,0(2), b = 1842,9(4), c = 3 059,7(6) pm, Z = 8, 1 129 Reflexe, R(Rw) = 0,0997(0,0886). 3, monoklin, Raumgruppe P21/c, a = 1 363,1(3), b = 1 342,8(3), c = 1 671,9(3) pm, β = 103,48°, Z = 2, 1 374 Reflexe, R(Rw) = 0,0708(0,0617).
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956210113
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    Kaliumamidotrioxogermanate(IV) - Wasserstoff-Brückenbindungen in K3GeO3NH2 und K3GeO3NH2 · KNH2 (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 137-142 
    Details
    ISSN: 0044-2313
    Keywords: Potassium amido trioxogermanate ; single crystals ; crystal structure ; hydrogen bridge bonding ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Potassium Amido Trioxo Germanates(IV) - Hydrogen Bridge Bonds in K3GeO3NH2 and K3GeO3NH2 · KNH2Colorless crystals of K3GeO3NH2 and of K3GeO3NH2 · KNH2 were obtained by the reaction of KNH2 with GeO2 in supercritical ammonia at 450°C and pNH3 = 6 kbar in high-pressure autoclaves within 15 resp. 5 days. The crystal structures of both compounds were solved by X-ray single crystal methods.K3GeO3NH2: P1, a = 6.390(1) Å, b = 6.684(1) Å, c = 7.206(1) Å, α = 96.47(1)°, β = 101.66(1)°, γ = 91.66(1)°, Z = 2, R/Rw = 0.020/0.022, N(I) ≥ 2σ(I) = 3023, N(Var.) = 82 K3GeO3NH2 · KNH2: P21/c, a = 10.982(6) Å, b = 6.429(1) Å, c = 12.256(8) Å, β = 106.12(1)°, Z = 4, R/Rw = 0.022/0.029, N(F) ≥ 3σ(F) = 1745, N(Var.) = 107.In K3GeO3NH2 tetrahedral ions GeO3NH23- are connected to chains by N—H … O bridge bonds with 2.18 Å ≤ d(H … O) ≤ 2.40 Å for d(N—H) ≡ 1.0 Å and by potassium ions while in K3GeO3NH2 · KNH2 bridge bonds between NH2 groups of GeO3NH23- and NH2- ions as acceptors occur with 2.41 Å ≤ d((N—)H … NH2-) ≤ 2.61 Å for d(N—H) ≡ 1.0 Å.
    Notes: Farblose Kristalle von K3GeO3NH2 und von K3GeO3NH2 · KNH2 wurden durch Umsetzung von KNH2 mit GeO2 in überkritischem Ammoniak bei 450°C und pNH3 = 6 kbar in Hochdruckautoklaven innerhalb von 15 bzw. 5 Tagen erhalten. Die Atomanordnungen beider Verbindungen konnten über Röntgenstrukturanalysen an Einkristallen geklärt werden.K3GeO3NH2: P1, a = 6,390(1) Å, b = 6,684(1) Å, c = 7,206(1) Å, α = 96,47(1)°, β = 101,66(1)°, γ = 91,66(1)°, Z = 2, R/Rw = 0,020/0,022, N(I) ≥ 2σ(I) = 3023, N(Var.) = 82 K3GeO3NH2 · KNH2: P21/c, a = 10,982(6) Å, b = 6,429(1) Å, c = 12,256(8) Å, β = 106,12(1)°, Z = 4, R/Rw = 0,022/0,029, N(F) ≥ 3σ(F) = 1745, N(Var.) = 107.In K3GeO3NH2 sind tetraedrische Anionen GeO3NH23- über H-Brückenbindungen N—H … O zu Ketten verknüpft mit 2,18 Å ≤ d(H … O) ≤ 2,40 Å bei d(N—H) ≡ 1,0 Å, die über Kalium zusammengehalten werden, während in K3GeO3NH2 · KNH2 Brückenbindungen zwischen NH2 von GeO3NH23- und eingelagertem NH2- auftreten mit 2,41 Å ≤ d((N—)H … NH2-) ≤ 2,61 Å bei d(N—H) ≡ 1,0 Å.
    Additional Material: 8 Ill.
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    Darstellung und Charakterisierung von P4O7S (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 479-483 
    Details
    ISSN: 0044-2313
    Keywords: Tetraphosphorus heptoxide monosulfide ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Syntheses and Characterization of P4O7SP4O7S was synthesized for the first time and characterized by X-ray structure determination (single-crystal methods) and 31P-n.m.r. (solution and MAS-solid) (P1; a = 687.2(1); b = 718.2(1); c = 809.1(1) pm; α = 92.58(1)°; β = 104.43(1)°; γ = 94.82(2)°; 2 907 diffractometer data; R1 = 0.030; wR2 = 0.102). The different influences of terminally bound oxygen and sulfur on the geometry of the P4O6 cage are discussed.
    Notes: P4O7S wurde erstmals dargestellt und durch Röntgenstrukturanalyse an Einkristallen sowie 31P-NMR (Lösung und MAS-Festkörper) charakterisiert (P1; a = 687,2(1); b = 718,2(1); c = 809,1(1) pm; α = 92,58(1)°; β = 104,43(1)°; γ = 94,82(2)°; 2 907 Diffraktometerdaten; R1 = 0,030; wR2 = 0,102). Der unterschiedliche Einfluß von terminalem Sauerstoff und Schwefel auf die Geometrie des Käfigs in P4O7S wird diskutiert.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956210325
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    Ba7Fe6F32 · 2H2O: Original isolated trimers [Fe3F16]7- in a new defective jarlite-type compound (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1025-1032 
    Details
    ISSN: 0044-2313
    Keywords: Barium iron fluoride ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ba7Fe6F32 · 2H2O: isolierte [Fe3F16]7--Trimere in einer neuen Verbindung vom Defekt-Jarlit-TypBa7Fe6F32 · 2H2O wurde aus wäßriger HF-Lösung in einer Teflon-Bombe (Berghof) bei 180°C dargestellt. Ein teilweiser F-/OH--Austausch erfolgt in verdünnterem HF-Medium und führt zu Ba7Fe6F32-x(OH)x · 2H2O. Die Verbindungen kristallisieren im monoklinen System, Raumgruppe C2/m (Z = 2) mit a = 17,023(1) Å, b = 11,482(1) Å, c = 7,624(1) Å, β = 101,13(1)° für x = 0 und a = 17,036(2) Å, b = 11,489(1) Å, c = 7,620(2) Å, β = 101,48(1)° für x ≍ 5,3. Die Struktur wurde aus 2 256 bzw. 1 343 unabhängigen Reflexen für x = 0 bzw. x ≍ 5,3 mit einem Siemens AED2 Vierkreisdiffraktometer (MoKα) bestimmt; für x = 0: R = 0,0235, Rw = 0,0240; für x ≍ 5,3: R = 0,0324, Rw = 0,0335. Die eng mit dem Jarlit-Typ verwandte Struktur wird aus isolierten Oktaedertrimeren [Fe3F16]7- aufgebaut, die durch Ba2+-Ionen verknüpft werden. Die Lage der Anionen und Wassermoleküle wird mittels Valenzband-Rechnungen diskutiert. Magnetische-und Mössbauer-Untersuchungen werden diskutiert.
    Notes: Ba7Fe6F32 · 2H2O was prepared from HF aqueous solution in a teflon bomb (Berghof) at 180°C. A partial exchange F-/OH- can be realized in more diluted HF medium and leads to Ba7Fe6F32-x(OH)x · 2H2O. The compounds crystallize in the monoclinic system, space group C2/m (Z = 2) with a = 17.023(1) Å, b = 11.482(1) Å, c = 7.624(1) Å, β = 101.13(1)° for x = 0 and a = 17.036(2) Å, b = 11.489(1) Å, c = 7.620(2) Å, β = 101.48(1)° for x ≍ 5.3. The structures were determined from 2 256 and 1 343 independent reflections for x = 0 and x ≍ 5.3 respectively, collected with a Siemens AED2 four-circle diffractometer with the MoKα radiation (R = 0.0235 and Rw = 0.0240 for x = 0 and R = 0.0324 and Rw = 0.0335 for x ≍ 5.3). The structure, closely related to that of the Jarlite-type, is built up from isolated octahedra trimers [Fe3F16]7-, connected together by Ba2+-cations. The location of anions and water molecules is discussed from bond valence calculations. Magnetic and Mössbauer studies are reported and discussed.
    Additional Material: 5 Ill.
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    SeBr3[AlBr4] und TeI3[AlI4] - zwei weitere Vertreter des SCl3[AlCl4]-Strukturtyps (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1042-1046 
    Details
    ISSN: 0044-2313
    Keywords: Tribromoselenium (+) ; Triiodotellurium (+) ; Tetrabromoaluminate (-) ; Tetraiodoaluminate (-) ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: SeBr3[AlBr4] and TeI3[AlI4] - two further Compounds in the SCl3[AlCl4] Structure TypeThe reaction of SeBr4 and AlBr3 in a closed glass ampoule at 150°C yields quantitatively SeBr3[AlBr4] in form of yellow moisture sensitive crystals. From Te, two equivalents of I2, and AlI3 one obtains TeI3[AlI4] in form of dark red, moisture sensitive crystals. Both compounds crystallize monoclinic in the space group Pc (SeBr3[AlBr4]: a = 670.7(7) pm, b = 663.9(5) pm, c = 1 428.6(2) pm, β = 101.21(9)°, TeI3[AlI4]: a = 731.9(1) pm, b = 730.8(1) pm, c = 1 565.5(3) pm, β = 102.01(2)°). They are isotypic and have the SCl3[AlCl4] structure type. The structures are built of tetrahedral AlX4- ions and of pyramidal EX3+ ions (E = S, Se, Te; X = Cl, Br, I). The chalcogen atoms are additionally coordinated by halogen atoms of surrounding AlX4- ions, corresponding to a strongly distorted octahedral coordination EX3+3.
    Notes: Durch Reaktion von SeBr4 mit AlBr3 in einer geschlossenen Ampulle bei 150°C entsteht SeBr3[AlBr4] in Form gelber, hydrolyseempfindlicher Kristalle in quantitativer Ausbeute. Aus Te, AlI3 und zwei Äquivalenten I2 entsteht unter gleichen Bedingungen TeI3[AlI4] in Form dunkelroter, ebenfalls hydrolyseempfindlicher Kristalle. Beide Verbindungen kristallisieren monoklin, Raumgruppe Pc (SeBr3[AlBr4]: a = 670,7(7) pm, b = 663,9(5) pm, c = 1 428,6(2) pm, β = 101,21(9)°, TeI3[AlI4]: a = 731,9(1) pm, b = 730,8(1) pm, c = 1 565,5(3) pm, β = 102,01(2)°). Sie sind isotyp zu SCl3[AlCl4]. Die Strukturen sind aus tetraedrischen AlX4--Ionen und aus pyramidalen EX3+-Ionen (E = S, Se, Te; X = Cl, Br, I) aufgebaut. Das Chalkogen ist dabei von Halogenatomen benachbarter AlX4--Ionen zusätzlich so koordiniert, daß es eine stark verzerrte oktaedrische EX3+3-Koordination aufweist.
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    Die Kristallstruktur von KPdMIVF7 (MIV = Zr, Hf) (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1047-1052 
    Details
    ISSN: 0044-2313
    Keywords: Zirconium fluoride ; hafnium fluoride ; ternary fluorides ; KPdMIVF7 (MIV = Zr, Hf) ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of KPdMIVF7 (MIV = Zr, Hf)Blue single crystals of KPdZrF7 are obtained by heating the binary fluorides in sealed Pt-tubes under dry argon (solid state reaction, T ≍ 720°C, t ≍ 14 d). The compound crystallizes orthorhombically in the space group Pnna-D2h6 (Nr. 52); lattice parameters are a = 1 132.3(5) pm, b = 797.5(2) pm, c = 639.8(1) pm; Z = 4 (Four cycle diffractometer data, AED2). According to [F4PdF2/1ZrF5] distortet [PdF6]-octaedra are connected with pentagonal-bipyramidal [ZrF7]-polyhedra via two bridging F-, resulting in [PdZrF11]-groups. These [PdZrF11]-groups built up a threedimensional-network with K+ in its spacings. KPdHfF7 crystallizes isotypically (a = 1 136.1(3) pm, b = 796.4(2) pm und c = 638.8(1) pm; four cycle diffractometer data, AED2).
    Notes: Durch Tempern der binären Fluoride im verschweißten Pt-Rohr unter Schutzgas (Ar, Festkörperreaktion, T ≍ 720°C, t ≍ 14d) erhält man blaue Einkristalle von KPdZrF7 [eigener Strukturtyp, orthorhombisch, Pnna-D2h6 (Nr. 52); a = 1 132,3(5) pm, b = 797,5(2) pm, c = 639,8(1) pm; Z = 4; Vierkreisdiffraktometerdaten AED2]. Pd2+ ist verzerrt oktaedrisch von 6 F- umgeben, wohingegen Zr4+ pentagonalbipyramidal von 7 F- koordiniert wird. Beide Koordinationspolyeder sind gemäß [F4PdF2/1ZrF5] kantenverknüpft und bilden mit weiteren solcher [PdZrF11]-Einheiten durch Eckenverknüpfung ein dreidimensionales Raumnetz, in dessen Lücken K+ eingelagert ist. Nach Vierkreisdiffraktometerdaten (AED2) kristallisiert KPdHfF7 isotyp (a = 1 136,1(3) pm, b = 796,4(2) pm und c = 638,8(1) pm).
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956210626
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    The Crystal Structure of Pb8FeIIFe2IIIF24: an ordered Fluorite-like Compound (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1053-1057 
    Details
    ISSN: 0044-2313
    Keywords: Lead iron fluoride, Pb8FeIIFe2IIIF24 ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Kristallstruktur von Pb8FeIIFe2IIIF24: eine geordnete fluoritähnliche VerbindungPb8FeIIFe2IIIF24 ist triklin: a = 20,118(3) Å, b = 5,597(1) Å, c = 9,440(2) Å, α = 89,75(2)°, β = 105,79(2)° γ = 89,38(2)°, Z = 2, unkonventionelle Raumgruppe C1. Die Struktur wurde aus Einkristalldaten unter Verwendung von 1 641 unabhängigen Reflexen gelöst (R = 0,048, Rw = 0,051). Sie wird aus Paketen von zwei Untergittern entlang der a-Achse gebildet: fluoritähnlichen [Pb8F10]n6n+-Schichten und unendlichen, aus zwei Metallsorten gebildeten [FeIIFe2IIIF14]n6n- -Doppelketten von eckenverknüpften Oktaedern entlang der b-Achse.
    Notes: Pb8FeIIFe2IIIF24 is triclinic: a = 20.118(3) Å, b = 5.597(1) Å, c = 9.440(2) Å, α = 89.75(2)°, β = 105.79(2)°, α = 89.38(2)°, Z = 2. The structure is solved in the unconventional space group C1, from X-ray single crystal data using 1 641 independent reflections (R = 0.048, Rw = 0.051). It is built up from the stacking of two subnetworks along the a axis: fluorite-like [Pb8F10]n6n+ layers and infinite dimetallic [FeIIFe2IIIF14]n6n- double-chains of corner-sharing octahedra running along the b axis.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956210627
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    Die Verbindung Natriumphenolat · 2 Phenol im binären System ihrer Komponenten (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1058-1062 
    Details
    ISSN: 0044-2313
    Keywords: Sodium phenoxide · 2 phenol ; crystal structure ; system sodium phenoxide/phenol ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Compound Sodium Phenoxide · 2 Phenol in the System of its ComponentsIn the whole system of sodiumphenoxide/phenol the substance sodium phenoxide · 2 phenol is found to be the only compound between the two components. Single crystalls could be obtained by using the growing method according to Bridgman-Stockbarger.The crystal structure of PhONa · 2PhOH contains two different chains. In both of them sodium is coordinated in form of a distorted tetrahedron; in the first one by 4 oxygen, in the second one by 3 oxygen atoms and a phenoxid molecule, which is linked to sodium via its π-electrons. In the result of this realizations conclusions concerning the Kolbe-Schmitt-Synthesis are possible.
    Notes: Die Phase Natriumphenolat · 2 Phenol stellt im gesamten System Natriumphenolat/Phenol die einzige Verbindungsbildung der beiden Komponenten dar. Das Bridgman-Stockbarger-Verfahren führte zur erfolgreichen Züchtung von Kristallen.Die Kristallstruktur der Substanz setzt sich aus zwei verschiedenen Ketten zusammen. In beiden ist Natrium verzerrt tetraedrisch koordiniert; zum einen durch 4 Sauerstoffe, zum anderen durch 3 Sauerstoffe und einen Phenylring, mit dessen π-Elektronensystem das Metallatom in einer bindenden Wechselwirkung steht. Die Kenntnis der Struktur ermöglicht Aussagen hinsichtlich der Kolbe-Schmitt-Synthese.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956210628
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  • 80
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    Ba5[CrN4]N: Das erste Nitridochromat(V) (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 511-515 
    Details
    ISSN: 0044-2313
    Keywords: Nitridochromate(V) ; preparation ; crystal structure ; magnetic properties ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ba5[CrN4]N: The First Nitridochromate(V)Ba5[CrN4]N is prepared by reaction of mixtures of Li3N, Ba3N2 and CrN/Cr2N (1 : 1) (molar ratio Li : Ba : Cr = 3 : 5 : 1) in tantalum crucibles at 700°C with flowing nitrogen (1 atm) within a period of 48 h. After cooling down to room temperature (60°C/h) black-shining single crystals of the ternary phase with a platy habit are obtained (monoclinic, C2/m; a = 1054.0(2) pm, b = 1170.9(3) pm, c = 937.7(2) pm, b̃ = 110,79(2)°; Z = 4). The crystal structure contains isolated complex anions [CrVN4]7- which nearly satisfy the ideal tetrahedral symmetry (Cr—N [pm]: 2 × 175.3(4), 2 × 175.8(5); N—Cr—N [°]: 106.8(2), 109.5(2), 2 × 109.9(2), 2 × 110,3(2)). The coordination sphere for each of the terminal nitride functions of the complex anions is completed by five neighbouring Ba2+ ions (distorted CrBa5 octahedra). The octahedra are connected via common CrBa2 faces as well as CrBa edges thereby forming condensed tetrameric octahedral groups. The isolated nitride ions which are also present in the crystal structure of Ba5[CrN4]N are in an octahedral environment of Ba2+ ions.The presence of a d1-System (Cr(V)) is confirmed by magnetic susceptibility data.
    Notes: Ba5[CrN4]N wird durch Umsetzung von Mischungen aus Li3N, Ba3N2 und CrN/Cr2N (1 : 1) im molaren Verhältnis Li: Ba: Cr = 3 : 5 : 1 bei 700°C im Tantaltiegel unter strömendem Sticksktoff (1 atm) dargestellt. Die Reaktionszeit beträgt 48 h. Nach Abkühlen auf Raumtemperatur (60°C/h) liegt die ternäre Phase in Form schwarz-glänzender Kristalle mit plattigem Habitus vor (monoklin, C2/m; a = 1054,0(2) pm, b = 1170,9(3) pm, c = 937,7(2) pm, b̃ = 110,79(2)°; Z = 4). Die Kristallstruktur enthält isolierte komplexe Anionen [CrVN4]7- mit nahezu idealer Tetraedersymmetrie (Cr—N [pm]: 2 × 175,3(4), 2 × 175,8(5); N—Cr—N [°]: 106,8(2), 109,5(2), 2 × 109,9(2), 2 × 110,3(2)). Die Koordinationssphäre der terminalen Nitrid-Funktionen der komplexen Anionen wird durch je fünf benachbarte Ba-Ionen zu verzerrten CrBa5-Oktaedern vervollständigt. Je zwei dieser Oktaeder sind über gemeinsame CrBa2-Flächen zu dimeren Einheiten verknüpft, die über gemeinsame CrBa-Kanten zu tetrameren Oktaedergruppierungen kondensiert sind. Die in der Kristallstruktur von Ba5[CrN4]N zusätzlich enthaltenen, isolierten Nitridionen sind oktaedrisch von Barium umgeben.Das Vorliegen eines d1-Systems (Cr(V)) wird durch Messungen der magnetischen Suszeptibilität belegt.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956210402
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    LiBC  -  ein vollständig interkalierter HeterographitProfessor Heinrich Oppermann zum 60. Geburtstag gewidmet (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1153-1159 
    Details
    ISSN: 0044-2313
    Keywords: Alkali metal boride carbide ; intercalated heterographite ; crystal structure ; electron density ; physical properties ; topochemical reactions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: LiBC  -  A Completely Intercalated HeterographiteLiBC is a new compound composed only from light main group elements. LiBC is synthesized from the elements in sealed niobium ampoules at 770 K, and short annealing at 1 770 K, forming hexagonal platelets with golden lustre. According to Li+(BC)-, boron and carbon form planar hetero graphite layers of the isoelectronic hexagonal boron nitride type. The inter-layer regions are completely filled by lithium (P63/mmc; a = 275.2 pm; c = 705.8 pm; hP6; ZrBeSi type). The deformation density of the valence electrons prove the π character of the B—C bonds, as well as a polarization according to (BC-). Chemical and physical properties indicate a certain range of homogeneity x(Li) ≤ 1. The thermal decomposition and chemical reactions lead to BC products not yet characterized. The oxidation of LiBC obviously runs by a mechanism similar to that of graphite.
    Notes: LiBC ist eine neue, nur aus den leichten Elementen der Hauptgruppen bestehende Verbindung. Sie entsteht aus den Elementen in verschweißten Niobampullen bei 770 K und anschließendem kurzzeitigen Tempern bei 1 770 K in Form goldglänzender, hexagonaler Plättchen. Entsprechend Li+(BN)- bilden Bor und Kohlenstoff ebene Heterographitschichten vom Typ des isoelektronischen hexagonalen Bornitrids. Die Bereiche zwischen den Schichten sind durch Lithium vollständig aufgefüllt (P63/mmc; a = 275.2 pm; c = 705.8 pm; hP6; ZrBeSi-Typ). Die Deformationsdichte der Valenzelektronen beweist für die B—C-Bindungen π-Charakter und Polarisierung entsprechend (BC-). Nach chemischen und physikalischen Eigenschaften zeigt LiBC eine gewisse Phasenbreite x(Li) ≤ 1. Beim thermischen Abbau und bei chemischen Reaktionen entstehen bisher noch nicht charakterisierte BC-Produkte. Die Oxidation von LiBC verläuft offenbar nach einem ähnlichen Mechanismus wie bei Graphit.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956210707
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    Arsenidostannate mit Arsen-analogen [SnAs]-Schichten: Darstellung und Struktur von Na[Sn2As2], Na0,3Ca0,7[Sn2As2], Na0,6Sr0,6[Sn2As2], Na0,6Ba0,4[Sn2As2] und K0,3Sr0,7[Sn2As2] (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 576-582 
    Details
    ISSN: 0044-2313
    Keywords: Arsenidostannates ; alkali - alkaline earth substitution ; [SnAs] nets isostructural grey arsenic ; crystal structure ; Zintl phases ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Arsenidostannates with [SnAs] Nets Isostructural to Grey Arsenic: Synthesis and Crystal Structure of Na[Sn2As2], Na0.3Ca0.7[Sn2As2], Na0.4Sr0.6[Sn2As2], Na0.6Ba0.4[Sn2As2], and K0.3Sr0.7[Sn2As2]The metallic lustrous compounds Na[Sn2As2], Na0.3Ca0.7[Sn2As2], Na0.4Sr0.6[Sn2As2], Na0.6Ba0.4[Sn2As2] and K0.3Sr0.7[Sn2As2] were prepared from melts of mixtures of the elements. The compounds crystallize in the trigonal system (space group R3m, No. 166, Z = 3) with lattice constants see in “Inhaltsübersicht”. The structures are isotypic to Sr[Sn2As2] containing puckered ∞2[SnAs] nets which are stacked with a sequence of six layers. The E(I)/E(II) atoms are located between each second ∞2[SnAs] layer in trigonal antiprismatic interstices formed by As atoms. In the resulting ∞2[Sn2As2] double layers the ∞2[SnAs] nets are stacked in such a way that additional Sn - Sn contacts arise.
    Notes: Die metallisch glänzenden Verbindungen Na[Sn2As2], Na0,3Ca0,7[Sn2As2], Na0,4Sr0,6[Sn2As2], Na0,6Ba0,4[Sn2As2] und K0,3Sr0,7[Sn2As2] wurden aus Schmelzreaktionen, ausgehend von Gemengen der Elemente erhalten. Die Verbindungen kristallisieren trigonal, Raumgruppe R3m (Nr. 166), Z = 3, mit den Gitterkonstanten (pm): TextNa[Sn2As2]a = 400,6(2)c = 2758,1(5)c/a = 6,885Na0,3Ca0,7[Sn2As2]a = 410,1(2)c = 2648,6(5)c/a = 6,458Na0,4Sr0,6[Sn2As2]a = 411,7(2)c = 2718,5(5)c/a = 6,603Na0,6Ba0,4[Sn2As2]a = 409,2(2)c = 2793,4(5)c/a = 6,826K0,3Sr0,7[Sn2As2]a = 417,6(2)c = 2714,6(5)c/a = 6,500 - In den im Sr[Sn2As2]-Typ kristallisierenden Verbindungen sind zum grauen Arsen isostrukturelle ∞1[SnAs]-Netze ausgebildet, die senkrecht zur c-Achse eine Sechserschichtfolge aufweisen. Jeder zweite ∞1[SnAs]-Schichtzwischenraum ist von E(I)/E(II)-Atomen in trigonal antiprismatischen Lücken aus As-Atomen belegt. In den resultierenden ∞2[Sn2As2]-Doppelschichtpaketen sind die benachbarten ∞2[SnAs]-Netze so zueinander orientiert, daß relativ kurze Sn - Sn-Kontake ausgebildet werden.
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    URL: http://dx.doi.org/10.1002/zaac.19956210415
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    Zirconiumphthalocyanine: Darstellung und Eigenschaften chloridhaltiger Phthalocyanine des drei- und vierwertigen Zirconiums; Kristallstruktur von cis-Di(triphenylphosphin)iminium-tri(chloro)phthalocyaninato(2-)zirconat(IV)-di(dichlormethan) (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 607-616 
    Details
    ISSN: 0044-2313
    Keywords: Phthalocyanines ; zirconium complexes ; cyclovoltammetry ; optical spectra ; vibrational spectra ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zirconiumphthalocyanines: Synthesis and Properties of Chloride Ligated Phthalocyanines of Ter- and Quadrivalent Zirconium; Crystal Structure of cis-Di(triphenylphosphine)iminium-tri(chloro)phthalocyaninato(2-)zirconate(IV)-di(dichloromethane)cis-Di(chloro)phthalocyaninato(2-)zirconium(IV) is obtained by the reaction of ZrCl4 with phthalodinitrile in 1-chloronaphthaline at 230°C. It reacts with molten di(triphenylphosphine)iminiumchloride ((PNP)Cl) yielding cis-di(triphenylphosphine)iminium-tri(chloro)phthalocyaninato(2-)zirconate(IV), cis-(PNP)[ZrCl3Pc2-]. This crystallizes with two molecules of dichloromethane in the monoclinic space group P21/n with the lattice constants a = 15.219(4) Å, b = 20.262(10) Å, c = 20.719(4) Å, b̃ = 93.46(2)°, Z = 4. The seven coordinated Zr atom is situated in a “square base-trigonal cap” polyhedron. The plane of the three chlorine atoms runs parallel to the plane of the four isoindole nitrogen atoms Niso. The Zr-Cl distances range from 2.49 to 2.55 Å, the Zr—Niso distances from 2.26 to 2.29 Å. Due to ion packing effects the Pc2- ligand shows an asymmetrical convex distortion. The PNP cation adopts the bent conformation. The P—N—P angle is 139°, the P—N distance 1.58 Å. As confirmed by the cyclovoltammograms cis-(PNP)[ZrCl3Pc2-] is oxidized (anodically or chemically by Cl2) to yield cis-tri(chloro)phthalocyaninato(1-)zirconium(IV) and reduced (cathodically or chemically by [BH4]-) yielding chlorophthalocyaninato(2-)zirconium(III) and cis-di(triphenylphosphine)iminium-di(chloro)phthalocyaninato(2-)zirconate(III). The optical spectra show the typical π-π*-transitions of the Pc2- resp. Pc- ligand not much affected by the different states of oxidation and coordination of zirconium. The same is true for the vibrational spectra of the Pc2- resp. Pc- ligand. In the f.i.r. spectra between 350 and 150 cm-1 the asym. and sym. Zr—Cl stretching and Cl—Zr—Cl deformation vibration as well as the asym. Zr—N stretching vibration of the [ZrClxN4] skeleton (x = 1-3) is assigned.
    Notes: cis-Di(chloro)phthalocyaninato(2-)zirconium(IV) bildet sich bei der Reaktion von ZrCl4 mit Phthalodinitril in 1-Chlornaphthalin bei 230°C. Es reagiert mit geschmolzenem Di(triphenylphosphin)iminiumchlorid ((PNP)Cl) zu cis-Di(triphenylphosphin)iminium-tri(chloro)phthalocyaninato(2-)-zirconat(IV), cis-(PNP)[ZrCl3Pc2-]. Dieses kristallisiert mit zwei Solvatmolekülen Dichlormethan in der monoklinen Raumgruppe P21/n mit den Gitterkonstanten a = 15.219(4) Å, b = 20,262(10) Å, c = 20,719(4) Å, b̃ = 93,46(2)°, Z = 4. Das siebenfach koordinierte Zr-Atom befindet sich in einem nach Art eines „square base-trigonal cap“ aufgespannten Koordinationspolyeder. Die Ebene der drei Chlor-Atome verläuft parallel zur Ebene der vier Isoindol-N-Atome (Niso). Die (Zr—Cl)-Abstände variieren zwischen 2,49 und 2,55 Å, die (Zr—Niso)-Abstände zwischen 2,26 und 2,29 Å. Aufgrund von Ionenpackungseffekten ist der Pc2--Ligand unsymmetrisch konvex verzerrt. Das (PNP)-Kation liegt in der gewinkelten Konformation vor. Der (P—N—P)-Winkel beträgt 139°, der (P—N)-Abstand 1,58 Å. In Übereinstimmung mit den Cyclovoltammogrammen bildet sich aus cis-(PNP)[ZrCl3Pc2-] durch anodische oder chemische (mit Cl2) Oxydation cis-Tri(chloro)phthalocyaninato(1-)zirconium(IV) und durch kathodische oder chemische (mit [BH4]-) Reduktion Chlorophthalocyaninato(2-)zirconium(III) und cis-Di(triphenylphosphin)iminium-di(chloro)-phthalocyaninato(2-)zirconat(III). Die optischen Spektren zeigen die typischen π-π*-Übergänge des Pc2--bzw. Pc--Liganden. Die verschiedenen Oxydations- und Koordinationszustände des Zirconiums üben hierauf keinen großen Einfluß aus. Dieses gilt auch für die Schwingungsspektren des Pc2-- bzw. Pc--Liganden. In den FIR-Spektren werden zwischen 350 und 150 cm-1 für das [ZrClxN4]-Gerüst (x = 1-3) die asym. und sym. (Zr—Cl)-Valenz- und (Cl—Zr—Cl)-Deformationsschwingung sowie die asym. (Zr—N)-Valenzschwingung zugeordnet.
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    Neue phosphidoverbrückte Mehrkernkomplexe des Ag und Zn. Die Kristallstrukturen von [Ag3(PPh2)3(PnBu2tBu)3], [Ag4(PPh2)4(PR3)4] (PR3 = PMenPr2, PnPr3), [Ag4(PPh2)4(PEt3)4]n, [Zn4(PPh2)4Cl4(PRR2)2] (PRR′2 = PMenPr2, PnBu3, PEt2Ph), [Zn4(PhPSiMe3)4Cl4(C4H8O)2] und [Zn4(PtBu2)4Cl4] (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1681-1688 
    Details
    ISSN: 0044-2313
    Keywords: Mulinuclear phosphido-bridged Ag- and Zn-complexes ; Ag—P-rings ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Phosphido-bridged Multinuclear Complexes of Ag and Zn. The Crystal Structures of [Ag3(PPh2)3(PnBu2tBu)3], [Ag4(PPh2)4(PR3)4] (PR3 = PMenPr2, PnPr3), [Ag4(PPh2)4(PEt3)4]n, [Zn4(PPh2)4Cl4(PRR′2)2] (PRR′2 = PMenPr2, PnBu3, PEt2Ph), [Zn4(PhPSiMe3)4Cl4(C4H8O)2] and [Zn4(PtBu2)4Cl4]AgCl reacts with Ph2PSiMe3 in the presence of tertiary Phosphines (PnBu2tBu, PMenPr2, PnPr3 and PEt3) to form the multinuclear complexes [Ag3(PPh2)3(PnBu2tBu)3] 1, [Ag4(PPh2)4(PR3)4] (PR3 = PMenPr2 2, PnPr3 3) and [Ag4(PPh2)4(PEt3)4]n 4. In analogy to that ZnCl2 reacts with Ph2PSiMe3 and PRR′2 to form the multinuclear complexes [Zn4(PPh2)4Cl4(PRR′2)2] (PRR′2 = PMenPr2 5, PnBu3 6, PEt2Ph 7). Further it was possible to obtain the compounds [Zn4(PhPSiMe3)4Cl4(C4H8O)2] 8 and [Zn4(PtBu2)4Cl4] 9 by reaction of ZnCl2 with PhP(SiMe3)2 and tBu2PSiMe3, respectively. The structures were characterized by X-ray single crystal structure analysis. Crystallographic data see “Inhaltsübersicht”.
    Notes: AgCl reagiert mit Ph2PSiMe3 in Gegenwart der tertiären Phosphane PnBu2tBu, PMenPr2, PnPr3 und PEt3 unter Bildung mehrkerniger Komplexe. Abhängig vom tertiären Phosphan erhält man dabei folgende Verbindungen: [Ag3(PPh2)3(PnBu2tBu)3] 1, [Ag4(PPh2)4(PR3)4] (PR3 = PMenPr2 2, PnPr3 3) und [Ag4(PPh2)4(PEt3)4]n 4. Analog hierzu reagiert ZnCl2 mit Ph2PSiMe3 und PRR′2 zu den Mehrkernkomplexen [Zn4(PPh2)4Cl4(PRR′2)2] (PRR′2 = PMenPr2 5, PnBu3 6, PEt2Ph 7). Ferner konnten durch Umsetzung von ZnCl2 mit PhP(SiMe3)2 bzw. tBu2PSiMe3 die Verbindungen [Zn4(PhPSiMe3)4Cl4(C4H8O)2] 8 und [Zn4(PtBu2)4Cl4] 9 erhalten werden. Die Strukturen von 1-9 konnten durch Kristallstrukturanalysen aufgeklärt werden.(1: Raumgruppe P1 (Nr. 2), a = 1 245,8(6) pm, b = 1 662,0(8) pm, c = 2 159,2(12) pm, α = 77,01(3)°, β = 81,59(3)°, γ = 69,07(3)°, 2: Raumgruppe P21/n (Nr. 14), a = 1 283,7(8) pm, b = 2 102,8(13) pm, c = 1 481,7(9) pm, β = 104,31(5)°, 3: Raumgruppe C2/c (Nr. 15), a = 2 925,4(12) pm, b = 1 297,0(6) pm, c = 2 426,5(9) pm, β = 100,00(3)°, 4: Raumgruppe P1 (Nr. 2), a = 1 046,0(5) pm, b = 1 086,1(7) pm, c = 1 733,0(12) pm, α = 71,76(5)°, β = 88,57(5)°, γ = 87,22(5)°, 5: Raumgruppe I2/a (Nr. 15), a = 2 435,2(9) pm, b = 1 908,3(8) pm, c = 3 534,3(16) pm, β = 97,04(3)°, 6: Raumgruppe C2/c (Nr. 15), a = 2 261,6(15) pm, b = 1 888,9(10) pm, c = 1 810,2(13) pm, β = 108,79(4)°, 7: Raumgruppe P1 (Nr. 2), a = 1 495,9(3) pm, b = 2 005,0(3) pm, c = 2 921,5(9) pm, α = 107,80(2)°, β = 92,36(2)°, γ = 103,99(1)°, 8: Raumgruppe P21/n (Nr. 14), a = 910,2(3) pm, b = 2 568,2(6) pm, c = 1 293,5(6) pm, β = 98,42(3)°, 9: Raumgruppe P21/n (Nr. 14), a = 1 227,3(6) pm, b = 1 205,3(9) pm, c = 1 584,5(7) pm, β = 109,32(3)°).
    Additional Material: 8 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956211012
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    Darstellung, Kristallstruktur und Eigenschaften von Kaliumhydrogencyanamid (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1703-1707 
    Details
    ISSN: 0044-2313
    Keywords: Potassium hydrogen cyanamide ; synthesis ; crystal structure ; IR-spectroscopy ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation, Crystal Structure, and Properties of Potassium Hydrogen CyanamideFor the preparation of KHCN2 melamine has been reacted with potassium amide in liquid ammonia. After evaporation of the solvent the resulting solid has been transformed at 210°C. KHCN2 (P212121, a = 708.7(2), b = 909.0(2), c = 901.4(2) pm, Z = 8, R = 0.039, wR = 0.016) is yielded as a coarse crystalline product. In the solid K+ and HCN2- ions occur. As expected two significantly differing bond-distances C—N (117.3(5) pm) and HN—C (128.7(5) pm) have been found in the anion. According to IR-spectroscopy a non linear group N—C—N (174.4(4)°) is observed.
    Notes: Zur Darstellung von KHCN2 wurde Melamin mit Kaliumamid in flüssigem Ammoniak umgesetzt und der nach Verdampfen des Lösungsmittels verbleibende Feststoff bei 210°C zur Reaktion gebracht. KHCN2 (P212121, a = 708,7(2), b = 909,0(2), c = 901,4(2) pm, Z = 8, R = 0,039, wR = 0,016) entsteht dabei grobkristallin. Im Festkörper findet man K+ - und HCN2--Ionen. Erwartungsgemäß liegen zwei signifikant unterschiedliche Bindungslängen C—N (117,3(5) pm) und HN—C (128,7(5) pm) im Anion vor. In Übereinstimmung mit IR-spektroskopischen Befunden ist die Gruppierung N—C—N nicht linear (174,4(4)°).
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956211015
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    Zur Thermochemie und Struktur von Berylliumchlorid (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1723-1726 
    Details
    ISSN: 0044-2313
    Keywords: Beryllium dichloride ; dimorphy ; enthalpy ; entropy ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Thermochemistry and Structure of Beryllium ChlorideBeCl2 is dimorphous, with a transition point at 405°C. The transition enthalpy and transition entropy have been determined by solution calorimetry: ΔUH° = 2.9 kJmol-1 and ΔUS° = 9.7 JK-1mol-1.The previously known SiS2-type structure of BeCl2 is that of the high temperature phase. The structure of the phase stable at room temperature has been determined from single crystal data. a = 1 062.4(6) pm, c = 1 804(2) pm, I41/acd, Z = 32, R = 0.038 (Mg(NH2)2-type). The structure consists of P4O10-like [Be4Cl6Cl4/2]-units, connected by their terminal anions.
    Notes: BeCl2 ist dimorph, die Umwandlungstemperatur liegt bei 405°C. Aus lösungskalorimetrischen Messungen ergibt sich als Differenz der Lösungsenthalpien eine Umwandlungsenthalpie von ΔUH° = 2,9 kJmol-1 und eine Umwandlungsentropie ΔUS298° = 9,7 JK-1 mol-1.Die bislang bekannte Struktur im SiS2-Typ ist die der Hochtemperaturphase. Die Struktur von bei Raumtemperatur stabilem T-BeCl2 wurde aus Einkristalldaten bestimmt. a = 1 062,4(6) pm, c = 1 804(2) pm, I41/acd, Z = 32, R = 0,038 (Mg(NH2)2-Typ). Es liegen (Be4Cl6Cl4/2)-Einheiten vor, die dem Bauprinzip von P4O10 entsprechen, aber über ihre terminalen Chlorid-Ionen verknüpft sind.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956211018
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  • 87
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    InIII-Phthalocyanine: Darstellung, Eigenschaften und Kristallstruktur von Tetra(n-butyl)ammonium-cis-di(nitrito-O,O′)phthalocyaninato(2-)indat(III) (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1708-1714 
    Details
    ISSN: 0044-2313
    Keywords: Indium(III) phthalocyanines, nitrito-O,O′ complexes ; cyclic voltammetry ; optical spectra ; vibrational spectra ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: InIII-Phthalocyanines: Synthesis, Properties, and Crystal Structure of Tetra(n-butyl)ammonium-cis-di(nitrito-O,O')phthalocyaninato(2-)indate(III)[In(Cl)Pc2-] reacts with (nBu4N)NO2 in acetone yielding green-blue (nBu4N)cis[In(NO2)2Pc2-], which crystallizes in the monoclinic space group P21/n (No. 14). Both nitrite anions are coordinated as chelating nitrito-O,O'(NO2) ligands to InIII in cis-geometry. Consequently InIII is octa-coordinated within a distorted “quadratic” antiprism and directed towards the Pc2--ligand. One of the NO2 ligands has equivalent N—O bonds similar to free nitrite, while the other has asymmetric N—O bonds. Both (In,O,N,O) rings are approximately planar with a dihedral angle of 80°. The Pc2- ligand is distorted in an asymmetrically convex manner. Partially overlapping pairs of Pc2- ligands related by an inversion center form double layers, which are separated by layers containing the (nBu4N)+ cations. The cyclic voltammogram shows three electrode processes, which are assigned to the redox pairs: Pc3-/Pc2- (-0.94 V) 〈 InI/InIII (-0.78 V) 〈 Pc2-/Pc- (0.64 V). The UV-VIS-NIR spectra and vibrational spectra are discussed.
    Notes: [In(Cl)Pc2-] bildet mit (nBu4N)NO2 in Aceton grün-blaues (nBu4N)cis[In(NO2)2Pc2-], welches monoklin kristallisiert (RG.: P21/n (14)). Die Nitrit-Anionen sind als chelatbildende Nitrito-O,O′ (NO2)-Liganden an InIII in cis-Koordination gebunden. Infolgedessen ist InIII oktakoordiniert und befindet sich in einem verzerrten “quadratischen” Antiprisma auf der dem Pc2--Liganden zugewandten Seite. Einer der (NO2)-Liganden hat ähnlich wie freies Nitrit äquivalente N—O-Bindungen, der andere nichtäquivalente. Beide (In,O,N,O)-Ringe sind nahezu planar (Diederwinkel: 80°). Der Pc2--Ligand ist unsymmetrisch konvex verzerrt. Partiell überlappende Paare einander zugewandter Pc2--Liganden bilden von den (NO2)-Liganden begrenzte Doppelschichten, die von den die (nBu4N)+-Kationen enthaltenden Schichten getrennt sind. Das Zyklovoltammogramm von cis[In(NO2)2Pc2-]- zeigt drei Elektrodenprozesse, die den Redoxpaaren: Pc3-/Pc2- (-0,94 V) 〈 InI/InIII (-0,78 V) 〈 Pc2-/Pc- (0,64 V) zugeordnet werden. Die UV-VIS-NIR- und Schwingungsspektren werden diskutiert.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956211016
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    Lithiumphthalocyanine: Synthese, Eigenschaften und Kristallstruktur von Bis(triphenylphosphin)iminiumphthalocyaninatolithaten mit verschiedenen Konformationen des Kations (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1715-1722 
    Details
    ISSN: 0044-2313
    Keywords: Phthalocyanines ; lithium complex ; crystal structure ; cyclic voltammetry ; UV-VIS-NIR spectra ; vibrational spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Lithiumphthalocyanines: Synthesis, Properties, and Crystal Structure of Bis(triphenylphosphine)iminiumphthalocyaninatolithates with Different Conformations of the CationReaction of tri(n-dodecyl)n-butylammoniumphthalocyaninatolithate, (TDBA)[LiPc2-] with bis(triphenylphosphin)iminiumbromide, (PNP)Br in dichloromethane yields (PNP)[LiPc2-]. It crystallizes in the triclinic space group P1 as dichloromethane solvate (1) and in the monoclinic space group P21/n as hydrate (2). The crystal structures of (1) and (2) are reported. Each salt contains two crystallographically slightly different discrete [LiPc2-]- anions, in which the square-planar coordinated Li+ cation is centered within the planar Pc2- ligand (Dav.(Li—Niso) = 1.945 Å). There are three different conformations for the (PNP) cation: (1) only contains the bent conformer (dav.(P—N) = 1.575 Å; ϕ(P—N—P) = 140.8°), while in (2) an hybrid (dav.(P—N) = 1.562 Å; ϕ(P—N—P) = 158.1°) and the linear conformer (dav.(P—N) = 1.547 Å; ϕ(P—N—P) = 176.8°) are present. The very soluble, blue-green salts melt at 265°C without decomposition. In accordance with cyclovoltammetric data thin films of (PNP)[LiPc2-] are oxidized by NO2 or Br2 to yield brown violet [LiPc-]. The electronic absorption spectra and the vibrational spectra are discussed.
    Notes: Tri(n-dodecyl)n-butylammoniumphthalo-cyaninatolithat, (TDBA)[LiPc2-] bildet mit Bis(triphenylphosphin)iminiumbromid, (PNP)Br in Dichlormethan (PNP)[LiPc2-]. Dieses kristallisiert triklin (RG.:P1) als Dichlormethan-Solvat (1) und monoklin (RG.: P21/n) als Hydrat (2). Nach den Röntgenstrukturanalysen von (1) und (2) enthält jedes Salz zwei kristallographisch unterschiedliche, diskrete [LiPc2-]--Anionen, in denen sich das quadratisch-planar koordinierte Li+-Kation im Zentrum des ebenen Pc2--Liganden befindet (Dgem(Li—Niso) = 1,945 Å). Das (PNP)-Kation tritt in drei verschiedenen Konformationen auf: (1) enthält nur das gewinkelte Konformer (dgem(P—N) = 1,575 Å; ϕ(P—N—P) = 140,8°), (2) dagegen neben dem linearen (dgem(P—N) = 1,547 Å; ω(P—N—P) = 176,8°) ein Hybrid-Konformer (dgem(P—N) = 1,562 Å; ϕ(P—N—P) = 158,1°). Die löslichen, blaugrünen Komplexsalze schmelzen unzersetzt bei 265°C. Dünnfilme von (PNP)[LiPc2-] werden in Übereinstimmung mit cyclovoltammetrischen Daten durch NO2 oder Br2 zu braun-violettem [LiPc-] oxydiert. Die elektronischen Absorptions- und Schwingungsspektren werden diskutiert.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956211017
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    Die Kristallstrukturen von [Cu2Cl2(AA · H+)2](NO3)2 und [AA · H+]Pikr- (AA · H+ = Allylammonium; Pikr- = Pikrat) (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1741-1745 
    Details
    ISSN: 0044-2313
    Keywords: Bis(diallylammonium)dichlorocopper(I) nitrate ; allylammonium picrate ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structures of [Cu2Cl2(AA · H+)2](NO3)2 and [AA · H+]Picr- (AA · H+ = Allylammonium; Picr- = Picrat)By an alternating current electro synthesis the crystal-line π-complex [Cu2Cl2(AA · H+)2](NO3)2 has been obtained from CuCl2 · 2H2O, allylamine (AA), and HNO3 in ethanolic solution. X-ray structure analysis revealed that the compound crystallized in the monoclinic system, space group P21/a, a = 7.229(3), b = 7.824(3), c = 26.098(6) Å, γ = 94.46(5)°, Z = 4, R = 0.025 for 2 023 reflections. The crystal structure is built up of CunCln chains which are connected by π-bonding bidentate AA · H+ … ON(O)O … H+ · AA units. For comparision with the above complex the structure of [AA · H+]Picr- (Picr- = picrate anion) is also reported.
    Notes: Die elektrochemische Disproportionierung Cu2+ + Cu0 → Cu1+ im System CuCl2—Allylamin(AA)—HNO3—Ethanol ergibt den π-Komplex [Cu2Cl2(AA · H+)2](NO3)2, dessen Kristallstruktur röntgenographisch bestimmt wurde. Die Verbindung kristallisiert im monoklinen Kristallsystem, Raumgruppe P21/a, a = 7,229(3), b = 7,824(3), c = 26,098(6) Å, γ = 94,46(5)°, Z = 4, R = 0,025 für 2 023 Reflexe. Die Kristallstruktur besteht aus CunCln-Ketten, die durch π-bindende, zweizähnige AA · H+ … ON(O)O · H+ · AA-Einheiten verknüpft sind. Zum Vergleich wird auch über die Struktur von [AA · H+]Pikr- (Pikr- = Pikratanion) berichtet.
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    URL: http://dx.doi.org/10.1002/zaac.19956211022
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    The Preparation and X-Ray Structure of [AsPh4][Ph2P(S)NSiMe3] · 0.5 THFDedicated to Professor Herbert W. Roesky on the Occasion of his 60th Birthday (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1813-1817 
    Details
    ISSN: 0044-2313
    Keywords: [AsPh4][Ph2P(S)NSiMe3] · 0.5 THF ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Darstellung und Röntgen-Strukturbestimmung von [AsPh4][Ph2P(S)NSiMe3] · 0,5 THFDie Reaktion von Ph2P(S)N(SiMe3)2 mit Kalium-tert-butoxid im molaren Verhältnis 1:1 ergibt K[Ph2P(S)NSiMe3], das mit [AsPh4]Cl zum AsPh4+-Salz umgesetzt wird. Die Kristallstruktur von [AsPh4][Ph2P(S)NSiMe3] ·0,5 THF besteht aus AsPh4+ und Ph2P(S)NSiMe3- mit d(P—S) = 1,980(4) Å und d(P—N) = 1,555(8) Å. Der P—N—Si-Winkel im Anion beträgt 136,3(5)°. Der elektrophile Angriff von Ph2P(S)Cl erfolgt am Schwefel des Ph2P(S)NSiMe3-. Die Oxidation des Anions mit Iod ergibt ein Disulfid, das bei Umsetzung mit Kalium-tert-butoxid wieder K[Ph2P(S)NSiMe2] ergibt.
    Notes: The reaction of Ph2P(S)N(SiMe3)2 with potassium tert-butoxide in a 1:1 molar ratio produces K[Ph2P(S)NSiMe3], which was converted to the AsPh4+ salt by metathesis with [AsPh4]Cl. The X-ray crystal structure of [AsPh4][Ph2P(S)NSiMe3] · 0.5 THF consists of noninteracting AsPh4+ and Ph2P(S)NSiMe3- ions with d(P—S) = 1.980(4) Å and d(P—N) = 1.555(8) Å. The PNSi bite angle in the anion is 136.3(5)°. Electrophilic attack by Ph2P(S)Cl occurs at the sulfur atom of Ph2P(S)NSiMe3-. The oxidation of the anion with iodine produces a disulfide which regenerates K[Ph2P(S)NSiMe2] upon treatment with potassium tert-butoxide.
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    URL: http://dx.doi.org/10.1002/zaac.19956211102
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    Cis-/Trans-Isomerie bei Bis-(trisalkoxy)-hexavanadaten: cis-Na2[V6IVO7(OH)6{(OCH2)3CCH2OH}2] · 8 H2O, cis-(CN3H6)3[VIVV5VO13{(OCH2)3CCH2OH}2] · 4,5 H2O und trans-(CN3H6)2[V6VO13{(OCH2)3CCH2OH}2] · H2OProfessor Herbert W. Roesky zum 60. Geburtstag gewidmet (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1818-1831 
    Details
    ISSN: 0044-2313
    Keywords: Polyoxovanadates ; alkoxy hexavanadates ; bis-(trisalkoxy)-hexavanadates: UV/VIS ; IR ; ESR ; magnetic measurements ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Cis-/Trans-Isomerism of Bis-(trisalkoxy)-hexavanadates: cis-Na2[V6IVO7(OH)6{(OCH2)3CCH2OH}2] · 8 H2O, cis-(CN3H6)3[VIVV5VO13{(OCH2)3CCH2OH}2] · 4.5 H2O and trans-(CN3H6)2[V6VO13{(OCH2)3CCH2OH}2] · H2OPolyoxovanadates with distorted Lindquist-structure, in which six of the twelve μ2-oxygen atoms are formally replaced by the oxygen atoms of two coordinated pentaerythritol ligands, can be prepared by a simple method in an aqueous medium. The “fully reduced”, six-fold protonated compound cis-Na2[V6VO7(OH)6{(OCH2)3CCH2OH}2] · 8 H2O (1), the mixed valence species cis-(CN3H6)3[VIVV5VO13{(OCH2)3CCH2OH}2] · 4.5 H2O (2) containing one localized VIV centre and the “fully oxidized” compound trans-(CN3H6)2[V6VO13{(OCH2)3CCH2 · OH}2] · H2O (3) have been synthesized and characterized by UV/VIS-, IR- and EPR-spectroscopy, by magnetic measurements, cyclic voltammetry and by a single-crystal X-ray structure analysis.The organic {(CH2)3CCH2OH}3+-groups tend to cap the triangular faces formed by μ2-oxygen atoms of the central approximately octahedral {V6O19}-unit. Therefore the anions of bis-(trisalkoxy)-hexavanadates can exist in a trans-form as well as in an isomeric cis-form referring to a “basic” plane of four vanadium atoms of the {V6}-octahedron. The different relative positions of the ligands have a significant influence on the redox potentials of the compounds.For structural details see “Inhaltsübersicht”.
    Notes: Die beschriebenen Trisalkoxy-polyoxovanadate mit verzerrter Lindqvist-Struktur, in der sechs der zwölf μ2-verbrückenden Sauerstoffatome formal durch die Sauerstoffatome von zwei koordinierten Pentaerythritolliganden ((HOCH2)3CCH2OH) ersetzt wurden, können auf einfache Weise im wäßrigen Medium dargestellt werden. Durch UV/VIS-, IR- und ESR-Spektroskopie sowie durch magnetische Messungen, Cyclovoltammetrie und Röntgenstrukturanalyse wurden die „vollständig reduzierte“, sechsfach protonierte Verbindung cis-Na2[V6IVO7(OH)6{(OCH2)3CCH2OH}2] ·8 H2O (1), das gemischtvalente, ein lokalisiertes V(IV)-Zentrum enthaltende Derivat cis-(CN3H6)3[VIVV5VO13{(OCH2)3CCH2OH}2] · 4,5 H2O (2) sowie die „vollständig oxidierte“ Verbindung trans-(CN3H6)2[V6VO13{(OCH2)3CCH2OH}2] · H2O (3) charakterisiert.Da die organischen {(CH2)3CCH2OH}3+-Gruppen, formal betrachtet, die jeweils aus drei μ2-O-Atomen gebildeten Flächen der zentralen, angenähert oktaedrischen {V6O19}-Einheit überdachen, können die Anionen der Bis-(trisalkoxy)-hexavandate sowohl in einer trans-Form als auch in einer stellungsisomeren cis-Form bezüglich einer aus vier Vanadiumatomen des {V6}-Oktaeders gebildeten „Basis“-Ebene auftreten. Die unterschiedliche Anordnung der Liganden hat einen signifikanten Einfluß auf die Redoxpotentiale der Verbindungen.1: cis-Na2[VI6VO7(OH)6{(OCH2)3CCH2OH}2] · 8 H2O: Raumgruppe P1, a = 987,2(2) pm, b = 1 080,6(2) pm, c = 1 654,3(3) pm, α = 94,83(1)°, β = 98,73(2)°, γ = 116,05(1)°, V = 1,5443(5) nm3, Z = 2, R = 0,067 für 5 913 unabhängige Reflexe [F 〉 4σ(F)].2: cis-(CN3H6)3[VIVV5VO13{(OCH2)3CCH2OH}2] · 4,5 H2O: Raumgruppe Pbca, a = 1 569,5(3) pm, b = 1 652,3(3) pm, c = 2 758,2(6) pm, V = 7,153(2) nm3, Z = 8, R = 0,126 für 2 698 unabhängige Reflexe [F 〉 4σ(F)].3: trans-(CN3H6)2[V6VO13{(OCH2)3CCH2OH}2] · H2O: Raumgruppe C2/c, a = 2 293,4(3) pm, b = 1 102,6(2) pm, c = 1 368,6(2) pm, β = 120,87(1)°, V = 2,9705(8) nm3, Z = 4, R = 0,046 für 2 206 unabhängige Reflexe [F 〉 4σ(F)].
    Additional Material: 8 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956211103
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  • 92
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    Structural Studies on Dimethyltin(IV) CarboxylatesDedicated to Professor Herbert W. Roesky on the Occasion of his 60th Birthday (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1875-1882 
    Details
    ISSN: 0044-2313
    Keywords: Bis(acetato)dimethyltin(IV) ; bis(trifluoroacetato)dimethyltin(IV) ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Strukturuntersuchungen an Dimethylzinn(IV)-carboxylatenUm die 119Sn-Mössbauer-Parameter und Strukturdaten für Dimethylzinn(IV)-Derivate zu korrelieren, wurden die Molekülstrukturen von Bis(acetato)dimethylzinn(IV) und Bis(trifluoroacetato)dimethylzinn(IV) durch Einkristall-Röntgen-Strukturanalysen bestimmt. Me2Sn(OOCCH3)2: monoklin, a = 26,282(4), b = 5,282(1), c = 14,434(3) Å, β = 101,17(2)°, Z = 8, Raumgruppe C2/c; [Me2Sn(OOCCF3)2]n: monoklin, a = 8,444(1), b = 17,689(1), c = 15,368(1) Å, β = 93,013(9)°, Z = 8, Raumgruppe Cc. Die Strukturen wurden mit Patterson-Methoden gelöst und verfeinert nach dem full-matrix least-squares-Verfahren bis zu R = 0,025 bzw. 0,027 (Rw = 0,023 and 0,030) für 2 298 bzw. 4 182 Reflexe mit I ≥ 3σ(F2).
    Notes: In order to correlate 119Sn Mössbauer parameters and structural data for dimethyltin(IV) derivatives, the molecular structures of bis(acetato)dimethyltin(IV) and bis(trifluoroacetato)dimethyltin(IV) were determined by single crystal X-ray diffration. Crystals of Me2Sn(OOCCH3)2 are monoclinic, a = 26.282(4), b = 5.282(1), c = 14.434(3) Å, β = 101.17(2)°, Z = 8, space group C2/c, and those of [Me2Sn(OOCCF3)2]n are monoclinic, a = 8.444(1), b = 17.689(1), c = 15.368(1) Å, β = 93.013(9)°, Z = 8, space group Cc. The structures were solved by the Patterson method and were refined by full-matrix least-squares procedures to R = 0.025 and 0.027 (Rw = 0.023 and 0.030) for 2 298 and 4 182 reflections with I ≥ 3σ(F2), respectively.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956211109
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  • 93
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    Die Molekulare Zusammensetzung von erstarrten Phosphor-Schwefel-Schmelzen und die Kristallstruktur von β-P4S6Professor H. J. Seifert zum 65. Geburtstag gewidmet (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1637-1643 
    Details
    ISSN: 0044-2313
    Keywords: Phosphorus sulfides ; 31P NMR spectroscopy ; phosphorus sulfur melts ; tetra phosphorus hexasulfide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Molecular Composition of Solidified Phosphorus-Sulfur Melts and the Crystal Structure of β-P4S6Phosphorus sulfur melts were annealed for one week at 673 K and then quenched in ice water. The solids were dissolved in CS2 and the concentrations of phosphorus sulfides were determined by 31P NMR spectroscopy. Samples containing between 44 and 70 mol% sulfur dissolved completely in CS2. Between 0 and 42 mol% remains an insoluble residue of red phosphorus. Above 72 mol% it consisted of sulfur chains linked by phosphorus atoms. The solutions contained mainly the congruently melting compounds P4S3, P4S7, and P4S10 having maximum concentrations at their stoichiometric compositions. Other compounds P4Sn (n = 4-9) which decompose on heating, according to the phase diagram, were also found in surprisingly high concentrations. One of these was β-P4S6 which crystallizes in the monoclinic space group P21/c with the lattice parameters a = 702.4(2), b = 1 205.6(2), c = 1 148.9(6) pm and β = 103.4(2)°.Reaction of white phosphorus with sulfur was also investigated. In contrast to the results of previous authors, who described the system P4-S8 below 373 K as eutectic, we found that the elements reacted below this temperature.
    Notes: Phosphor-Schwefel-Schmelzen wurden eine Woche bei 673 K getempert und anschließend in Eiswasser abgeschreckt, dann in CS2 gelöst und die Konzentration der Phosphorsulfide mit Hilfe der 31P-NMR-Spektroskopie bestimmt. Proben mit Zusammensetzungen zwischen 44 und 70 Mol-% Schwefel lösten sich vollständig auf. Zwischen 0 und 42 Mol-% Schwefel traten als unlöslicher Rückstand roter Phosphor, oberhalb von 72 Mol-% Schwefel über Phosphoratome vernetzte Schwefelketten auf. Die löslichen Bestandteile waren hauptsächlich die kongruent schmelzenden Verbindungen P4S3, P4S7 und P4S10. Die maximalen Konzentrationen lagen bei den jeweiligen stöchiometrischen Zusammensetzungen. Andere P4Sn (n = 4-9) Verbindungen, deren Molekülkristalle sich beim Erwärmen peritektisch oder peritektoid zersetzen, wurden ebenfalls mit höheren Konzentrationen gefunden, dazu gehörte β-P4S6, das in der monoklinen Raumgruppe P21/c mit den Gitterkonstanten a = 702,4(2), b = 1 205,6(2), c = 1 148,9(6) pm und β = 103,4(2)° kristallisiert.Die Reaktion von weißem Phosphor mit Schwefel wurde ebenfalls untersucht. Im Gegensatz zu Angaben anderer Autoren, die das P4-S8-System unterhalb von 373 K als einfach eutektisch beschreiben, wurden in diesem Temperaturbereich Reaktionen zwischen den Komponenten beobachtet.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956211004
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  • 94
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    Synthese, Struktur und magnetische Eigenschaften von [CrCl(μ-Cl)(TMEDA)]2 (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 2061-2064 
    Details
    ISSN: 0044-2313
    Keywords: Chromium(II) chloride TMEDA complex ; crystal structure ; magnetism ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Structure, and Magnetic Properties of [CrCl(-μCl)(TMEDA)]2The title complex [CrCl(μ-Cl)(TMEDA)]2 (1) is obtained in an equimolar reaction of CrCl2(THF) with TMEDA in high yield. 1 crystallises in the monoclinic space group P21/c with a = 843.2(2), b = 1 109.(2), c = 1 147.4(3) pm, β = 102.99(2)° and Z = 2. The molecular structure of 1 contains two, slightly distorted quadratic pyramidal CrL5-subunits, which are linked via two unsymmetrical Cl-bridges. The μ-Cl-functions take the apical position of one and a basal position of the second CrL5-unit, wherein the apical Cr-Cl bond (277.6(1) pm) is destinctly longer than the basal Cr-Cl bond (240.6(1) pm). The terminal Cr-Cl bond is still shorter (237.5(1) pm). The Cr…Cr distance is far beyond any bonding interaction. This is confirmed by means of magnetic susceptibility measurements, which show four unpaired electrons per Cr centre; however, a small antiferromagnetic coupling of J/k = -7.3 K can be calculated. This coupling is suggested to be originated by a 90°-σ-superexchange via the asymmetric μ-Cl functions.
    Notes: Den Titelkomplex [CrCl(μ-Cl)TMEDA]2 (1) erhält man in einer äquimolaren Reaktion von CrCl2(THF) mit TMEDA in hohen Ausbeuten. 1 kristallisiert in der monoklinen Raumgruppe P21/c mit a = 843,2(2), b = 1 109,4(2), c = 1 147,4(3) pm, β = 102.99(2)° und Z = 2. Die Molekülstruktur von 1 enthält zwei leicht verzerrte quadratisch pyramidal koordinierte CrL5-Untereinheiten, die über zwei unsymmetrische Cl-Brücken verbunden sind. Die μ-Cl-Funktionen nehmen die apikale Position der einen und eine basale Position der anderen CrL5-Einheit ein, wobei die apikale Cr-Cl-Bindung (277,6(1) pm) deutlich länger als die basale Cr-Cl-Bindung (240,6(1) pm) ist. Die terminale Cr-Cl-Bindung ist noch kürzer (237,5(1) pm), Der Cr—Cr-Abstand mit 381,7(1) pm liegt deutlich außerhalb einer bindenden Cr-Cr-Wechselwirkung. Dieses wird durch magnetische Suszeptibilitätsmessungen bestätigt, die pro Cr-Zentrum vier ungepaarte Elektronen nachweisen; allerdings kann eine kleine antiferromagnetische Kopplung von J/k = -7,3 K berechnet werden. Diese Kopplung wird vermutlich durch einen 90°-σ-Superaustausch über die Cl-Brücken erwirkt.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956211214
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  • 95
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    Preparation, crystal structure, and infrared characterization of the first thiocyanato-oxy-antimonate(III) [(CH3)4N]2[Sb6O4(NCS)12] (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 2070-2074 
    Details
    ISSN: 0044-2313
    Keywords: Antimony(III) thiocyanate complex ; crystal structure ; IR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Darstellung, Kristallstruktur und IR-Charakterisierung des ersten Thiocyanato-oxyantimonats(III), [(CH3)4N]2[Sb6O4(NCS)12][(CH3)4N]2[Sb6O4(NCS)12] ist der erste Thiocyanato-oxyantimonat(III)-Komplex. Die Synthese, wichtige IR-Daten und die Struktur werden mitgeteilt. Die Verbindung kristallisiert in der triklinen Raumgruppe P1, Z = 2 (C10H12N7O2S6Sb3), a = 11,314(6), b = 12,846(3), c = 8,679(2) Å, α = 91,93(3)°, β = 90,31(3)°, γ = 99,13(3)°. Die Struktur wird aus zentrosymmetrischen [Sb6O4(NCS)12]2--Anionen und isolierten Tetramethylammonium-Kationen aufgebaut. Das grundlegende Strukturelement des Anions wird von drei SbOSbO-Ringen gebildet, die zu einem in zick-zack-Form, leicht gefalteten Band verbunden sind. Etwas Besonderes ist die Ungleichheit der sechs Thiocyanat-Liganden, obwohl alle N-gebunden an Antimon sind. Drei Thiocyanate sind terminal, während drei andere asymmetrisch N-verbrückend zwischen zwei Zentren sind; zwei von diesen verbinden die Anionen über Sb⋅⋅⋅S-Kontakte. Für die Antimonatome sind drei unterschiedliche Umgebungen vorhanden, einmal die Bindung an einen Stickstoff und drei Sauerstoffe, zweitens an einen Sauerstoff und drei Stickstoffe und drittens an je zwei Sauerstoffe und Stickstoffe.
    Notes: The salt [(CH3)4N]2[Sb6O4(NCS)12] is the first identified thiocyanato-oxy-antimonate(III) complex. Reported are details of the synthesis, relevant infrared data and its x-ray structure. The compound crystallizes in the triclinic space group P1 with Z = 2 (C10H12N7O2S6Sb3) and unit cell dimensions a = 11.314(6), b = 12.846(3), c = 8.679(2) Å; α = 91.93(3)°, β = 90.31(3)° and γ = 99.13(3)°. It contains centrosymmetric [Sb6O4(NCS)12]2- anions packed with isolated tetramethyl-ammonium cations. The fundamental structural element of the anion is provided by the fusion of three SbOSbO rings forming a zig-zag portion of a ribbon, only slightly pleated. Peculiar is the unequivalence of the six thiocyanate ligands, though all primarily N-bonded to antimony atoms. Three thiocyanates are terminal while other three are asymmetrically N-bridging between two centers; two of this latter type are also interconnecting the anions via Sb⋅⋅⋅S contacts. There are three different antimony environments, the primary bonding at Sb being to one nitrogen and three oxygens, to one oxygen and three nitrogens and to two atoms of each type.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956211216
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  • 96
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    Ternäre Thalliumplatin- und Thalliumpalladiumchalkogenide Tl2M4X6. Synthesen, Kristallstruktur und Bindungsverhältnisse (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 2083-2088 
    Details
    ISSN: 0044-2313
    Keywords: Transition metal chalcogenides ; platinum ; palladium ; melting reaction ; crystal structure ; Extended-Hückel-calculations ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ternary Thallium Platinum and Thallium Palladium Chalcogenides Tl2M4X6. Syntheses, Crystal Structures, and Bonding RelationsThe compounds Tl2Pt4S6, Tl2Pt4Se6, Tl2Pt4Te6 and Tl2Pd4Se6 can be synthesized by a melting reaction from the elements or by the reaction of thallium carbonate, transition metal powder and chalcogen powder in the temperature range between 400°C and 950°C. X-Ray investigations on single crystals and powdered samples revealed a new structure type for the compounds, that can be understood as stacking variant of the already known atom arrangement of the alkaline metal platinum chalkogenides A2Pt4X6 (A ≙ alkaline metal, X ≙ S, Se). The short distances thallium-platinum and thallium-palladium, respectively, as well as the results of Extended-Hückel-calculations indicate covalent bonds between the main group and transition metal atoms.
    Notes: Die Verbindungen Tl2Pt4S6, Tl2Pt4Se6, Tl2Pt4Te6 und Tl2Pd4Se6 sind durch Schmelzreaktionen aus den jeweiligen Elementen oder durch die Umsetzung von Thalliumcarbonat, Übergangsmetall- und Chalkogenpulver im Temperaturbereich zwischen 400°C und 950°C darstellbar. Röntgenographische Untersuchungen an Einkristallen und an pulverförmigen Proben ergaben, daß die Verbindungen in einem neuen Strukturtyp kristallisieren, der als Stapelvariante schon bekannter Atomanordnungen der Alkalimetallplatinchalkogenide A2Pt4X6 (A ≙ Alkalimetall, X ≙ S, Se) aufgefaßt werden kann. Die geringen Atomabstände Thallium-Platin bzw. Thallium-Palladium deuten in übereinstimmung mit den Ergebnissen von Extended-Hückel-Rechnungen auf eine kovalente Bindung zwischen dem Hauptgruppen- und dem übergangsmetall hin.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956211218
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  • 97
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    Monomeres Trilithium-tris[tert-butyldimethylsilylamido]phenylsilan, PhSi[NLi(THF)SiMe2CMe3]3 -- Darstellung und KristallstrukturProfessor Herbert W. Roesky zum 60. Geburtstag gewidmet (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 2093-2096 
    Details
    ISSN: 0044-2313
    Keywords: Monomeric trilithium-tris(silylamido)silane ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Monomeric Trilithium-tris[tert-butyldimethylsilylamido]phenylsilane, PhSi[NLi(thf)SiMe2CMe3]3 - Synthesis and Crystal StructureLithiated tert-butyldimethylsilylamine reacts with trifluorophenylsilane in a molar ratio 2:1 or 3:1 to give the bis- and tris(silylamino)silanes 1 [(Me3CSiMe2NH)2SiFPh] and 2 [(Me3CSiMe2NH)3SiPh]. The trilithium derivative 3 [Me3CSiMe2NLi(thf)]3SiPh is obtained in the reaction of 2 with n-BuLi in hexane/thf. 3 crystallizes as a monomer forming three planar four-membered (LiNSiN)-rings. The results of the crystal structure of 3 are discussed.
    Notes: Lithiiertes tert-Butyldimethylsilylamin reagiert mit Trifluorphenylsilan im molaren Verhältnis 2:1 bzw. 3:1 zu den Bis- und Tris(silylamino)silanen 1 [(Me3CSiMe2NH)2 · SiFPh] und 2 [(Me3CSiMe2NH)3SiPh]. In der Reaktion von 2 mit n-BuLi in Hexan/THF entsteht das Trilithiumderivat 3 [Me3CSiMe2NLi(THF)]3SiPh. 3 kristallisiert als Monomer und bildet im Kristall drei planare, viergliedrige (LiNSiN)-Ringe. Die Ergebnisse der Kristallstrukturanalyse von 3 werden mitgeteilt.
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    URL: http://dx.doi.org/10.1002/zaac.19956211220
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  • 98
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    Zur Polymorphie von Sm2Se3 (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 1977-1979 
    Details
    ISSN: 0044-2313
    Keywords: Samarium sesquiselenide ; chemical transport ; crystal structure ; polymorphism ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Polymorphism of Sm2Se3Two modifications of Sm2Se3 could be obtained in form of single crystals by chemical transport reaction. We prepared starting from Sm2Se3 powders red brown crystals of Sm2Se3 in the defective Th3P4 type structure with the space group I43d and a = 878.2 pm as well as starting from SmSe1.9 and samarium metal black, prismatic crystals of Sm2Se3 in the U2S3 type structure with the space group Pnma and a = 1 127.3 pm, b = 409.1 pm and c = 1103.2 pm.
    Notes: Zwei Modifikationen von Sm2Se3 konnten durch chemischen Transport in Form von Einkristallen erhalten werden. Es wurden einmal ausgehend von pulverförmigem Sm2Se3 rotbraune, plättchenförmige Einkristalle von Sm2Se3 im defekten Th3P4-Strukturtyp mit der Raumgruppe I43d und a = 878,2 pm dargestellt, zum anderen ausgehend von SmSe1,9 und Samariummetall schwarze, prismenförmige Einkristalle von Sm2Se3 im U2S3-Strukturtyp mit der Raumgruppe Pnma und a = 1 127,3 pm, b = 409,1 pm und c = 1 103,2 pm.
    Additional Material: 5 Tab.
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    URL: http://dx.doi.org/10.1002/zaac.19956211125
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  • 99
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    Über die Magnetischen Eigenschaften der Cobaltate Na6CoS4, Na6CoSe4 und K6CoS4Professor Robert Juza zum 90. Geburtstag gewidmet (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 409-411 
    Details
    ISSN: 0044-2313
    Keywords: Alkali metal cobalt chalcogenides, Na6CoS4, Na6CoSe4, K6CoS4 ; preparation ; crystal structure ; magnetic properties ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Magnetic Properties of the Cobaltates Na6CoS4, Na6CoSe4, and K6CoS4The alkali metal cobalt chalcogenides Na6CoS4, Na6CoSe4, and K6CoS4 crystallize in the space group P63mc with Z = 4. The structure is characterized by isolated [CoX4]-tetrahedra.The magnetic susceptibilities show Curie-Weiss behaviour. The deviations at low temperatures are caused by antiferromagnetic interactions. The magnetic moments are discussed with regard to ligand-field parameters.
    Notes: Die Alkalicobaltchalkogenide Na6CoS4, Na6CoSe4 und K6CoS4 kristallisieren in der Raumgruppe P63mc mit Z = 4. Als charakteristische Baugruppen treten „isolierte“ tetraedrische [CoX4]-Einheiten auf.Die Temperaturabhängigkeiten der magnetischen Suszeptibilitäten lassen sich mit einem Curie-Weiss-Verhalten beschreiben. Bei tiefen Temperaturen treten Abweichungen von diesem Verhalten auf, die auf antiferromagnetische Wechselwirkungen zurückzuführen sind. Die magnetischen Momente werden im Hinblick auf Ligandenfeldparameter diskutiert.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19956210312
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  • 100
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    Ein neuer Typ ternärer Cobaltsulfide A9Co2S7 (A \documentclass{article}\pagestyle{empty}\begin{document}$ \buildrel \wedge \over = $\end{document} K, Rb, Cs) mit trigonalplanaren [CoS3]-Baugruppen des zwei- und dreiwertigen CobaltsProfessor Peter Paetzold zum 60. Geburtstag gewidmet (1995)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 405-408 
    Details
    ISSN: 0044-2313
    Keywords: Ternary cobalt sulphides ; preparation ; crystal structure ; magnetic properties ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: A New Type of Ternary Cobalt Sulphide, A9Co2S7 (A \documentclass{article}\pagestyle{empty}\begin{document}$ \buildrel \wedge \over = $\end{document} K, Rb or Cs), containing Trigonal-Planar [CoS3] Units of Two- and Three-Valent CobaltThe passage of a stream of hydrogen over an alkali carbonate/cobalt/sulphur melt resulted in the preparation of the compounds K9Co2S7, Rb9Co2S7 and Cs9Co2S7. The structure of the potassium compound (Space group P213, Z = 4) could be determined from X-ray diffraction experiments on single crystals whilst X-ray investigations of powdered samples of the rubidium and caesium compounds indicate isotypic atomic arrangements with K9Co2S7. The characteristic structural elements of these compounds are trigonal-planar [CoS3]-units of two- and three-valent cobalt. The results from investigations of the magnetic properties of these ternary cobalt sulphides are in agreement with those expected for mixed-valent CoII/CoIII structures. The analogously-composed ferrates are closely structurally-related to these sulphides and show corresponding magnetic properties [1].
    Notes: Durch Schmelzreaktionen von Alkalicarbonat mit Cobalt und Schwefel im Wasserstoffstrom gelang die Darstellung der Verbindungen K9Co2S7, Rb9Co2S7 und Cs9Co2S7. Die Struktur der Kaliumverbindung konnte über röntgenographische Untersuchungen an Einkristallen bestimmt werden (Raumgruppe P213, Z = 4). Untersuchungen an pulverförmigen Proben lassen für die Rubidium- und die Cäsiumverbindung isotype Atomanordnungen erkennen. Als charakteristische Strukturelemente treten trigonal planare [CoS3]-Baugruppen des zwei- und dreiwertigen Cobalts auf. Untersuchungen zum Magnetismus sind in Übereinstimmung mit der Annahme eines gemischtvalenten Aufbaus, der auch bei den analog zusammengesetzten, in einem eng verwandten Strukturtyp kristallisierenden Ferraten auftritt [1].
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19956210311
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