bluuebunny/crossref_metadata_2025_split huggingface dataset:
Acetonylperoxyl Radicals, CH3COCH2O2: A Study on the y-Radiolysis and Pulse Radiolysis of Acetone in Oxygenated Aqueous Solutions
Authors: Zegota Henryk , Schuchmann Man Nien , Schulz Dorothea , Sonntag Clemens von 
Published: March 2015

Abstract
Hydroxyl radicals from the radiolysis of N2O/O2 (4:1)-saturated aqueous solutions of acetone (10−3 mol dm −3) react with the solute by H-abstraction thereby forming acetonyl radicals. As shown by pulse radiolysis, the acetonyl radicals rapidly add oxygen (k = 3 x 109 dm3mol−1s−1) thereby forming acetonylperoxyl radicals which decay by second-order kinetics (2 k = 8 x 108 dm3mol−1s−1). Under steady-state radiolysis conditions (0.24 Gy s−1) the products (G values in parentheses) are methylglyoxal (2.5), hydroxyacetone (0.5), form aldehyde (1 .6), acids (1 .7), carbon dioxide (0 .5), organic (hydro)peroxides (0.4), hydrogen peroxide (2 .2), and G (oxygen uptake) has been determined at 5.2. In the decay of the acetonylperoxyl radicals the major process (slightly less than one half) leads in a concerted reaction to two molecules of methyl­ glyoxal and one molecule of hydrogen peroxide. The Russell mechanism which yields one molecule of methylglyoxal, hydroxyacetone and oxygen contributes about one fifth as does the breakdown into two molecules of form aldehyde, one molecule of oxygen and two acetyl radicals. Carbon dioxide, formaldehyde and acetic acid are among the products which result from the acetylperoxyl radicals formed upon oxygen addition to the acetyl radicals. A bout one tenth of the organic peroxyl radicals is converted into hydroperoxides by O2
⨪ produced as a byproduct in the water radiolysis.
Polysulfonylamine, VIII [1] Ein Molekül mit einer extrem langen Silicium-Stickstoff-Bindung. Festkörperstrukturen von N-Trimethylsilyl- und N-Methyl-dimesylamin / Polysulfonylamines, VIII [1] A Molecule with an Extremely Long Silicon-Nitrogen Bond. Solid State Structures of N-Trimethylsilyl- and N-Methyl-dimesylamine
Authors: Schomburg Dietmar , Blaschette Armand , Wieland Elke 
Published: March 2015

Abstract
The crystal and molecular structures of two dimesylamine derivatives, RN(SO2CH3)2, (R = Si(CH3)3 (1a), R-CH3 (1b)) were determined. Com pound 1a displays a very long Si-N bond which is well outside the range normally found in comparable com pounds (185.1 pm, mean value for two crystallographically independent m olecules). The unusually large bond length can be explained by the absence of (d -p)π interactions between silicon and nitrogen. In both com pounds the bonding geometry around the nitrogen atoms is essentially planar
[8+2]-CycIoadditionen mit Benzylidenmalonsäurederivaten: Steuerung der Stereochemie durch die Carbonsäurestrukturteile [1] / [8+2]-C ycloadditions with Benzylidene Malonic Acid Derivatives: The Role of Carboxylic Groups in Stereoselectivity [1]
Authors: Daub Jörg , Gierisch Sebastian , Knöchel Thomas , Salbeck Erika 
Published: March 2015

Abstract
The stereochemistry of the regiospecific [8+2]-cycloaddition of 8 -methoxyheptafulvene (2) with Michael type olefins is elaborated. The stereoselectivities are decreasing in the series a-cyanacrylic acid ester (9), 1,1-dicyanethene derivatives (1), 5-phenylmethylene-1,3-dioxane- 4,6-dione (6 ). The mechanistic impact is discussed. The structure of the tetrahydroazulenes 3-5, 7, 8 and 10, which are formed in good chemical yields are determ ined, mainly by 1H NMR. The molecular structure of 3c is determ ined by X-ray crystallography
Spin Labeled Bovine Serum Albumin, Spin Labeled Bovine Serum Albumin Chelating Agents and Their Gadolinium Complexes. Potential Contrast Enhancing Agents for Magnetic Resonance Imaging
Authors: Sosnovsky George , Rao N. Uma Maheswara , Lukszo J. , Brasch Robert C. 
Published: March 2015

Abstract
Bovine Serum Albumin (BSA) was spin labeled using the active esters 3 and 5 containing a nitroxyl radical to give the spin labeled BSA derivatives 4 and 6. Spin labeled C D TA , DTPA and TTHA chelating agents 10, 13 and 16 and the corresponding BSA derivatives 17, 18 and 19 and their gadolinium complexes 20, 21 and 22 were synthesized. All these BSA derivatives were evaluated as possible contrast enhancing agents for NMR imaging by measurement of spin-lattice (T1) and spin-spin (T2) relaxations and by calculations of relaxivities i.e., slopes of 1/T1 versus concentration plots. The spin labeled BSA-complexon-gadolinium conjugates 20, 21 and 22 were found to have better relaxation times and relaxivities than the BSA spin labeled derivatives 4, 6, 17, 18 and 19. The spin count for the BSA derivatives 4, 6, 17, 18 and 19 and for their gadolinium conjugates 20, 21 and 22 was found to be between 9 -1 0 spins/molecule of the protein. The gadolinium conjugates 20, 21 and 22 of spin labeled BSA possess high relaxivities combined with a nitroxyl marker that could be used with EPR to assess pharmacokinetic behaviors of these potential contrast agents
Natural Abundance 13C—13C Coupling Constants Observed via ID and 2D INADEQUATE Experiments in Stigmasterol and 1,4-Androstadiene-3,11,17-trione
Authors: Neszmélyi Andras , Hull William E. , Lukacs Gabor , Voelter Wolfgang 
Published: March 2015

Abstract
For two steroids, stigmasterol and 1,4-androstadiene-3,11,17-trione, natural abundance 13C -13C coupling constants are determ ined by 1D and 2D INADEQUATE experiments. Besides full assignment of the 13C resonances of these steroids is achieved
Ligandensubstitution an cis-Mo(CO)2(PPh3)2(MeCN)(η2-SO2), Kristall- und Molekülstruktur von cis-Mo(CO)2(PMe3)3(η2-SO2) / Ligand Substitution at cis-Mo(CO)2(PPh3)2(MeCN)(η2-SO2), Crystal and Molecular Structure of cis-Mo(CO)2(PMe3)3(η2-SO2)
Authors: Baumann Franz-Erich , Burschka Christian , Schenk Wolfdieter A . 
Published: March 2015

Abstract
Mo(CO)2(PPh3)2(MeCN)(η2-SO2), reacts with a number of unidentate or tridentate phosphines with displacement of both MeCN and PPh3. Mixtures of up to three different isomers are obtained the structures of which are assigned by IR , 1H, 13C, and 31PNMR , and in one case by X-ray crystallography. The results support earlier observations concerning the relationship between the disposition of donor and acceptor ligands around the metal and the bonding mode of SO2 .
The Crystal and Molecular Structure of Dichloro Monothiodibenzoylmethanato Indium Monothiodibenzoylmethane InCl2L(LH)
Authors: Mishra Anil K. , Gupta Vishnu D . , Nöth Heinrich 
Published: March 2015

Abstract
Indium trichloride reacts with 2 moles of monothiodibenzoylm ethane (LH) in the presence of sodium acetate to yield In Cl2L(LH). According to an X-ray structure analysis the molecule possesses a hexacoordinated indium atom with two chlorine atoms in cis position and two sulfur atoms in trans position. The symmetry of the molecule is C2 imposed by a crystallographic twofold axis. The unique hydrogen atom , assumed to form an intermolecular hydrogen bridge between oxygen atoms could not be detected in the structure analysis.
Synthesis of Water Soluble Spin Labeled Glucose Derivatives as Potential NMR Contrast Enhancing Agents
Authors: Sosnovsky George , Rao N. Uma Maheswara , Lukszo Jan , Brasch Robert C. 
Published: March 2015

Abstract
Synthetic methodologies for the preparation of nitroxyl labeled derivatives of D -(+)-glucose, α -D -(+)-m ethylglycoside, 2-amino-2-deoxy-D -(+)-glucose, and D -(+)-glucuronic acid are presented. The spin labels in these compounds are attached variably at the 1, 2, 3, and 6 positions of the glucose framework. These new compounds, being water soluble and producing marked en­hancement of spin-lattice (T ,) and spin-spin (T2) proton relaxation in deionized water and human plasma have potential utility as contrast altering pharmaceuticals for magnetic resonance imaging and as spin probes in biomolecular research. These spin labeled carbohydrates may demonstrate in vivo biodistribution characteristics reflecting tissue-specific differences in glucose metabolism .
Synthese und Struktur von [Fe(SPh)2(NO)2]- dem „Monomeren“ des Roussinschen Phenylesters/ Synthesis and Structure of [Fe(SPh)2(NO)2]- , the “Monomer” of Roussin’s Phenyl Ester
Authors: Strasdeit Henry , Krebs Bernt , Henkel Gerald 
Published: March 2015

The complex (Et4N )[Fe(SPh)2(NO)2] (2) has been obtained as black crystals by treatment of K[Fe4S3(NO)7]·H2O with potassium hydroxide in molten diphenyldisulfide and subsequent addition of methanol and tetraethylammonium chloride. 2 is orthorhombic, space group Pbca, Z = 8, with a = 18.853(3), b = 17.958(3), and c = 13.283(2) Å at 140 K. The X-ray structure of 2 has been refined to R1 (R2) = 2.7% (3.1% ). It reveals a pseudotetrahedral S2N2 arrangement around the iron atom (Fe -S 2.280, Fe -N 1.679 Å (mean values), S -Fe -S 109.73(2)°, N -Fe -N 117.36(9)°) and Fe -N -O groups of the linear type (N -O 1.180 Å , Fe -N - O 169.0° (mean values)). The N - O bond order is 2.2. Structural properties as well as the low Mößbauer isomeric shift ( + 0.08 mm/s relative to Fe metal) are indicative of strong Fe - N π-back bonding and a major contribution of the mesomeric form Fe = N = Ō̱
.
Benzoatokomplexe des Rutheniums, 2. Mitt. Synthese, Eigenschaften und Kristallstruktur von Ru2(C6H5COO)2(CO)4, Ru2(C6H5COO)2(CO)6 und Ru2(CH3COO)2(CO)6/Benzoato Complexes of Ruthenium, Part 2 Synthesis, Properties and Crystal Structure of Ru2(C6H5COO)2(CO)4, Ru2(C6H5COO)2(CO)6 and Ru2(CH3COO)2(CO)6
Authors: Spohn Martin , Vogt Thomas , Strähle Joachim 
Published: March 2015

Abstract
The reaction of Ru3(CO)12 with molten benzoic acid yields Ru2(C6H5COO)2(CO)4 (1) and Ru2(C6H5COO)2(CO)6 (2). Ru2(CH3COO)2(CO)6 (3) was obtained in small yield by annealing Ru2(CH3COO)2(CO)4 over a period of 3 weeks at 145 °C in a sealed glass am poule. 1 forms orthorhombic, orange needles crystallizing in the space group Pbca, with the lattice constants a = 974.9, b = 2090.5, c = 1830.1 pm, Z = 8 . 2 crystallizes as monoclinic, yellow needles in the space group C2/m with a = 1879.2, b = 1168.3, c = 1029.3 pm, β = 103.77°, Z = 4. 3 is obtained in the form of yellow platelets which crystallize in the space group P 21/c and with lattice constants a = 792.3, b = 2802.6, c = 1440.9 pm, β = 100.65°, Z = 8. All three complexes consist of dimeric units Ru2(RCOO)2(CO)4 with bridging carboxylato groups in cis positions. In the case of 1 these units are linked together by additional Ru -O bonds between neighbouring dimers to form polymer chains. 2 and 3 are isolated complexes with the axial positions occupied by CO ligands. The diamagnetism as well as the Ru -Ru distances (1: 263.9 pm; 2: 270.4 pm; 3: 269.0 and 268.8 pm) are in agreement with a Ru-Ru single bond and the electron configuration σ2π4δ2δ∗2. Polymer 1 reacts reversibly with CO at 1 bar pressure to form 2.
Darstellung von Chalkogenostibanen des Typs R2SbER′ (R = CH3, C2H5; E = S, Se, Te; R′ = CH3, C6H5) durch Austauschreaktionen zwischen Distibanen und Dichalkogeniden/ Preparation of Chalcogenostibanes of the Type R2SbER′ (R = CH3, C2H5; E = S, Se, Te; R′ = CH3, C6H5) by Exchange Reactions of Distibanes and Dichalcogenides
Authors: Breunig Hans Joachim , Gülec Sabahittin 
Published: March 2015

Abstract
Chalcogenostibanes of the type R2SbER′ (R = CH3, C2H5; E = S, Se, Te; R′ = C H3, C2H5) have been prepared by complete exchange reactions of the corresponding distibanes and dichalcogenides. The derivatives (CH3)2SbTeCH3 , and (C2H5)2SbTeCH3 are thermochromic.
Synthese und Struktur von Dicarbonyl(η5-pentaphenylcyclopentadienyl)rhodium, (η5-C5Ph5)Rh(CO)2
Authors: Behrens Ulrich , Edelmann Frank 
Published: March 2015

Abstract
(η5-C5Ph5)Rh(CO)2 has been prepared in 62% yield by treatment of [Rh(CO)2Cl]2 with NaC5Ph5 in THF. The title com pound crystallizes in the rhombic space group Pcab with the lattice parameters a = 2064.7(7) pm , b = 2065.2(8) pm, c = 1407.6(6) pm and Z = 8 . The crystal structure consists of discrete (η5-C5Ph5)Rh(CO)2 molecules and the Rh(CO)2 fragment adopts an eclipsed conformation relative to the cyclopentadienyl ring.
Spectral, Magnetic and Thermogravimetric Studies of Some Dimeric Oxovanadium(IV) Complexes
Authors: Nath P. K. , Mishra N. C. , Chakravortty V. , Dash K. C. 
Published: March 2015

Abstract
The tridentate dibasic Schiff base anthranilic acid salicylideneimine (H2SB) reacts with VOCl2 in the presence o f NaOAc and imidazole (or its derivatives) to form dimeric oxovanadium (IV) complexes of the type [VO(S B)(D)]2. These green or yellow -green compounds have a magnetic moment of 1.4 B.M . at room temperature, and are non-electrolytes in MeOH . The compounds are characterised on the basis of electronic and IR spectra as well as EPR spectroscopy. The IR spectra shows a strong band due to v(V = O) at 880 cm-1 in addition to the bands of H2SB and imidazole. [VO(SB)(Im)]2 shows a single unresolved EPR signal at g = 1.9715 whereas compounds containing other imidazole derivatives show both a broadening and shifting of the signal. The thermogravimetric measurements indicate the stability of the complexes and their stepwise thermal decomposition.
Metallkomplexe mit biologisch wichtigen Liganden, XLIII Metallkomplexe mit ungeschützten acyclischen Monosaccharid-Derivaten (Amin-, Oxim-, Schiffbase-, Thiazolidin-und 1,3-Dithian-Liganden)/Metal Complexes with Biologically Important Ligands, XLIII Metal Complexes with Unprotected Acyclic Derivatives of Monosaccharides (Amine, Oxime, Schiffbase, Thiazolidine and 1,3-Dithiane Ligands)
Authors: Nagel Yvonne , Beck Wolfgang 
Published: March 2015

Abstract
The synthesis and spectroscopic data of palladium (II), platinum (II), nickel(II), cobalt(II), copper(II) and gold(I) complexes with D-glucose oxime, 2-amino-2-deoxy-D-glucose oxime, 1,2-diamino-1,2-deoxy-D-glucitole, L-cysteine-D-glucose, D-glucose trimethylene mercaptale. Schiffbases from 1,2-diamino-1,2-deoxy-D -glucitole and acetylacetone or from D-glucosone and 1.3-diaminopropane are reported.
Erdalkaliquadratate, II SrC4O4 · 3H2O Typ I [1] / Alkaline-Earth Squarates, II SrC4O4 · 3H2O Type I [1]
Authors: Robl Christian , Weiss Armin 
Published: March 2015

Abstract
In SrC4O4-3H2O (type I), Sr2+ has CN 8. It is surrounded by 3 water molecules and 5 oxygen atoms of 4 different squarate dianions. The C-O and C-C bond lengths are typical of extensive delocalization of the π-electron system. The connection of Sr2+ and C4O4
2- leads to infinite layers, obviously interlinked by hydrogen bonding.
The oxygens of the squarate behave differently: two are Sr-chelating, but simultaneously bound to two additional Sr2+, one is connected with one Sr2+ only, and the fourth is not bound to any Sr2+. The single crystal character remained in principle unchanged during dehydration to SrC4O4 · 1 H2O and subsequent rehydration to the trihydrate. Grinding of a crystal treated in this way led to a new modification of SrC4O4 ·3 H2O.
Ein neues quaternäres Oxocadmat: Cs2K2Cd3O5 [1] / A New Quaternary Oxocadmate: Cs2K2Cd3O5 [1]
Authors: Seipp Erhard , Hoppe Rudolf 
Published: March 2015

Abstract
Cs2K2Cd3O5 has been prepared from mixtures of the binary oxides in a silver-tube (550 °C. 17 days). The unit cell is triclinic, P1̄ (a = 983.2, b = 918.0, c = 653.5 pm. α = 108.3°, β = 113.7°, γ = 99.9°. The crystal structure was refined to R = 5.9% and /?u = 5.8% (four-circle-diffractome­ter data, 2616 unique of 3359 measured reflexions). The Effective Coordination Numbers (ECoN) and the Madelung Part of Lattice Energy (MAPLE) are calculated and discussed.
Synthese und Kristallstruktur von Mg[Si(CH3)3]2 · (CH3)2NCH2CH2CH2N(CH3)2 / Synthesis and Crystal Structure of Mg[Si(CH3)3]2 · (CH3)2NCH2CH2CH2N(CH3)2
Authors: Rösch Lutz , Pickardt Joachim , Imme Sigrid , Börner Ute 
Published: March 2015

Abstract
Mg(SiMe3)2 · TMDAP was synthesized by reaction of Hg(SiMe3)2 with magnesium in 1,3-bis-(dimethylamino)propane/diethyl ether. The crystal structure of the compound was investigated.
Polyphosphinhaltige Trichlorostannatoplatin(II)-Komplexe: Synthese und NMR(119Sn, 31P)-Charakterisierung / Trichlorostannatoplatinum(II) Complexes Containing Polyphosphines: Synthesis and NMR (119Sn, 31P) Characterization
Authors: Brüggeller Peter 
Published: March 2015

Abstract
Trichlorostannatoplatinum(II) complexes containing bis(2-diphenylphosphinoethyl)phenyl- phosphine, etp, and the tripod ligand tris(2-diphenylphosphinoethyl)phosphine, PP3, respective­ly, have been prepared and characterized by 119Sn{1H} and 31P{1H} NMR spectroscopy. [(etp)PtCl](BPh4) (1a) reacts with SnCl2 via oxidative addition to give [(etp)PtSnCl3](BPh4) (1b). The 31P NMR spectral patterns of type 1 complexes are consistent with AX2 spin-systems and square planar structures in solution. There is 31P NMR evidence that in the presence of (Ph4P)Cl 1b adds further SnCl2. The possibility of the formation of [(etp)Pt(SnCl3)2] (2) is discussed. [(PP3)PtCl](BPh4) (3a) reacts with SnCl2 to give [(PP3)PtSnCl3](BPh4) (3b). The 31P NMR spec­tral patterns of 3a and 3b are consistent with AX3 spin-systems and trigonal bipyramidal struc­tures.
Reductive Dehalogenation of α-Haloketones by Sodium Borohydride and Tin(II) Chloride in Tetrahydrofuran
Authors: Ono Aoi , Yamaguchi Ritsuko , Shirai Yoshiko 
Published: March 2015

Abstract
α-H aloketones and α-halocarbonyl compounds are effectively reduced to dehalogenation to their corresponding parent ketones or carbonyl compounds in good yield by sodium borohydride and tin(II) chloride in tetrahydrofuran.
Some New Derivatives of Harmaline Series of Bases
Authors: Siddiqui Salimuzzaman , Siddiqui Bina S. , Begum Sabira 
Published: March 2015

Abstract
In the course of pharmaco-chemical studies in the structure and activity relationship in harmaline series of β-carboline bases, a number of new derivatives of harmaline have been obtained and characterized through chemical and spectral studies. Pharmacological screening carried out on one of these (9) shows that it has mild physiological activity without any toxicity.
Empirical Parameters of Lewis Basicity of Binary Solvent Mixtures, Part II Mixtures with Water
Authors: Wrona Piotr K. , Krygowski Tadeusz M. , Zielkowska Urszula 
Published: March 2015

The Kamlet and Taft basicity parameters βKT, for twelve mixtures of organic solvents with water are reported. Also the data for water-butanols (n-BuOH. i-BuOH. and s-BuOH) and alcohols (MeOH, EtOH. n-PrOH. and i-PrOH)-n-hexane mixtures are given. It was found that in the case of mixtures of 1.4-dioxane. acetone, tetrahydrofuran. dimethylsulfoxide. and acetonitrile with water, the basicity parameters of the mixture are higher than that of pure solvents in a region of smaller concentrations of water.
These results, together with earlier reported results for THF and Et2O mixtures with MeOH are discussed in terms of breaking off the structure of the more structurized solvent (water and MeOH). All these mixtures, except the W-THF mixture, show the excess thermodynamic func­tions (ΔHE and ΔSh) analogous to MeOH-CCl4 mixtures, where depolymerization of MeOH clusters was postulated.
Relativity of different basicity scales in respect to the acidic probe molecule is also shortly discussed
Structural and Transport Studies for Ternary Graphite Intercalated Phases (CoCl2, AlCl3)
Authors: Pernot Paul , Vangelisti René 
Published: March 2015

Metal dihalide low-volatility is the major characteristic slowing down their intercalation into graphite (GICs: graphite intercalation compounds). An original synthesis using volatile heterocomplexes between metal dihalide (CoCl2) and gaseous dimer Al2Cl6 increases strickingly CoCl2 intercalation rate but entails cointercalation of significative amount of AlCl3 in the compounds MGICs (mixture graphite intercalation compounds). Structural studies along c-axis, in plane and out the plane (3 D stacking) display a similar behaviour as in the CoCl2 containing binary compounds. Microstructural studies confirm the separation of CoCl2 and AlCl3 in distinct domains. Other ternary phases with alternate CoCl2 and AlCl3 layers and characterized by a similar AlCl3/CoCl2 ratio can be obtained using biintercalation method: (GBICs: graphite biintercalation compounds).
X-Ray diffraction shows that the biintercalation involves a complete lost of correlations in the successive CoCl2 or graphite layers. Transport studies of ternary phases (MGICs and GBICs) display an anomalous behaviour as T is lowered below the magnetic ordering temperature Tc especially for in plane resistivity.
Synthese, Struktur und thermisches Verhalten von Thiophosphorsäuretriamid SP(NH2)3 [1] / Synthesis, Structure, and Thermal Behaviour of Phosphorothionic Triamide SP(ΝΗ2)3 [1]
Authors: Schnick Wolfgang 
Published: March 2015

Phosphorothionic triamide SP(NH2)3 is obtained by slow addition of SPCl3 dissolved in dry CH2Cl2 to a satured solution of NH3 in CH2Cl2 at —50°C. Ammonium chloride is removed from the resulting precipitate by treatment with HNEt2 followed by extraction with CH2Cl2. Coarse crystalline SP(NH2)3 is obtained after recrystallization from dry methanol. The crystal structure of SP(NH2)3 has been determined by single crystal X-ray methods (Pbca; a = 922.3(1), b = 953.8(1), c = 1058.4(2) pm, Z = 8). In the crystals the molecules show non-crystallographic point symmetry C8. The P—S bond (195.4(1) pm) is slightly longer than in SPCl3. From P—N bond lengths of about 166 pm a significant electrostatic strengthening of the P—N single bonds is assumed. Weak intermolecular hydrogen bonding interactions (N —H · · · N ≥ 329.5 pm; N — H · · · S ≥ 348.3 pm) are observed.
Investigation of thermal properties shows a melting temperature of 115°C for SP(NH2)3. According to combined DTA/TG and MS investigations above this temperature the compound decomposes by evolution of H2S and NH3 to yield amorphous phosphorus(V)nitride.
Umsetzungen von Ferrocenyl-lithium mit Carbonyleisen-Komplexen / Reactions of Ferrocenyl Lithium with Carbonyliron Complexes
Authors: Herberhold Max , Feger Wolfgang , Thewalt Ulf 
Published: March 2015

The reaction of cis-Fe(CO)4Br, with ferrocenyl lithium, FcLi, leads to the binucleara hexacarbonyldiiron complexes Fe2,(CO)6(μ-Br)(μ-CFc) (7), Fe,(CO)6(μ-COFc)2 (8) and Fe2(CO)6(μ-C2Fc2O) (9)b. Addition of FcLi to Fe(CO)5 gives the ferrocenoyl tetracarbonylferrate anion which was characterized as the salt NEt4
+[Fe(CO)4(FcCO)]- (10); 9 is obtained after reaction of the anion with Meerwein’s salt, Me3O+BF4
-.
The reaction of Fe2(CO)9 with FcLi, followed by methylation with Me3O+BF4
-, results in the formation of Fe2(CO)8[μ2-C(OMe)Fc] (11) which can be extracted from the product mixture using pentane. Chromatography of the product mixture over silica, however, leads preferentially to the formation of trinucleara complexes of the type Fe3(CO)9(μ3-COMe)(μ3-CR) (R = Fc (12), OMe (13) and O(CH2)4OMe (14)) in addition to 9; the same products are obtained starting from Fe3(CO)12. No complexes could be isolated which contained a direct iron σ-ferrocenyl bond. The structures of the new complexes were deduced from their infrared, mass, 1H and 13C NMR spectra. The bis(ferrocenoyl)-bridged compound 8 was also characterized by an X-ray crystallographic structure analysis.
Ferrocenyl-aryl-plumbane / Ferrocenyl-aryl-plumbanes
Authors: Utri Gerhard , Schwarzhans Karl-Eberhard , Allmaier Günter M. 
Published: March 2015

The first example of a diplumba[1.1]ferrocenophane[cpPb(ø2)cp]2Fe2 has been prepared from ø2PbCl2 and 1,1′-dilithioferrocene 2 TMEDA. The preparation of further four ferrocenyl-phenyl-plumbanes, including the hitherto unknown compounds (ø3Pbcp)2Fe, Fc2Pb2ø2 and [(ø3Pb)cpFecp]FcPbø2 has been achieved by reaction of a mixture of monolithioferrocene · TMEDA and 1,1′-dilithioferrocene 2 TMEDA with ø 2PbCl2 and ø3PbCl, respectively.
These compounds have been investigated by 1H, 13C and 207Pb NMR spectroscopy as well as by half-wave potential measurements, EI, FD and PD mass spectrometry.
The results were discussed in terms of the possibility of Pb/Fe metal orbital overlap.
There is evidence from the VT 1H NMR spectra for conformational flexibility of the diplumba[ 1.1 ]ferrocenophane.