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  • Inorganic Chemistry  (35)
  • 1995-1999  (35)
  • 1985-1989
  • 1950-1954
  • 1930-1934
  • 1915-1919
  • 1910-1914
  • 1996  (35)
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  • 1995-1999  (35)
  • 1985-1989
  • 1950-1954
  • 1930-1934
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  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 622 (1996), S. 845-852 
    ISSN: 0044-2313
    Keywords: Nickel orthoperiodate ; i.r., Raman spectra ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: NiH3IO6 · 6 H2O  -  Crystal Structures and Vibrational SpectraThe crystal structure of NiH3IO6 · 6 H2O has been determined by X-ray single-crystal diffraction (Pc, Z = 2, a = 516.74(9), b = 981.5(2), c = 1052.5(2) pm, β = 116.496(8)°) on the basis of 4169 unique reflections (R = 1.96%). The structure is built up of distorted Ni(H2O)62+ and H3IO62- octahedra linked by hydrogen bonding. IR and Raman spectra of both the title compound and isostructural MgH3IO6 · 6 H2O as well as of deuterated specimens are given. There are up to 14 different OH(OD) modes in the spectra of isotopically dilute samples due to the 15 different hydrogen positions of the structure. The internal modes of the meridional H3IO62- ions (pseudo C2v symmetry) are discussed with respect to that double T-shaped entity, which gives rise to only two instead of 3I—O, I—O(H), and OH stretches in the IR and Raman spectra, i.e. the same as for facial (C3v) structured ions.
    Notes: Die Kristallstruktur (Pc, Z = 2) von NiH3IO6 · 6 H2O wurde mittels Röntgen-Einkristallmessungen auf der Basis von 4169 symmetrieunabhängigen Reflexen bestimmt (R = 1,96%). IR- und Raman-Spektren von NiH3IO6 · 6 H2O und der isotypen Verbindung MgH3IO6 · 6 H2O sowie von deuterierten Präparaten werden mitgeteilt. Die Spektren isotypenverdünnter Proben zeigen bis zu 14 OH(OD)-Streckschwingungen entsprechend den 15 verschiedenen Wasserstoff-Positionen der Struktur. Die meridionalen H3IO62--Ionen (Pseudosymmetrie C2v) besitzen wegen der T-förmigen Anordnung der je 3 IO-und IOH-Gruppen nur je 2 IO-, IO(H)- und OH-Streckschwingungen in den IR- und Raman-Spektren und können daher schwingungsspektroskopisch nicht von H3IO62--Ionen mit facialer Struktur (C3v) unterschieden werden.
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  • 2
    ISSN: 0044-2313
    Keywords: Sn(P2)3Sn cage system ; NMR data, crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure of Hexa-t-butyl-1,4-dichloro-1,4-distanna-2,3,5,6,7,8-hexaphosphabicyclo[2.2.2]octane - a New Cage Compound with the Sn(P2)3Sn SkeletonThe reaction of the diphosphide K2[(tBuP)2] 1 with SnCl4 leads by a redox process mainly to (tBuP)3,4 and other sideproducts. However, at the same time a threefold [2 + 1]-cyclocondensation reaction takes place yielding the new cage compound hexa-t-butyl-1,4-dichloro-1,4-distanna-2,3,5,6,7,8-hexaphosphabicyclo[2.2.2]octane, ClSn(tBuP—PtBu)3SnCl 2. 2 could be obtained in a pure form and characterized 31P and 119Sn NMR spectroscopically; 2 was also characterized by a single crystal structure analysis.
    Notes: Bei der Reaktion zwischen dem Diphosphid K2[(tBuP)2] 1 und SnCl4 finden überwiegend Redoxreaktionen statt, die zu (tBuP)3,4 und weiteren Nebenprodukten führen. Gleichzeitig findet aber auch eine dreifache [2 + 1]-Cyclokondensation statt, bei der die neuartige Käfigverbindung Hexa-t-butyl-1,4-dichloro-1,4-distanna-2,3,5,6,7,8-hexaphospha-bicyclo[2.2.2]octan, ClSn(tBuP—PtBu)3SnCl 2 gebildet wird. 2 konnte in reiner Form isoliert und 31P- und 119Sn-NMR-spektroskopisch sowie durch eine Einkristallstrukturanalyse charakterisiert werden.
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  • 3
    ISSN: 0044-2313
    Keywords: Phosphorus tin heterocycles ; syntheses ; crystal structure ; NMR ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis of the Stannatetraphospholanes (tBuP)4SnR2 (R = tBu, nBu, C6H5) and (tBuP)4Sn(Cl)nBu Molecular and Crystal Structure of (tBuP)4Sn(tBu)2The reaction of the diphosphide K2[tBuP-(tBuP)2-PtBu] 4 with the halogenostannanes (tBu)2SnCl2, (nBu)2SnCl2, (C6H5)2SnCl2 or nBuSnCl3 in a molar ratio of 1 : 1 leads via a [4 + 1]-cyclocondensation reaction to the stannatetraphospholanes (tBuP)4SnR2 3 b-3 d and (tBuP)4Sn(Cl)nBu 3 e, respectively, with the binary 5-membered P4Sn ring system. 3 b was characterized by a single crystal structure analysis; the 5-membered ring exists in a planar conformation. The compounds 3 b-3 e were identified by NMR and also by mass spectroscopy; the 31P{1H}-NMR spectra of 3 b-3 d showed an AA′MM′ (AA′MM′X), 3 e on the other hand an ABCD (ABCDX) spin system.
    Notes: Bei der Reaktion zwischen dem Diphosphid K2[tBuP-(tBuP)2-PtBu] 4 und den Halogenstannanen (tBu)2SnCl2, (nBu)2SnCl2, (C6H5)2SnCl2 bzw. nBuSnCl3 im Molverhältnis 1 : 1 findet eine [4 + 1]-Cyclokondensationsreaktion statt, bei der die Stannatetraphospholane (tBuP)4SnR2 3b-3d bzw. (tBuP)4Sn(Cl)nBu 3 e mit dem binären Fünfringgerüst P4Sn gebildet werden. Von 3 b wurde eine Einkristallstrukturanalyse durchgeführt; das Fünfringgerüst zeigt eine planare Konformation. Die Verbindungen 3 b-3 e wurden Massen- und NMR-spektroskopisch charakterisiert; 3 b-3 d liefern im 31P{1H}-NMR-Spektrum ein AA′MM′-(AA′MM′X)-, 3 e dagegen ein ABCD- (ABCDX)-Spinsystem.
    Additional Material: 3 Ill.
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  • 4
    ISSN: 0044-2313
    Keywords: Trifluoromethyl tellurium compounds ; crystal structure ; NMR spectra ; metathesis reactions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure of CF3TeTeCF3. Synthesis, Characterization, and Properties of CF3TeITe2(CF3)2 crystallizes in the monoclinic space group P21/a with four formular units in the unit cell. The lattice constants are a = 10.13(1) Å, b = 11.489(7) Å, c = 6.822(8) Å and β = 101.20(8)°. CF3TeI is prepared by a quantitative reaction of Te2(CF3)2 with equimolar amounts of iodine. This compound is very instable, no isolation is possible. NMR spectra have been registrated. From metathesis reactions CF3TeX (X = C≡CC6H5, t-C4H9, SCN, SC6F5) are prepared.
    Notes: Te2(CF3)2 kristallisiert in der monoklinen Raumgruppe P21/a mit vier Formeleinheiten in der Elementarzelle. Die Gitterkonstanten betragen a = 10,13(1) Å, b = 11,489(7) Å, c = 6,822(8) Å und β = 101,20(8)°. Bei der Umsetzung von Te2(CF3)2 mit der äquimolaren Menge Iod entsteht CF3TeI in quantitativer Ausbeute, eine Isolierung gelingt nicht. Die NMR-Spektren zeigen eine starke Lösungsmittelabhängigkeit. Durch Metathesereaktionen werden die Verbindungen CF3TeX (X = C≡CC6H5, t-C4H9, SCN, SC6F5) synthetisiert.
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  • 5
    ISSN: 0009-2940
    Keywords: Triazacyclohexanes ; Chromium complexes ; Amides ; Hexamethyldisilane ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of N,N′,N′′-trimethyl-1,3,5-triazacyclohexane chromium trichloride ((Me3TAC)CrCl3, 1) with LiN(SiMe3)2 or NaN(SiMe3)2 in petroleum ether yields nearly quantitatively [Cr{N(SiMe3)2}3] (2) with loss of the Me3TAC ligand. Compound 2 could be crystallized from hexamethyldisilane as [Cr{N(SiMe3)2}3] · (Me6Si2)0,5 which allowed the refinement of the X-ray crystal structure in the trigonal space group P-31c (no. 163) (a = 16.012(3) Å, c = 8.4796(12) Å, V = 1882.8(6) Å3, Z = 2) without severe disorder.
    Additional Material: 3 Ill.
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 485-487 
    ISSN: 0009-2940
    Keywords: Dimetallations ; Insertions ; Rhenium ; Isothiocyanates ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Molecules containing dimetallated hydrocarbyl groupings are of great chemical interest[1-3]. These groupings often represent intermediates in important catalytic processes[4]. Recently, we have shown that substituted dimetallated olefins can be formed by alkyne insertion into the metal-metal bonds of certain dinuclear complexes[2,5]. Complexes having dimetallated hydrocarbyl groups combined with heteroatoms are quite rare[6]. Herein is described the formation of a dimetallathioimidate grouping by the insertion of an organic isothiocyanates into an unsupported metal-metal bond. Organic isothiocyanates are useful reagents in organic synthesis[7], but the organometallic chemistry of these molecules is not yet well developed[8].
    Additional Material: 3 Ill.
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1093-1098 
    ISSN: 0009-2940
    Keywords: Indium tris(thiobenzoate) ; Triethylammonium tetrakis(thiobenzoato)indate ; Tin, butyl-, tris(thiobenzoate) ; Tin, dichloro-, bis(thiobenzoate) ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Indium(III) and tin(IV) thiocarboxylates were prepared and characterized on the basis of their IR, 13C- and 19Sn-NMR data. Indium tris(thiobenzoate) (1) decomposes into a sulfido complex In (S)[S(O)CPh] (2a). The corresponding tris(thioacetate) In[S(O)CMe]3 is thermally too unstable to be isolated. The anionic tetrakis complex [Et3NH]{In[S(O)CPh]4} (3) was characterized by X-ray crystallography which revealed a distorted tetrahedral coordination at the In atom. X-ray diffraction analysis of the complexes BuSn[S(O)CPh]3 (4) and Cl2Sn[S(O)CPh]2 (7) showed distorted tetrahedral and cis-octahedral structures, respectively.
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  • 8
    ISSN: 0009-2940
    Keywords: Lanthanum complexes ; Neodymium complexes ; Erbium complexes ; Pyrazolate, 3,5-di-tert-butyl-, complexes of ; Pyrazolate, 3,5-diphenyl-, complexes of ; 1,2-Dimethoxyethane, complexes of ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The complexes [Ln(Ph2pz)3 (DME)2] and [Ln(tBu2pz)3 (DME)] (Ln = La, Nd, Er; Ph2pzH = 3,5-diphenylpyrazole; tBu2pzH = 3,5-di-tert-butylpyrazole; DME = 1,2-dimethoxyethane) have been prepared by reaction of the lanthanoid metal with bis(pentafluorophenyl)mercury and the pyrazole in DME. The molecular structures of [Er(Ph2pz)3 (DME)2] (3) and [Nd(tBu2pz)3 (DME)]∞ (5) have been determined by X-ray diffraction. Complex 3 has nine-coordinate Er with three chelating Ph2pz ligands and one chelating and one η1-bound DME. There is a trigonal prismatic arrangement of the oxygen donors and the centres of the N - N bonds. 5 was found to be a linear polymer with transoid DME ligands bridging Nd(tBu2pz)3 units in a novel manner. The centres of the N - N bonds (which are essentially coplanar with Nd), and the oxygen donor atoms adopt an arrangement intermediate between trigonal-bipyramidal and square-pyramidal [O - Nd - O 153.5(2)°].
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  • 9
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 21-24 
    ISSN: 0009-2940
    Keywords: Orthoamides ; Trisaminomethanes, tricyclic ; Guanidinium cation, alkylation ; Copper(II) complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The orthoamides 2a, b (R = Ph and PhCH2) have been prepared by alkylation of the guanidinium salt 4+BPh4- with PhNa and PhCH2Na, respectively. The crystal structures of the two orthoamides have been determined by X-ray crystallography. Their reaction with CuCl2 gives 1:1 complexes. The crystal structure of the complex with 2a shows a square planar geometry around the copper atom with η2-2a and two chlorides and weak interactions two the third nitrogen atom and a C-H bond of 2a in the axial positions.
    Additional Material: 3 Ill.
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  • 10
    ISSN: 0009-2940
    Keywords: Thietane ; Catalysis ; Tungsten ; Macrocycle ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The following four compounds have been synthesized: M(CO)5L (3 and 4, where M = Cr and W, and L = H2), W(CO)5(12S3) (5, where 12S3 = 1,5,9-trithia-cyclododecane), and [W(CO)5]2(12S3) (6). The molecular structures of 4 and 5 were established by single-crystal X-ray diffraction analyses. Both compounds contain a W(CO)5 group coordinated to one of the sulfur atoms of the hetero-cycle. The ability of the compounds M(CO)6, 1 and 2 (M = Cr and W), and 3 - 5 to catalytically produce ring opening cyclooligomerization (ROC) of thietane into 12S3 and 24S6, (24S6 = 1,5,9,13,17,21-hexathiacyclotetracosane) has been investigated. Compounds 1 - 3 have relatively low activity. Compounds 4 and 5 have the highest activity and selectivity for 12S3 formation. Crystal Data for 4: space group = P212121, a = 12.906(2) Å, b = 13.730(4) Å, c = 6.427(1) Å, Z = 4, 1306 reflections, R = 0.033; for 5: space group = P1¯, a = 12.703(1) Å, b = 13.510(2) Å, c = 5.833(1) Å, α = 101.75(1)°, β = 97.54(1)°, γ = 101.70(1)°, Z = 2, 2225 reflections, R = 0.023.
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