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  • 1995-1999  (2,170)
  • 1935-1939
  • 1995  (2,170)
  • Analytical Chemistry and Spectroscopy  (1,554)
  • Inorganic Chemistry  (567)
  • crystal structure  (158)
  • Nuclear reactions
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  • 1995-1999  (2,170)
  • 1935-1939
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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 
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    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 
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    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.
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    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 
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    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.
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    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.
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    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.
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    URL: http://dx.doi.org/10.1007/BF01665969
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  • 18
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    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 
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    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
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    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
    Masthead (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995) 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280101
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  • 32
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    Electronic Resource
    Tripodal Triamidostannates as Building Blocks in the Generation of Sn - M-Bonded Heterobimetallics (M = Fe, Ru) (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 29-34 
    Details
    ISSN: 0009-2940
    Keywords: Tripodal ligands ; Triamidostannates ; Metal-metal bonds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: By in situ lithiation of the trifunctional amines H3CC(CH2NHSiMe3)3, PhC(CH2NHSiMe3)3, and HC{SiMe2NH(p-Tolyl)}3 and subsequent reaction with SnCl2 the corresponding triamidostannates were obtained. These were coupled with CpM(CO)2Cl (M = Fe, Ru) to yield the M - Sn-bonded heterobimetallics 9-14 of which H3CC(CH2NSiMe3)3SnFe(CO)2Cp (9) was characterized by a single-crystal X-ray structure analysis. Of the in situ-generated amidostannates only [HC{SiMe2N(p-Tolyl)}3Sn][Li(THF)3] (8) could be isolated as a uniform product and characterized analytically and spectroscopically.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951280105
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  • 33
    Electronic Resource
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    The Structures of [X2Y—N—YX2]+ Cations (X = F, Cl; Y = S, Se). A Comparison of X-ray and ab Initio Studies[1] (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 35-40 
    Details
    ISSN: 0009-2940
    Keywords: Selenium-nitrogen compounds ; Sulfur-nitrogen compounds ; Calculations, ab initio ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The structures of cationic species of the series [X2Y—N—YX2]+ (X = F, Cl; Y = S, Se) have been computed ab initio using all electron treatments for first-row elements and sulfur and quasi-relativistic pseudopotentials for Se and Cl. Splitvalence basis sets with polarization and diffuse functions were employed. The MP2 results for the (non-isostructural!) cations [Cl2Se—N—SeCl2]+ (1: Cs) and [F2S—N—SF2]+ (2: C2v) are in excellent agreement with the experimental (X-ray) observations. Both structures represent local minima. A deeper minimum for either of the cations is represented by another C2v isomer which for crystal lattice energy reasons is stable in the isolated state only. The geometries of the hitherto unknown species [Cl2S—N—SCl2]+ (3) and [F2Se—N—SeF2]+ (4) have been assessed by ab initio HF calculations. In analogy to 2, cations 3 and 4 are predicted to prefer C2v symmetry. Therefore, 1 exhibits unusual structural features. According to strictly localized natural bond orbital analysis (NBO), the central nitrogen atoms in 1 and 2 possess two lone pairs of electrons (LP: one sp hybrid and one p orbital). The relatively short Se—N and S—N bond distances in 1 (1.741-1.760 Å) and 2 (1.551 Å) can best be attributed to LP(N)→s̰*(Y—X) negative hyperconjugation (1: Y = Se, X = Cl; 2: Y = S, X = F).
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280106
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  • 34
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    Die fördernde Rolle von Phosphinoester-Liganden bei der Synthese neutraler Carben-, Vinyliden- und Allenyliden-Ruthenium(II)-KomplexeHerrn Professor Hubert Schmidbaur zum 60. Geburtstag gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 49-62 
    Details
    ISSN: 0009-2940
    Keywords: Ruthenium(II) complexes, octahedral ; Phosphino esters as mono- and bidentate ligands ; Fluxional behaviour ; Carbene complexes ; Vinylidene complexes ; Allenylidene complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Vinylidene Transition-Metal Complexes, XXXV[1].  -  The Supporting Role of Phosphino Ester Ligands for the Synthesis of Neutral Carbene, Vinylidene and Allenylidene Ruthenium(II) ComplexesThe reaction of [RuCl2(PPh3)3] (1) with the phosphino esters iPr2P(CH2)nCO2R (2-4) leads to complete (n = 1; R = CH3, C2H5) or partial (n = 2; R =CH3) displacement of the PPh3 ligands and formation of the octahedral ruthenium(II) complexes [RuCl2{k2(P,O)-iPr2PCH2CO2R}2] (5, 6) and [RuCl2(PPh3){k(P)-iPr2PCH2CH2CO2Me}{k2(P,O)-iPr2PCH2CH2CO2Me}] (7). Treatment of 5 with LiBr and LiI affords the dibromo- and diiodoruthenium derivatives 8 and 9. While compound 5 reacts with CO and SO2 by cleavage of one Ru - O bond to yield the 1:1 adducts [RuCl2(L){k(P)-iPr2PCH2CO2Me}{k2(P,O)-iPr2PCH2CO2Me}] (10, 11), the reaction of the dibromo derivative 8 with CO in solution gives the dicarbonyl complex [RuBr2(CO)2{k(P)-iPr2PCH2CO2Me}2](13). If CO is passed over 8 in the solid state, the corresponding monocarbonyl compound 14 is formed. The hydridoruthenium(II) complex 16, which is obtained from equimolar amounts of [RuHCl(CO)(PiPr3)2] (15) and 2, reacts with HC≡CMe by insertion to give the vinyl derivative [RuCl{E - CH=CHMe}(CO)(PiPr3){k2(P,O)-iPr2CH2CO2Me}] (17). Treatment of 5 with HC̊' (R' = H, Me, tBu, Ph) and of 6, 8, 9 with HC≡CPh affords upon photochemical activation the octahedral vinylidene complexes [RuX2-(=C=CHR){k(P)-iPr2PCH2CO2R}{k2(P,O)-iPr2PCH2CO2R}] (18-21 and 23-25) in good to excellent yield. At room temperature, these compounds (with the exception of 25) are highly fluxional in solution. From 31P-NMR measurements, the free energies of activation ΔG
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280108
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  • 35
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    Reaktionen von R2Al—AlR2 (R = CH(SiMe3)2) mit Trimethylsilylazid  -  Insertion in die Al—Al-Bindung und Abbau zum trimeren Dialkylaluminiumazid (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 81-85 
    Details
    ISSN: 0009-2940
    Keywords: Aluminium-aluminium bond ; Insertion of trimethylsilyl azide ; Trimeric dialkylaluminium azide ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reactions of R2Al—AlR2 (R = CH(SiMe3)2) with Trimethylsilyl Azide  -  Insertion into the Al—Al Bond and Formation of a Trimeric Dialkylaluminium AzideTetrakis[bis(trimethylsilyl)methyl]dialuminium(4) (1) reacts with trimethylsilyl azide under insertion of one nitrogen atom into the Al—Al bond. As shown by NMR spectra and crystal structure the product contains three and four coordinated Al atoms due to the coordination of the α-nitrogen atom of the azide group to one of the Al atoms. An electronically delocalized N3-system is formed with a N—N bond length of 132.0 pm and a bond order of 1.5 for both N—N bonds. With an excess of trimethylsilyl azide further reaction is observed only under mild irradiation conditions with an exchange of the azide group between Si and Al and formation of Me6Si2 and the dialkylaluminium azide 3, which is better synthesized by the reaction of Me3Si—N3 with Cl—Al[CH(SiMe3)2]2. The sterically highly shielded aluminium azide 3 is a trimer in the solid state showing a non-planar 12-membered Al3N9 heterocycle with short N—N bonds (114 pm).
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280112
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  • 36
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    Transition-Metal Complexes with the Novel Scorpionate Ligand Dihydrobis-(tetrazolyl)borate: Synthesis and Characterization of Infinite Two-Dimensional Metal-Ligand Frameworks and One-Dimensional Water SubstructuresDedicated to Professor Dr. Herbert Schumann on the occassion of his 60th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 323-328 
    Details
    ISSN: 0009-2940
    Keywords: Poly(azolyl)borates, metal complexes of ; Bis(tetrazolyl)borate, metal complexes of ; Metal-nitrogen coordination ; Coordination polymers ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Dihydrobis(tetrazolyl)borate metal compounds of the composition [M(L)2{μ-H2B(CHN4)2}2]n for M = Mn, Fe, Co, Zn, Cd with L = H2O and for M = Cu with L = NH3 are obtained from metal salts and K[H2B(CHN4)2]. Single-crystal X-ray studies reveal the formation of two-dimensional rhombic grid sheets through the bridging action of the bis(tetrazolyl)borate ligands. Each metal atom is octahedrally coordinated with two trans L ligands and four H2B(CHN4)-2 nitrogen donors. Two additional, hydrogen-bonded water molecules occupy the rhombic openings in the compounds with M = Mn, Fe, Co, Zn, and Cd. The water of crystallization is held in place through hydrogen bonding from the water ligands and to the nitrogen atoms to give a substructure of parallel kinked water chains. Temperature-variable magnetic measurements show a Curie-Weiss behavior for the paramagnetic complexes with M = Mn, Fe, Co, and Cu.
    Additional Material: 8 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951280402
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    New Organophosphorus Ligands: Cyclopropanation and Other Reactions of Cumulenes Bearing Diphenylphosphanyl Substituents (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 365-371 
    Details
    ISSN: 0009-2940
    Keywords: Cumulenes ; Butadienes ; Vinylcyclopropane ; Vinylidenecyclopropane ; Bicyclopropyl, phosphanyl-substituted ; Cyclopropanation ; Phosphane ligands ; Phosphane chalcogenides ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Hydrophosphorylation of 1,4-bis(diphenylphosphanyl)butadiyne with diphenylphosphane leads to the butadiene (Ph2P)2C=CH—CH=C(PPh2)2 (1). Treatment of 1 with dimethylsulfonium methylide gives the vinylcyclopropane (Ph2P)2C=CH—CH(CH2)C(PPh2)2 (2). Compound 2 reacts with aqueous hydrogen peroxide, elemental sulfur, or selenium to afford the tetrachalcogenides (Ph2XP)2C=CH—CH(CH2)C(PXPh2)2 with X = O (3), X = S (4), X = Se (5), respectively. While the tetraphosphane 1 and the vinyl-cyclopropane compound 2 cannot be converted into a bis-(cyclopropyl) compound with an excess of Me2S=CH2, the tetrasulfide 4 readily affords a mixture of (1R,1′R)-/(1S,1′S)-and meso-2,2,2′,2′-tetrakis(diphenylthiophosphinyl)-1,1′-bicyclopropyl (6, 7) in good yield. Treatment of 1,1,4,4-tetrakis-(diphenylphosphanyl)butatriene with dimethylsulfonium methylide leads to the vinylidenecyclopropane (Ph2P)2C=C=C(CH2)C(PPh2)2 (8). Compound 8 is converted into its tetrasulfide (Ph2SP)2C=C=C(CH2)C(PSPh2)2 (9) by treatment with elemental sulfur. The crystal structures of 1, 2, 4, 7, and 8 have been determined by single-crystal X-ray diffraction.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280408
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    Mono- und Diferriophosphane und -thioxophosphoraneHerrn Professor Dr. Ekkehard Lindner zum 60. Geburtstag gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 413-416 
    Details
    ISSN: 0009-2940
    Keywords: Ferriophosphanes ; Ferriophosphoranes ; Thioxophosphane ligand ; Decarbonylation reaction ; Sulfurization ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Mono- and Diferriophosphanes and -thioxophosphoranesHerrn Professor Dr. Ekkehard Lindner zum 60. Geburtstag gewidmet.The substitution of organic substituents in phosphanes or thioxophosphoranes by the 17-electron fragments CpFe-(CO)2 (—Fp) leads to isolobal ferriophosphanes or -thioxophosphoranes. The mono- and diferriophosphanes FpnPPh3-n [n = 1 (3), 2 (4)] are obtained by deprotonation of the mono- and diferriophosphonium salts [FpnPPh3-nH]X [n = 1 (1), 2 (2)] with DBU. They are oxidized by sulfur giving the mono- and diferriothioxophosphoranes FpnPPh3-n(S) [n = 1 (5), 2 (6)]. Sulfide 5 arises also from the reaction of CpFe(CO)2Cl and Ph2PH(S)/DBU. The one-sided decarbonylation reaction of 6 leads to FpFp′PPh(S) (7, Fp′ = CpFeCO). The Fp substituents (17 electrons) in 3-7 coordinate as one-electron donors to the PhnP- or PhnP(S) units (n = 1, 2). The bridging functions in 4 and 6 are hitherto unknown. The molecular structures of the complexes 5-7 were determined by X-ray structure analyses.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951280413
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  • 39
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    About some Electrophilic Substitution Reactions with [(CF3S)3C+][AsF-6] (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 435-436 
    Details
    ISSN: 0009-2940
    Keywords: Trifluoromethylthio group ; Carbenium ions ; Diphenylmethane ; Dyes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Tris(trifluoromethylthio)carbenium hexafluoroarsenate (1) reacts with N,N-dimethylaniline and anisole to form the corresponding diphenylmethanes 2, 3 with the SCF3 group at the methine carbon atom. During the reaction of 1 with benzene, compounds such as C6H5C(SCF3)3 and C6H5SCF3 are formed along with benzophenone, a product of hydrolysis of the diphenylmethane compound.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280417
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  • 40
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    Synthesis and Structure of the First Dimetalated Diphosphane Disulfide [(η5-C5Me5)(CO)2FeP(H)(S)]2 (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 441-442 
    Details
    ISSN: 0009-2940
    Keywords: Diphosphane disulfides ; Metallophosphoranes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The first transition metal derivative meso-[(η5-C5Me5)(CO)2FeP(H)(S)]2 (2) of the unknown diphosphane disulfide [PH2(S)]2 results from treatment of (η5-C5Me5)(CO)2FePH2 (1) with 1.5 equivalents of elemental sulfur. Compound 2 was characterized by means of spectroscopy (IR, 31P, 31P{1H}, 13C{1H}, 1H NMR) as well as X-ray diffraction analysis.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951280419
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  • 41
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    Preparation and Molecular Structures of Tetrahydrofuran, Diethylene Diglycol Dimethyl Ether and 18-Crown-6 Complexes of Strontium and Barium TetrahydridoborateDedicated to Prof. Dr. Nils Wiberg on the occasion of his 60th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 455-460 
    Details
    ISSN: 0009-2940
    Keywords: Strontium bis(tetrahydridoborate)-2 tetrahydrofuran, chain polymer of ; Strontium bis(tetrahydridoborate)-bis(diglyme) ; Barium bis(tetrahydridoborate)-bis(diglyme) ; Strontium bis(tetrahydridoborate)-1,4,7,13,16-hexaoxacyclooctadecane ; Metal-hydrogen-boron bridges ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The strontium and barium tetrahydridoborate complexes M(BH4)2 · 2 diglyme and M(BH4)2 · 18-crown-6 (M = Sr, Ba) have been prepared from the solvates M(BH4)2 · 2 THF by ligand displacement. 11B-NMR and IR data reveal strongly polar bonding of the BH4 groups to the metal centers, and X-ray structural analyses of the diglyme and crown ether compounds show molecular units in which the BH4 group is in contact via three H atoms with the metal center. In contrast, M(BH4)2 · 2 THF compounds are chain polymers in the solid state, and each metal center is surrounded by 2 THF molecules in trans position and four BH4- groups each of which forms bridges with two metal centers. Estimations of the effective radius for the BH4 group indicate a high polarity for the M-BH4 interaction.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280504
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    Photochemische Reaktionen von Übergangsmetall-Organyl-Komplexen mit Olefinen, 1312. Mitteilung: Lit.Photochemisch induzierte [5+2],homo[5+21-Cycloaddition von 3-Hexin an Tricarbonyl(η5-2,4-cycloheptadien-l-yl)mangan (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 515-518 
    Details
    ISSN: 0009-2940
    Keywords: Manganese ; Cycloheptadienyl ; Alkyne ; [5+2],homo[5+2] Cycloadditions ; Tricyclo[5.3.1.04,10]undeca-2,5-dien-11-yl ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Photochemical Reactions of Transition Metal Organyl Complexes with Olefins, 1312. Mitteilung: Lit. . - Photochemically Induced [5+2], homo[5+2] Cycloaddition of 3-Hexyne to Tricarbonyl(η 5-2,4-cycloheptadien-1-yl)manganeseTricarbonyl(η5-2,4-cycloheptadien-1-yl)manganese (1) reacts upon UV irradiation in hexane at 243 K with two equivalents of 3-hexyne (2) in successive [5+2],homo[5+2] cycloadditions to give tricarbonyl(η2:2:1-1,2,3,11-tetraethyltricyclo-[5.3.1.04,10]undeca-2,5-dien-11-yl)manganese (3). Its crystal and molecular structure was determined by an X-ray diffraction analysis, in solution it was studied also by IR and NMR spectroscopy.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951280513
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    Masthead (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995) 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280601
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    1,4,2-Diazaphospholothiazoles and -pyridines by a Hantzsch-Type Condensation Using Chloromethyldichlorophosphane (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 581-587 
    Details
    ISSN: 0009-2940
    Keywords: Anellated azaphospholes ; Hantzsch-type [3 + 2] cyclocondensation ; Chloromethyldichlorophosphane ; Regioselectivity ; 31P-, 1H-, 13C-NMR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The [3 + 2] cyclocondensation of 2-amino-1,3-thiazoline, 2-aminopyridines, 2- and 4-aminopyrimidines, 2-aminopyrazine, and 2-aminoquinoline with chloromethyldichlorophosphane in the presence of triethylamine yields regiospecifically 5,6-dihydrothiazolo[2,3-e][1,4,2]diazaphosphole (3), 1,4,2-diazaphospholo[4,5-α]pyridines (12), 1,4,2-diazaphospholo[4,5-α]pyrimidines (15), 1,4,2-diazaphospholo[4,5-e]pyrimidine (17), 1,4,2-diazaphospholo[4,5-α]pyrazine (19), and [1,4,2]diazaphospholo[4,5-α]quinoline (22), respectively. Using 2-amino-1,3-thiazole (4) and 2-aminobenzothiazoles 8, we obtained mixtures of the 1,5- and 4,5-anellated 1,4,2-diazaphospholes 5/6, 9a/10a and 9b/10b, while in the case of the methyl derivative 8c only the [1,4,2]diazaphospholo[5,4-b][1,3]benzothiazole 10c was formed. In the reaction of 2-aminothiazole and 2-aminopyrazine with Chloromethyldichlorophosphane the bis(diazaphospholo)-substituted chloromethylphosphanes 7 and 20 could be detected. The new anellated 1,4,2-diazaphospholes are colorless to pale yellow crystalline moisture-sensitive solids.
    Additional Material: 6 Tab.
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    URL: http://dx.doi.org/10.1002/cber.19951280610
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    Reactions at Silicon-Silicon Bonds, V. Selective Trichlorosilylation of Alkyl(diorganylamino)chlorophosphanes with Hexachlorodisilane or with Trichlorosilane/Triethylamine. - Two Routes to New Functional Trichlorosilylphosphanes (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 615-619 
    Details
    ISSN: 0009-2940
    Keywords: Reductive silylation ; Aminochlorophosphanes ; Silylphosphanes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of alkyl(diorganylamino)chlorophosphanes R(R2′N)PCl 1 (1a: R = tBu, R′ = Et, 1b: R = iPr, R′ = iPr; 1c: R = iPr, R′ = Ph) with hexachlorodisilane, afforded alkyl(diorganylamino)trichlorosilylphosphanes R(R2′N)PSiCl3 2 (2a: R = tBu, R′ = Et; 2b: R = iPr, R′ = iPr; 2c: R = iPr, R′ = Ph) and silicon tetrachloride. An intermediate formed in the reaction of 1b with hexachlorodisilane, the adduct iPr(iPr2N)(Cl)P-Si(Cl)3-SiCl3 (3b = 1b · Si2Cl6), was detected by 31P- and 29Si-NMR spectra that indicate pentacoordinated silicon bound to tetracoordinated phosphorus and tetracoordinated silicon. Trichlorosilylphosphanes 2 are also available from 1 under very mild conditions by reductive trichlorosilylation with trichlorosilane in the presence of triethylamine. Compounds 2 were identified analytically, by mass spectroscopy, multinuclear NMR, and an X-ray structure determination of 2c.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951280614
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    Reactions of Complex Ligands, LXIVPart LXIII: Ref.. Synthesis of 5,5′-Diphenyl-2,2′-bifuran, a Biaryl Compound with Remarkable Fluorescence Properties (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 641-643 
    Details
    ISSN: 0009-2940
    Keywords: Carbene ligands ; Tungsten complexes ; 2,2′-Bifuran ; Copper coupling reaction ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The 2-oxacyclic α,β-unsaturated carbene complex 1 reacts with an excess of dimethylamine to give the diphenylbifuran 2. The structure of 2 was established by independent synthesis from 2-phenylfuran (4) via regioselective lithiation and transmetalation to zinc and tin organometallics 6a-c and final oxidative copper coupling reactions.
    Additional Material: 1 Tab.
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    URL: http://dx.doi.org/10.1002/cber.19951280618
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    Synthesis of 2- and 3-Stannolenes via Addition of Trimethyltin Alkoxides to 3-Diethylboryl-4-ethyl-1,1-dimethylstannole (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 679-687 
    Details
    ISSN: 0009-2940
    Keywords: Stannole, diethylboryl-substituted ; Trimethyltin alkoxides ; 2-, 3-Stannolenes, organometallic-substituted ; NMR, coupling constants, 2J(Sn,Sn), sign determination ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Trimethyltin alkoxides (2) react stereoselectively with 3-diethylboryl-4-ethyl-1,1-dimethylstannole (1) via addition of the Me3Sn group to C(2) to the C(2) = C(3) bond and a 1,2 shift of an ethyl group from boron to C(3) to give the 2-stannolenes 3. The molecular structure of 3f' [R = (S)-2-Bu] was determined by single-crystal X-ray analysis, confirming the cis positions of the Et(RO)B and the Me3Sn group. These 2-stannolenes 3 undergo, upon heating to ca. 80°C, facile rearrangement by irreversible allylic migration of the Et(RO)B group to the 3-stannolenes 4 in which the cis positions of the boryl and the stannyl group are retained. All 2-stannolenes (in contrast to the 3-stannolenes) are readily deprotoborylated to give the 3-stannolene 5. The structures of 3, 4, and 5 follow conclusively from 1H-, 11B-, 13C-, and 119Sn-NMR spectra. The negative sign of the geminal coupling constants 2J(SnSn) was determined in the case of 3, 4, and 5 by 2D 119Sn/1H heteronuclear shift correlations.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951280705
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    Synthesis of Structures of (Acyloxy)boranesDedicated to Prof. Dr. A. Schmidpeter on the occasion of his 65th birthday.Synthesis of Structures of (Acyloxy)boranes (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 751-762 
    Details
    ISSN: 0009-2940
    Keywords: Trifluoroacyloxy-9-borabicyclo[3.3.1]nonane ; Pivaloyloxy-9-borabicyclo[3.3.1]nonane dimer ; Bis(9-borabicyclo[3.3.1]nonyl]oxalate ; Tetrakis(9-borabicyclo[3.3.1]nonyl)-dihydroxyoxalate ; Bis(9-borabicyclo[3.3.1]nonyl)-2,2-dimethylmalonate tetramer ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 9-Borabicyclo[3.3.1]nonane (9-BBNH) reacts with monocarboxylic acids to afford 9-(acyloxy)-9-borabicyclo[3.3.1]nonanes which are dimers in the solid state as shown by X-ray crystal structures of the benzoate and pivalate. More complex reactions were observed by allowing 9-BBNH to react with dicarboxylic acids in THF or monoglyme. Thus, (9-BBN)2 oxalate 3 contains a fully delocalized oxalate unit with equal C-O and B-O bond lengths. Traces of water convert it into the tetrakis(9-BBN) oxalate 5. A rather unusual structure is veryfied by 9-BBN 2,2-dimethylmalonate 7 which according to its molecular structure is a tetramer featuring a 32-membered ring system. In contrast, reactions of oxalic acid with thexylborane leads to reduction of the acid and formation of a bicyclic dioxaborolo-dioxaborolane 10. Several intermediates were detected by 11B-NMR spectroscopy as well as in reactions of BH3 · THF or BH3 · SMe2 with oxalic acid.  -  It follows from the present study that (acyloxy)boranes derived from dicarboxylic acids are strong Lewis acids with an unexpected variety of structural features.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951280803
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    A T-Shaped Selenenyl Halide: Synthesis and Characterisation of a Proposed Reaction Intermediate (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 741-742 
    Details
    ISSN: 0009-2940
    Keywords: Selenenyl halides ; Nucleophilic substitution ; Complex intermediate ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The T-shaped selenenyl halide (1), which may be regarded as a model substance for the transition state in nucleophilic displacement at divalent chalcogen atoms, has been isolated and subjected to X-ray structure determination.
    Additional Material: 1 Tab.
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    URL: http://dx.doi.org/10.1002/cber.19951280715
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    Zinc Complexes of Drugs Containing Nitrogen Heterocycles (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 779-785 
    Details
    ISSN: 0009-2940
    Keywords: Zinc complexes ; Drug ligands ; Captopril ; Isoniazid ; Nalidixic acid ; Mercaptopurine ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Four drugs whose actions have a relation to the status of zinccontaining species in the human body were used as ligands in zinc complexes. Captopril (H2Cap) forms the compound [ZnCap] (1) presumed to be a coordination polymer with O and S coordination. Isoniazid, in the presence of zinc salts, is converted to 1,2-diisonicotinoyl hydrazide (H2Nih) which forms polymeric [Zn(Nih)NH3] (2) with trigonal-bipyramidal ZnO2N3 coordination. Nalidixic acid (HNal) and zinc perchlorate yield [Zn(HNal)2(H2O)2](ClO4)2 · 2 H2O (3) containing zinc in an octahedral ZnO6 environment. Mercaptopurine (H2Mer), in the presence of ammonia, forms [Zn(Mer)(NH3)2] . H2O (4) which is a coordination polymer containing tetrahedral ZnN4 units. The structures of [Zn(Nih)NH3], [Zn(HNal)2(H2O)2](ClO4)2 . 2 H2O, and [Zn(Mer)(NH3)2] . 2 H2O were determined diffractometrically.
    Additional Material: 4 Ill.
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    Enantioselective Deprotonation of Benzyl Phosphates by Homochiral Lithium Amide Bases  -  Configurational Stability of Benzyl Carbanions with a Dialkoxyphosphoryloxy Substituent and Their Rearrangement to Optically Active α-Hydroxy Phosphonates (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 823-830 
    Details
    ISSN: 0009-2940
    Keywords: Phosphate-phosphonate rearrangement ; Carbanions, benzylic, configurational stability of ; Phosphonaes Lithium amides, homochiral ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Benzyl dialkyl phosphates are deprotonated enantioselectively by homochiral lithium amides of isopropyl(1-phenylethyl)amine or bis(1-phenylethyl)amine. The short-lived benzylic carbanions formed are virtually configurationally stable relative to the rearrangement to optically active phenyl-hydroxymethylphosphonates. The enantiomeric excesses are up to 50%. The pro-(S) hydrogen is removed by amides having (S) configuration. Homochiral diethyl (S)-phenyl[D1]-methyl phosphate [(S)-16c] is deprotonated by both LDA and n-BuLi with a high primary kinetic isotope effect (kH/D ≍ 50) and isomerizes to the corresponding α-hydroxy phosphonate with an enantiomeric excess of up to 85%.
    Additional Material: 1 Tab.
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    URL: http://dx.doi.org/10.1002/cber.19951280814
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    Tris(1,10-phenanthroline)iron(II) Complexes  -  Broad Variation of the Redox Potential by 4,7-Substitution at the Phenanthroline Ligands[1] (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 845-850 
    Details
    ISSN: 0009-2940
    Keywords: Phenanthroline synthesis ; Tris(phenanthroline)iron(II) complexes ; Redox potential ; Cyclic voltammetry ; Electron transfer, outer-sphere ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The new 4,7-donor-substituted phenanthrolines 2a-h were synthesized and the corresponding tris(1,10-phenanthroline)iron(II) complexes 3a-h studied by cyclic voltammetry. In more detail three novel aza-crown ether-linked (phenanthroline)iron complexes were investigated, the redox potentials of which could be fine-tuned by the addition of group-Ia,IIa metal cations. All iron(II) complexes showed reversible waves at scan rates between 50 and 500 mV · s-1 and could be reversibly oxidized and reduced by chemical means.
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    URL: http://dx.doi.org/10.1002/cber.19951280816
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    Bis(cyclopentadienyl)methane-Bridged Dinuclear Complexes, 10Part 9: B. Stempfle, H. Werner, Gazz. Chim. Ital., 1995, 125, in press. The Bis(cyclopentadienyl)methane Link between Lewis Basic and Lewis Acidic Metal CentersDedicated to Prof. Dr. Herbert Schumann on the occasion of his 60th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 877-881 
    Details
    ISSN: 0009-2940
    Keywords: Bis(cyclopentadienyl)methane ; Heterobimetallic complexes ; Imido complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The mononuclear rhodium complexes [(C5H5CH2C5H4)-Rh(CO)2] (1) and [(C5H5CH2C5H4)Rh(PhC≡CPh)(PiPr3)] (2) readily react with nBuLi or TlOEt to yield the corresponding lithium salts 3 and 4 or thallium salts 5 and 6. The reaction of these salts with [(C5H5)Nb(NtBu)Cl2] (7) leads to the formation of the heterodinuclear compounds [{CH2(C5H4)2}-{Rh(CO)2}{(C5H5)Nb(NtBu)Cl}] (8) and [{CH2(C5H4)2}-{Rh(PhC≡CPh)(PiPr3)}{(C5H5)Nb(NtBu)Cl}] (9), respectively. Treatment of 3-6 with [Mo(NtBu)2Cl2] (10) gives the heterodinuclear Rh/Mo complexes [{CH2(C5H4)2}{Rh(CO)2}-{Mo(NtBu)2Cl}] (11) and [{CH2(C5H4)2}{Rh(PhC≡CPh)-(PiPr3)}{Mo(NtBu)2Cl}] (12). The analogous reaction of [Mo(NMes)2Cl2(DME)] (13) with 3-6 yields the corresponding complexes [{CH2(C5H4)2}{Rh(CO)2}{Mo(NMes)2Cl}] (14) and [{CH2(C5H4)2}{Rh(PhC≡CPh)(PiPr3)}{Mo(NMes)2Cl}] (15). From the monometallated ligand [(C5H5CH2C5H4)M] (M = Li: 16; M = Tl: 17) and the imidometal compounds 7, 10 and 13, the mononuclear complexes [(C5H5CH2C5H4)(C5H5)Nb-(NtBu)Cl] (18) and [(C5H5CH2C5H4)Mo(NR)2Cl] (R = tBu: 19; R = Mes: 20) have been obtained.
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    URL: http://dx.doi.org/10.1002/cber.19951280905
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    Addition von Hydrofullerid [C60H]- an koordinierte, ungesättigte Kohlenwasserstoffe: Bindung von Fulleren an Metallkomplexe über KohlenwasserstoffbrückenHerrn Professor Herbert Walter Roesky zum 60. Geburtstag gewidmet (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1059-1060 
    Details
    ISSN: 0009-2940
    Keywords: Fullerene ; Hydrofulleride ; Manganese complex ; Rhenium complex ; Iron complexes ; Ruthenium complex ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Addition of Hydrofulleride [C60H]- to Coordinated, Unsaturated Hydrocarbons: Binding of Fullerene to Metal Complexes through Hydrocarbon BridgesHerrn Professor Herbert Walter Roesky zum 60. Geburtstag gewidmet.Hydrofulleride [C60H]- is added to the hydrocarbon ligands of the cationic complexes [(OC)5Re(η2-C2H4)]+, [(OC)3Mn-(η6-C6H6)]+, [(OC)3M(η5-C6H7)]+ (M = Fe, Ru), [(OC)3Fe(η5-C7H9)]+, and [(η5-C5H5)Fe(η6-C5H4CH2)]+.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951281017
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    Controlled Conversion of the Transient 2-Mesityl-1,1-bis(trimethylsilyl)silene into a Tetrahydro-2,3-disilanaphthalene, a 1,2-Disilacyclobutane, or a 1,3-Disilacyclobutane (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1083-1088 
    Details
    ISSN: 0009-2940
    Keywords: Silenes ; Silene dimerization ; 1,2-Disilacyclobutanes ; 1,3-Disilacyclobutanes ; 2,3-Disilanaphthalene, tetrahydro- ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Mesityl[tris(trimethylsilyl)silyl]methanol (1) reacts with strong bases with elimination of trimethylsilanolate according to a Peterson-type mechanism, the outcome of the reaction being dependent on solvent, temperature, and nature of the organometallic base applied. Thus, 1 was converted by treatment with MeLi in ether at -78°C to (E)-1,2,3,8a-tetra -hydro-1-mesityl-5,7,8a-trimethyl-2,2,3,3-tetrakis (trimethylsi-lyl)-2,3-disilanaphthalene (3), formally a [2 + 4] cyclodimer of the transient silene (Me3Si)2Si=CHMes (2). The reaction of 1 with PhMgBr in THF after some days resulted in the formation of (Z)-3,4-dimesityl-1,1,2,2-tetrakis(trimethylsilyl) -1,2-disilacyclobutane (6) as the main product besides small quantities of 3, the polysilane (Me3SiSi(SiMe3)2CH2Mes (10), and the alkoxysilane (Me3Si)3SiCH(Mes)OSi(Si-Me3)2CH2Mes (7). Compound 6, the formal [2 + 2] cycloadduct of 2, can also be obtained by thermal treatment of 3 and is considered to be the thermodynamically more stable silene dimer whereas 3 is the kinetically preferred product. At high LiBr concentrations in the reaction mixture 1 was converted by PhMgBr in THF to (E)-2,4-dimesityl-1,1,3,3-tetrakis(tri- methylsilyl)-1,3-disilacyclobutane (13) besides 6 and [bis(tri-methylsilyl)silyl]mesityl(trimethylsiloxy)methane (11). The unforeseen formation of 13 is discussed as proceeding via the silene-lithium bromide adduct (Me3Si)2Si(Br)CH(Li)Mes (12). In the absence of LiBr 1 was converted by MeLi in THF at -78°C to 11 and the trisilane (Me3Si)2Si(Me)CH2Mes (4b). Probable pathways of the formation of all new compounds are discussed. For 6 and 13 the results of the X-ray structural analyses are given.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951281105
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    Metallkomplexe mit biologisch wichtigen Lisganden, LXXXLXXIX. Mitteilung: Lit.. (η3:η3-C10H16)Ru(IV)-Komplexe mit α-Aminocarboxylaten, α-Aminosäureestern und Peptidestern als Liganden (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1117-1125 
    Details
    ISSN: 0009-2940
    Keywords: 1,7-Dimethylocta-2,6-diene-1,8-diyl ; Ruthenium complexes ; α-Amino carboxylates ; α-Amino acid esters ; Peptide esters ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Metal Complexes Containing Biologically Important Ligands, LXXXLXXIX. Mitteilung: Lit. .  -  (η3:η3-C10H16)Ru(IV) Complexes with α-Amino Carboxylates, α-Amino Acid Esters, and Peptide Esters as LigandsReactions of the chloro-bridged bis(allyl) complex [(η3:η3-C10H16)Ru(Cl)(μ-Cl)]2 with α-amino carboxylates and α-amino acid esters afford the complexes (η3:η3-C10H16)(Cl)RuNH2CHRCO2 (2) and (η3:η3-C10H16)(Cl)2-RuNH2CHRCO2R′ (3). Abstraction of chloride from 3 by Ag+ gives the N,O-chelates [(η3:η3-C10H16)(Cl)RuNH2CHRCO2R′]+BF4 (4). Cysteine methyl ester forms the N,S-chelate complex (η3:η3-C10H16)(Cl)RuNH2CH(CO2CH3)CH2S (5), and with histidine methyl ester a dinuclear complex 6 with N,N-histidine bridge is obtained. Compound 3d with L-PheOEt as ligand was characterized by X-ray diffraction.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951281110
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    [MeO(CH2CH2O)3(CH2)3C5Me4]FeCl: A Halfsandwich Iron (II) Chloride Complex of Remarkable Stability (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1135-1136 
    Details
    ISSN: 0009-2940
    Keywords: Hemilabile ligands ; Cyclopentadienyl ligands, functionalised ; Iron compounds ; Halfsandwich complex ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reaction of iron(II) chloride with one equivalent of [MeO-(CH2CH2O)3(CH2)3C5Me4]Li in THF yields the title halfsand-wich complex 1, which is stable in solution up to room temperature. Compound 1 reacts with C5H5Li and CO to give [MeO(CH2CH2O)3(CH2)3C5Me4]Fe(C5H5) (2) and [MeO-(CH2CH2O)3(CH2)3C5Me4]Fe(CO)2CI (3), respectively, in high yields.
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    URL: http://dx.doi.org/10.1002/cber.19951281113
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    [Cp4Fe4(E2)2] Clusters with Triangulated Dodecahedral Fe4E4 Skeletons (E = P, As)Dedicated to Professor Herbert Schumann on the occasion of his 60th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1145-1148 
    Details
    ISSN: 0009-2940
    Keywords: P2, As2, P2S2, and P2Se2 ligands ; Iron complexes ; Triangulated dodecahedra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The thermolysis of [CpFe(CO)2]2 (1) and P4 or As4 affords the iron clusters [Cp4Fe4(E2)2], E = As (2a), P (2b), the Fe4E4 skeleton of which consists of a triangulated dodecahedron. S8 and gray Se oxidize the P2 ligands of 2b with formation of [Cp4Fe4(P2X2)2], X = S (3a), Se (3b), complexes with the hitherto unknown P2X2 ligands, 2a, b and 3a, b have been characterized by X-ray crystallography.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951281202
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    Functionalized Diorganozinc Compounds: Key Reagents for the Synthesis of Enantiomerically Pure 2,5-Disubstituted cis- and trans-Tetrahydrofurans (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1021-1028 
    Details
    ISSN: 0009-2940
    Keywords: Synthesis, stereoselective ; Catalysis ; Tetrahydrofurans ; Dialkylzinc reagents ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 1,4-Diol derivatives 4a-i were synthesized stereoselectively by either reagent- or catalyst-controlled routes using the addition of functionalized diorganozinc reagents to aldehydes. The stereoselectivities along the reagent-controlled synthetic path were in the range between 80:20 and 95:5. The stereoselectivities along the catalyst route exceeded 95:5. The 1,4-diol derivatives 4 thus obtained were transformed into enantiomerically pure cis- and trans-2,5-disubstituted tetrahydrofurans (16-20) by means of an intramolecular Williamson reaction.
    Additional Material: 1 Tab.
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    Contributions to the Chemistry of Boron, 231Part 230: Ref.. Synthesis and Structures of Borylated HydrazinesDedicated to Professor H. P. Fritz on the occasion of his 65th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1187-1194 
    Details
    ISSN: 0009-2940
    Keywords: Hydrazines ; N,N'-bis(diphenylboryl)-N,N'-dimethyl- ; N,N'-bis(diphenylboryl)-N',N'-dimethyl- ; N,N'-bis(dimethylphenylsilyl)- ; N,N'-bis(chloromesitylboryl)-N'-phenyl-N'-(trimethylsilyl)- ; 1,2,4,5,3,6-Tetrazadiborinane, 1,2,4,5-tetrakis(tert-butyldimethylsilyl)-3,6-difluoro- ; Triazadiborolidine, dihydro-, derivative ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The diboration of the diazene PhN = NSiMe3 (15) by diborane(4) derivatives provides a new synthetic route to N,N'-diborylated hydrazines. The product formed depends on the type of the diborane(4) compound. Thus, addition of dimesityldiboron dichloride to 15 in a 1:1 ratio afforded (mesCIB)PhN-N(SiMe3)(BClmes) (16) while bis(dimethyl-amino)diboron dichloride was found to react in a 1:2 ratio to give a triazadiborolidine derivative 17. In addition, it was demonstrated that in the solid state Me2N-N(BPh2)2 (8) is a derivative of a three-membered dihydroazadiboriridine C while its isomer, (Ph2B)MeN-NMe(BPh2) (7), forms no BN coordinative bond. The new 3,6-difluoro-1,2,4,5-tetraza-3,6-diborine 13 shows a twist conformation. The molecular structures of all these compounds were determined by X-ray crystal structure analysis, and the influence of the B substituent on the conformation is discussed.
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    URL: http://dx.doi.org/10.1002/cber.19951281209
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    Metal Complexes of Functional Isocyanides, XXV. Amino(hydrazino)carbene Complexes (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1061-1068 
    Details
    ISSN: 0009-2940
    Keywords: N-Isocyanides ; N-Isocyanodialkylamine complexes ; Carbene complexes ; Imaging-Plate data collection ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The N-isocyanodialkylamine metal complexes [M(CO)5CN-NR2] (M = Cr, W), trans-[MI2(CNNR2)2] (M = Pd, Pt), trans-[Pt(Cl)(CNNR2)(PPh3)2]BF4, and cis-[PtCl2(CNNR2)(PPh3)] [R = Et, iPr; 2 R = -{CHMe(CH2)3CHMe}-] react with primary amines to give the amino(hydrazino)carbene metal complexes [M(CO)5(C(NHR′)NHNR2}] (R′ = Me, nPr, Cy) (1-9), trans-[PtI2{C(NHMe)NHNR2}2] (10-12) and trans, and the amine adducts cis-[PtCl2{C(NHMe)NHNC(H)(Me) (CH2)3CHMe}(PPh3)] H2NMe (14), and trans-[PdI2{C (NHMe)NHNC(H)(Me)(CH2)3CHMe}2] 2 H2NMe (15). With secondary amines the amino(hydrazino)carbene metal complexes trans (18) and trans-[PtCl{C(NEt2)NHNEt2} (PPh3)2]BF4 (19) Were isolated. The complexes trans-[PtI2{C(NHCy)NHNiPr2}CNNiPr 2] (20) and trans-[PdI2 (NH2Cy){C(NHCy)NHNiPr2}] (21) were obtained by reaction of trans-[MI2(CNNiPr2)2] (M = Pd, Pt) with cyclohexylamine. The structures were assigned on the basis of IR, NMR- (1H, 13C, 31P), and mass spectroscopy as well as an X-ray structural analysis of 21.
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    Metallocenophanes, VIIPart VI: Ref.. Preparation and Characterisation of the Disilver(I) Complexes of Conjugated Polyenes with [2.2.2]Paracyclophanyl End Groups (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1079-1082 
    Details
    ISSN: 0009-2940
    Keywords: [2.2.2]Paracyclophanes ; Polyenes ; Silver complexes ; X-Ray structural analysis ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The preparation of the disilver(I) complexes 3 and 4, polyene metal complexes that are terminally substituted with [2.2.2]paracyclophanyl units, is described. NMR spectro-scopic studies on the disilver perchlorate complex 3b showed that (a) the sites of complexation are the cyclophane groups and (b) the olefinic spacers do not overly perturb the overall complexation properties of the individual [2.2.2]paracyclo-phanyl groups. The crystal structures of the disilver hexafluo-roantimonate complexes 4a-b were determined. The use of the hexafluoroantimonate counterion and solvent mixtures containing toluene both proved crucial in obtaining single crystals; toluene is incorportated into the crystal lattices.
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    Highly Substituted Tris(pyrazolyl)methane Ligands and Some Zinc Complexes Thereof (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1095-1103 
    Details
    ISSN: 0009-2940
    Keywords: Zinc complexes ; Tridentate ligands ; Tris(pyrazolyl)methane ; Reactivity ; Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Tris(pyrazolyl)methane ligands in which two or three of the pyrazole carbon atoms bear organic substituents (L1-L7) were synthesized from chloroform and the corresponding pyrazole under phase transfer conditions. Their behavior towards zinc salts was found to span the range from no reaction at all to hydrolytic destruction. One hydrolysis product isolated and structurally characterized was the perchlorate complex [(HPz5)3Zn-OClO3]ClO4 (1), other ones were the 2:1 complexes (HPz3)2ZnBr2 (2) and (HPz6)2Zn(NO3)2 (3, HPzn = substituted pyrazole). Zinc perchlorate and tris(trimethylpy-razolyl)methane (L2) formed the octahedral binary complex [L22Zn](ClO4)2 (4) as evidenced by a structure determination. Zinc halides produced the 1:1 complexes L1 · ZnBr2 (5), L4 · ZnCl2 (6), and L4 · ZnBr2 (7), which according to the structure determinations of 6 and 7 contain tetrahedral ZnN2Hal2 units with only bidentate tris(pyrazolyl)methane ligands. In contrast, the zinc nitrate complex L4 · Zn(NO3)2 (8) was found to have an octahedral structure with mono- and bidentate nitrate and tridentate L4. The bromide complex 7 was converted by silver perchlorate hydrate into the labile compound [L4 · ZnBr]ClO4 (9) and then into the unstable product [L4 · Zn-OH2](ClO4)2 (10), both presumed to contain zinc in a tetrahedral ZnN3Br or ZnN3O environment, respectively. The ease of hydrolytic self-destruction prevented the exploitation of the reactivity of 9 and 10 in analogy to that of the corresponding tris(pyrazolyl)borate zinc complexes.
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    Unusual Complexation Behavior of Metallomacrocycles Based on Isothiosemicarbazides with Respect to Alkali and Alkaline Earth Metal Ions: Novel 2:1 Associates (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1089-1093 
    Details
    ISSN: 0009-2940
    Keywords: Metallomacrocycles ; Nickel complexes ; Complexation reactions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reactions between alkali and alkaline earth metal ions and nickel(II) macrocycles based on S-alkylated isothiosemi-carbazides with different crown ether cavity size were studied in propylene carbonate by spectrophotometric and calorimetric titrations. Metallomacrocycles 1 and 2 exhibit normal behavior on 1:1 complexation with alkali- and alkaline earth metal ions and resemble in this respect 15C5 and 18C6, respectively. The most stable complexes are formed by these “ligands” when the diameter of the cation and the crown ether hole have approximately the same size. The most striking feature of the complexation processes studied is the formation of 1:2 metal-ligand associates even in the case of the smallest cations. These associates are very different from “normal” crown ether sandwich complexes. In reality, the particle formed is an associate between a 1:1 complex, in which the corresponding metal ion is well accommdated inside the ligand cavity, and a second metallomacrocyclic ligand. Their formation is disfavored by enthalpic contributions. A special kind of “switch” from these associates to normal sandwich complexes takes place in the case of 1, when the cation diameter compared to hole size increases. The macrocycle 2 forms this kind of associates with all akali and alkaline earth ions.
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    URL: http://dx.doi.org/10.1002/cber.19951281106
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    Synthesis and Reactivity of Silicon Transition Metal Complexes, 3433. Mitteilung: Lit.. Pentachlordisilanyl- und Disilanyl-Komplexe von Molybdän und Wolfram: Darstellung, Struktur und spektroskopische CharakterisierungHerrn Professor Hubert Schmidbaur zum 60. Geburtstag gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1109-1115 
    Details
    ISSN: 0009-2940
    Keywords: Silicon transition metal complexes ; Metallodisilanes ; Nucleophilic metallation ; Cl/H exchange at silicon ; Raman spectroscopy ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis and Reactivity of Silicon Transition Metal Complexes, 34[*].  -  Pentachlorodisilanyl and Disilanyl Complexes of Molybdenum and Tungsten: Synthesis, Structure, and Spectroscopic CharacterizationReaction of the lithium metallates Li[M(PMe3)(CO)2C5R5] [M = Mo, W; R = H (1a, b), Me (1c, d)] with Si2Cl6 (2) leads to the formation of the pentachloro(metallo)disilanes 5R5(OC)2(Me3P)M - SiCl2 - SiCl3 (3a - d), which are transformed into the metallo disilanes C5R5(OC)2(Me3P)M - SiH2 - SiH3 (4a - d) on treatment with LiAlH4. The disilanes 4a - d are reconverted into 3a - d in the presence of tetrachloromethane. Extensive spectroscopic investigations (NMR, Raman, and IR spectroscopy) were performed to establish the transition-metal effect especially with respect to the H5Si2 ligand. The molecular structure of C5Me5(OC)2(Me3P)W - SiCl2 - SiCl3 (3d) was determined by single-crystal X-ray diffraction.
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    URL: http://dx.doi.org/10.1002/cber.19951281109
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    Octacarbonylbis {μ-(tris(trimethylsilyl)methyl]indany l} dimanganese with Two Monoalkyl Indium Groups Bridging the Mn-Mn Bond (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1137-1139 
    Details
    ISSN: 0009-2940
    Keywords: Tetraindane(4) ; Indium(I) ; Mn-Mn bond ; Indium alkyl bridge ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Tetrahedra-tetrakis[tris(trimethylsilyl)methyl]tetraindane(4) (1) reacts with decacarbonyldimanganese(0) to yield the bright red crystalline title compound 2, in which two carbonyl ligands are replaced by two InR fragments. The crystal structure determination of 2 shows two Mn(CO)4 groups (Mn-Mn 313.7 pm) bridged by two monoalkylindium units and a planar Mn2In2 molecular center.
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    URL: http://dx.doi.org/10.1002/cber.19951281114
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    Thioselonocarboxylic Ester, Selenetane, and Dihydrodiselenine Complexes Prepared from Pentacarbonyl(selenobenzaldehyde)tungsten with π-Donor-Substituted Alkynes (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1149-1156 
    Details
    ISSN: 0009-2940
    Keywords: Selenoaldehyde complex ; Thioselonocarboxylic ester complexes ; Selenetane complex ; Dihydrodiselenine complex ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Pentacarbonyltungsten-coordinated selenobenzaldehyde, [(CO)5W{Se=C(Ph)H}] (1), reacts with tBu-C≡C-SMe (2) by insertion of the C≡C into the Se=C bond to form in a highly regio- and stereoselective manner the α,β-unsaturated thioselonocarboxylic ester complex (Z)(C=C)-[(CO)5W{≡1-Se=C(SMe)C(tBu)=C(Ph)H}] (3). The thioselonocarboxylic ester ligand is cleaved intact from the metal by treatment of 3 with [NEt4]Br. Three complexes are formed in the reaction of 1 with Me-C≡C-SMe (5): the thioselonocarboxylic ester complex [(CO)5W{≡1-Se=C(SMe)C(Me)=C(Ph)H}] (6) as a mixture of the (E) and (Z)(C=C) isomers, a selenetane complex (7) and a dihydrodiselenine complex (8). The product distribution depends on the ratio 1:5 and on the solvent. The reaction of 1 with the bis(organylthio)alkynes RS-C≡C-SR (9) [R = Me (a), iPr (b), 2,6-C6H3Me2 (c)] yields mixtures of the (E) and (Z)(C=C) isomers of the α,β-unsaturated α-organylthio thioselonocarboxylic ester complexes [(CO)5W{≡1-Se=C(SR)C(SR)=C(Ph)H)] (10a-c). In contrast, the reaction of 1 with tert-butoxyethyne, H-C≡C-OtBu (11), affords a bis(pentacarbonyltungsten) 5,6-dihydro-1,2-diselenine complex (12). Compound 12 is probably formed by consecutive reaction of 1 with 11 to give the selonocarboxylic ester complex [(CO)5W{≡1-Se=C(OtBu)C(H)=C(Ph)H}] which then further reacts as a heterodiene by highly regioselective [4 + 2] cycloaddition with the Se=C bond of a second molecule of 1 to give 12. In the reaction of 1 with 5 and 9a the isomer with a trans arrangement of C(=Se)SMe and Ph is the kinetically controlled reaction product [(E)-6 and (Z)-10a, respectively]. The formation of (E)-6 and (Z)-10a is followed by isomerization until an (E)/(Z) equilibrium is reached. Complexes 3 and 7 were characterized by X-ray structural analyses.
    Additional Material: 1 Ill.
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    Tin for Organic Synthesis, 13Part 12: Ref.. A New and Regioselective Method for the Synthesis of Aromatic, Heteroaromatic, and Olefinic Sulfonamides by Electrophilic Destannylation (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1195-1198 
    Details
    ISSN: 0009-2940
    Keywords: Electrophilic aromatic substitution ; Electrophilic vinylic substitution ; Trialkylstannanes, application of ; Sulfonamides, synthesis of ; Sulfodestannylation, application of ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A mild and effective method for the preparation of aromatic and olefinic sulfonamides is described. The reaction of trialkylaryl- (4a-f), heteroaryl- (4g), and vinylic stannanes (4h) with sulfuryl chloride and secondary amines provides the corresponding sulfonamides in an ipso-specific manner.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951281210
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    Ylidylphosphorsulfide, -selenide, -disulfide, -sulfidselenide und -diselenide (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1207-1219 
    Details
    ISSN: 0009-2940
    Keywords: Ylide-substituted phosphorus ; Phosphorus sulfides ; Phosphorus selenides ; Thioxophosphanes ; Selenoxo-phosphanes ; Dithioxophosphoranes ; Diselenoxophosphoranes ; Alkylation reactions ; Selenadiphosphirane ; 2,5,7-Triselena-1,3,4,6-tetraphosphanorbornane ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Ylidylphosphorus Sulfides, Selenides, Disulfides, Sulfide Selenides, and DiselenidesWe report on the first stable monomeric phosphorus mono-chalcogenides 2, 8 and the first stable dichalcogenides 4, 10 without bulky or intramolecularly coordinating substituents. They are stabilized by a high contribution of the zwitterionic resonance formula, which follows both from the NMR spectra and from an X-ray structure determination. Their preparation starts from triphenylphosphoniumylidyl-dichlorophosphanes 1. For the monochalcogenides they are treated with sodium sulfide or selenide or better with bis(trimethylsilyl) sulfide or selenide. In case of the C-phenyl and C-meta-tolyl representatives and also of the C-trimethylsilyl compound a number of secondary, partly novel products are obtained. - The dichalcogenides result from the reaction with sodium disulfide and diselenide, respectively, or from the oxidation of the monochalcogenides. - Alkylation of the monochalcogenides results in ylidylalkylchalcogenophosphenium salts 13, 15. In solution they are in equilibrium with more or less of the covalent form 14, 16, depending on the anion and on the solvent. Alkylation is often accompanied by secondary reactions. A diselenide loses selenium on alkylation.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951281212
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    Synthesis and Reactivity of Silicon Transition Metal Complexes, 3332. Mitteilung: Lit.. Metallo Silanols and Metallo Siloxanes, 87. Mitteilung: Lit.. Metallo-silanole vom Typ C5R5(OC)2(Me3P)M - SiPh2OH (M = Cr, Mo, W): Darstellung nach der Dimethyldioxiran-Methode und Überführung in funktionalisierte Metallo-disiloxaneHerrn Professor Max Schmidt zum 70. Geburtstag gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1251-1255 
    Details
    ISSN: 0009-2940
    Keywords: Oxofunctionalization ; Dimethyldioxirane ; Metallo silanes ; Metallo silanols ; Metallo siloxanes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis and Reactivity of Silicon Transition Metal Complexes, 3332. Mitteilung: Lit. .  -  Metallo Silanols and Metallo Siloxanes, 8 7. Mitteilung: Lit. .  -  Metallo Silanols of the Type C5R5(OC)2(Me3P)M-SiPh2OH (M = Cr, Mo, W): Preparation According to the Dimethyldioxirane Route and Conversion into Metallo Disiloxanes Herrn Professor Max Schmidt zum 70. Geburtstag gewidmet.The metallo silanes C5R5(OC)2(Me3P)M-SiPh2H (4a-c), are converted into the corresponding metallo silanols C5R5(OC)2-(Me3P)M-SiPh2OH [R = H, M = Cr (6a); R = Me, M = Mo (6b); M = W (6c)] by oxofunctionalization with dimethyldioxirane (5). Treatment of 6b, c with the chlorosilanes Me2Si(R)Cl [R = H (3b), [R = Cl (3c)] in the presence of triethylamine gives access to the metallo disiloxanes C5Me5(OC)2(Me3P)M-SiPh2OSiMe2R (M = Mo, R = H (7a); M = W, R = Cl (7b)]. The structure of tungsten silanol 6c is determined by X-ray diffraction analysis.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951281217
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    Synthesis and Characterization of β-Phosphaenones An Investigation on the Conjugative Properties of the P=C Bond (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 465-476 
    Details
    ISSN: 0009-2940
    Keywords: Phosphaalkenes, C-halo, C-metal ; Phosphaacrylic acid ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Thermally and air-stable β-phosphaenones were synthesized by functionalization of Mes*P=CCl2 (1; Mes* = supermesityl = 2,4,6-tri-tert-butylphenyl). At low temperature, 1 was lithiated by halogen-metal exchange with n-butyllithium to give the phosphanylidene carbenoid (Z)-Mes*P=C(Cl)Li [(Z)-2] which reacted with acid chlorides to furnish the C-carbonyl-substituted phosphaalkenes (Z)-Mes*P=C(Cl)R (3: P = COtBu; 4: R = COPh; 5: R = COOEt). The reaction of (Z)-2 with carbon dioxide furnished the carboxylate 6, which was converted by treatment with pivaloyl chloride or trimethylsilyl chloride into the phosphaalkenes 7 and 8 functionalized at the carbon atom by an anhydride or a trimethylsilyl ester function, respectively. Acidification of 6 or hydrolysis of 8 with water in chloroform solution afforded the novel carboxylic acid (Z)-Mes*P=C(Cl)COOH (9). Spectroscopic investigations (NMR, UV, IR) of 3-9 and the X-ray structures of 3 and 4 are presented. Based on these properties and on theoretical calculations, the occurrence of conjugation in the β-phosphaenone system is discussed and compared with the well-known conjugation in normal enones.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951280506
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    Reactions of Phosphaalkenes with HexafluoroacetoneDedicated to Professor H. M. R. Hoffmann on the occasion of his 60th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 499-502 
    Details
    ISSN: 0009-2940
    Keywords: Phosphaalkenes ; Cycloadditions ; Insertion reactions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The dimethylamino-substituted phosphaalkene 1 reacts with hexafluoroacetone (HFA) with addition at the P=C bond to form the 1,5,2-dioxaphosphorinane 2. The structure of 2 was confirmed by an X-ray crystal structure analysis. The six-membered ring displays an envelope conformation with the phosphorus atom out of the plane, but the phosphorus is disordered over two sites. Reaction of P-trimethylsilyl-substituted phosphaalkenes with HFA proceeds with retention of the P=C double bond and insertion of HFA into the P—Si bond. Two isomeric products are obtained and are characterized by 1H-, 13C-, 19F-, and 31P-NMR spectroscopy, IR spectroscopy, mass spectrometry, and elemental analysis.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951280511
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    Monomere (Acetylacetonato)kupfer(I)-Komplexe von Alkinen und 1,4-Diinen (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 525-529 
    Details
    ISSN: 0009-2940
    Keywords: Copper complexes ; Acetylacetonate ; Alkynes ; 1,4-Diynes ; Titanocenes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Monomeric (Acetylacetonato)copper(I) Complexes of Alkynes and 1,4-DiynesMonomeric (η2-Me3SiC≡CSiMe3)Cu(acac) (3) is formed by the reaction of dimeric [(η2-Me3SiC≡CSiMe3)CuBr]2 (1) with two equivalents of Na(acac) (2). In a similar manner Me2-Si(C≡CSiMe3)2 (4) reacts with CuCl (5) and 2 to afford Me2Si[(η2-C≡CSiMe3)Cu(acac)]2 (6). In compounds 3 and 6 an alkyne unit is η2-coordinated to a monomeric Cu(acac) moiety with a copper atom in a planar environment. With the organometallic 1,4-diyne (η5-C5H4SiMe3)2Ti(C≡CSiMe3)2 (7), compound [(η5-C5H4SiMe3)2Ti(C≡CSiMe3)2]Cu(acac) (8) is formed. In 8 both Me3SiC≡C ligands of the 3-titanapenta-1,4-diyne fragment are η2-coordinated to a monomeric Cu-(acac) building block. The copper atom in 8 possesses a pseudo-tetrahedral environment (shown by X-ray analysis), built by the two Me3SiC≡C ligands of the (η5-C5H4SiMe3)2-Ti(C≡CSiMe3)2 moiety and the two oxygen atoms of the acetylacetonato ligand. 8 is additionally formed by the reaction of 3 or 6 with 7, or by treatment of [(η5-C5H4SiMe3)2Ti(C≡C-SiMe3)2]CuCl (9) with Na(acac) (2). The application of 3, 6, and 8 as precursors for the preparation of copper films in the CVD process of copper(I) is discussed.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951280515
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    Chiral Organometallic Reagents, XIIIPart XII: Ref.. Structural Aspects of Differentially Solvated Benzyllithium Contact Ion Pairs (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 551-556 
    Details
    ISSN: 0009-2940
    Keywords: Benzyllithium compounds ; Ion pairs ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The solvation and ion pair nature of α-(phenylthio)benzyllithium (2d) in THF solution were investigated by NMR-spectroscopic methods. The effect of additives such as diethylene-glycol dimethyl ether or of 12-crown-4 was studied. The results were compared to those of benzyllithium compounds 4 and 6, containing a pentaoxapentadecane ansa chain. These compounds exist as contact ion pairs in which lithium is held at the anionic carbon. This is reflected in the 6Li,13C coupling and 1H,6Li-HOESY contacts in the NMR spectra.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280604
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    Sulfur Compounds, Part 186Part 185: K. Bergemann, M. Kustos, P. Krüger, R. Steudel, Angew. Chem., in print.. The Synthesis of Cyclic Organosulfur Compounds from (C5H5)4Ti2C2S4 by Ligand Transfer Reactions (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 561-564 
    Details
    ISSN: 0009-2940
    Keywords: Titanocene complexes ; Organosulfur ligands ; Ligand transfer ; Organosulfur heterocycles ; Sulfur-sulfur bonds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The tetrathiaoxalate complex Cp4Ti2C2S4 (1) reacts with an equimolar amount of COCl2 to give the blue-green mononuclear complex Cp2TiC2S4CO (4). This reaction is analogous to the known reactions of 1 with SCl2 or S2Cl2. However, when 1 was treated with equimolar amounts of the bifunctional sulfenyl chlorides 1,2-C2H4(SCl)2 (5), 1,3-C3H6(SCl)2 (6) or 1,2-C6H4(SCl)2 (7), the bi- or monocyclic tetrakisdisulfanes C6H8S8 (9b), C8H12S8 (10), and C14H8S8 (11), respectively, were obtained. The X-ray crystal structure analysis of 11 · CS2 showed that 11 possesses Ci symmetry with a central exocyclic CC double bond similar to tetrathiafulvalenes: C6H4(μ-S2)2C=C(μ-S2)2C6H4.
    Additional Material: 2 Ill.
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    Norbornadiene(bipyridyl)molybdenum(II) Complexes: Synthesis, Structure and Reactivity of [Mo(CO)(C7H8)(C10H6R2N2)X2] (X = I, Br)Dedicated to Professor Dr. Helmut Werner on the occasion of his birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1007-1013 
    Details
    ISSN: 0009-2940
    Keywords: Tetracarbonyl(norbornadiene)molybdenum(0) ; Oxidative addition of I2 ; Dihalogeno(bipyridyl)molybdenum(II) complexes ; 7-Coordinated complexes ; Neutral and cationic molybdenum(II) complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of [Mo(CO)4(C7H8)] (1) with I2 gave the norbornadienemolybdenum(II) complex [Mo(CO)2(C7H8)I2]n≥1 (2), which existed in an equilibrium of two isomeric forms. In acetonitrile, 2 reversibly formed the adduct [Mo(CO)2-(C7H8)(NCCH3)I2] (3), whereas on treatment with 2,2′-bipyridine or 4,4′-di-2,2′-tBu-bipyridine, it gave stable 7-coordinated molybdenum(II) complexes, [Mo(CO)(C7H8)-(C10H8N2)I2] (4) and [Mo(CO)(C7H8)(C10H6tBu2N2)I2] (5), in good yield. In similar reactions, the related dibromomolybdenum compounds [Mo(CO)(C7H8)(C10H8N2)Br2] (6) and [Mo-(CO)(C7H8)(C10H6tBu2N2)Br2] (7) were prepared by oxidation of 1 with two equivalents of CuBr2. The X-ray structural analysis of 6 reveals that the geometry around the molybdenum atom is nearly perfectly pentagonal bipyramidal, with the CO and one of the bipyridyl rings perpendicular to the plane formed by the other ligands. The compounds 5 and 6 react with AgSbF6 by halogen abstraction to give cationic complexes, {[Mo(CO)(C7H8)(C10H8N2)Br]SbF6}n≥1 (8) and {[Mo(CO)(C7H8)(C10H6tBu2N2)I]SbF6}n≥1 (9): In acetone, 8 and 9 reversibly formed the adducts [Mo(CO)(C7H8)(C10H8N2)(acetone)Br]SbF6 (8′) and [Mo(CO)(C7H8)(C10H6tBu2N2)(acetone)I]SbF6 (9′); while on treatment with PMe3, the stable monomeric complexes, [Mo(CO)(C7H8)(C10H8N2)(PMe3)Br]SbF6 (10) and [Mo(CO)(C7H8)(C10H6tBu2N2)(PMe3)I]SbF6 (11), were isolated in almost quantitative yield. In the presence of KBr, compound 8′ reverted to the dibromo complex 6, whereas 9′ reacted to produce a 1:1:2 mixture of 5, 7 and the bromo(iodo) complex [Mo(CO)(C7H8)(C10H6tBu2N2)BrI] (12). The same mixture is available from the reaction of 5 with one equivalent of 7.
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    Graphical Abstract (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. A149 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951281018
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    Amino Substituted Tricarbonyl(cyclobutadiene)iron Complexes: Pd-Catalyzed Coupling of Iodocyclobutadiene Complexes with Amines (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1055-1058 
    Details
    ISSN: 0009-2940
    Keywords: Aminations ; Palladium catalysis ; Organometallic amines ; Coupling reactions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The coupling of the iodides 1 with amines under palladium catalysis affords the novel aminated cyclobutadiene derivatives 2 in preparative useful yields.
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    URL: http://dx.doi.org/10.1002/cber.19951281016
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    Masthead (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995) 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951281101
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    Chiral Carbanions, 1. Configurational Stability and Reactions of α-Acyloxy-Substituted α-Methylbenzyllithium Compounds (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1069-1077 
    Details
    ISSN: 0009-2940
    Keywords: Esters, 1-phenylethyl ; Carbanions, α-methyl-α-oxybenzyl, Configurational stability ; Ester - hydroxy ketone rearrangement ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Racemic and optically active 1-phenylethyl esters of pivalic, ( - )-camphanic and 2,4,6-triisopropylbenzoic acid were prepared. The esters 7a of pivalic acid were deprotonated with lithium 2,2,6,6-tetramethylpiperidide (Li-TMP) to form α-oxy-α-methylbenzyllithium compounds which are partly con-figurationally stable prior to acylation with starting material. Camphanic ester (-)-7b cannot be deprotonated by Li-TMP and tBuLi is added to the ester function to afford ketone (-)-12a. 1-Phenylethyl 2,4,6-triisopropylbenzoates 16 were transformed within minutes to carbanions 19 by using sBuLi/TMEDA in THF, hexane, toluene and sBuLi without TMEDA in toluene/20% diethyl ether at -78°C. The carbanions are configurationally stable only in toluene/20% diethyl ether and racemise partly in the other solvents. They react with a variety of electrophiles with either retention [MeOD, AcOD, (MeO)2CO, CICO2Me] or inversion (Me3SnCl) of configuration. Carbanions 19 rearrange on warming to -20°C to hydroxy ketone 24 with racemisation.
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    Metal Complexes with Tetrapyrrole Ligands, LXIX. Facile Synthesis and 13C-NMR Spectrum of Dichloro(octaethylporphyrinato)zirconium(IV) (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1131-1133 
    Details
    ISSN: 0009-2940
    Keywords: Zirconium(IV) octaethylporphyrin complex ; Dichlorozirconium(IV) porphyrin complex ; Precursor of organometallic compounds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The synthesis of dichloro(2,3,7,8,12,13,17,18-octaethylpor-phyrinato)zirconium(IV), Zr(oep)Cl2, from zirconium tetrachloride and octaethylporphyrin, H2(oep), is described. The reported synthesis is a new and simple route to this precursor of organometallic compounds. Zr(oep)Cl2 was characterized by elemental analyses, 1H- and 13C-NMR, UV/Vis, and mass spectra. Hydrolysis yielded a mixture of mono- and binuclear hydroxy zirconium(IV) porphyrins.
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    URL: http://dx.doi.org/10.1002/cber.19951281112
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    Derivatives of Aza-nido-tetraborane and Diaza-arachno-pentaborane from Tri-tert-butylazadiboriridine (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1-9 
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    ISSN: 0009-2940
    Keywords: 1-Aza-nido-tetraboranes ; 2,5-Diaza-arachno-pentaboranes ; 2,5-Diaza-nido-hexaboranes ; Boryl[diborane(4)yl]amine ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The Lewis acids RBH2 are added to the basis B-B bond of tri-tert-butylazadiboriridine, NB2tBu3 (1a), to give 5-alkyl-1,2,3-tri-tert-butyl-1-aza-nido-tetraboranes of type 3 (two endo-H atoms at B5) or type 4 (one H atom in a B2-B5 bridging position, one exo-H atom at B5), either as a mixture of 3 and 4 (3, 4b-d: R = Me, tBu, CMe2iPr) or with the isomer 4 in high excess (4e, f: R = Ph, sBu). The reaction of dialkylboranes R2BH with 1a yields 5,5-dialkyl-1,2,3-tri-tert-butyl-1-aza-nido-tetraboranes of type 4 (one H atom in a B2-B5 bridging position; 4g, h: R2 = Et2, cycloocta-1,5-diyl). In boiling THF, trialkylboranes BR3 transform 1a into NB2tBu2R which, expectedly, dimerizes spontaneously to give a dialkyltetra-tert-butyl-2,5-diaza-nido-hexaborane of type 2 (2a, b: R = Me, Et). The products of the addition of aminoboranes H2B=NRR' to 1a are identified as alkyl derivatives of 2,5-diaza-arachno-pentaborane, N2B3tH2tBu3RR' (5a-d, R/R' = H/Pr, H/tBu, Me/Me, Et/Et). The aminoborane H2B = NiPr2 with a sterically more demanding amino group hydroborates the B-B bond of 1a to give the acyclic product iPr2N=BH-B(tBu)-N(tBu)=B(tBu)H (6). In contrast to the B atoms, the N atoms in the electron-deficient cluster skeletons of 2-5 need not take part in (3c,2e) bonds of the s̰ type. The molecular structures of 4c, 5d, and 6 are confirmed by X-ray structural analyses.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951280102
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  • 83
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    New Pathways in Tellurium-Chalkogen-Nitrogen Chemistry: Preparations, Structures, and Properties of Telluraheterocycles (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 11-22 
    Details
    ISSN: 0009-2940
    Keywords: Thiaselenatelluradiazoles ; Thiaselenatelluratetrazocinium ; Tellurium(IV) compounds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Treatment of Se(NSO)2 with TeF4 in CH2Cl2 yields the compounds (4a) and (5b), while with TeBr4 after six months (2d) is formed. An almost quantitative yield of Cl4Te2N4S2 (6) is obtained from either Cl6Te2N2S (1a) and (CH3)3SiNSNSi(CH3)3 in CH2Cl2 at 20°C (2 d) or TeCl4 and (CH3)3SiNSO (molar ratio 1:2) in CH2Cl2 at 60°C (3 d). The use of (CH3)3SiOSi(CH3)3 as solvent in the last mentioned procedure gives 1a and small amounts of Cl2Te(NSO)2. Similarly, F2Te(NSO)2 is prepared from TeF4 and (CH3)3SiNSO in CH2Cl2. Dechlorination of 1a with (C6H5)3Sb leads to (2a), which is also produced from TeCl4 and [(CH3)3Si]2NSN[Si(CH3)3]2. When TeF4 is used instead of TeCl4 (molar ratio 3:1) the salt (7a) is formed. Similarly, (7b) is prepared from 2a and AsF5 or Ag+[AsF-6] in SO2. A new method for the preparation of bicyclic type 1 telluraheterocycles involves bromination of 2a yielding Cl2Br4Te2N2S (1b). Dehalogenation with (C6H5)3Sb converts 1b into (2b). When 2b is treated with Br2 in CH2Cl2 an oxidative halogenation takes place with formation of Br6Te2N2S (1c). Metathetical exchange between 2b and Ag+[AsF-6] gives (7c). Isostructural S(NSO)2 reacts with TeCl4 for several weeks at 60°C in CH2Cl2 to form S4N4. TeCl4 and [S5N+5][Te3Cl-3], in contrast to the corresponding reaction with Se(NSO)2. The molecular structures of 4a, 7b, 8, and [S5N+5][Te3Cl-13] have been determined by X-ray diffraction methods. Spectroscopic data for all new compounds are presented.
    Additional Material: 9 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951280103
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  • 84
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    Tellurium Polycations by Oxidation of Tellurium with Tungsten Halides Syntheses and Crystal Structures of Te6(WOCl4)2 and Te6I2(WCl6)2 (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 23-27 
    Details
    ISSN: 0009-2940
    Keywords: cyclo-Hexatellurium(2+) ; 1,4-Diiodo-cyclo-hexatellurium(2+) ; Hexachlorotungstate(V) ; Tetrachlorooxotungstate(V) ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: WOCl4 reacts at 200°C with tellurium in a sealed, evacuated ampoule with the formation of Te6(WOCl4)2. The structure consists of six-membered tellurium rings in a boat conformation with significant transannular interactions and of pyramidal WOCl4 units which are linked by linear asymmetric O...;W=O bridges to polymeric (WOCl4)n, chains. The observed paramagnetism is consistent with the ionic formulation Te2+6[(WOCl-4)2]n. In the reaction of WCl6, I2 and Te in a 2:1:6 ratio Te6I2(WCl6)2 is formed at 150°C. The crystal structure consists of Te6I2+2cations and of slightly distorted octahedral WCl-6 anions. The Te6I2+2 ions are isostructural with Se6I2+2 and consist of a six-membered ring of Te atoms in the chair conformation with two I atoms bound in the 1,4-positions.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951280104
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  • 85
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    Two Alternatives of Heteroallene Insertion in Metal  -  Ligand Bonds of Five-Coordinate Ruthenium(II) and Osmium(II) Complexes [MXY(CO)(PiPr3)2]Herrn Professor Nils Wiberg zum 60. Geburtstag gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 41-47 
    Details
    ISSN: 0009-2940
    Keywords: Ruthenium complexes ; Osmium complexes ; Insertion reactions ; Carbon disulfide ; Carbon dioxide ; Methyl isothiocyanate ; Zwitterionic ligands ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The five-coordinate chloro(hydrido)- and hydrido(iodo)ruthenium(II) and -osmium(II) compounds [MHX(CO)(PiPr3)2] (1, 2, 6, 7) react with CS2 to give the octahedral dithioformato complexes [MCl(CO)(PiPr3)2(η2-S2CH)] (3, 4, 8, 9) in excellent yields. In the initial step, an addition of the heteroallene to the metal center occurs which is followed by insertion of CS2 into the M - H bond. On treatment of the dichlororuthenium(II) derivative [RuCl2(CO)(PiPr3)2] (10), which is prepared from RuCl3 · aq and PiPr3 in methanol, with carbon disulfide insertion into one of the Ru - PiPr3 bonds takes place to give the six-coordinate ruthenium(II) complex 12 with zwitterion -S2CPiPr3+ as a chelating ligand. While the reaction of [OsH(SPh)(CO)(PiPr3)2] (13) with MeSCN leads to addition of the thionitrile to the metal center, the starting material reacts with MeNCS by insertion of the heteroallene into the Os - SPh bond to give two stereoisomers 15a, b, in which the nitrogen atom of the chelate ring is either cis or trans to the hydrido ligand. The octahedral methoxydithiocarbonato- and formatoosmium(II) compounds 16 and 17 are prepared from 2 and CS2 or CO2 in the presence of NaOMe. The crystal and molecular structures of 4 (M = Os), 12 and 15a have been determined.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951280107
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  • 86
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    Synthese und Struktur von Cobalt(III)-Komplexen mit doppelt deprotoniertem Anhydroerythrit, Methyα-D-mannopyranosid und Methyl-β-D-galactopyranosid (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 75-79 
    Details
    ISSN: 0009-2940
    Keywords: Cobalt(III) complexes ; Dianionic polyolato ligands ; Anhydroerythritol ; α-DMannopyranoside, methyl ; α-DGalactopyranoside, methyl ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Polyol Metal Complexes, XII[1].  -  Synthesis and Structure of Cobalt(III) Complexes with Doubly Deprotonated Anhydroerythritol, Methyl α-DMannopyranoside, and Methyl α-DGalactopyranosideThe polyols anhydroerythritol (AnEryt), methyl α-D-mannopyranoside (Me-α-D-Manp), and methyl α-D-galactopyrano-side (Me-α-DGalp) are deprotonated twice to form the cobalt(III) complexes [(en)2Co(AnErytH-2)]I (1), δ-[(en)2- Co(Me-α-DManp3,4H-2)]ClO4 · NaClO4 · 2H2O (2), and δ-[(en)2Co(Me-α-DGalp2,3H-2)]ClO4·H2O (3), resp., in aqueous, alkaline solutions of trans-[(en)2CoCl2]Cl. The crystal structures of 1-3 have been determined by X-ray diffraction.
    Additional Material: 4 Tab.
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    URL: http://dx.doi.org/10.1002/cber.19951280111
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  • 87
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    Contribution to the Chemistry of Boron, 222.  -  Chemistry of Diborane(4) Derivatives: Mixed Tetraaminodiboranes(4) and Additions of Diborane(4) Derivatives to an Amino-imino-borane (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 93-93 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280115
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  • 88
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    Protolysis of Tri-tert-butylazadiboriridine: Formation of a B-H-B Bridge in Unusual Coordination (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 99-103 
    Details
    ISSN: 0009-2940
    Keywords: Tri-tert-butylazadiboriridine ; (Hydroboryl)(methoxyboryl)amine ; 2,3-μ-Hydro-1,2,3-azoniadiborata-l-cyclopropenes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The B—B bond of tri-tert-butylazadiboriridine [—NR—BR—BR—] (R = tBu; 1) is oxidized by MeOH to give the (hydroboryl)(methoxyboryl)amine H—BR=NR-BR(OMe) (2a). μ-2,3-Hydroazoniadiborata-1-cyclopropenes [=NR—BR(X)—μH—BR=] (3a, 3c-e) are formed by the action of the acids HX upon 1. A similar hydrogen bridge as in 3a-e is formed during the hydroboration of 1 by catecholborane, yielding 3f. A B atom is identified in the products 3a-f to be planarly coordinated by four atoms, two of which are forming a BHB three-center bond with that B atom. This is a novel bonding situation in boron chemistry. The structures of the products are deduced from 1H-, 11B-, and 13C-NMR spectra and are confirmed by X-ray structural analyses of 2a, 3a, and 3c.
    Additional Material: 2 Tab.
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    URL: http://dx.doi.org/10.1002/cber.19951280203
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  • 89
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    Synthese und Struktur zweikerniger Kupfer(II)-Komplexe eines neuen Hexaaza-Makrocyclus mit verbrückenden Oxalat- und Acetat-Ionen (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 115-119 
    Details
    ISSN: 0009-2940
    Keywords: Polyazamacrocycles ; Dinucleating ligands ; Copper complexes ; Oxalate complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis and Structure of Dinuclear Copper(II) Complexes of a Novel Hexaaza Macrocycle Containing Bridging Oxalate and Acetate IonsNon-template Schiff base [2 + 2] condensation of pyridine-2,6-dicarbaldehyde with 1,4-diamino-2-butyne yields the hexaazamacrocyclic ligand 1, which is converted to 2 by NaBH4 reduction of the imino groups. Two dinuclear copper(II) complexes of 2 containing oxalate and acetate ions, [(2)Cu2(μ-C2O4)](BPh4)2 (3) and [(2)Cu2(μ-CH3CO2)(OH2)](PF6)2.25-(NO3)0.75 (4), were characterized by X-ray crystallography. The oxalate ligand in 3 forms a (μ-η4:η4) bridge between the copper atoms. Compound 4 contains a syn-anti-bridging acetate ion. The Cu-Cu distances are 5.315 Å in 3 and 4.746 Å in 4, respectively. Oxalate can be separated from other carboxylates in aqueous solution by selective binding to the [(2)Cu2] unit and precipitation of 3.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280205
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  • 90
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    Synthesis, X-Ray Crystal Structure and Magnetic Characterization of the First “Ni3S4N3” Nickel Thiolate Cluster (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 125-129 
    Details
    ISSN: 0009-2940
    Keywords: Nickel cluster ; Nickel thiolate ; Hydrogenase ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The tridentate N,O,S-ligand (RS)-2-[(2-mercapto-1-methylamino)ethyl]phenol (rac-1) was prepared from ortho-hydroxy-chloroacetophenone in three steps. When this ligand was treated with nickel(II) acetate, the novel “Ni3S4N3” cluster rac-3 was obtained. The X-ray crystal structure of rac-3 unambiguously revealed the pseudo-C3 symmetric structure of this novel nickel cluster, which is made up by three nickel ions, one sulfide sulfur atom, and three homochiral ligand molecules, each contributing one thiolate sulfur atom and one amine nitrogen atom to the ligation of the metal ions. According to NMR-spectroscopic results, this highly symmetric structure is maintained in solution. The magnetic studies revealed diamagnetic behavior in the solid state, although antiferromagnetic interaction of the metal centers cannot absolutely be excluded.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280207
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  • 91
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    Stereospecific Ligand Substitutions in Manganese(I) Complexes (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 151-155 
    Details
    ISSN: 0009-2940
    Keywords: Tripodal ligands ; Phosphane ligands ; Thioethers ; Manganese complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Treatment of fac-[(P2SPh-P,P')Mn(CO)3Br] and fac-[(PS2Ph-P,S)Mn(CO)3Br] [P2SPh: Z = PPh2; PS2Ph: Z = SPh in CH3C-(CH2PPh2)(CH2SPh)(CH2Z)] with silver hexafluorophosphate yields the η3-tripodal manganese complexes [(P2SPh-P,P',S)Mn(CO)3]PF6 (7) and [(PS2Ph-P,S,S')Mn(CO)3]PF6 (9), respectively, whereas the reaction of CH3C(CH2PPh2)2-(CH2SH) with Mn(CO)5Br gives directly [CH3C(Ph2-PCH2)2(CH2S)-P,P',S]Mn(CO)3 (11). Both ionic complexes 7 and 9 undergo stereospecifically ligand substitution upon treatment with Br-, I-, N-3, SCN- and CN- to give syn-fac-[(P2SPh-P,P')Mn(CO)3X] and syn-fac-[(PS2Ph-P,S)Mn(CO)3X] (X = Br, I, SCN, N3, CN) respectively, but the neutral complex 11 fails to undergo such a substitution reaction with these ions. However, reaction of I- with the complex [(PSMe)-P,P',S]Mn(CO)3]BF4 (20) [P2SMe = CH3C(CH2-PPh2)2(CH2SCH3)), which is obtained from the S-alkylation of 11 with (CH3)3OBF4, affords syn-fac-[(P2SMe)-P,P']Mn(CO)3I (22s) exclusively. The possible reaction mechanism of this ligand substitution is discussed.
    Additional Material: 1 Tab.
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    URL: http://dx.doi.org/10.1002/cber.19951280211
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  • 92
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    Oxacycloalkenyliden-Komplexe von Chrom, Molybdän und Wolfram: Synthese, Anellierung mit Alkinen und Diels-Alder-Reaktionen mit Dienen (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 157-161 
    Details
    ISSN: 0009-2940
    Keywords: Carbene ligands ; Chromium complexes ; Molybdenum complexes ; Tungsten complexes ; Annulation reaction ; Diels-Alder reaction ; Oxacyclopentenylidene ligands ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reactions of Complex Ligands, LXI[1]. - Oxacycloalkenylidene Complexes of Chromium, Molybdenum, and Tungsten: Synthesis, Their Annulation with Alkynes and Diels-Alder Reaction with DienesLithiiated propargylic ether 1 reacts with M(CO)6 (M = Cr, Mo, W) to give the 2-oxacyclic carbene complexes 2-4 containing an α,β-double bond and a cyclic acetal structure which serves as a protected benzoyl group. Reaction of the chromium complex 2 with tolan leads to an acyl hydroquinone derivative 5. The tungsten complex 3 undergoes a [4 + 2] cycloaddition with cyclopentadiene to give two diastereomeric oxatricyclic carbene complexes 6 and 7 with an endo/exo selectivity of 3:1. The stereochemistry of the Diels-Alder reaction is controlled by the configuration of the acetal carbon center.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280212
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  • 93
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    Darstellung und Komplexierung von 1,4-Dimethyl-2,3-bis(isopropyliden)-1,4-diboratetralinHerrn Professor Nils Wiberg zum 60. Geburtstag gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 183-185 
    Details
    ISSN: 0009-2940
    Keywords: 1,4-Diboranaphthalines ; 2,7-Diboradodeca-1,3,9,11-tetraenes ; Cobalt complexes ; Rhodium complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis and Complexation of 1,4-Dimethyl-2,3-bis(isopropylidene)-1,4-diboratetraline1,4-Dimethyl-2,3-bis(isopropylidene)-1,4-diboratetraline (2) is obtained from o-dilithiumbenzene and 2,5-dimethyl-3,4-bis(chloromethylboryl)-2,4-hexadiene in 61% yield. Its complexation with cyclopentadienylbis(ethene)cobalt leads to the triple-decker bis(η5-cyclopentadienylcobalt)-μ-η6,η6-1,4-dimethyl-2-isopropenyl-3-isopropyl-1,4-dihydro-1,4-dibora-naphthaline (3) in low yield. However, the reaction of 2 with (C5H5)Rh(C2H4)2 and (C5Me5)Co(C2H4)2 originates complexes of a tricyclic ligand formed from 2 via conrotatoric [2 + 2] cycloaddition of the isopropylidene groups. (η5-Cyclo-pentadienylrhodium)-η6-tricyclo-[6.4.0.03,6]-2,4,4,5,5,7-hexamethyl-2,7-diboradodeca-1,3,9,11-tetraene (4), (η5-pentamethylcyclopentadienylcobalt)-η6-tricyclo-[6.4.0.03,6]-2,4,4,5,5,7-hexamethyl-2,7-diboradodeca-1,3,9,11-tetraene (5) and its related dinuclear complex 6 could be isolated in 29, 10, and 31%, respectively. Their constitutions are derived from spectroscopic data and proven by X-ray structure analysis of 4.
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    URL: http://dx.doi.org/10.1002/cber.19951280216
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    Zerfall von Nitrosylazid, N4O: Existieren auch cyclische Stickstoff-Oxide? (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 201-203 
    Details
    ISSN: 0009-2940
    Keywords: Nitrogen oxides ; Calculations, ab initio ; Tetranitrogen monoxide ; Dinitrogen monoxide ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Decomposition of Nitrosyl Azide, N4O: Are Cyclic Nitrogen Oxides Existent?The unimolecular decomposition of nitrosyl azide (tetranitrogen monoxide), N4O, was studied at the electron-correlated, spin-restricted RMP2 level with the 6-31G(d,p) and 6-31+G* basis sets. Frequency calculations were performed at 6-31+G* on the optimized structures. It is demonstrated that the experimentally established trans-trans-N4O (Cs) may either interconvert into cis-cis-N4O which upon decomposition forms cyclic N4O (C2v) as an intermediate species to finally give N2O (C∞v) and N2, or trans-trans-N4O may directly dissociate into cyclic N2O (C2v) and N2. All structures determined were rationalized by energy hypersurface calculations.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951280220
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    Reactions of Diazo Compounds and Chiral Rhenium Alkylidene Complexes of the Formula [(η5-C5H5)Re(NO)(PPh3)(=CHR)]+ PF-6 A Versatile and Highly Stereoselective Route to Alkene Complexes (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 213-220 
    Details
    ISSN: 0009-2940
    Keywords: Rhenium complexes ; Alkylidene complexes ; Diazo compounds ; Alkene complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The methylidene complex [(η5-C5H5)Re(NO)(PPh3)(=CH2)]+ PF-6 or the Re—CD2 analog react with diazo compounds N2CHR [R — H, Si(CH3)3, COPh, CO2C2H5] in CH2Cl2 at -80°C to give alkene complexes [(η5-C5H5)Re(NO)(PPh3)(η2-H2C=CHR)]+ PF-6 or D2C=CHR analogs. The two Re=C geometric isomers of benzylidene complex [(η5-C5H5)Re-(NO)(PPh3)(=CHPh)]+ PF-6 and CH2N2 react to give opposite configurational diastereomers of styrene complex [(η5-C5H5)Re(NO)(PPh3)(η2-H2C=CHPh)]+ PF-6. Stereochemical features of these reactions are analyzed in detail, and are interpreted in terms of models involving (a) attack of the diazo compound upon the Re=C face opposite to the bulky PPh3 ligand, (b) an antiperiplanar disposition of the Re=C and C—N2 bonds in the transition state, utilizing the diazo carbon face that minimizes interactions of the substitutent (R) and cyclopentadienyl ligand, and (c) N2 loss from the resulting intermediate [(η5-C5H5)Re(NO)(PPh3)(CHR′CHRN2)]+ PF-6 via a conformer with antiperiplanar P—Re—CHR′—C and Re—CHR′—CHR—N linkages, with anchimeric assistance of the rhenium fragment d orbital HOMO from the backside.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280303
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    Contributions to the Chemistry of Boron, 227Part 226: Ref.. The P-centered Chemistry of [(Di-tert-butylphosphanyl)imino]-(2,2,6,6-tetramethylpiperidino)boraneDedicated to Professor Helmut Werner on the occasion of his 60th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 205-212 
    Details
    ISSN: 0009-2940
    Keywords: Borane, [(di-tert-butylphosphanyl)imino](2,2,6,6-tetramethylpiperidino) dimer ; Phosphonium, di-tert-butylmethyl[(2,2,6,6-tetramethylpiperidinoborylene)imino]iodide ; Haloboration ; Hydroboration ; Metal carbonyl complexes of [(di-tert-butylphosphanyl)imino](2,2,6,6-tetramethylpiperidino)borane ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The elements oxygen, sulfur, and selenium add to the P atom of the title borane 1. In contrast to the formation of tmp—B≡N—P(X)tBu2 (X = S, Se), the P oxide (X = O) dimerizes to [tmp—B≡N—P(O)tBu2]2 (5) with an eight-membered flat boat-shaped B2N2P2O2 ring. Borane 1 reacts readily with Mel to yield a phosphonium salt 8 and with BBr3 to give an adduct 9 with a B—P bond. In contrast, bis(dichloroboryl)-methane not only adds to 1 to generate a coordinate B—P bond but also chloroborates the B≡N triple bond, the final product being a new five-membered heterocycle 10. Similarly, the BH3 component of BH3·SMe2 first adds to the P atom of 1 followed by reaction of a second mol of BH3·SMe2 which hydroborates the B≡N triple bond. Finally, metal carbonyl fragments add only to the P atom of 1, demonstrating also that the chemistry of the molecule 1 is dominated by the basicity of its P center.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280302
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    Synthese und Charakterisierung stabiler Bis(phosphonio)isophosphindolylium-Carbonylmetallate und eines kationischen Bis(phosphonio)isophosphindolylium-Gold-KomplexesHerrn Professor Alfred Schmidpeter zum 65. Geburtstag gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 259-266 
    Details
    ISSN: 0009-2940
    Keywords: Bis(phosphonio)isophosphindolylium cation ; Gold complexes ; Bis(phosphonio)isophosphindolylium carbonylmetallates ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis and Characterisation of Stable Bis(phosphonio)isophosphindolyliumcarbonylmetallates and a Cationic Bis(phosphonio)isophosphindolylium-Gold ComplexHerrn Professor Alfred Schmidpeter zum 65. Geburtstag gewidmet.Reaction of 1,3-bis(triphenylphosphonio)isophosphindolylium bromide, [L+][Br-] (1a), with Tl[Co(CO)4], Na[MoCp-(CO)3], or Na[WCp(CO)3] (5a-c) yields the corresponding ionic isophosphindolylium-carbonylmetallates, 6a-c. Whereas 1a fails to react with neutral metal carbonyls, a mixture of ionic complexes of the type [LAuX+][AuYZ-] (7a, X, Y, Z = Cl or Br) is formed by reaction with two equivalents of AuCl. Treatment of AuCl with the triflate [L+][OTf-] (1b), which is accessible from 1a via anion metathesis, furnishes [LAuCl+][OTf-] (7b). Both the carbonylmetallate 6c and the complex 7b have been characterized by X-ray structure analyses. 7b displays enhanced reactivity as compared to 1b towards MeOH and H2O, forming the addition products 8 and 9a, b, the latter existing as two different diastereomers. Reactions of 7b with LiF, (Me2N)3P=O, and (Et2N)2C=NH), respectively, proceed via ligand exchange to yield equilibrium mixtures containing the cations [L+] and [LAuCl+].
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280309
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    Darstellung von phosphor- und fluorhaltigen Calix[4]aren-Derivaten. Konformationsanalyse, Trennung der Konformere und Röntgenstrukturanalyse an einem KonuskonformerHerrn Professor Helmut Werner zum 60. Geburtstag gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 267-273 
    Details
    ISSN: 0009-2940
    Keywords: Calix[4]arenes ; Supramolecular chemistry ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Preparation of Phosphorus -  and Fluorine-Containing Calix[4]arene Derivatives. Conformational Analysis, Separation of the Conformers, and X-Ray Crystal Structure Analysis of a Cone ConformerHerrn Professor Helmut Werner zum 60. Geburtstag gewidmet.The Calix[4]arene 1 reacts with hexamethyldisilazane or (diethylamino)trimethylsilane to form the bis-trimethylsilyl-ated derivative 2. Treatment of 2 with PF2C1 gives the mono-and bis-difluorophosphites 3 and 4, which react with elimination of Me3SiF or PF3 to yield the monofluorophosphite derivative 5. All four OH hydrogen atoms in 1 are replaced by lithium on reaction with nBuLi with formation of the tetrali-thiated product 6. This has been allowed to react with the Pchlorophosphorinanones 7-9. From 7 the cone conformer 10a is formed, whereas in the case of 8 and 9 a mixture of all four possible conformars 11a-d and 12a-d is obtained. The pure conformers 12a-d are isolated. By refluxing the cone conformer 12a in tetrachloroethane a conformational conversion is effected. In order to evaluate its coordinating ability, 12a was allowed to react with dichloro(cycloocta-1, 5-diene)platinum(II) to form the trans-disubstituted complex 13. In the case of 12a (acetonitrile solvate) a single-crystal X-ray structure analysis has been conducted. The molecule displays a cone conformation, whereby two of the opposing phenyl rings are approximately parallel and the other two approximately perpendicular to each other.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280310
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    Synthese kationischer η2-Phosphinocarben-Komplexe des Molybdäns und WolframsHerrn Professor Hubert Schmidbaur zum 60. Geburtstag gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 289-292 
    Details
    ISSN: 0009-2940
    Keywords: η2-Phosphinocarbene complexes of molybdenum and tungsten ; Carbyne complexes ; Chlordimethylphosphane ; Chlordiphenylphosphane ; Electrophilic addition ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis of Cationic η2-Phosphinocarbene Complexes of Molybdenum and TungstenHerrn Professor Hubert Schmidbaur zum 60. Geburtstag gewidmet.The reaction of chlordimethylphosphane or chlordiphenyl-phosphane and sodium tetraphenylborate with dicarbonyl(η5-cyclopentadienyl)carbyne complexes of molybdenum and tungsten enables the direct conversion of a M=CR group into a M=C(R)—PR2 unit providing dicarbonyl substituted η2-phosphinocarbene complexes in high yields. In the absence of Na[BPh4] a base induced carbonyl carbene coupling reaction affords η3-phosphinoketene complexes.
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280313
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  • 100
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    Charge-Transfer-Komplexe von Metalldithiolenen, XVIII. Ionenpaare von Dithiolencobaltaten mit Bipyridinium-Akzeptoren (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 303-307 
    Details
    ISSN: 0009-2940
    Keywords: Cobalt dithiolenes ; Charge-transfer complexes ; Electrical conductivity ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Charge-Transfer Complexes of Metal Dithiolenes, XVIII. - Ion Pairs of Dithiolene Cobaltates with Bipyridinium AcceptorsIon pair charge-transfer (IPCT) complexes of the type {A2+[Co(mnt)2]2-}, mnt2- = cis-1,2-dicyano-1,2-ethenedithiolate, A2+ = a bipyridinium derivative, posses IPCT bands in the range from 590 to 950 nm. An X-ray structure analysis of {BQ2+[Co(mnt)2]2-}, BQ2+ = 6,7,8,9-tetrahydrodipyrido[1,2-a:2,1-c][1,4]diazocinium, reveals that the strongly twisted acceptor and planar donor do not form mixed stacks, as usually observed in less twisted systems. Electrical conductivities of pressed powder pellets are in the range of 10-15 to 10-7 Ω-1 cm-1 and do not exhibit a simple correlation with the driving force of electron transfer between the ion pair components. The cis-trans isomerization of an ethene-bridged methyl viologen acceptor leaves the conductivity almost unchanged.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280315
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