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  • 1
    Electronic Resource
    Electronic Resource
    Bis(4-hydroxy-3-methoxybenzaldehyde thiosemicarbazonato-N1,S)nickel(II) tetraethanol solvate (2000)
    Oxford [u.a.] : International Union of Crystallography (IUCr)
    Acta crystallographica 56 (2000), S. 549-550 
    Details
    ISSN: 1600-5759
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Notes: The title complex crystallizes as a tetraethanol solvate, [Ni(C9H10N3O2S)2]·4C2H6O, with the metal on a centre of inversion. Two singly deprotonated ligands coordinate the metal atom in a planar fashion. The metal complexes are organized into layers by an extended network of hydrogen bonds involving the NH2 groups, the phenolic OH groups and the solvent molecules.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1107/S0108270100001657
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  • 2
    Electronic Resource
    Electronic Resource
    Stable one-step technetium-99m labeling of His-tagged recombinant proteins with a novel Tc(I)–carbonyl complex (1999)
    [s.l.] : Nature America Inc.
    Nature biotechnology 17 (1999), S. 897-901 
    Details
    ISSN: 1546-1696
    Source: Nature Archives 1869 - 2009
    Topics: Biology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: [Auszug] We have developed a technetium labeling technology based on a new organometallic chemistry, which involves simple mixing of the novel reagent, a 99m Tc(I)–carbonyl compound, with a His-tagged recombinant protein. This method obviates the labeling of unpaired engineered cysteines, which ...
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1038/12890
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  • 3
    Electronic Resource
    Electronic Resource
    Application of technetium and rhenium carbonyl chemistry to nuclear medicine. Preparation of [NEt4]2[TcCl3(CO)3] from [NBu4][TcO4] and structure of [NEt4][Tc2(μ-Cl)3(CO)6]; structures of the model complexes [NEt4][Re2(μ-OEt)2(μ-OAc)(CO)6] and [ReBr({-CH2S(CH2)2Cl}2)(CO)3] (1997)
    Springer
    Transition metal chemistry 22 (1997), S. 597-601 
    Details
    ISSN: 1572-901X
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A detailed investigation of the one-pot synthesis of [NEt4]2[MX3(CO)3] [M=Tc (1a) or Re (1b); X= Cl−, Br−] is presented. The intermediates [NEt4][Tc2-(μ-Cl)3(CO)6] (2a), [NBu4][Tc3(μ3-H)(μ-H)3(CO)9] (3) and [Tc3(μ-H)3(CO)12] (4) have been isolated and characterized. The X-ray structure of (2a) is described. Complex (2a) crystallizes in the monoclinic space group P21/c with a=19.491(6), b=18.323(2) and c=17.497(9)AÅ, and β=97.59(2)°. Quantitative conversion of (2a), (3) and (4) into the aqua-ion [M(OH2)3(CO)3]+ [M=Tc (5a) or Re (5b)] is described. To evaluate an optimal and simple chelating group for the “fac-M(CO)3” moiety, the reaction with the bidentate thioether ligand Cl(CH2)2S(CH2)2S(CH2)2Cl (qyp) has been investigated and the structure of the neutral complex [ReBr(qyp)(CO)3] (6) is described. Complex (6) crystallizes in the monoclinic space group P21/c with a=15.935(6), b=2.788(4) and c= 7.955(10)AÅ, and β=98.57(1)°. To extend the knowledge about substitution chemistry of organometallic complexes in aqueous solution, the acetato ligand [OOCCH3]− has been reacted with (1b), resulting in the formation of the dinuclear, acetato-bridged complex [NEt4][Re2(μ-OH)2(μ-OAc)(CO)6], which converted into [Re2(μ-OEt)2(μ-OAc)(CO)6]− (7) after recrystallization from EtOH. The X-ray structure of (7) has been determined. Complex (7) crystallizes in the monoclinic space group P21/c with a=16.288(3), b=12.4272(10) and c=13.620(3)AÅ, and β=76.63(1)°. For a future application of the small “fac-M(CO)3” moiety, it seems thus advantageous to combine these two ligand groups in one simple chelating function.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1018573026710
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  • 4
    Electronic Resource
    Electronic Resource
    Darstellung und Strukturen von (Et4N)2[Re(CO)3(NCS)3] und (Et4N)[Re(CO)2Br4] (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 813-818 
    Details
    ISSN: 0044-2313
    Keywords: Rhenium complexes ; carbonyls ; X-ray diffraction ; ligand exchange ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Syntheses and Structures of (Et4N)2[Re(CO)3(NCS)3] and (Et4N)[Re(CO)2Br4]Rhenium(I) and rhenium(III) carbonyl complexes can easily be prepared by ligand exchange reactions starting from (Et4N)2[Re(CO)3Br3]. Using nonoxidizing reagents the facial ReI(CO)3 unit remains and only the bromo ligands are exchanged. Following this procedure, (Et4N)2[Re(CO)3(NCS)3] can be obtained in high yield and purity using trimethylsilylisothiocyanate. The compound crystallizes in the monoclinic space group P21/n, a = 18.442(5), b = 17.724(3), c = 18.668(5) Å, β = 92.54(1)°, Z = 8. The NCS- ligands are coordinated via nitrogen.The reaction of [Re(CO)3Br3]2- with Br2 yields the rhenium(III) anion [Re(CO)2Br4]-. The tetraethylammonium salt of this complex crystallizes in the noncentrosymmetric, orthorhombic space group Cmc21, a = 8.311(1), b = 25.480(6), c = 8.624(1) Å, Z = 4. The carbonyl ligands are positioned in a cis arrangement. Their strong trans influence causes a lengthening of the Re—Br bond distances by at least 0.05 Å.
    Notes: Ausgehend von (Et4N)2[Re(CO)3Br3] lassen sich durch einfache Ligandenaustauschreaktionen weitere Rhenium(I)- und Rhenium(III)-Carbonylkomplexe herstellen. In Abwesenheit starker Oxidationsmittel bleibt die faciale Re1(CO)3-Einheit bei gleichzeitigem Austausch der Bromoliganden erhalten. Mit Trimethylsilylisothiocyanat kann so (Et4N)2[Re(CO)3(NCS)3] in guten Ausbeuten und hoher Reinheit hergestellt werden. Die Verbindung kristallisiert monoklin in der Raumgruppe P21/n, a = 18,442(5), b = 17,724(3), c = 18,668(5) Å, β = 92,54(1)°, Z = 8. Die NCS--Liganden sind jeweils über ihr Stickstoffatom an das Metall gebunden.Die Umsetzung von [Re(CO)3Br3]2- mit Br2 führt zum Rhenium(III)-Anion [Re(CO)2Br4]-. Das Tetraethylammoniumsalz dieses Komplexes kristallisiert orthorhombisch in der nichtzentrosymmetrischen Raumgruppe Cmc21, a = 8,311(1), b = 25,480(6), c = 8,624(1) Å, Z = 4. Die Carbonylliganden befinden sich in cis-Stellung zueinander. Ihr starker trans-Einfluß bewirkt eine Aufweitung der Re—Br-Bindungslänge um mindestens 0,05 Å.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19966220511
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  • 5
    Electronic Resource
    Electronic Resource
    Derivate des Imidazols. XXIV [1].[Li12O2Cl2(ImN)8(THF)4] · 8 THF: Ein Peroxo-Komplex des Lithiums mit neuartiger KäfigstrukturProfessor Welter Siebert zum 60. Geburtstag gewidmet (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1121-1124 
    Details
    ISSN: 0044-2313
    Keywords: Lithium ; imidazole derivatives ; peroxo complexes ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Imidazole Derivatives. XXIV. [Li12O2Cl2(ImN)8(THF)4] · 8 THF: a Peroxo Lithium Fragment in a Novel Cage Structure1,3-dimethyl-2-iminoimidazoline (8, ImNH) reacts with methyl lithium to give [ImNLi]n (9). In tetrahydrofuran, crystals of C56H96Cl2Li12N24O6 · 8 C4H8O (10) are obtained. The structure of 10 consists of a Li12Cl2N8O2 core in which a peroxo unit is incorporated into a stack of ladder fragments. Over all, four tetrahydrofuran and eight imidazoline ligands are attached at the lithium and nitrogen atoms.
    Notes: 1,3-Dimethyl-2-iminoimidazolin (8, ImNH) reagiert mit Methyllithium in Diethylether zu [ImNLi]n (9). In Tetrahydrofuran werden Kristalle von [Li12O2Cl2(ImN)8(THF)4] · 8 THF (10) erhalten. In 10 liegt ein Li12Cl2N8O2-Käfig in Form gestapelter Leiterfragmente mit O22 als zentraler Einheit vor. Hieran sind über die Lithium- und Stickstoffatome insgesamt vier Tetrahydrofuran- und acht Imidazolin-Liganden koordiniert.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976230719
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  • 6
    Electronic Resource
    Electronic Resource
    Gemischtligandkomplexe des Technetiums. XV. Zur Reaktion von [TcNCl2(Me2PhP)3] mit Dialkyldithiocarbamaten und N,N-DialkylthiocarbamoylbenzamidinenProfessor Eberhard Hoyer zum 65. Geburtstag gewidmet (1996)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1257-1262 
    Details
    ISSN: 0044-2313
    Keywords: Technetium ; nitrido complexes ; mixed-ligand complexes ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Mixed-ligand Complexes of Technetium. XV. The Reaction of [TcNCl2(Me2PhP)3] with Dialkyldithiocarbamates and N,N-Dialkylthio-carbamoylbenzamidines[TcN(Cl)(Me2PhP)2(Et2dtc)], [TcN(Me2PhP)(Et2dtc)2], and [TcN(Et2dtc)2] can be prepared by stepwise ligand exchange reactions starting from dichlorotris(dimethylphenylphosphine)nitridotechnetium(V), [TcNCl2(Me2PhP)3], and diethyldithiocarbamate. In contrast to this, only one intermediate, [TcN(Cl)(Me2PhP)2(HEt2tcb)], could be isolated during the reaction with N,N-Diethlthiocarbamoylbenzamidine, which yields the bis chelate [TcN(HEt2tcb)2].[TcN(Me2PhP)(Et2dtc)2] crystallizes in the monoclinic space group P21/c; a = 17.369(5) Å, b = 15.024(1) Å, c = 9.906(3) Å, β = 76.47(1)º, Z = 4. The phosphine is coordinated equatorially. The multiply bonded nitrogen ligand (Tc—N(1) 1.624(3) Å) strongly labilizes the trans positioned donor atom (distance Tc—S(4) 2.826(1) Å).[TcN(HEt2tcb)2] crystallizes in the triclinic space group P1 with a = 9.749(4) Å, b = 11.264(4) Å, c = 12.359(4) Å, α = 75.34(2)º, β = 79.69(2)º, γ = 87.55(2)º, Z = 2. The metal is five-coordinate with the nitrido donor atom occupying the apex of a square pyramid. It's basal plane is formed by the cis-coordinated chelate ligands. The technetium is situated over the basal plane by about 0.6 Å. The Tc≡N distane was found to be 1.610(5) Å.
    Notes: Von Dichlorotris(dimethylphenylphosphan)-nitridotechnetium(V), [TcNCl2(MePhP)3] werden durch schrittweisen Ligandenaustausch mit Diethyldithiocarbamat Komplexe der Zusammensetzung [TcN(Cl)(Me2PhP)2(Et2dtc)], [TcN(Me2PhP)(Et2dtc)2] und [TcN(Et2dtc)2] dargestellt. Die Reaktion mit N,N-Diethylthiocarbamoylbenzamidin, H2Et2tcb, liefert dagegen in guten Ausbeuten das Bis-Chelat. Als einziges Intermediat der Reaktion läßt sich [TcN(Cl)(Me2PhP)2-(HEt2tcb)] isolieren.[TcN(Me2PhP)(Et2dtc)2] kristallisiert in der monoklinen Raumgruppe P21/c mit a = 17,369(5) Å, b = 15,024(1) Å, c = 9,906(3) Å, β = 76,47(1)º, Z = 4. Der Me2PhP-Ligand ist äquatorial koordiniert. Die auffällig kurze Mehrfachbindung zwischen Technetium und Stickstoff (Bindungslänge Tc—N(1) 1,624(3) Å) wirkt sich stark labilisierend auf das trans-ständige Donoratom aus (Abstand Tc—S(4) 2,826(1) Å).[TcN(HEt2tcb)2] kristallisiert in der triklinen Raumgruppe P1, mit a = 9,749(4) Å, b = 11,264(4) Å, c = 12,359(4) Å, α = 75,34(2)º, β = 79,69(2)º, γ = 87,55(2)º, Z = 2. Das Koordinationspolyeder ist eine quadratische Pyramide, deren Spitze vom Nitridoliganden besetzt ist. Ihre Grundfläche wird von den Donoratomen der cis-koordinierten Chelatliganden gebildet. Das Metall befindet sich um etwa 0,6 Å über der Grundfläche. Der Tc≡N-Abstand beträgt 1,610(5) Å.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19966220725
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  • 7
    Electronic Resource
    Electronic Resource
    Synthese, Strukturen und Reaktivität von [(2,4,6-Ph3C6H2)Te(μ2-O)X]2 (X = Br und I) (1997)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 623 (1997), S. 1968-1972 
    Details
    ISSN: 0044-2313
    Keywords: Tellurium ; organotellurium compounds ; tellurium oxides ; X-ray structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Structures, and Reactivity of [(2,4,6-Ph3C6H2)Te(μ2-O)X]2 (X = Br, I)[(2,4,6-Ph3C6H2)Te]2 reacts with iodine affording the aryltellurenic halide (2,4,6-Ph3C6H2)TeI, which is oxidized by oxygen to yield [(2,4,6-Ph3C6H2)Te(μ2-O)I]2. It crystallizes with two molecules of dichloromethane in the monoclinic space group P21/c with a unit cell of the dimensions a = 911.3(4); b = 1153.3(2); c = 2244.1(9) pm; β = 93.53(2)°, Z = 2). The analogues bromo compound [(2,4,6-Ph3C6H2)Te(μ2-O)Br]2 is obtained by the reaction of [(2,4,6-Ph3C6H2)Te(μ2-O)I]2 with NH4Br. It crystallizes with two molecules of xylene in the monoclinic space group P21/n (a = 1067.5(5); b = 1018.4(4); c = 2486.5(8) pm; β = 101.71(2)°; Z = 2). Both compounds are built up by two (2,4,6-Ph3C6H2)TeX units (X = Br, I) which are linked by two oxgen bridges to form centrosymmetric molecules. The Te—O—Te angles are 102°. Distinct Te—O bond lengths have been found (191.4(2) and 208.6(2) pm in [(2,4,6-Ph3C6H2)Te(μ2-O)I]2 and 189.8(4)/208.4(5 pm in the bromo compound).
    Notes: Das Ditellurid [(2,4,6-Ph3C6H2)Te]2 bildet mit Iod das Aryltellurenylhalogenid (2,4,6-Ph3C6H2)TeI, das mit Sauerstoff weiter zu [(2,4,6-Ph3C6H2)Te(μ2-O)I]2 reagiert. Die Verbindungen kristallisiert mit zwei Molekülen Dichlormethan in der monoklinen Raumgruppe P21/c: a = 911,3(4); b = 1153,3(2); c = 2244,1(9) pm; β = 93,53(2), Z = 2. Die analoge Bromverbindung [(2,4,6-Ph3C6H2)Te(μ2-O)I]2 entsteht bei der Umsetzung von [(2,4,6-Ph3C6H2)Te(μ2-O)I]2 mit NH4Br. Sie kristallisiert mit zwei Molekülen Xylen in der monoklinen Raumgruppe P21/n: a = 1067,5(5); b = 1018,4(4); c = 2486,5(8) pm; β = 101,71(2)°; Z = 2. Beide Verbindungen sind aus jeweils zwei (2,4,6-Ph3C6H2)TeX-Einheiten (X = Br, I) aufgebaut, die über zwei Sauerstoffbrücken verbunden sind. Im Zentrum der Te2O2-Ringe befindet sich jeweils ein Inversionszentrum. Die Te—O—Te-Winkel betragen 102°. Es wurden jeweils zwei unterschiedliche Te—O-Abstände gefunden 191,4(2) und 208,6(2) pm in [(2,4,6-Ph3C6H2)Te(μ2-O)I] bzw. 189,8(4) und 208,4(5 pm in der Bromverbindung).
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19976231222
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