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  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 1038-1046 
    ISSN: 0044-2313
    Keywords: Binuclear antimony(V) complexes ; structure ; dynamics ; NMR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: d, h-μ-Benzylalkoxophosphonato-e-μ-alkoxo-f-μ-oxo-bis[trichloroantimony(V)] CompoundsThe binuclear antimony(V) complexes Cl3Sb(O)[R3(R1O)PO2](OR2)SbCl3 1 - 6 with R1 = R2 = CH3, C2H5 and R3 = C6H5CH2, (CH3)3C6H2CH2 in solution slowly exchanges the R2 groups between the oxygen atoms of the Sb2O2 ring. The SbOPOSb ringsystem makes rapid pseudorotation. The isomeres are detected by nmr spectroscopy. 1 (R1 = R2 = CH3) crystallizes in the orthorhombic space group Pnma with a = 1247.0, b = 1324.1, c = 1207.9 pm and Z = 4. 2 (R1 = CH3, R2 = C2H5) and 5 (R1 = R2 = CH3, R3 = (CH3)3 · C6H2CH2) crystallizes triclinic in the space group P-1 with a = 984.1, b = 1026.7, c = 1079.9 pm, α = 87.93, β = 75.70, γ = 87.62° and Z = 2 and a = 1164.6, b = 1296.9, c = 1712.9 pm, α = 109.9, β = 96.3, γ = 100.2° and Z = 4 resp., with two crystallographically independent molecules in the asymmetric unit.
    Notes: Die zweikernigen Antimon(V)-Komplexe Cl3Sb(O)[R3(R1O)PO2](OR2)SbCl3 1 bis 6 mit R1 = R2 = CH3, C2H5 und R3 = C6H5CH2, (CH3)3C6H2CH2 tauschen bei RT in Lösung langsam die R2-Gruppen aus. Daneben erfolgt rasches Umklappen des SbOPOSb-quasi-Fünfringes. Die Isomerenbildung wird NMR-spektroskopisch nachgewiesen. 1 (R1 = R2 = CH3) kristallisiert orthorhombisch in der Raumgruppe Pnma mit a = 1247,0, b = 1324,1, c = 1207,9 pm und Z = 4. 2 (R1 = CH3, R2 = C2H5) und 5 (R1 = R2 = CH3, R3 = (CH3)3C6H2CH2) kristallisieren triklin in der Raumgruppe P-1 mit a = 984,1, b = 1026,7, c = 1079,9 pm, α = 87,93, β = 75,70, γ = 87,62° und Z = 2 bzw. a = 1164,6, b = 1296,9, c = 1712,9 pm, α = 109,9, β = 96,3, γ = 100,2° und Z = 4 mit zwei kristallographisch unabhängigen Molekülen in der asymmetrischen Einheit.
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 615 (1992), S. 93-96 
    ISSN: 0044-2313
    Keywords: Rhodium(III) complex ; tris(N,N-diethyl-N′-benzoylthioureato)rhodium(III) ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure of Tris(N,N-Diethyl-N′-benzoylthioureato) Rhodium(III)Rh(C12H15N2OS)3 crystallizes in the trigonal space group P-3. The cell parameters are a = 16.660(2), c = 8.479(1) Å and Z = 2. The structure was solved with Patterson and direct methods and refined to a final R-value of 7.05%. RhIII is octahedrally coordinated to three N,N-Diethyl-N′ -benzoylthiourea molecules, which are bidentately coordinated through their oxygen and sulfur atoms. The Rh—S and Rh—O bond lengths are 2.284 Å and 2.033 Å, respectively.
    Notes: Rh(C12H15N2OS)3 kristallisiert in der trigonalen Raumgruppe P-3 mit den Gitterkonstanten a = 16,660(2), c = 8,479(1) Å, Z = 2. Die Struktur wurde mit Patterson und Direkten Methoden gelöst und bis zu einem R-Wert von 7,05% verfeinert. RhIII bildet mit dem Liganden N,N-Diethyl-N′ -benzoylthioharnstoff einen oktaedrisch koordinierten Neutralkomplex, in dem drei Ligandmoleküle bidental über Schwefel und Sauerstoff an das Zentralatom gebunden sind. Der Rh—S-Abstand beträgt 2,284 Å, der Rh—O-Abstand 2,033 Å.
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 610 (1992), S. 145-150 
    ISSN: 0044-2313
    Keywords: Iodinetrimethylsilane · β-picoline ; -.γ-picoline ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of Me3SiI · β-Picoline and Me3SiI · γ-Picoline A Comparison between the Lewis-Bases Pyridine, β-Picoline, and γ-PicolineThe reaction of Iodinetrimethylsilane with β- und γ-Picoline (Pic) leads to solid 1 : 1 compounds Me3SiI · β-Picoline 1, Me3SiI · γ-Picoline 2. The reaction was performed at room temperature. Yellow single crystals were obtained by sublimation. Single crystal X-ray investigations confirm that both compounds are ionic [Me3SiPic]+I-. The comparison of β-Picoline with γ-Picoline and Pyridine (Py) demonstrates that the presence of a methyl group and also its position has no significant influence on the Si—N bond length in compound 1, 2 and on the adduct Me3SiI · Py.
    Notes: Iodtrimethylsilan reagiert mit β- und γ-Picolin (Pic) bei Raumtemperatur zu festen 1 : 1 Addukten (M3SiI · β-Picolin 1, Me3SiI · γ-Picolin 2), die durch Sublimation leicht gelblich gefärbte Einkristalle bilden. Die Röntgenstrukturanalyse beider Verbindungen beweist eine ionische Struktur des Typs [Me3SiPic]+ I-. Der Vergleich von β-Picolin mit γ-Picolin und Pyridin (Py) zeigt, daß die Anwesenheit einer Methylgruppe und auch deren Position keinen signifikanten Einfluß auf die Si—N-Bindungslänge in Verbindung 1, 2 und dem Addukt Me3SiI · Py hat.
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 786-790 
    ISSN: 0044-2313
    Keywords: Bis(N,N-diethyl-N′-benzoylselenoureato)-zinc(II) ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of Bis(N,N-Diethyl-N′-benzoylselenoureato)zinc(II).Zn(C12H15N2OSe)2 crystallizes in the acentric orthorhombic space group Pca21. The cell parameters are a = 16.914(5), b = 13.492(4), c = 11.705(5) Å and Z = 4. The structure was solved with Patterson and direct methods and was refined to a final R-value of 7,05%. ZnII is coordinated to two N,N-Diethyl-N′-benzoylselenoureato molecules, which are bidentately coordinated through their oxygen and selenium atoms to form a distorted tetrahedron. The Zn—Se bond lenghts are 2.394(3) and 2.369(4) Å, the Zn—O bond lengths are 1.971(11) and 1.974(12) Å.
    Notes: Zn(C12H15N2OSe)2 kristallisiert in der azentrischen orthorhombischen Raumgruppe Pca21 mit den Gitterkonstanten a = 16,914(5), b = 13,492(4), c = 11,705(5) Å, Z = 4. Die Struktur wurde mit Patterson und Direkten Methoden gelöst und bis zu einem R-Wert von 7,05% verfeinert. Zink bildet mit dem Liganden N,N-Diethyl-N′-benzoylselenoharnstoff einen bidental koordinierten Komplex, in dem zwei Ligandmoleküle über Selen und Sauerstoff in Form eines verzerrten Tetraeders an das Zentralatom gebunden sind. Die Zn—Se-Abstände betragen 2,394(3) und 2,369(4) Å, die Zn—O-Abstände 1,971(11) und 1,974(12) Å.
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 791-795 
    ISSN: 0044-2313
    Keywords: Bis(N,N-Diethyl-N′-benzoylselenoureato)-cadmium(II) ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of Bis(N,N-Diethyl-N′-benzoylselenoureato)cadmium(II).Cd(C12H15N2OSe)2 exists in a dimeric oxygen bridged form and crystallized in the monoclinic space group P21/n. The cell parameters are a = 12.506(3), b = 11.563(2), c = 18.924(4) Å, β = 91.59(3)°, Z = 4. The structure was solved with Patterson and direct methods and was refined to a final R-value of 6.58%. Cadmium is coordinated by 3 oxygen and 2 selenium atoms and exhibits the unusual coordination number 5. The coordination polyhedron is a distorted trigonal bipyramid, to bipyramids are connected by a common edge. The Cd—Se bond lengths are 2.591(1) and 2.565(1) Å, the Cd—O bond lengths are 2.263(6), 2.272(5) und 2.438(5) Å.
    Notes: Cd(C12H15N2OSe)2 liegt als sauerstoff-verbrücktes Dimer vor und kristallisiert in der monoklinen Raumgruppe P21/n mit den Gitterkonstanten a = 12,506(3), b = 11,563(2), c = 18,924(4) Å, β = 91,59(3)°, Z = 4. Die Struktur wurde mit Patterson und Direkten Methoden gelöst und bis zu einem R-Wert von 6,58% verfeinert. Die Cadmiumatome sind von jeweils 3 Sauerstoff- und 2 Selenatomen koordiniert und besitzen die ungewöhnliche Koordinationszahl 5. Das Koordinationspolyeder ist eine verzerrte trigonale Bipyramide, zwei Bipyramiden sind über eine gemeinsame Kante miteinander verknüpft. Die Cd—Se Abstände betragen 2,591(1) und 2,565(1) Å, die Cd—O Abstände 2,263(6), 2,272(5) und 2,438(5) Å.
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 619 (1993), S. 1689-1692 
    ISSN: 0044-2313
    Keywords: Thallium(I) complex ; (N,N-Diethyl-N′-benzoylselenoureato) thallium(I) ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of (N,N-Diethyl-N′-benzoylselenoureato)thallium(I).Tl(C12H15N2OSe) exists in a dimeric form and crystallizes in the triclinic space group P-1. The cell parameters are a = 6.501(6), b = 9.901(7), c = 12.233(9) Å, α = 91.59(2), β = 80.11(6), γ = 85.28(5)° and Z = 2. The structure was solved with Patterson and direct methods and was refined to a final R-value of 5.30%. Two complex molecules are connected by Tl—Se bonds to form a planar four membered ring with diagonally arranged Tl and Se atoms. The considerably bended chelate rings are nearly at right angle to the central four membered ring. The Tl—Se bond lengths are 3.105(3) and 3.118(3) Å, the Tl—O bond length is 2.532(9) Å.
    Notes: Tl(C12H15N2OSe) liegt als Dimer vor und kristallisiert in der triklinen Raumgruppe P-1 mit den Gitterkonstanten a = 6,501(6), b = 9,901(7), c = 12,233(9) Å, α = 91,59(2), β = 80,11(6), γ = 85,28(5)°, Z = 2. Die Struktur wurde mit Patterson und Direkten Methoden gelöst und bis zu einem R-Wert von 5,30% verfeinert. Zwei Komplexmoleküle sind über Tl—Se-Bindungen zu einem planaren Vierring aus diagonal angeordneten Thallium- und Selenatomen verknüpft. Die stark abgewinkelten Chelatringe sind nahezu rechtwinklig zum zentralen Vierring angeordnet. Die Tl—Se-Abstände betragen 3,105(3) und 3,118(3) Å, der Tl—O-Abstand beträgt 2,532(9) Å.
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 611 (1992), S. 95-98 
    ISSN: 0044-2313
    Keywords: N,N-Diethyl-N′-benzoylformamidin-tetrachloroaurate(III) ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Complex Formation of Gold with N,N-Dialkyl-N′-benzoylthioureas: The Crystal Structure of N,N-Diethyl-N′-benzoylformamidin-tetrachloroaurate(III)N,N-Diethyl-N′-benzoylformamidin-tetrachloroaurate(III) AuCl4C12H17N2O crystallizes in the monoclinic space group P21/c. The cell parameters are a = 7.764(2), b = 14.473(4) and c = 16. 105(9) Å β = 100.75(4) 0. The structure was solved with direct methods and refined to a final R-value of 3.38%.
    Notes: N,N-Diethyl-N′-benzoylformamidin tetrachloroaurat(III) AuCl4C12H17N2O kristallisiert in der monoklinen Raumgruppe P2/c mit den Gitterkonstanten a = 7,764(2), b = 14, 473(4) und c = 16, 105(9) Å β = 100, 75(4)°. Die Struktur wurde mit Direkten Methoden gelöst und bis zu einem R-Wert von 3,38% verfeinert.
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 611 (1992), S. 99-102 
    ISSN: 0044-2313
    Keywords: N,N-Diethyl-N′-benzoylthioureatogold(I) chloride ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Complex Formation of Gold with N,N-Dialkyl-N′-benzoylthioureas: The Crystal Structure of N,N-0Diethyl-N′-benzoylthioureatogold(I) ChlorideN,N-Diethyl-N′-benzoylthioureatogold(I) chloride AuCiS12H16N2O crystallizes in the monoclinic space group P21/c. The cell parameters are a = 18.407(4), b = 5.456(1) and c = 196.322(3) Å, β = 113.6/8(1)°. The structure was solved with direct techniques and refined to final R-value of 5.92%. Gold(I) forms a monodentately sulfur-coordinated complex with the ligand N,N-Diethyl-N′-benzoylthiourea. The coordination sphere around Au(I) shows a nearly linear arrangement of sulfur and chloride.
    Notes: N,N-Diethyl-N′-benzoylthioureatogold(I)-chlorid AuCISC12H16N2O kristallisiert in der monoklinen Raumgruppe P21/c mit den Gitterkonstanten a = 18,407(4), b = 5,456(1) und c = 16,322(3) Å, β = 113,68(1)0. Die Struktur wurde mit direkten Methoden gelöst und bis zu einem R-Wert von 5,92% verfeinert. Gold(I) bildet mit dem Liganden N,N-Diethyl-N′-benzoylthioharnstoff einen monodental über Schwefel koordinierten Komplex. Die Ligandatome Schwefel und Chlor sind nahezu linear an das Zentralatom gebunden.
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  • 9
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 737-742 
    ISSN: 0044-2313
    Keywords: Indium ; tris(N,N-diethyl-N′-benzoylselenoureato)indium(III) ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of Tris(N,N-Diethyl-N′-benzoylselenoureato)indium(III)In(C12H15N2OSe)3 crystallizes in the monoclinic space group P21/c. The cell parameters are a = 11.792(2), b = 36.797(4), c = 18.574(2) Å, β = 92.15(2)° and Z = 4. The structure was solved with Patterson and direct methods and was refined to a final R-value of 3.41%. The asymmetric unit contains two complex molecules. The indium atoms are bidentally coordinated by three N,N-Diethyl-N′-benzoylselenourea molecules to form distorted octahedra with facial arrangement of the selenium and oxygen donor atoms. The chelate rings diverge strongly from planarity. The In—Se bond lengths vary from 2.643(1) to 2.657(1) Å, the In—O bond lengths from 2.179(4) to 2.203(4) Å, respectively.
    Notes: In(C12H15N2OSe)3 kristallisiert in der monoklinen Raumgruppe P21/c mit den Gitterkonstanten a = 11,792(2), b = 36,797(4), c = 18,574(2) Å, β = 92,15(2)°, Z = 4. Die Struktur wurde mit Patterson und Direkten Methoden gelöst und bis zu einem R-Wert von 3,41% verfeinert. In der asymmetrischen Einheit befinden sich zwei In(C12H15N2OSe)3-Komplexmoleküle. Jeweils drei N,N-Diethyl-N′-benzoylseleno-harnstoff-Moleküle sind bidental über Selen- und Sauerstoffatome an die Zentralatome koordiniert. Das Koordinationspolyeder ist ein verzerrter Oktaeder mit facialer Anordnung der Donoratome. Die Chelatringe weichen deutlich von der Planarität ab. Die In—Se-Abstände in den beiden Oktaedern liegen zwischen 2,643(1) und 2,657(1) Å, die In—O-Abstände variieren von 2,179(4) bis 2,203(4) Å.
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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 177-182 
    ISSN: 0044-2313
    Keywords: Bis(N,N-diethyl-N′-benzoylselenoureato)nickel(II) ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of Bis(N,N-diethyl-N′ -benzoylselenoureato)nickel(II)Ni(C12H15N2OSe)2 crystallizes in the monoclinic space group P21/c. The cell parameters are a = 11.399(3), b = 16.016(4), c = 14.910(6) Å, β = 104.64(3)° and Z = 4. The structure was solved with Patterson and direct methods and was refined to a final R-value of 5.43%. Nickel is coordinated to two N,N-diethyl-N′ -benzoylselenourea molecules to form a bidentally coordinated chelate complex with cis arrangement of the donor atoms. Coordinaton around the nickel atom is planar while the chelate rings diverge from planarity. The ethyl groups of one diethylamino group are disordered. The Ni—Se bond lengths are 2.244(1) and 2.264(1) Å, the Ni—O bond lengths are 1.871(4) and 1.883(4) Å, respectively.
    Notes: Ni(C12H15N2OSe)2 kristallisiert in der monoklinen Raumgruppe P21/c mit den Gitterkonstanten a = 11,399(3), b = 16,016(4), c = 14,910(6) Å, β = 104,64(3)°, Z = 4. Die Struktur wurde mit Patterson und Direkten Methoden gelöst und bis zu einem R-Wert von 5,43% verfeinert. Nickel bildet mit dem Liganden N,N-Diethyl-N′-benzoylselenoharnstoff einen bidental koordinierten Chelatkomplex, in dem zwei Ligandmoleküle über Selen- und Sauerstoffatome in cis-Anordnung an das Zentralatom koordiniert sind. Die Koordinationssphäre um das Nickelatom ist planar, die Chelatringe weichen dagegen deutlich von der Planarität ab. Die Ethylgruppen einer Diethylaminogruppe sind fehlgeordnet. Die Ni—Se-Abstände betragen 2,244(1) und 2,264(1) Å, die Ni—O-Abstände 1,871(4) und 1,883(4) Å.
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