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  • 1
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    Series available for loan
    Untersuchungen zur Herstellung und Auswertung von Röntgenstereogrammen im Bereich der medizinischen Röntgendiagnostik (1974)
    Hannover
    Associated volumes
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    Call number: SR 99.0139(55)
    In: Wissenschaftliche Arbeiten der Fachrichtung Vermessungswesen der Universität Hannover
    Type of Medium: Series available for loan
    Pages: III, 120 S.
    Series Statement: Wissenschaftliche Arbeiten der Lehrstühle für Geodäsie, Photogrammetrie und Kartographie an der Technischen Universität Hannover 55
    Language: German
    Location: Lower compact magazine
    Branch Library: GFZ Library
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  • 2
    Electronic Resource
    Electronic Resource
    Chiral Chelate Ligands Based on a Neopentane Framework; Introducing Indenyl and Fluorenyl Donor Groups (1999)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 1999 (1999), S. 2187-2199 
    Details
    ISSN: 1434-1948
    Keywords: Ansa compounds ; Cp-derived chelate ligands ; Neopentane chemistry ; Spiro compounds ; Tripodal ligands ; Cyclopentadienyl compounds ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The neopentane-derived functionalized oxetane O(CH2)2C(CH3)(CH2OMs), 1, reacts with indenyllithium (LiInd) or fluorenyllithium (LiFlu) to produce the derivatives O(CH2)2C(CH3)(CH2R) (R = indenyl, fluorenyl), 2. The oxetane ring of 2 undergoes nucleophilic ring-opening by reaction with LiPR′2 to give the chiral chelate ligands (HOCH2)(CH3)C(CH2R)(CH2PR′2) (R = indenyl, fluorenyl), 5. Nucleophilic ring-opening by LiInd or LiFlu is possible too, resulting in the functionalized ansa-Cp ligands (HOCH2)(CH3)C(CH2R)(CH2R′) (R, R′ = indenyl, fluorenyl), 12. Electrophilic ring-opening of 2 with HBr to give (HOCH2)(CH3)C(CH2R)(CH2Br) (R = indenyl, fluorenyl), 3, is also possible. The alcohol function of 3 may be activated directly, whereas activation of this group in 5 is only possible after BH3 protection of the phosphane function. The mesylates (MsOCH2)(CH3)C(CH2R)(CH2Br) (R = indenyl, fluorenyl), 4, undergo, under basic conditions, spiro cyclization to produce spirocyclobutane derivatives 9 with the α-carbons of the five-membered cycles acting as the spiro centres. Substitution of the mesylate group of 4 by PR2 nucleophiles is therefore not possible. Ansa-Cp derivative (MsOCH2)(CH3)C(CH2Ind)(CH2Flu), 12c also reacts with LiPPh2 with spiro cyclization to produce 9d, instead of giving the substitution product. Tripodal ligands (CH3)C(CH2R)(CHPPh2)2 (R = indenyl, fluorenyl), 11, are accessible by the reaction of (MsOCH2)(CH3)C(CH2PPh2)2 with LiInd or LiFlu. All compounds are fully characterized by the usual spectroscopic and analytical techniques including single-crystal X-ray analyses in several cases.
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  • 3
    Electronic Resource
    Electronic Resource
    Neopentane-Based Tripodal CpL2 Ligands: Synthesis and Reactions of CH3C(CH2-η5-C5H4)(CH2-η1-PPh2)2RuCl; Hindered Rotation of Vinylidene Ligands (2000)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 2000 (2000), S. 33-50 
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    ISSN: 1434-1948
    Keywords: Tripod ligands ; Hindered rotation of vinylidene ligands ; CpML2 chelate ligands ; Ruthenium ; Carbenes ; Carbene-type ligands ; Cyclic voltammetry ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The tripodal ligand [CH3C(CH2C5H4)(CH2PPh2)2]- reacts with RuCl2(PPh3)3 to produce CH3C(CH2-η5-C5H4)(CH2-η1-PPh2)2RuCl, [tripodCpL2RuCl], 1. Complex 1 undergoes substitution of the chlorine function with various nucleophiles L′ to produce [tripodCpL2RuL′]+. The carbonyl derivative (L′ = CO) 2, isonitrile (L′ = RNC) 3, nitrile compounds (L′ = RCN) 4, and a tolane adduct (L′ = η2-PhC≡CPh) 5 are obtained when 1 is treated with the appropriate ligands in polar solvents. Halide acceptors (e.g. TlPF6) are generally needed to promote these reactions. The cyanide derivative tripodCpL2RuCN (3a) is alkylated by F3CSO3CH3 to give the isonitrile derivative [tripodCpL2RuCNMe]+3b. Terminal alkynes HC≡CR produce vinylidene compounds [tripodCpL2RuL′]+, where L′ = C=CHR (R = tBu, 7b; R = Ph, 7c), or allenylidene derivatives, L′ = C=C=CPh2 (6), depending on the nature of R (R = CPh2OH for synthesis of 6). Trimethylsilylacetylene gives the parent vinylidene species, L′ = C=CH2 (7a), which is transformed to the Fischer-type carbene compound, L′ = C(OMe)Me (8), upon treatment with methanol. The vinylidene species 7 are deprotonated by NaOMe to produce the alkynyl compounds tripodCpL2RuC≡CR (9). Methylation of 9 with F3CSO3CH3 results in the vinylidene derivatives L′ = C=C(Me)R (R = tBu, 7d; R = Ph, 7e), having two organic substituents at the terminal carbon centre. For all vinylidene compounds with two different substituents at their terminal carbon atom, hindered rotation of the single-faced vinylidene π-ligand about its Ru-C bond is observed. Analysis by 31P-NMR spectroscopic coalescence measurements as well as line-shape analyses reveals activation enthalpies of around 40 kJmol-1 for this rotation, with small activation entropies of around ±10 Jmol-1K-1. Solid-state structures of nine compounds of the type [tripodCpL2RuL′]+n (n = 0, 1) demonstrate the remarkable conformational rigidity of the tripodCpL2Ru template. They also show that the possible strain imposed by linking the Cp ligand and the two donor groups L in one and the same chelate scaffolding does not appear to impose a serious steric strain on these templates.
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  • 4
    Electronic Resource
    Electronic Resource
    Synthesis of the Germanium(I) Compounds [Ge2Hal4]2- and Their Reductive Condensation to Octahedral [Ge6]2- Clusters in an Organometallic Environment (2000)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 2000 (2000), S. 879-887 
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    ISSN: 1434-1948
    Keywords: Germanium(I) ; Tetrahalgenodigermanate(2-) ; Octahedral [Ge6]2- clusters ; Organometallic derivatives ; Carbonyl complexes ; Chromium ; Tungsten ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: GeI2 reacts with [M2(CO)10]2- (M = Cr, W) leading to reductive coupling of two GeI2 units to produce the [Ge2I4]2- ligands of [{(OC)5M}I2Ge-GeI2{M(CO)5}]2- (1a and 2a). The [Ph4P] salts of these anions have been characterised by X-ray structure analyses as have the [Ph4P] salts of [{(OC)5M}Cl2Ge-GeCl2{M(CO)5}]2- (1b and 2b) obtained from the iodo derivatives 1a and 2a by halide metathesis with [Ph4P]Cl. Treatment of GeI2 with [W2(CO)10]2- in the presence of 2,2′-bipyridine leads to [{(OC)5W}I2Ge-Ge(bipy){W(CO)5}] (3). The digermanium ligands in 1-3 contain germanium in the unconventional formal oxidation state +I. Reductive condensation of [{(OC)5Cr}I2Ge-GeI2{Cr(CO)5}]2- (1a) by addition of [Cr2(CO)10]2- leads to the octahedral cluster [{(OC)5Cr}6Ge6]2- (4) in a yield of 40%. The sequence of reactions as reported describes the first systematic approach to the synthesis of [E6]2- clusters.
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  • 5
    Electronic Resource
    Electronic Resource
    Four-Coordinate Group-14 Elements in the Formal Oxidation State of Zero - Syntheses, Structures, and Dynamics of [{(CO)5Cr}2Sn(L2)] and Related Species (1998)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 1998 (1998), S. 703-720 
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    ISSN: 1434-1948
    Keywords: Germanium ; Tin ; Lead ; 119Sn NMR ; Dynamic NMR ; Salt metathesis ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The sodium salts Na2[{(CO)5M}2EX2] (M = Cr, Mo, W; E = Ge, Sn, Pb; X = Cl, I, OOCCH3) react with 2,2′-bipyridine (bipy) to form neutral compounds [{(CO)5M}2E(bipy)] (E = Sn: 1a-1c; E = Ge: 3a; E = Pb: 4). 1,10-Phenanthroline (phen) analogues of compounds 1a-1c and 3a [{(CO)5M}2E(phen)] (E = Sn: 1d-1f, E = Ge: 3b) are as well accessible. The 2,2′-bipyridine ligand in 1 may be formally replaced by two pyridine (py) ligands resulting in [{(CO)5M}2Sn(py)2] (1g: M = Cr, 1h: M = W). The bis-bidentate ligand 2,2′-bipyrimidine (bpmd) is found to coordinate just one [{(CO)5M}2Sn] entity in [{(CO)5M}2Sn(bpmd)] (2b: M = Cr, 2c: M = W). The biimidazolato (biim) ligand binds two [{(CO)5Cr}2Sn] moieties in [{(CO)5Cr}2Sn(biim)Sn{Cr(CO)5}2]2-, 2a. It is shown by 1H-NMR that the pyrimidine entities in these compounds (2b, 2c) are able to rotate by a full 180° turn-around with respect to one another. This process must involve complete de-coordination of at least one of the two nitrogen donors in again at least one of the chelate cycles, the activation energy for this process being around 60 kJ/mol. By 119Sn-NMR spectroscopy of almost all of the tin compounds described it is shown that equilibria between [{(CO)5M}2Sn(L2)] and [{(CO)5M}2Sn(L)] + L exist in all cases. From the temperature dependence of the δ values it is concluded that the activation barriers for this association/dissociation process is below 10 kJ/mol. The structures of all new compounds are documented by X-ray analyses and all compounds are characterized by the usual analytical and spectroscopical techniques.
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  • 6
    Electronic Resource
    Electronic Resource
    The 1,3-Sn2O2-Heterocycle as a Ligand in Organometallic Compounds - Dimerization of the Inidene Species [{(CO)5M}2SnOR]- (M = Cr, W) (1998)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 1998 (1998), S. 1057-1066 
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    ISSN: 1434-1948
    Keywords: Pentacarbonylmetal-tin bonding ; Alkoxytin compounds ; Inidene compounds ; 119Sn NMR ; Bonding ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Dimerized inidene complexes [(CO)5M-Sn(OR)-M(CO)5]22- (M = Cr, W; R = Et, iPr), 1, are obtained from [{(CO)5M}2SnCl2]2- by different routes. Dimerization occurs via alkoxy-donor tin-acceptor bonding by which a planar Sn2O2 ring is formed. The Sn-{M(CO)5} bonds are made in a plane vertical to this ring such that, with the R-O groups being almost coplanar with the Sn2O2 ring, the overall geometry of the compounds shows idealized D2h symmetry. - The 119Sn-NMR resonances of 1 are found at rather low fields (M = Cr: δ ≈ 1400; M = W: δ ≈ 1170) indicating a low-lying tin-centered orbital in the LUMO range. Correspondingly EHT analyses show that the 3-center-4π system, which characterizes monomeric inidene species [LnM-E(X)-MLn]n, is still prevalent in the dimeric species 1. The low-lying π*-type LUMOs of 1 are the rationale for the observed 119Sn-NMR low-field shifts of 1. The dimeric compounds 1 react with 2,4-pentanedione to form chelate compounds of the same type as those characteristically obtained from monomeric inidene complexes: [{(CO)5Cr}2SnOEt]22- (1a) reacts to give [{(CO)5Cr}2Sn(acac)]- (2). The experimental results are verified by X-ray analyses in addition to the usual spectroscopic and analytical investigations.
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  • 7
    Electronic Resource
    Electronic Resource
    Zwei Extreme in der Zinnchemie: Ein nichtbindender Sn-Sn-Abstand von 285 pm und eine 119Sn-NMR-Verschiebung δ = 3301 in metallorganischen Derivaten von Sn(0)Herrn Prof. Dr. G. P. Schiemenz gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 187-191 
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    ISSN: 0009-2940
    Keywords: Tin complexes ; Transition metal complexes ; NMR, 119Sn ; Sn(0) compounds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Two Extremes in Tin Chemistry: A Non-bonding Sn-Sn Distance of 285 pm and a 119Sn-NMR Shift δ = 3301 in Organome-tallic Derivatives of Sn(0)The reaction of Na[{Cp'(CO)2Mn}2H] with SnCl2, which produces the inidene compound [Cp'(CO)2Mn\documentclass{article}\usepackage{amsmath}\pagestyle{empty}\begin{document}$ {\rm C}\ddot - {\rm C} $\end{document}Sn(Cl)\documentclass{article}\usepackage{amsmath}\pagestyle{empty}\begin{document}$ {\rm C}\ddot - {\rm C} $\end{document}Mn-(CO)2Cp']- under standard workup procedures, results in the formation of [{Cp'(CO)2MnSn}2{μ2-Mn(CO)2Cp'}2{μ2-Cl}]- (1) when quenched with unpolar solvents. While, formally, 1 contains tin in its oxidation state zero, it may be conceived as composed of an Sn2-2 entity, which is linearly end-on coordinated to two Cp'(CO)2Mn 16-electron species; in addition the tin centers are bridged by two μ2-Mn(CO)2Cp' moieties and a μ2-Cl function. The resulting connectivity Sn2{μ2-Mn(CO)2Cp'}2{μ2-Cl} thus corresponds to a [1.1.1]propellane scaffolding. While there is no obvious need for a tin-tin bond in this propellane-type cage, a short Sn-Sn contact of only 285 pm is observed. While the 119Sn-NMR signal of 1 could not be recorded, the peculiar bonding in this type of compounds is generally mirrored in their unconventional 119Sn-NMR shift whereever signals can be observed: it is found that [{Cp*(CO)2Mn}3(μ3-Sn)], which contains trigonally planar-coordinated μ3-Sn as a naked ligand atom, has its 119Sn-NMR resonance at δ = 3301 well beyond the known range of 119Sn-NMR shifts. This finding is interpreted in terms of a relatively week Snpπ-Mndπ π bonding which leads to low-energy unoccupied molecular orbitals as the prerequisit for a large paramagnetic contribution to the NMR shift.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280217
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  • 8
    Electronic Resource
    Electronic Resource
    Divalent Tin and Lead Compounds EX2 Acting as Bridging Ligands in [{(CO)5M}2EX2]2- (E = Sn, Pb; M = Cr, Mo, W): Preparation and PropertiesDedicated to Professor G. E. Herberich on the occasion of his 60th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 687-699 
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    ISSN: 0009-2940
    Keywords: Tin ; Lead ; 119Sn NMR ; Salt metathesis ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of Na2[M2(CO) 10] (M = Cr, Mo, W) with SnHal2 (Hal = Cl, Br) is a well established procedure for the synthesis of anions of type A, [{(CO)5M)SnHal3]-. Conditions are described which, for the same type of procedure, result in the additional formation of dianions of type B, [{(CO)5M}2SnHal2]2-. Procedures for separating these two types of anions in the form of their stable [Ph4P]+ or [nBu4N]+ salts by appropriate salt metathesis are presented. The structures of theses species have been characterized by X-ray analysis of three salts containing type A anions and two salts containing type B anions. The reactivity of the type B salts containing the bulky cations [Ph4P]+ or [nBu4N]+, respectively, is remarkably low; the salts are, however, transformed into highly reactive sodium salts by further metathesis with Na[BPh4]. In such salts the halide substitutents are easily exchanged as shown by the synthesis of ]})CO(5Cr}2oxinato]- (4)- from [Na-(THF)x]2[{(CO)5Cr}2SnCl2] and sodium 8-oxoquinolate, Na[C9H6NO]. The structure of the anion, 4 is compared to the structure of [[(CO)5Cr)SnCl2· THF] and sodium 8-oxochinolate. The preparation of the dinuclear anions [{(CO)5Cr}2E(OOCCH3)2]2- (E = Sn, 2g; E = Pb, 3) is accomplished by the reaction of [Ph4P]2[Cr2(CO)10] with the corresponding acetates E(OOCCH3)2. While 2g and 3 are formal analogues of the type-B anions, their structures reveal an asymmetrical η2-coordination of the two acetato ligands, in each case ending up in a 4+2 coordination for the main group centres, instead of the four-coordination observed for [{(CO)5M}2SnHal2]2-, All compounds have been characterized by usual spetroscopic and analytical techniques. X-ray analyses have been performed for selected examples. 119Sn-NMR data are presented for all of the compounds which contain tin-centred ligands.
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    URL: http://dx.doi.org/10.1002/cber.19971300604
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  • 9
    Electronic Resource
    Electronic Resource
    η4-Coordination of Dienes and Heterodienes to the TripodCobalt(I) Template [CH3C(CH2PPh2)3Co]+: Synthesis, Structure, and Dynamics (1999)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 2000 (1999), S. 523-536 
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    ISSN: 1434-1948
    Keywords: Tripod ligands ; Dienes ; Heterodienes ; η4-Coordination ; Hindered rotation ; Line-shape analysis ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: CH3C(CH2PPh2)3CoCl (1) is easily accessible from CH3C(CH2PPh2)3CoCl2 by reduction with activated zinc powder. Upon dehalogenation with TlPF6, 1 reacts with dienes to give [tripodCoI-(η4-diene)]+ (2). The heterodienes acrolein and methyl vinyl ketone produce the analogous η4-heterodiene compounds 3. When crotonaldehyde is used as the potential η4-diene ligand, decarbonylation is observed leading to [tripodCoI-(CO)2]+ (4). Reaction of [tripodCoaq](BF4)2 with allyl mercaptan produces [tripodCoI-(η4-thioacrolein)]+ (3a) through dehydrogenation of the ligand precursor. 1,2-Diketones such as benzil and phenanthrenequinone do not coordinate in a η4 fashion but rather generate η2-coordinate enediolato ligands by an electron-transfer process, resulting in compounds of the type {tripodCoIII-[η2-RC(O)=C(O)R]}+ (5). All the compounds have been characterized by standard analytical and spectroscopic techniques, including X-ray analysis in some cases. Compounds 4 and 5 show trigonal-bipyramidal coordination in the solid state, whereas the coordination polyhedra in compounds 2 and 3 are better described as square-pyramidal. While a minimum of two phosphorus resonances might be expected for each of these coordination geometries, only one time-averaged signal is normally observed. Only with the η4-coordinated heterodienes acrolein, methyl vinyl ketone, and thioacrolein present in 3 is there a resolution of the signals of the three chemically distinct phosphorus nuclei at low temperatures. By 31P-NMR line-shape analysis, the activation barriers for the rotational reorientation of the heterodienes are found to be around ΔH≠ = 47 kJmol-1 for all three compounds 3.
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  • 10
    Electronic Resource
    Electronic Resource
    Cooperative Binding of Nitrile Moieties Within a Bimetallic Pocket: Enforcing Side-On π-Interaction With a High-Spin Nickel(II) Site (2000)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 2000 (2000), S. 771-781 
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    ISSN: 1434-1948
    Keywords: Cooperative effects ; Coordination modes ; Nickel ; Bimetallic complexes ; π interactions ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Different cooperative binding modes of nitriles within the bimetallic pocket of a pyrazolate-based compartmental dinickel(II) site have been studied. The H3O2-bridged dinuclear complex 1 reacts with cyanamide to yield 4, in which a secondary hydrogencyanamido(1-) bridge spans the two metal centers at an unusually short metal-metal distance imposed by the primary ligand matrix. In 5, a single 2-cyanoguanidine (cnge) molecule is N-bound to one nickel(II) ion through its nitrile part and is coordinated to the adjacent metal site through an amido nitrogen. The characteristics of the coordination spheres of the metal centers suggest an additional side-on π-bonding interaction of the nitrile moiety with the second high-spin nickel(II) ion. This unusual interaction is corroborated by comparing the IR bands for the ν(C≡N) stretching vibration of 5 with those of complex 6, which has two end-on bound cnge molecules, and those of the related mononuclear complex 7, which lacks a second nickel(II) ion. The nature of the π-bonding interaction in 5 is further analyzed by DFT calculations on relevant model systems. Even though the π-bonding is found to be very weak, it does include some backbonding from occupied 3d MOs at the second high-spin nickel(II) ion to the π* MOs of the nitrile. Such an unconventional π-interaction is suggested to be enforced by the constrained fixation of the nitrile unit within the highly organized coordination pocket of the bimetallic framework. In contrast, the bifunctional 2-hydroxybenzonitrile is accommodated by the distinct binding of the nitrile and phenolate functions to the different metal centers in 8, which confirms that the simultaneous binding of both an OR-function and an end-on bound nitrile is indeed feasible within the active site pocket. Such a situation is reminiscent of the bimetallic effect that has been assumed to enable the cooperative hydration of nitriles at the dinickel(II) site of 1. Complexes 4·(ClO4)2, 5·(ClO4)2, 6·(ClO4)3, 7·(ClO4)(BPh4), and 8·(ClO4)2 have been characterized structurally by X-ray crystallography.
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