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  • Atomic, Molecular and Optical Physics  (441)
  • crystal structure  (128)
  • 1990-1994  (569)
  • 1965-1969
  • 1992  (569)
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  • 1990-1994  (569)
  • 1965-1969
Year
  • 1
    ISSN: 1573-904X
    Keywords: pharmaceutical salt selection ; salts of p-aminosalicylic acid ; hydrates ; crystal structure ; thermal stability
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The potassium (K), sodium (NA), calcium (CA), and magnesium (MG) salts of p-aminosalicylic acid were obtained, and their thermal behavior was characterized by means of differential scanning calorimetry (DSC) and thermogravimetric analysis (TG). Their crystal and molecular structures were determined by single-crystal X-ray diffraction after powder patterns had shown them to be nonisomorphous. Different degrees of hydration were observed for the solid salts, and an assessment of hydrate stability to dehydration was made from thermogravimetric studies. The onset temperature of dehydration (T t) of each salt varied within the series and exhibited correlation with X-ray determined structure. The observed onset of dehydration of MG and CA was higher than that of NA and is consistent with stronger ion-dipole interactions for the divalent salts. Crystallographic determination of the bond lengths between the metal ion and the water oxygens were 2.4 and 2.9 Å for NA, between 2.0 and 2.1 Å for MG, and 2.4 Å for CA. The open nature and presence of a channel feature in the structure of the sodium salt may have facilitated escape of water molecules from the crystal. Particle presentation (e.g., size, crystallinity) was also shown to affect dehydration behavior.
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  • 2
    Electronic Resource
    Electronic Resource
    Springer
    Pharmaceutical research 9 (1992), S. 365-371 
    ISSN: 1573-904X
    Keywords: celiprolol ; crystal structure ; two-dimensional nuclear magnetic resonance (2D NMR)
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal structure and nuclear magnetic resonance (NMR) spectra and assignments of celiprolol, N′-[3-acetyl-4[3-[N-t-butylamino-2-hydroxypropoxy]phenyl]-N, N-diethylurea, are reported. Celiprolol crystallizes in the monoclinic space group, P2l/a, with a = 9.081(2), b = 13.800(4), and c = 17.471(5) Å and β = 95.04(2)°. Structure was solved by direct methods; structure refinement to R of 0.058. Intermolecular hydrogen-bonding in the crystal is discussed. The 1H, 13C, and two-dimensional (2D) NMR spectra of the hydrochloride have been obtained and definitive signal assignments made.
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  • 3
    ISSN: 1573-9171
    Keywords: crystal structure ; molecular complexes ; phosphinimines ; protonation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract X-ray diffraction analysis has been used to determine the crystal structures of the 1:1-composition products of protonation by perchloric acid of isomeric triphenyl-N-(4-methylpyridyl-2)phosphinimine (1) and triphenyl-N-(3-methylpyridyl-2)phosphinimine (2). The structures were refined toR=0.048 andR=0.052, respectively, using 2274 (1) and 2647 (2) reflections. The protonation centers are located at the sites of N atoms of the pyridine ring (1) and the phosphinimino group (2). The distribution of the bond lengths in the cations suggests that a significant contribution is made by a phosphonic structure with positive charges localized on the P atoms. N-H...O hydrogen bonds, with lengths of 2.890(4) and 3.020(3) Å, connect cations and anions in both structures.
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  • 4
    ISSN: 1573-9171
    Keywords: synthesis ; crystal structure ; 1,12-difluoro-1,1,3,5,5,8,8,10,12,12-decanitro-3,10-diazadodecane-6,7-diol dinitrate
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A two-step synthesis has been proposed to obtain 1,12-difluoro-1,1,3,5,5,8,8,10,12,12-decanitro-3,10-diazadodecane-6,7-diol dinitrate, starting from 1,1,4,4-tetranitrobutane-2,3-diol and N-(methoxymethyl)-2-fluoro-2,2-dinitroethyl-amine, followed by nitration of the Mannich base formed. An x-ray-diffraction investigation of the dinitrate obtained was carried out.
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  • 5
    ISSN: 1573-9171
    Keywords: macrocyclic polyethers ; crystal structure ; biological activity ; IR spectra ; complex with calcium thiocyanate
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The antihypoxic and anticonvulsant activity of eight new amidophosphoryl derivatives of crown ethers was investigated. It was found that some of them exhibit pronounced antihypoxic activity. The results of an x-ray structural and IR spectroscopic study of dibenzo-N-phenylphosphonyl-14-crown-5 (a=9.818,b=16.062,c=15.925 Å; γ=124.90°;V=2072 Å3;M=417.2;d=1.33 g/cm3 forZ=4, 1955 independent reflections [I〉3σ(I)] in a DAR-UM inCuK α radiation,P2 1/b space group,R=5.2%) and dibenzo-N-adamantylphosphonyl-14-crown-5 compounds (a=11.077,b=15.936,c=16.771 Å; γ=56.05°;V=2456 Å3;M=486.3;d=1.31 g/cm3 forZ=4, 2164 independent reflections [I〉3σ(I)] in a DAR-UM inCuK α radiation,P21/b space group,R=5.1%) are reported. Some details of the structure of the dibenzo-N-phenylphosphonyl-14-crown-5-complex with calcium thiocyanate and water are discussed; a polyhedron with a coordination number of six was found for the first time for calcium complexes with macrocyclic ligands. The combined examination of the results of the biological, x-ray structural, and IR spectroscopic study of macrocyclic, 14-member ligands suggested that the nature of the substituents at phosphorus affect the conformational state of the macrocycle, which remains unchanged in complexation in the investigated conditions.
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  • 6
    ISSN: 1573-9171
    Keywords: X-ray crystallographic analysis ; 1,1′-divinyl-2,2′-biimidazolyl ; crystal structure ; molecular structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal and molecular structures of 1,1′-divinyl-2,2′-biimidazolyl (L) were determined by x-ray crystallographic analysis. It was established that the molecule of L has crystallographic symmetry 2 and a cisoid conformation with an angle of rotation of 128° between the imidazole rings. The length of the C2-C2′ bond is increased to 1.485(11) Å compared with the length of the analogous bond in unsubstituted 2,2′-biimidazolyl (1.423 Å). Localization of the N=C multiple bond is observed [1.297(9) Å]. The other N-C bonds of the ring are almost equalized (1.374 Å) and are close to the standard values for bonds of the C sp 2-N type in imidazoles. The angle between the plane of the heterocycle and the plane passing through the atoms of the vinyl group amounts to 7°.
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  • 7
    ISSN: 1573-1111
    Keywords: Charles Pedersen ; crown ethers ; phenol-pendant cyclam-zinc(II) complex ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The molecular structure of phenol-pendant cyclam-zinc(II) complex,4a, has been determined by X-ray structure analysis. Crystals of4a · ClO4 · CH3OH (C16H27N4OZn · ClO4 · CH3OH) are monoclinic, space groupP21/nn, with four molecules in the unit cell of dimensionsa=31.198(2) Å,b=8.426(1) Å,c=8.214(1) Å, andβ=93.96(1)°. The structure was solved by the heavy atom method and refined anisotropically toR=0.044,R w=0.062 for 1551 independent reflections. The complex assumes a five-coordinate, square pyramidal geometry, where zinc(II) is surrounded by the cyclam moiety in a planar fashion with the pendant phenolate anion occupying an axial position. An extremely short Zn-O(phenolate) bond distance of 1.983(5) Å, in conjunction with the 0.288 Å displacement of Zn(II) above the cyclam N4 plane toward the phenolate, accounts for the extremely low pK a value of 5.8 for the pendant phenol. These facts about4a, in comparison with the previous findings for the Ni(II) (4b) and Cu(II) complexes (4c) with the same ligand, illustrate well the characteristics of zinc(II) ion coordination properties.
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  • 8
    ISSN: 1573-1111
    Keywords: Host-guest inclusion compound ; p-,m-,o-xylene ; deoxycholic acid ; symmetry factor ; energy transfer ; photophysical factor ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The isomerization processes induced by UV photons in inclusion compounds of the host-guest type are examined, with special attention to the photophysics of the energy transfer process between the host and the guest, as well as to the influence of the host molecular cavity symmetry and the guest molecular symmetry. In particular, the experimental study has been carried out on the isomerization processes ofp-,m-, ando-xylene inside the molecular cavities of deoxycholic acid. The results have been compared with those obtained by irradiating the xylenes in an inert solution of hexane. The main difference is the elimination of by-products when the photochemical process is carried out in the solid state inclusion compound; however, the high purity of the isomerization product corresponds to a decrease in its yield with respect to the reaction in solution, due to the energy transfer process from the host to the guest moiety.
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  • 9
    ISSN: 1573-1111
    Keywords: Dioxocyclam ; 5,7-dioxo-1,4,8,11-tetra-azacyclotetradecane ; platinum tetrachloride ; crystal structure ; paramagnetic properties of ionic stacked structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The paramagnetic complex salt of diprotonated dioxocyclam (1,11-dihydro-5,7-dioxo-1,4,8,11tetra-azacyclotetradecane), Pt(II) tetrachloride and water has been synthesized in strongly acidic medium and identified by X-ray structure analysis. The crystals of [(C10H22N4O2)2+(PtCl4)2−]·H2O are monoclinic, space groupP21 c,M r=585.23,a=9.516(1) Å,b=11.926(1) Å,c=16.622(2) Å,β=102.88(2)°,V=1839(1)Å3,Z=4,D x=2.114 g cm−3, λ(MoK α)=0.70930 Å,μ=83.1 cm−1,F(000)=1128,T=292 K,R=0.019 for 2808 observed reflections withI 〉 3δ(I). Alternating moieties of diprotonated dioxocyclam and a PtCl 2− 4 anion form columns running down the c axis. Water molecules are localized in the intercolumnar space and contribute to the extensive hydrogen bond network. The macrocycle conformation is characterized by two sequences of torsional angles, corresponding to two different subunits. The shorter sequence idealized as (-sc, ap, -ac, + ac, ap, +sc) [sc( ±60°), ac( ±120°), ap(180°)], describing the C pseudosymmetric part of the molecule, is centered on a -CH2 group between the two peptide O-C-N-H fragments. The opposite C pseudosymmetric subunit has a nearly (-sc, ac, -SC, ap)2 conformation. Pt is square planar coordinated by four Cl atoms, Pt-Clαve = 2.306(8) Å. The shortest Pt ... Pt distance is 7.200(1) Å.
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  • 10
    ISSN: 1573-1111
    Keywords: Inclusion compound ; hydroxy compound ; crystal structure ; thermal analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal and molecular structures of the title host compound (I), C35H26O, and its inclusion complexes with water (II), C35H26O·H2O and dimethylsulphoxide (III), C35H26O·C2H6OS are reported. (I) is monoclinicC2/c,a = 9.725(1),b = 20.031(3),c = 26.545(3) Å, β = 90.60(1)0,V = 5170 Å3,Z = 8; (II) is triclinic, $$P\bar 1$$ ,a = 10.206(1),b = 10.324(2),c = 14.425(2) Å, α = 101.68(1), β = 89.92(2), γ = 116.34(1)0,V = 1327 Å3,Z = 2; (III) is monoclinicP21/n,a = 17.832(5),b = 10.109(3),c = 17.901(5) Å, β = 111.93(2)0,V = 2993 Å3,Z =4. The structures were solved by direct methods and refined to final residuals of 0.045, 0.048, and 0.071, respectively. Thermal analysis of the complexes corroborates the crystallographic results.
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  • 11
    ISSN: 1573-1111
    Keywords: Inclusion compounds ; calixarene ; crystal structure ; hydrogen bonding ; amines
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The structure of thep-t-butyldihomooxacalix[4]arene triethylamine (1 : 2 complex has been determined by X-ray crystallography. Crystals are monoclinic, space groupCc,a = 22.821(3),b = 15.257(3),c = 16.365(2) Å,β = 97.44(1)°,V = 5650(1) Å3,Z = 4,D calc = 1.03 g cm−3. One triethylamine (Et3N) molecule has one of its ethyl groups pointing inside the cavity of a calixarene molecule; its nitrogen atom is directed exo to this calixarene molecule and is involved in a hydrogen bond with one of the hydroxy groups of a neighbouring calixarene molecule. This scheme leads to columns of alternating host and guest molecules. The other Et3N molecule is in the interhost space. This feature allows us to define the title compound as a complex/clathrate hybrid.
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  • 12
    ISSN: 1573-1111
    Keywords: Crown compound ; potassium thiocyanate ; crown cation complex ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Single crystal X-ray analysis of the hydrated KSCN complex of benzodinaphthopyridino-21-crown-7 (1) (1 : 1 : 1) is reported. Crystals of the complex are orthorhombic,Pnma, withα = 16.946(4),b = 22.298(4),c = 10.390(8) Å andD c = 1.184 g cm−1,Z = 4. The host macroring (1) has a mirror symmetry and exists in a so-called ‘dentists chair’ conformation. The cation (K−) is coordinated to all the six ether oxygen atoms and also weakly to the pyridine N atom. The SCN− anion group has a statistical type of disorder with opposite orientations of S and N such that nitrogen and sulphur are coordinated to K+. Packing of the host molecules is in columns to form quasi channels with K+, SCN−, and H2O being located inside the stacks.
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  • 13
    ISSN: 1573-1111
    Keywords: Calix[4]arene ; crystal structure ; second-sphere coordination ; nickel(II) ; copper(II) ; pyridine
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The title compounds crystallize such that bilayers of calixarenes are separated by hydrophilic layers. In each case the transition metal has, in addition to a primary sphere of ligands, a second-sphere coordination by a calixarene. [(H2O)5Ni(NC5H5)]2(Na)[calix[4]arene sulfonate]·3.5 H2O,1, crystallizes in the triclinic space groupP $$\bar 1$$ witha = 12.487(4),b = 14.281(2),c = 15.055(5) Å, α = 85.66(2), β = 80.07(2), γ = 80.48(2)°, andD c = 1.64 g cm−3 forZ = 2. Refinement based on 2441 observed reflections led to a finalR value of 0.066. There are two different environments for the nickel-containing cations: one is positioned within the hydrophilic layer with the pyridine ligand intercalated into the hydrophobic calixarene bilayer and the other is also positioned within the hydrophilic layer, but the pyridine ligand is inserted into the hydrophobic cavity of the calix[4]arene. [(H2O)4Cu(NC5HS)2](H3O)3[calix[4]arene sulfonate]·10 H2O,2, crystallizes in the triclinic space groupP $$\bar 1$$ witha = 15.438(4),b = 15.727(6),c = 12.121(9) Å, α = 112.74(4), β = 102.02(4), γ = 85.34(4)°, andD c = 1.57 g cm−3 forZ = 2. Refinement based on 3925 observed reflections led to a finalR value of 0.107. The structure is similar to that of 1 except that the one copper-containing cation spans the hydrophilic layer and is intercalated into the bilayer of calixarenes on one side and positioned into the calixarene cavity on the other.
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  • 14
    ISSN: 1573-1111
    Keywords: 1,2-Dialkylated calix[4]arene ; crystal structure ; ethanol inclusion complex ; intramolecular hydrogen bonding patterns
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal structure of the title compound (1 · C2H5OH) has been determined by single-crystal X-ray analysis and refined to anR-value of 0.074 for 2732 observed reflections [I 〉 2.0σ(I)]. Crystals are triclinic, space group P $$\bar 1$$ , witha = 13.6150(18),b = 13.7195(11),c = 16.5497(16) Å, α = 73.132(7),β = 66.165(9), γ = 65.580(8)° andZ = 2. Calix[4]arene (1) adopts a relatively open distorted cone conformation in the solid state, with two pendantsyn-proximal O-CH2-Py groups. The major conformation determining features in (1 · C2H5OH) are the presence of (a) an intramolecular O-H...O hydrogen bond between adjacent proximal phenolic oxygens, O...O 2.719(7) Å and (b) an intramolecular O-H...N hydrogen bond between a phenolic oxygen and a proximal pyridinyl nitrogen, O...N 2.810(8) Å. The intramolecular hydrogen bonding and the interplanar angles of 65.1(3) and 50.7(3)° between opposite aromatic rings facilitate the inclusion of an ethanol molecule within the calixarene cup.
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  • 15
    ISSN: 1573-1111
    Keywords: Cation binding ; crown ether ; crystal structure ; lariat ether ; synthesis ; triaza-18-crown-6
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Details of a new synthetic approach to 4,10,16-triaza-18-crown-6 (‘triaza-18-crown-6’) are reported, along with the preparation and binding properties of the following derivatives having the indicated sidearms: CH2C≡CH, CH2CH2OH, CH2CH2OCH3, COCH2OCH3,CH2COOCH2CH3, CH2C6H5, and CH2C6H4−2−NO2. A key intermediate in the synthesis of triaza-18-crown-6 is 4-N-toluenesulfonyl-1,7,13-trioxa-4,10,16-triazacyclooctadecane-9,17-dione. This compound is found by solid state structure analysis to fold to form an intramolecular, doubly-hydrogen bonded complex in which the two N-H protons interact with the two tosyl group oxygens. Details of the structure are reported.
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  • 16
    Electronic Resource
    Electronic Resource
    Bognor Regis [u.a.] : Wiley-Blackwell
    ISSN: 0887-6266
    Keywords: poly(2,6-oxynaphthoate) ; crystal structure ; whiskers ; lamellae ; unit cell ; transitions ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Electron diffraction from single crystal lamellae and whiskers of poly(2,6-oxynaphthoate) reveals the presence of at least 3 unit cells. The equatorial reflections in the patterns from the whiskers correspond to the dominant (phase I) hk0 diffraction pattern from the lamellae; phase I is monoclinic with 2 chemical repeats per physical repeat. The intensity distributions in the hk0 patterns of phase I and II resemble those of the same phases in poly(p-oxybenzoate). The hk0 reflections of phase III suggest a common internapthalene unit spacing, but variable lateral (and possibly axial) shifts; apparently related orthorhombic and monoclinic patterns, with variable γ*, are observed. At elevated temperature, above the crystalliquid crystal transition (ca. 330°C), quadrant reflections are retained; the change in the hk0 pattern from any given crystal is gradual, extending over some 40°C. Above the liquid crystal-liquid crystal transition (ca. 460°C) the pattern can be interpreted in terms of nematic or possibly smectic A packing. © 1992 John Wiley & Sons, Inc.
    Additional Material: 19 Ill.
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  • 17
    ISSN: 1572-8862
    Keywords: Heterometallic-heterobridging cubane-type tetranuclear cluster ; preparation ; crystal structure ; molecular orbital calculation ; quasi-aromaticity ; copper ; molybdenum
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract By the reaction of cluster [Mo3OS3](dtp)4(H2O) used as starting material with CuI using [3+1] mode, two novel heterometallic-heterobridging cubane-type tetranuclear cluster compounds [CuMo3OS3]·I·(μ-OAc)[S2P(OC2H5)2]3·L [(I)L=py, (II)L=DMF] [dtp=S2P(OC2H5)2; OAc=OOCCH3] containing [CuMo3OS3] core have been obtained. Compounds (I) and (II) have been characterized by IR, EPR, UV-VIS, electrochemistry and X-ray crystallography. By comparison of these two compounds with the analogous [CuMo3S4] series in the structure and molecular orbital calculation, the influence of mixed S/O bridging on the structure is discussed. It is demonstrated that the {Mo3S3} cluster ring in [Mo3OS3]4+ possesses a similar quasi-aromaticity to [Mo3S4]4+. Crystal data: for (I), space group= $$P\overline 1 $$ ,a=13.781(8)Å,b=14.523(6)Å,c=12.098(6)Å, α=98.37(4)°, β=109.41(5)°, γ=105.00(5)°,V=2133(2)Å3,Z=2,R=0.058; for (II), space group= $$P\overline 1 $$ ,a=13.215(4)Å,b=17.818(8)Å,c=9.873(4)Å, α=106.06(4)°, β=109.78(3)°, γ=82.00(3)°,V=2100(2)Å3,Z=2,R=0.045.
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  • 18
    ISSN: 1573-9171
    Keywords: synthesis ; crystal structure ; UV spectra ; 2,6-di-tert-butyl-4-[α-(2-hydroxy-1-naphthyl)methyl]phenol ; 2,6-di-tert-butyl-4-[α-morpholino-α-(2-hydroxy-6-bromo-1-naphthyl)methyl]phenol ; 2,6-di-tert-butyl-4-α-(2-hydroxy-1-naphthyl)-1,4-methylenequinone ; 2,6-di-tert-butyl-4-α-(2-acetyloxy-1-naphthyl)-1,4-methylenequinone
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Mannich bases exhibiting photo- and thermochromic properties in solutions were synthesized from 3,5-di-tert-butyl-4-hydroxybenzaldehyde and 2-naphthols. An investigation of an acetyl derivative of methylenequinone, modeling a product of photo- and thermochromic transformations, proved that the color change of solutions of the Mannich bases is due to reversible dissociation into colored methylenequinones and morpholine. On the basis of data of x-ray diffraction analysis of one of the Mannich bases, characteristics of their molecular structure were determined, and reasons were stated for their effect on the dissociation mechanism.
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  • 19
    ISSN: 1573-9171
    Keywords: hexafluorotitanates ; synthesis ; crystal structure ; 19F NMR ; IR spectroscopy
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Mixed alkali hexafluorotitanates of the composition LiMTiF6 are synthesized, which crystallize with the orthorhombic symmetry. The lattice parameters of these materials are determined. It is shown that substitution of the Li+ cation in Li2TiF6 by Na+, K+, Rb+, and Cs+ leads to various degrees of distortion of the hexafluoroion. It is determined (19F NMR data) that the change in the dynamic state of the octahedral [TiF6]2− ions is related to their transition from the hindered-rotational to the isotropic state.
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  • 20
    ISSN: 1573-9171
    Keywords: organic metals ; radical-cation salts ; bis(ethylenedithio)tetrathiafulvalene = ET ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The electrochemical oxidation of ET [bis(ethylenedithio)tetrathiafulvalene] in bromobenzene (electrolyte Bu 4 N[HgBr 3 ]) gave the radical-cation salt (ET) 8 [Hg 2 Br 6 ·PhBr] 2 (1), a new organic metal with a temperature range of 300–125 K. At 125 K a metal—dielectric transition is observed. Crystallographic data for (1):a=19.171(6),b=12.668(4),c=17.777(6) Å, α=118.03(3), β=89.45(2), γ=101.21(3)°, P $$\overline 1 $$ ,Z=1,d calc=2.30 g/cm 3 . The crystal structure of (1) is laminar. In the conducting organic layer the ET radical cations are linked into bands by shortened intermolecular S···S contacts of the “side-to-side” type. The anionic layer consists of centrosymmetric complexes [Hg 2 Br 6 ·C 6 H 5 Br] 2 4− . The Hg 1 and Hg 2 atoms are characterized by a trigonal configuration of the Hg-Br bond which is built up, on account of secondary Hg···Br interactions, into trigonal-bipyramidal for Hg 1 and trigonal-pyramidal (tetrahedral) for Hg 2 . Interaction between the anionic and cationic layers is effected through Br 6 ...S 8 contacts [3.491(7) Å)].
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  • 21
    ISSN: 1573-9171
    Keywords: organic metals ; bis(ethylenedithio)tetrathiafulvalene (ET) ; crystal structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The composition and structure of the radical-ion salt (ET) 2 [Hg(SCN) 2 Cl], a new organic metal withT M-D=50 K, were established in an x-ray structure investigation. Principal crystallographic data:a=36.69(1),b=8.302(8),c=11.732(8) Å, β=90.02(6)°, space groupCc, Z=4,d calc=2.08 g/cm 3 ,R=0.067. The crystal structure of the salt consists of an alternation of organic (cationic) and inorganic (anionic) layers along the axisa. The anionic layer consists of the polymeric chains in which the [Hg(SCN) 2 Cl]− ions are linked together along the axisc through secondary Hg···N bonds with lengths of 2.75(3) and 2.98(8) Å. On account of these interactions the trigonal configuration of the bonds of the Hg atom is built up to trigonal-bipyramidal. In the organic layer with a structure of the κ type the ET cations form dimers with an interplanar distance of 3.53 Å. ET cations belonging to neighboring dimers are linked together through shortened intermolecular S...S contacts with lengths of 3.40–3.50(2) Å.
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  • 22
    ISSN: 0044-2313
    Keywords: Bis(phthalocyaninato)cerium(IV) ; crystal structure ; u.v.-vis., m.i.r., f.i.r., resonance Raman spectra ; cyclovoltammetry ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation, Properties and Crystal Structure of Bis(phthalocyaninato)cerium(IV)The anodic or chemical oxidation with dibenzoylperoxide of solutions of bis(phthalocyaninato)cerate(III) in dichloromethane yields selectively sparely soluble bis(phthalocyaninato)cerium(IV), [Ce(Pc(2-))2]. Green, monoclinic needles cristallize with a = 18.783(12) Å b = 18.739(16) Å c= 15.618(10) Å ß114.30(7)°; Z = 4; space group C2/c. [Ce(Pc(2-))2] is a sandwich complex in which the cerium Atom is eightfold coordinated by the isoindole nitrogens of the two staggered convex Pc-rings. The u.v.-vis., m.i.r., f.i.r. and resonance Raman spectra are consistent with the structure.
    Notes: Schwerlösliches Bis(phthalocyaninato)cer(IV), [Ce(Pc(2-))2] wird durch anodische oder chemische Oxydation mit Dibenzoylperoxid von Bis(phthalocyaninato)cerat(III), gelöst in Dichlormethan, dargestellt. Es kristallisiert in grünen monoklinen Nadeln in der Raumgruppe C2/c mit den Gitterkonstanten a = 18,783(12) Å; b = 18,739(16) Å c = 15,618(10) Å β = 14,30(7)°; Z = 4. [Ce(Pc(2-))2] ist ein sandwichartiger complex in dem das cer-Atom von den Isoindol-Stickstoff-Atomen der beiden konvex verzerrten, auf Lücke stehenden Pc- Ringe achtfach-koordiniert ist. Die UV-VIS-, MIR-, FIR- und Resonanz-Raman-Spektren stehen im Einklang mit dieser Struktur.
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  • 23
    ISSN: 0044-2313
    Keywords: Cesium hydroxide hydrates ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Hydrates of Weak and Strong Bases. VII. Concerning the System Cesium Hydroxide - Water: The Crystal Structures of CsOH · 2H2O and CsOH · 3H2OIn the context of structural studies of hydrates of the alkali metal hydroxide the crystal structure of CsOH · 2H2O and CsOH · 3H2O have been determined for the first time. The diffractometer data, obtained at -150 · C,made it possible to locate and refine also all the H-atoms. The dihydrate was found to probably form only one phase, melting incongruently at 2,5 · C. It is orthorhombic with space group Pca21 and Z = 8 formula units per unit cell. The lattice constants are a = 13.238, b = 6.747 and c = 9.121 A. With 1870 independent observed reflection a final R value of 0.013 was obtained. The trihydrate, melting congruently et -5.5 ·C, is monoclinic with space group P21/n,Z = 4 and lattice constants a = 8.637, b = 5.984, c = 10.061 Å and ß = 96.57 ·. With 2098 independent observed reflection the final R is 0.026. In both hydrate structures there are no simple characteristic coordination polyhedra for the cations; in each case it is rather the hydrogen-bonded and fully ordered anionic water structure which shows up as the determining building principle. Both these water structures are altogether three-dimensional, but primarily contain layers. The anionic layers are formed by condensation of small and medium rings, namely four-, five- and seven-membered rings in CsOH · 2H2O and four-, five- and six membered ones in CsOH · 3H2O. They are linked together by one set each of extra H2O molecules between the layers as well as by the Cs+ ions.
    Notes: In Zusammenhang mit Untersuchungen zur Struktur von Hydraten der Alkalimetallhydroxide wurden die Kristallstrukturen von CsOH · 2H2O und CsoH · 3H2O erstmalig bestimmt. Die bei - 150°C erhaltenen Diffraktometerdaten erlaubten dabei auch die Lokalisierung und Verfeinerung Sämtlicher H-Atome. Das nach eigenen Untersuchungen wahrscheinlich nur einphasig vorliegende Dihydrat schmilzt inkongruent bei 2,5°C und kristallisiert orthorhombisch mit der Raumgruppe Pca21 und Z = 8 Formeleinheiten pro Elementarzelle sowie den Gitterkonstanten a = 13,238, b = 6,747 und c = 9,121 ß. Mit 1870 unabhängigen beobachteten Reflexen wurde ein abschließender R-Wert von 0,013 erreicht. Das bei - 5,5°C kongruent schmelzende Trihydrat ist monoklin mit der Raumgruppe P21/n und Z = 4. Die Gitterkonstanten betragen a = 8,637, b = 5,984, c = 10,061 A und ß = 96,57°. Mit 2098 unabhängigen beobachteten Reflexen liegt der abschließende R-Wert bei 0,026. In beiden Hydratstrukturen gibt es keine einfachen charakteristischen Koordinationspolyeder für die Kationen; vielmehr wird jeweils die durch H-Brücken gebildete und vollständig geordnete anionische Wasserstruktur zum bestimmenden Bauprinzip. Beide Wasserstrukturen sind insgesamt dreidimensional, enthalten primär aber Schichten. Die aus Kondensierten Kleinen und mittleren Ringen, nämlich Vier-, Fünf - und Siebenringen (CsOH · 2H2O) bzw. Vier-, Fünf- und Sechsringen (CsOH · 3H2O), bestehenden anionischen Schichten werden jeweils über einen Satz weiterer H2O-Moleküle zwischen den Schichten sowie über die Cs+-Ionen miteinander verknüpft.
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  • 24
    ISSN: 0044-2313
    Keywords: Copper weberites, Na2CuGaF7, Na2CuInF7 ; crystal structure ; magnetic investigation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Kupferweberite: Kristallstruktur und magnetische Untersuchung von Na2CuGaF7 und Na2CuInF7Die Kristallstruktur von zwei neuen Kupferweberiten Na2CuGaF7 und Na2CuInF7 wurde bestimmt. Na2CuGaF7: monokline Raumgruppe C2/c; a = 1232,5(5), b = 731,8(1), c = 1278,0(5) pm, β = 109,29(2)°, Z = 8. Na2CuInF7: orthorhombische Raumgruppe Pmnb; a = 731,8(1) pm, b = 1060,2(2) pm, c = 771,2(1) pm Z = 4. Die Strukturen wurden verfeinert mit 1175 Reflexen bis zu R = 0,043 (wR = 0,035) für Na2CuGaF7 und mit 1917 Reflexen bis zu R = 0,034 (wR = 0,025) für Na2CuInF7. Die Strukturen bestehen aus [CuF5]n3n--Ketten, die im Na2CuInF7 parallel zur a-Achse orientiert sind und in zwei alternierenden Richtungen im Na2CuGaF7. Die Natriumatome besitzen entweder siebenfache oder achtfache Koordination. Obwohl starke antiferromagnetische Wechselwirkungen innerhalb der Ketten beobachtet werden, gibt es keine Hinweise auf eine dreidimensionale Ordnung.
    Notes: The crystal structures of two new copper weberites Na2CuGaF7 and Na2CuInF7 have been determined. Na2CuGaF7 has the monoclinic space group C2/c: a = 1232.5(5) pm, b = 731.8(1) pm, c = 1278.0(5) pm, β = 109.29(2)° and Z = 8. Na2CuInF7 crystallizes in the orthorhombic space group Pmnb: a = 731.8(1) pm, b = 1060.2(2) pm, c = 771.2(1) pm and Z = 4. The structures have been refined from 1175 reflections to R = 0.043 (wR = 0.035) for Na2CuGaF7, and from 1917 reflections to R = 0.034 (wR = 0.025) for Na2CuInF7. The structures consist of [CuF5]n3n- chains which are parallel the a-axis in Na2CuInF7 and oriented in two alternating directions in Na2CuGaF7. Sodium atoms exhibit either seven-fold or eight-fold coordination. Although strong antiferromagnetic interactions are observed inside the chains, there is no evidence for three-dimensional ordering.
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  • 25
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 610 (1992), S. 99-102 
    ISSN: 0044-2313
    Keywords: Aminosilane ; tetrakis(pentafluorophenylamino)silane ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of Tetrakis(pentafluorophenylamino)silaneColourless single-crystals of Tetrakis(pentafluorophenylamino) silane were obtained from the reaction of SiCl4 with monolithiated pentafluoroaniline at low temperatures. The aminosilane has been characterized by various spectroscopic methods and its crystal structure has been determined by x-ray diffraction (for details see “Inhaltsübersicht”). Thermal condensation has not been achieved. However, reaction of silicon(IV)-chloride with pentafluoroaniline in the presence of triethylamine yielded the respective tricyclosilazane.
    Notes: Tetrakis(pentafluorphenylamino)silan wurde erstmals (Umsetzung von Siliciumtetrachlorid mit monolithiiertem Pentafluoranilin) synthetisiert und durch verschiedene spektroskopische Techniken sowie Röntgenstrukturanalyse charakterisiert (I41/a; a = 19,6383(9), c = 6,5551(7) Å; 1842 Diffraktometerdaten; R = 0,054). Versuche zur thermischen Kondensation blieben ohne Erfolg, jedoch führte die Reaktion von Silicium (IV)-chlorid mit Pentafluoranilin in Gegenwart von Triethylamin als Hilfsbase zu dem entsprechenden Tricyclosilazan.
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  • 26
    ISSN: 0044-2313
    Keywords: 2,2′-Bipyridyl molybdenum difluoridedioxide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Crystal Structure of [MoO2F2(2,2′-bipyridyl)]The title compound crystallizes in the space group P21/n with a = 869.6(1), b = 1390.1(3), c = 959.0(1) pm, β = 110.967(5)°, Z = 4; structure determination with 1718 observed independent reflections, R = 0.031. The compound consists of molecules having two cis oxo ligands and a bipyridyl chelate in the MoO2 plane.
    Notes: Die Titelverbindung kristallisiert in der Raumgruppe P21/n mit a = 869,6(1); b = 1390,1(3); c = 959,0(1) pm; β = 110,967(5)°, Z = 4; Strukturbestimmung mit 1718 beobachteten unabhängigen Reflexen, R = 3,1%. Die Verbindung besitzt eine Molekülstruktur mit cis-ständigen Oxoliganden und dem Bipyridylchelat in der MoO2-Ebene.
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  • 27
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 610 (1992), S. 103-111 
    ISSN: 0044-2313
    Keywords: Alkali metal orthoarsenate ; crystal structure ; MAPLE calculations ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Alkalioxoarsenates (V). On Rb2Li[AsO4] and Cs2Li[AsO4]By heating of well-grounded mixtures of the binary oxides (A2O, Li2O2, and As2O3; A : Li : As = 2 : 1 : 1; Ni-tube, 550°C, 21 d; A = Rb, Cs) colourless single crystals of Rb2Li[AsO4] and Cs2Li[AsO4] were obtained for the first time. These new orthoarsenates(V) crystalize orthorhombic (space group C mc21—C2v12, No. 36) with Z = 4. As expected they are isotypic with the according orthovanadates(V) [2] A2Li[VO4], A = Rb, Cs. The lattice constants of Rb2Li[AsO4]: a = 582.1(4) pm, b = 1171.1(7) pm, c = 792.4(5) pm and Cs2Li[AsO4]: a = 596.4(2) pm, b = 1223.4(2) pm, c = 819.7(3) pm were taken from Guinier-Simon powder data. The structure was determined by four-circle-diffractometer data [Siemens AED II, MoKα, 6290 I0 (hkl), R = 3.5%, Rw = 3.2% to Rb2Li[AsO4]; 3518 I0 (hkl), R = 2.8%, Rw = 2.6% to Cs2Li[AsO4]; parameters see text]. The Madelung Part of Lattice Energy, MAPLE, and Effective Coordination Numbers, ECoN, these calculated via Mean Fictive Ionic Radii, MEFIR, as well as charge distribution CHARDI are calculated and discussed.
    Notes: Durch Tempern inniger Gemenge der binären Oxide (A2O, Li2O2 und As2O3; A : Li : As = 2 : 1 : 1; Ni-Bombe, 550°C, 21 d; A = Rb, Cs) wurden Rb2Li[AsO4] und Cs2Li[AsO4] erstmals in Form von farblosen Einkristallen erhalten. Die neuen Orthoarsenate(V) kristallisieren orthorhombisch (Raumgruppe C mc21—C2v12, Nr.36) mit Z = 4 und sind erwartungsgemäß isotyp zu den entsprechenden Orthovanadaten(V) [2] A2Li[VO4] mit A = Rb, Cs. Die Gitterkonstanten für Rb2Li[AsO4]: a = 582,1(4) pm, b = 1171,1(7) pm, c = 792,4(5) pm und Cs2Li[AsO4]: a = 596,4(2) pm, b = 1223,4(2) pm, c = 819,7(3) pm wurden aus Guinier-Simon-Pulverdaten ermittelt. Die Struktur wurde mittels Vierkreisdiffraktometerdaten [Siemens AED II, MoKα, 6290 I0 (hkl), R = 3,5%, Rw = 3,2% für Rb2Li[AsO4]; 3518 I0 (hkl), R = 2,8%, Rw = 2,6% für Cs2Li[AsO4]; Parameter siehe Text] bestimmt. Der Madelunganteil der Gitterenergie, MAPLE, und Effektive Koordinationszahlen, ECoN, diese über Mittlere Fiktive Ionenradien, MEFIR, sowie die Ladungsverteilung CHARDI werden berechnet und diskutiert.
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  • 28
    ISSN: 0044-2313
    Keywords: Nitrosyl-fluoride complex of rhenium ; synthesis ; IR spectrum ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [Na(15-crown-5)][ReFCl3(NO)(CH3CN)] Synthesis, IR Spectrum, and Crystal StructureThe title compound has been prepared by the reaction of [ReCl3(NO)2(CH3CN)] with the equivalent amount of sodium fluoride in the presence of 15-crown-5 in boiling acetonitrile, forming blue crystals. They were characterized by IR spectroscopy and by an X-ray structure determination. Space group P21/n, Z = 4,2117 observed independent reflections, R = 0.037, wR = 0.029. Lattice dimensions at 20°C: a = 834.0(2), b = 1600.0(3), c = 1670.0(3) pm; β = 104.19(3)°. The compound forms an ion pair via one Na—F contact of 234.4 pm and one Na—Cl contact of 293.4 pm; the nitrosyl ligand ist in trans-position to the F atom of the anion [ReFCl3(NO)(CH3CN)]-.
    Notes: Die Titelverbindung wird aus [ReCl3(NO)2(CH3CN)] mit der äquivalenten Menge Natriumfluorid bei Gegenwart von 15-Krone-5 in siedendem Acetonitril in Form blauer Kristalle hergestellt und durch das IR-Spektrum und eine Kristallstrukturanalyse charakterisiert. Raumgruppe P21/n, Z = 4, 2117 beobachtete unabhängige Reflexe, R = 3,7%, wR = 2,9%. Gitterabmessungen bei 20°C: a = 834,0(2); b = 1600,0(3); c = 1670,0(3) pm; β = 104,19(3)°. Die Verbindung bildet ein Ionenpaar mit einem Na—F-Kontakt von 234,4 pm und einem Na—Cl-Kontakt mit 293,4 pm; der Nitrosylligand befindet sich in trans-Stellung zum Fluorliganden des [ReFCl3(NO)(CH3CN)]--Ions.
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  • 29
    ISSN: 0044-2313
    Keywords: Thiolato ; selenolato ; bromo ; iodo complexes of vanadium(V) ; 1H, 51V NMR ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and NMR Spectroscopic Studies of tert-Butylimino-cyclopentadienylvanadium(V) Compounds tC4H9N=VCpX2 (X=SR, SeC6H5, Br, I)Syntheses of the cyclopentadienylvanadium(V) compounds tC4H9N=VCpX2 (X=SR, SeC6H5, Br, I) tC4H9N=VCp (StC4H9) and tC4H9N=VCp[S—(CH2)3—S] (4) are described starting from tC4H9N=VCpCl2. tC4H9N=VCl3 reacts with BBr3 and BI3 by halogen exchange forming the trihalogenides tC4H9N=VX3 (X=Br, I). All compounds obtained are characterized by 1H and 51V NMR spectroscopy. 4 has been found by X-ray diffraction analysis to be a distorted tetrahedral vanadium complex with a chair conformation of the VS2C3-ring.
    Notes: Die Darstellung der Cyclopentadienyl-vanadium(V)-Verbindungen tC4H9N=VCpX2 (X=SR, SeC6H5, Br, I), tC4H9N=VCp(StC4H9) und tC4H9N=VCp[s—(CH2)3—S] (4) wird beschrieben; als Ausgangsverbindung wird tC4H9N=VCpCI2 eingesetzt. tC4H9N=VCl3 reagiert mit BBr3 und Bl3 unter Halogenaustausch und Bildung der Trihalogenide tC4H9N=VX3 (X=Br, I). Alle dargestellten Verbindungen werden 1H- und 51V-NMR-spektroskopisch charakterisiert. Die Röntgenstrukturanalyse von 4 zeigt das Vanadiumatom in einer verzerrt tetraedrischen Anordnung der Liganden; der VS2C3-Ring liegt in der Sesselkonformation vor.
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  • 30
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 609 (1992), S. 59-62 
    ISSN: 0044-2313
    Keywords: Ruthenium ; oxygen ; chlorine ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: About Ba6Ru2PtO12Cl2Single crystals of Ba6Ru2PtO12Cl12 were prepared by a BaCl2 flux and investigated by X-ray methods (D3d3—P3M1; a = 5,805; c = 15.006 Å; Z = 1). The characteristic face shared M3O12-octahedratriples show an ordered (Ru/Pt/Ru) occupation. Calculation of the Coulomb term of lattice energy support the charge distribution (5+/4+/5+) ions engage three point sites with different coordinations. The connection to other compounds are discussed.
    Notes: Durch Schmelzmittelreaktion mit BaCl2 wurde Ba6Ru2PtO12Cl2 an Einkristallen dargestellt und röntgenographisch untersucht (D3d3-P3m1; a = 5,805; c = 15,006 Å; Z = 1). Die charakteristischen flächenverknüpften M3O12-Oktaedertripel weisen eine geordnete Besetzung mit Ru/Pt/Ru auf. Berechnungen des Coulombanteils zur Gitterenergie unterstützen eine Ladungsverteilung in den M3O12-Baugruppen von (5+/4+/5+). Ba2+ -Ionen besetzen drei Punktalgen mit jeweils unterschiedlicher Koordination. Der Zusammenhang mit anderen Strukturen wird diskutiert.
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  • 31
    ISSN: 0044-2313
    Keywords: Thallium tetrafluoromanganate(III), TlMnF4 ; crystal structure ; magnetic structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Kristall- und magnetische Struktur von TlMnF4, einer Verbindung mit SchichtstrukturDie Kristallstruktur und die magnetischen Eigenschaften des Fluoromanganates(III) TlMnF4 wurden untersucht. Die Struktur wurde in der monoklinen Raumgruppe I2/a, Elementarzelle mit a = 539,7(2); b = 544,1(2); c = 1248,4(5) pm, β = 90,19(3)° (Z = 4) auf R/wR 0,057/0,043 verfeinert. TlMnF4 zeigt eine Schichtstruktur, die durch Eckenverknüpfung von MnF6-Oktaedern über ihre vier äquatorialen Ecken gebildet wird. Die Mn—F-Abstände innerhalb des Oktaeders liegen im Bereich von 178 bis 215 pm. Die magnetische Austauschenergie (J/K) innerhalb der Schicht wurde durch Anpassung der experimentellen Suszeptibilitätsdaten im Temperaturbereich von 10-300 K auf der Basis des Heisenbergmodells für quadratische Schichten zu -0,45 K bestimmt. Dreidimensionale antiferromagnetische Ordnung tritt bei 4,2(5) K ein. Die magnetische Zelle entspricht der kristallographischen, jedoch mit primitivem Translationsgitter. Die magnetische Struktur wurde auf R = 0,058 in der magnetischen Raumgruppen P2′/a′ verfeinert. Die magnetischen Momente an MnIII sind colinear zur b-Achse und zeigen antiparallele Ordnung innerhalb der Schichten.
    Notes: The crystal structure and the magnetic properties of the fluoromanganate(III) TlMnF4 have been investigated. The structure has been refined down to R/wR of 0.057/0.043 in the monoclinic I2/a space group with the unit cell constants a = 539.7(2) pm; b = 544.1(2) pm; c = 1248.4(5) pm; β = 90.19(3)° (Z = 4). TlMnF4 is characterized by a layer structure formed of MnF6 octahedra sharing their four equatorial corners. Within each octahedron the Mn—F distances range from 178 pm to 215 pm. The intralayer magnetic interaction (J/K) has been evaluated to be approximately -0.45 K by fitting the experimental susceptibility in the 10-300 K range using the quadratic layer Heisenberg model. A 3 D-antiferromagnetic ordering occurs at Tn = 4.2(5) K. The magnetic cell corresponding to the nuclear one but with a primitive symmetry. The magnetic structure has been refined down to R = 0.0528 in the P2′/a′ magnetic group. The MnIII moments are colinear to the b-axis and show antiparallel ordering within the layers.
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  • 32
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 612 (1992), S. 21-24 
    ISSN: 0044-2313
    Keywords: Barium ; manganese ; neodymium ; oxygen ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On a New Oxometallate of Manganese (II): Ba5Mn4Nd8O21Single crystals of Ba5Mn4Nd8O21 were prepared for the first time by CO2-Laser technique using H2-atmosphere. It was investigated by a single crystal X-ray diffractometer study. Ba5Mn4Nd8O21 crystallizes with tetragonal symmetry space group: C54h—I4/m; a = 14.2104 Å; c = 5.8581 Å; Z = 2. Mn2+ is found in square pyramids of oxygen.
    Notes: Ba5Mn4Nd8O21 wurde erstmals mit CO2-Lasertechnik in H2-Atmosphäre dargestellt und an Einkristallen röntgenographisch untersucht. Es kristallisiert tetragonal in der Raumgruppe C54h—I4/m; a = 14,2104 Å; c = 5,8581 Å; Z = 2. Mn2+ liegt in tetragonal pyramidaler Sauerstoffkoordination vor.
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  • 33
    ISSN: 0044-2313
    Keywords: Iodocuprates(I) ; solvated cations ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structure Investigations of Iodocuprates(I). XV Iodocuprate(I) with Solvated Cations: [Li(CH3CN)4]1∞[Cu2I3] and [Mg{(CH3)2CO}6][Cu2I4][Li(CH3CN)4]1∞[Cu2I3] 1 and [Mg((CH3)2CO)6][Cu2I4] 2 were prepared by reactions of CuI with LiI in acetonitrile and of CuI with MgI2 in acetone. 1 crystallizes orthorhombic, Pnma, a = 552.7(2), b = 1258.8(8), c = 2516(1) pm, z = 4. [Li(CH3CN)4]+ cations are located between rod packings of CuI4 tetrahedra double chains 1∞ [(CuI2/2I2/4)2]- parallel to the axis. Short intermolecular anion/cation contacts were observed. The crystal structure of 2 (monoclinic, P21/n, a = 1840(2), b = 1059.2(2), c = 1879(2)pm, β = 112.94(4)°, z = 4) is built up by [Mg((CH3)2CO)6]2+ cations forming a simple hexagonal sphere packing. The binuclear anions [Cu2I4]2- occupy holes in the trigonal prismatic channels formed by the cations.
    Notes: [Li(CH3CN)4]1∞[Cu2I3] 1 und [Mg((CH3)2CO)6][Cu2I4] 2 wurden durch Umsetzung von CuI mit LiI in Acetonitril bzw. von CuI mit MgI2 in Aceton dargestellt. 1 kristallisiert orthorhombisch, Pnma, a = 552,7(2), b = 1258,8(8), c = 2516(1) pm, z = 4. Zwischen Stabpackungen von CuI4-Tetraederdoppelketten 1∞[(CuI2/2I2/4)2]- parallel zur a-Achse sind [Li(CH3CN)4]+ -Kationen unter Ausbildung kurzer, intermolekularer Anionen-Kationen-Kontakte eingelagert. In der Kristallstruktur von 2 (monoklin, P21/n, a = 1840(2), b = 1059,2(2), c = 1879(2) pm, β = 112,94(4)°, z = 4) sind [Mg((CH3)2CO)6]2+ -Kationen in der Art einer hexagonal einfachen Kugelpackung angeordnet. In die dabei gebildeten, trigonal prismatischen Kanäle sind die zweikernigen Anionen [Cu2I4]2- eingebaut.
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  • 34
    ISSN: 0044-2313
    Keywords: (Trifluoroethyl)aminosilane ; silane tetramin; alkylsilazalane ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preliminary Stages of Polymeric Silazanes with Fluoroalkyl Side Chains and their Condensation BehaviourTetrakis(2,2,2-trifluoroethyl)aminosilane has been synthesized by aminolysis of silicon tetrachloride with 2,2,2-trifluorethylamine. The characterisation of the silane tetramine was carried out spectroscopically and by X-ray-methods. The thermal condensation has been investigated between 60°C and 300°C. At 300°C the formation of oligospirocycloorganoazanes was observed which have been identified spectroscopically. The new silane tetramine reacts with trimethylalumina in toluene. The product has been characterized by crystal structure analysis to be a dimeric (C18H26N8F24Si2Al2). (P1; a = 920.39(9), b = 943.32(2), c = 1235.4(1) pm, α = 68.8(7)°, β = 86.9(4)°, γ = 62.6(4)°, Z = 1, 3923 independent reflections; R = 0.059, Rw = 0.054)
    Notes: Tetrakis[(2,2,2-trifluorethyl)amino]-silan wurde durch Aminolyse von Siliciumtetrachlorid mit 2,2,2-Trifluorethylamin dargestellt, spektroskopisch und röntgenographisch charakterisiert, sowie das thermische Kondensationsverhalten im Bereich von 60 - 300°C untersucht. Bei 300°C konnte die Bildung von Oligospirocyclo-silaorganoazanen massenspektrometrisch nachgewiesen werden. Das neu erhaltene Silantetramin wurde bei 80°C mit Trimethylaluminium im Verhältnis 1 : 1 in Toluol umgesetzt. Nach der Kristallstrukturanalyse liegt das erhaltene Alkylsilazalan im Kristall als Dimeres C18H26N8F24Si2Al2 vor. (P1; a = 920,39(9), b = 943,32(2), c = 1235,4(1) pm, α = 68,8(7)°, β = 86,9(4)°, γ = 62,6(4)°; Z = 1, 3923 unabhängige Reflexe, R = 0,059, Rw = 0,054)
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  • 35
    ISSN: 0044-2313
    Keywords: Potassium cyclodecaphosphate tetrahydrate ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Darstellung und Kristallstruktur von Kaliumcyclodecaphosphat-tetrahydrat: K10P10O30 · 4H2ODie Herstellung und Kristallstruktur von K10P10O30 · 4H2O, das zweite Beispiel eines Phosphates mit einem 20gliedrigen Ringanion, wird beschrieben. Es kristallisiert monoklin in der Raumgruppe C2/c, Gitterkonstanten: a = 15,342(5), b = 11,846(5), c = 19,264(5) Å Σ β = 91,27(3)°. Die Elementarzelle enthält 4 Formeleinheiten.Die Kristallstruktur wurde unter Verwendung von 4379 unabhängigen Reflexen gelöst, der R-Wert beträgt 0,034.Die P10O30-Ringanionen sind in Schichten annähernd parallel zur (101) Ebene angeordnet. Die Verknüpfung der Schichten erfolgt über KO8 und KO7 Polyeder sowie Wasserstoffbrückenbindungen. Das P10O30-Ringanion hat zweizählige Eigensymmetrie verursacht durch eine zweizählige Achse, die durch zwei gegenüberliegende Brückensauerstoffatome des Ringes führt.
    Notes: Chemical preparation and crystal structure of K10P10O30 · 4H2O are described. This compound, the second example of a cyclophosphate with a twenty membered ring, is monoclinic C2/c, with Z = 4, and the following unit-cell dimensions: a = 15.342(5), b = 11.846(5), c = 19.264(5) Å, β = 91.27(3)·.The crystal structure was solved by using 4379 unique reflections the final R value being 0.034.The P10O30 ring anions spread in layers approximately parallel to the (101) planes. These layers are interconnected by the various KO8 and KO7 polyhedra and by the hydrogen bonds. The P10O30 ring anion has a twofold internal symmetry induced by a twofold axis passing through two opposite bonding oxygen atoms of the ring.
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  • 36
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 612 (1992), S. 113-117 
    ISSN: 0044-2313
    Keywords: Silver bismuthate ; mixed valent bismuth ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Ag25Bi3O18, a Mixed Valent BismuthateApplying oxygen pressures of 10 MPa black crystals of Ag25Bi3O18 are prepared for the first time by solid state reaction of Ag2O and ‘Bi2O5’. The crystal structure determination (P3, a = 11.5887(2), c = 6,2386(1) å, Z = 1, 1369 diffractometer data, Rw = 0.034) proves the presence of trivalent (d(Bi-O) = 2.21, and 2.51 å (3×)) and pentavalent bismuth (d(Bi-O) = 2.13 å (6×)). The structure allows a change in the oxidation states (Bi3+ → Bi5+) by pressure induced shift of the oxygen atoms leading to a delocalisation of the 6s2 valence electrons. First evidence for this phenomenon is given by the pressure dependence of the NIR reflectivity. The thermal decomposition was recorded by DTA/TG and measurements of the resistivity were performed.
    Notes: Schwarze Einkristalle von Ag25Bi3O18 wurden neu dargestellt (Festkörperreaktion zwischen Ag2O und „Bi2O5“ bei 350°C unter einem Sauerstoffdruck von 10 MPa). Nach dem Ergebnis der Röntgenstrukturanalyse (P3, a = 11,5887(2), c = 6,2386(1) å, Z = 1,1369 Diffraktometerdaten, Rw = (0,034) liegt zweifelsfrei dreiwertiges Bismut (d(Bi-O) = 2,21 und 2,51 å, je 3×) neben fünfwertigem (d(Bi-O) = 2,13 å (6×)) je 3×) neben fünfwertigem (d(Bi-O) = 2,13 å (6×)) vor. Strukturchemisch ist ein displaziver, druckinduzierter Valenzwechsel unter Delokalisierung von Valenzelektronen möglich, für den durch charakteristische druckabhängige NIR Reflexionen ein erster experimenteller Beleg gegeben ist. Das Abbauverhalten wurde mittels DTA/TG untersucht, ferner wurden Leitfähigkeitsmessungen durchgeführt.
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  • 37
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 612 (1992), S. 118-122 
    ISSN: 0044-2313
    Keywords: Bismuth subhalide ; bismuth cluster ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Kristallstruktur von Bi14I4. Kondensierte Bismut-ClusterDie Kristallstruktur von Bi14I4  -  des Endgliedes der bekannten Bismuthalogenide  -  wurde mit röntgenographischen Methoden bestimmt (Einkristall, P21/m, Z = 1, a = 13,309(3) å, b = 11,447 (3) å, c = 4,342 (1) å, γ = 92,08 (3)°, R/Rw = 0,060/0,060 für 369 Reflexe, sinθ/λ ≤ 0,593, MoKα). Die Struktur besteht aus kondensierten Bismut-Clustern und ist aus unendlichen, eindimensionalen Bismut-Netzen aufgebaut, die sich entlang der c-Achse erstrecken und an den Enden Iodatome tragen.Die Besonderheiten der Bismutsubhalogenide, die auch kondensierte Cluster enthalten, werden in bezug auf Bindungslängen und Bindungswinkel besprochen. Die Einwirkung des einsamen Elektronenpaares des Bismutatoms auf die Gestalt der Koordinationspolyeder wird ebenso diskutiert wie der Zusammenhang zwischen der Koordination und der Oxidationsstufe der Bi-Atome.
    Notes: The crystal structure of Bi14I4  -  the final known member of binary bismuth halides  -  was determined by the single crystal X-ray diffractometer technique (P21/m, Z = 1, a = 13.309(3) Å, b = 11.447 (3) å, c = 4.342(1) å, γ = 92.08(3)°, R/Rw = 0.060/0.060 for 369 reflections, sinθ/λ≤ 0.593, MoKγ). The structure consists of condensed bismuth clusters and is build up from infinite one-dimensional bismuth nets running along the c-axis and limited by iodine atoms in another direction.The common structural features of bismuth subhalides containing condensed clusters are also considered based on the analysis of interatomic distances and bond angles. The influence of the lone pair of electrons of the bismuth atom on the geometry of bismuth coordination polyhedra, and the connection between bismuth atoms coordination and the formal oxidation state of these atoms is discussed.
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  • 38
    ISSN: 0044-2313
    Keywords: Caesium tetraoxoplumbate ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Correction of the Crystal Structure of “Cs4PbO3” and the Structural Relationship between the Modifications of Cs4PbO4The compound that has been described as Cs4PbO3 really is Cs4PbO4. It does not crystallize in the space group P21, as assumed, but in P21/c. The observed fictitiuous violation of the extinction law for the c glide plane is due to twinning. The structure was refined using the original data as well as new data from an untwinned crystal. The denomination β-Cs4PbO4 is used to distinguish this structure from another known modification (α-Cs4PbO4). Both structures, α-Cs4PbO4 and β-Cs4PbO4, can be derived from the sphere packing of γ-plutonium when certain voids in its packing are occupied with oxygen atoms.
    Notes: Bei der früher als Cs4PbO3 beschriebenen Substanz handelt es sich tatsächlich um Cs4PbO4. Dieses kristallisiert nicht, wie angenommen, in der Raumgruppe P21, sondern in P21/c. Die beobachtete scheinbare Verletzung des Auslöschungsgesetzes für die c-Gleitspiegelebene ist auf Verzwillingung zurückzuführen. Die Struktur wurde sowohl mit den ursprünglichen Daten wie auch mit neuen Daten eines unverzwillingten Kristalls verfeinert. Die Bezeichnung β-Cs4PbO4 dient zur Unterscheidung von einer bereits bekannten Modifikation (α-Cs4PbO4). Beide Strukturen, α-Cs4PbO4 und β-Cs4PbO4, lassen sich von der des γ-Plutoniums ableiten, wenn bei dieser bestimmte Lücken mit Sauerstoffatomen besetzt werden.
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  • 39
    ISSN: 0044-2313
    Keywords: Lanthanoide bromoaluminates ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Crystal Structure of LnAl3Br12 (Ln = La, Ce, Pr, Nd, Sm, Gd) and Thermal Decomposition to LnBr3LnAl3Br12 (Ln = La, Ce, Pr, Nd, Sm, Gd) was prepared in crystalline form for the first time. The crystal structures of LaAl3Br12, PrAl3Br12, and NdAl3Br12 were determined on single crystals by X-ray methods. The isotypic compounds crystallize with trigonal symmetry, space group P 3112, Z = 3. A structural comparison to lanthanoide chloroaluminates of equal composition is given and thermal decomposition of LnAl3Br12 (Ln = Nd) to the corresponding lanthanoide tribromide is described.
    Notes: Die Bromide LnAl3Br12 (Ln = La, Ce, Pr, Nd, Sm, Gd) wurden erstmals in kristalliner Form dargestellt und die Kristallstrukturen von LaAl3Br12, PrAl3Br12 anhand von röntgenographischen Einkristalluntersuchungen bestimmt. Alle kristallisieren in der trigonalen Raumgruppe P 3112, Z = 3. Ein struktureller Vergleich mit Lanthanoidchloroaluminaten der gleichen Zusammensetzung und der thermische Abbau von LnAl3Br12 (Ln = Nd) zum entsprechenden Lanthanoidtribromid werden beschrieben.
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  • 40
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 613 (1992), S. 60-62 
    ISSN: 0044-2313
    Keywords: Copper ; tantalum ; niobium ; oxygen ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Crystal Structure of Cu3NbTaO8Single crystals of Cu3NbTaO8 were prepared by solid state reaction. X-ray investigations led to triclinic symmetry, space group C1i—P1 with a = 5.179; b = 5.474; c = 6.003 Å; α = 72.85°; β = 83.39°; γ = 65.77°; Z = 1. Nb5+ and Ta5+ occupy one point position statistically. Both ions show an octahedral oxygen surrounding. Cu(1) is inside an elongated CuO6 octahedra and Cu(2) is coordinated by 5 O2- forming a distorted square pyramid. The polyhedra connection is shown and discussed.
    Notes: Einkristalle von Cu3NbTaO8 wurden durch Feststoffreaktion dargestellt. Die röntgenographische Untersuchung führte zu trikliner Symmetrie, Raumgruppe C1i  -  P1 mit a = 5,179; b = 5,474; c = 6,003 Å; α = 72,85°; β = 83,39°; γ = 65,77°; Z = 1. Nb5+ und Ta5+ besetzen eine Punktlage statistisch. Beide Ionen sind oktaedrisch von O2- koordiniert. Cu(1) zeigt ein stark gestrecktes CuO6-Oktaeder, während Cu(2) tetragonal pyramidal koordiniert ist. Die Polyederverknüpfung wird gezeigt und diskutiert.
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  • 41
    ISSN: 0044-2313
    Keywords: Nickel complex, Ni(BPSH)2 · H2O ; bis(benzoylpyridin-p-toluensulfonylhydrazido)nickel ; heterocyclic sulfonamido chelates ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Bis(benzoylpyridin-toluensulfonylhydrazido)nickel Ni(BPSH)2 · H2O  -  Relations between Structure, Redox, and Extraction Properties of Heterocyclic Sulfonamido ChelatesThe crystal structure of Ni(BPSH)2 · H2O was determined by x-ray diffraction: monoclinic, space group P21/c (Nr. 14); a = 15.077(4) Å, b = 14.901(3) Å, c = 16.335(3) Å, β = 95.74(1)°. R = 0.047 for a total of 5564 observed reflexions. Ni(BPSH)2 · H2O has a distorted tetrahedral structure with two six-membered chelate rings, one of them with a boat from. The electron system of the building blocks CNN⊖ within the chelate rings approaches that of a diazallyl group. The result is a high electron density on the sp2-hybridized donor atom N⊖ and, as a consequence, a short Ni—N⊖-distance (1.908 or 1.924 Å). The electronic properties of N⊖ also explain the high NH-acidity of the acid H(BPSH) (pks = 9,51 in 75 per cent dioxane) and the ligand field strength of BPSH⊖ which is low compared to that of other bidentate sulfonamido ligands and which is reflected in the paramagnetism of Ni(BPSH)2 · H2O.The redox behavior of metal chelates of the type, which is represented by Ni(BPSH)2 · H2O, is caused by a building block of the ligand which is also present in bipyridyl or in the 1,4-diaza-1,3-dienes. The central atoms M11 have only the function of interference factors.
    Notes: Die Kristallstruktur von Ni(BPSH)2 · H2O wurde durch Röntgenbeugung bestimmt: monoklin, Raumgruppe P21/c (Nr. 14), a = 15,077(4) Å, b = 14,901(3) Å, c = 16,335(3) Å, β = 95,74(1) ° R = 0,047 für 5564 beobachtete Reflexe. Ni(BPSH)2 ° H2O besitzt eine verzerrt tetraedrische Struktur mit zwei Chelatsechsringen, von denen einer in der Wannenform vorliegt. Die Baugruppen CNN⊖ innerhalb der Ringe weisen ein Elektronensystem auf, das sich an das einer Diazallylfunktion annähert. Die Folge davon ist eine hohe Elektronendichte auf dem sp2-hybridisierten Stickstoffhaftatom N⊖ und ein kurzer Ni—N⊖-Abstand (1,908 bzw. 1,924 Å). Die elektronischen Eigenschaften von N⊖ erklären weiterhin die hohe NH-Acidität der Säure H(BPSH) pks = 9,51 in 75% (Dioxan) und die verglichen mit anderen Sulfonamidochelatliganden geringe Ligandenfeldstärke von BPSH⊖, die sich im Paramagnetismus von Ni(BPSH)2 · H2O äußert.Das Redoxverhalten der Metallchelate des durch Ni(BPSH)2 · H2O repräsentierten Typs wird durch ein Bauelement des Liganden bestimmt, das sich im α, α′-Dipyridyl und in den 1,4-Diaza-1,3-dienen wiederfindet. Metallionen M2+ wirken über das Diazalylsystem lediglich als Störfaktoren.
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  • 42
    ISSN: 0044-2313
    Keywords: Rhenium tetrachloride chelate complexes ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Chelate Complexes of Rhenium Tetrachloride. The Crystal Structures of ReCl4(DME) and ReCl4(DPPE) · TolanBright green crystals of ReCl4(DME) have been prepared by the reaction of rhenium pentachloride with dimethoxyethane (DME) in dichloromethane. ReCl4(DPPE) · tolan was obtained in form of red crystals by the reaction of the alkyne complex [ReCl4(Ph—C≡C—Ph)(POCl3)] with bis(diphenylphosphino)ethane (DPPE) in dichloromethane. The complexes were characterized by X-ray structure determinations.ReCl4(DME): Space group I42d, Z = 8, 829 observed unique reflexions, R = 0.022. Lattice dimensions at 19.5°C: a = b = 960.60(6), c = 2337.2(6) pm. The complex forms monomeric molecules with DME as chelating ligand; the Re—O bond lengths are 213.1 pm. The chlorine atoms, arranged in trans position to the chelating ligand, have slightly shorter Re—Cl bonds than the chlorine atoms in cis position (232,1 pm).ReCl4(DPPE) · tolan: Space group P21/n, Z = 4,4313 observed unique reflexions, R = 0.040. Lattice dimensions at -80°C: a = 1095.7(1), b = 1764.2(2), c = 1898.0(2) pm, β = 99.229(8)°. The compound consists in form of monomeric molecules [ReCl4(DPPE)] and diphenylacetylene molecules, which are incorporated in the lattice. The two phenyl rings of the tolan molecules are twisted towards each other along the C—C axis with a dihedral angle of 21°. The DPPE molecules are bonded to the rhenium atom in a chelating fashion with medium Re—P lengths of 250.4 pm. The chlorine atoms, arranged in trans position to this ligand, with Re—Cl bond lengths of 234.5 pm are slightly longer than the Re—Cl bonds in cis position with 232.3 pm.
    Notes: ReCl4(DME) wird in Form leuchtend grüner Kristalle durch Reaktion von Rheniumpentachlorid mit Dimethoxyethan (DME) in Dichlormethan hergestellt. ReCl4(DPPE) · Tolan erhielten wir als rote Kristalle bei der Reaktion des Alkinkomplexes [ReCl4(Ph—C≡C—Ph)(POCl3)] mit Bis(diphenylphosphino)ethan (DPPE) in Dichlormethan. Die Komplexe wurden durch röntgenographische Strukturanalysen charakterisiert.ReCl4(DME): Raumgruppe I42d, Z = 8, 829 beobachtete unabhängige Reflexe, R = 2,2%. Gitterkonstanten bei 19,5°C: a = b = 960,60(6); c = 2337,2(6) pm. Der Komplex bildet monomere Moleküle mit dem DME-Liganden als Chelat und Re—O-Abständen von 213,1 pm. Die hierzu trans-ständig angeordneten Chloratome haben mit 228,1 pm etwas kürzere Re—Cl-Bindungen als die cis-ständigen Cl-Atome (232,1 pm).ReCl4(DPPE) · Tolan: Raumgruppe P21/n, Z = 4, 4313 beobachtete, unabhängige Reflexe, R = 4,0%. Gitterkonstanten bei -80°C: a = 1095,7(1); b = 1764,2(2); c = 1898,0(2) pm, β = 99,229(8)°. Der Komplex bildet monomere Moleküle [ReCl4(DPPE)] und in das Gitter eingelagerte Diphenylacetylenmoleküle, deren Phenylringe einen Diederwinkel von 21° zueinander bilden. Die DPPE-Moleküle sind chelatartig am Rheniumatom gebunden mit Abständen Re—P von im Mittel 250,4 pm. Die hierzu trans-ständig angeordneten Chloratome sind mit Re—Cl—Abständen von 234,5 pm etwas länger als die cis-ständigen Re—Cl-Bindungen mit 232,3 pm.
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  • 43
    ISSN: 0044-2313
    Keywords: Tin(IV) alkoxides ; partially hydrolized tin(IV) alkoxide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Investigations into Tin(IV) Alkoxides. II. Isolation and Characterization of the Compound Sn3O(OiBu)1010 · 2i-BuOH. The First Example of a Partially Hydrolized Tin(IV) AlkoxideThe partial hydrolysis product Sn3O(OiBu)10 · 2i-BuOH was obtained by slow hydrolysis of the reaction product of tin tetrachloride with sodium isobutoxide. The compound forms colourless, moisture sensitive crystals, which easily release the coordinated solvent molecules in dry air. Its crystal and molecular structure has been determinated by single crystal X-ray diffraction. The compound crystallizes in the triclinic space group P1 with a = 1363.5(7), b = 1462.7(10), c = 1637.7(7) pm, α = 95.40(5)°, β = 96.79(4)°, γ = 102.12(5)° and Z = 2. The crystal structure consists of discrete, trimeric molecules with octahedrally coordinated tin atoms which are connected to each other corresponding to the formulation Sn3(μ3-O)(μ2-OiBu)3(O1Bu)7 · (i-BuOH)2 by three isobutoxide groups bridging two metal atoms and a single threefold bridging oxygen atom
    Notes: Das partielle Hydrolyseprodukt Sn3O(OiBu)10 · 2i-BuOH des Zinn(IV)-isobutanolats wurde bei der schonenden Hydrolyse des Reaktionsproduktes von Zinntetrachlorid mit Natriumisobutanolat erhalten. Die Verbindung bildet farblose, feuchtigkeitsempfindliche Kristalle, die in trockener Luft unter Abspaltung der Lösungsmittelmoleküle rasch verwittern. Die Kristall- und Molekülstruktur wurde durch Röntgenstrahlbeugung an einem Einkristall bestimmt. Die Verbindung kristallisiert in der triklinen Raumgruppe P1 mit den Gitterkonstanten a = 1363,5(7), b = 1462,7(10), c = 1637,7(7) pm, α = 95,40(5)°, β = 96,79(4)°, γ = 102,12(5)° und Z = 2. Die Kristallstruktur besteht aus diskreten, trimeren Molekülen, in denen die oktaedrisch koordinierten Zinnatome entsprechend der Formulierung Sn3(μ3-O)(μ2-OiBu)3(OiBu)7(i-BuOH)2 über drei, je zwei Metallatome verbrückende Isobutanolat-Gruppen und ein einzelnes dreifach verbrückendes Sauerstoffatom miteinander verbunden sind.
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  • 44
    ISSN: 0044-2313
    Keywords: Sodium iron chalcogenides, Na6FeS4, Na6FeSe4 ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis, Structure, and Magnetic Properties of the Sodium Iron Chalcogenides Na6FeS4 and Na6FeSe4The compounds Na6FeS4 and Na6FeSe4 have been synthesized by fusion reactions of sodium carbonate with iron and chalcogen in a stream of hydrogen.Structural investigations on single crystals show that both compounds crystallize in an atomic arrangement isotypic with Na6ZnO4 (space group P63mc). The structure is characterized by isolated [FeX4]-tetrahedra.The magnetic susceptibilities show Curie-Weiss behaviour. The deviations at low temperatures are obviously caused by antiferromagnetic interactions.
    Notes: Durch Schmelzreaktionen von Natriumcarbonat mit Eisen und Chalkogen im Wasserstoffstrom gelang die Darstellung von Na6FeS4 und Na6FeSe4.Röntgenstrukturuntersuchungen an Einkristallen ergaben daß die beiden Verbindungen isotyp kristallisieren. Die Atomanordnung entspricht der des Na6ZnO4 (Raumgruppe P63mc). Als charakteristische Baueinheit treten isolierte [FeX4]6--Tetraeder auf.Die Temperaturabhängigkeiten der magnetischen Suszeptibilitäten lassen sich mit einem Curie-Weiss-Verhalten beschreiben. Bei tiefen Temperaturen treten Abweichungen von diesem Verhalten auf, die offensichtlich auf antiferromagnetische Wechselwirkungen zurückzuführen sind.
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  • 45
    ISSN: 0044-2313
    Keywords: Pentagold molybdenum cluster ; trigold cobalt cluster ; [(Ph3PAu)5Mo(CO)4]PF6 ; (Ph3PAu)3Co(CO)3 ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Cluster Synthesis by Photolysis of R3PAuN3. VIII. Synthesis and Crystal Structure of [(Ph3PAu)5Mo(CO)4]PF6 · CH2Cl2 and (Ph3PAu)3Co(CO)3Photolysis of a mixture of Ph2PAuN3 and Mo(CO)6 in THF yields [(Ph3PAu)5Mo(CO)4]+ (1), which can be crystallized from CH2Cl2/diisopropylether as orange 1 · PF6 · CH2Cl2 with the space group P21/c and a = 1681.4(5), b = 2215.6(12), c = 2761.5(9) pm, β = 91.54(3)°, Z = 4. The Au5Mo center of cluster 1 forms a capped trigonal bipyramid with the Mo atom in equatorial position and almost equal Mo—Au distances between 279.9(5) and 284.6(7) pm to all five Au atoms. The Au—Au distances range from 272.2(4) to 301.3(4) pm. The Mo(CO)4 group causes three v(C0) at 1975, 1915 and 1890cm-1. Reaction of Ph3PAuCo(CO)4 with Ph3PAuPF6 affords the known cluster cation [(Ph3PAu)4Co(CO)3]+ in high yield. It can be degraded with C1- to the neutral cluster (Ph3PAu)3Co(CO)3 (2). 2 forms air stable, yellow crystals with the space group P21/n and a = 1359.4(4), b = 2041.0(5), c = 1853.2(6)pm, β = 91.47(1)°, Z = 4. The Au3Co core of 2 has a tetrahedral structure with distances Co—Au between 250.4(1) and 254.0(2) pm and Au—Au between 279.5(1) and 285.1(1) pm. v(C0) are observed at 1963, 1905 and 1891 cm-1. Reaction of 2 with [(Ph3PAu)4Co(CO)3]+ yields the condensed cluster [(Ph3PAu)6AuCo2(CO)6]+.
    Notes: Die Photolyse einer Mischung von Ph3PAuN3 und Mo(CO)6 in THF ergibt den Cluster [(Ph3PAu)5Mo(CO)4]+ (l), der nach Zugabe von PF6- aus CH2Cl2/Diisopropylether als oranges 1 · PF6 · CH2Cl2 mit der Raumgruppe P21/c und a = 1681,4(5), b = 2215,6(12), c = 2761,5(9) pm, β = 91,54(3)°, Z = 4 kristallisiert. Das Au5Mo - Gerüst von 1 bildet eine einfach überkappte trigonale Bipyramide mit dem Mo - Atom in äquatorialer Position und nahezu gleich langen Mo—Au-Abständen von 279,9(5) bis 284,6(7) pm zu allen fünf Au-Atomen. Die Au—Au-Abstände liegen zwischen 272,2(4) und 301,3(4) pm. Die Valenzschwingungen v(Co) der Mo(CO)4-Gruppe werden bei 1975, 1915 und 1890cm-1 beobachtet. Reaktion von Ph3PAuCo(CO)4 mit Ph3PAuPF6 liefert das bereits bekannte Clusterkation [(Ph3PAu)4C(CO)3]+ in hoher Ausbeute. Es kann durch Umsetzung mit Cl- zum Neutralcluster (Ph3PAu)3Co(CO)3 (2) abgebaut werden. 2 bildet luftstabile, gelbe Kristalle rnit der Raumgruppe P21/n und a = 1359,4(4), b = 2041,0(5), c = 1853,2(6)pm, β = 91,47(1)°, Z = 4. Das Au3Co-Gerüst weist eine tetraedrische Struktur mit Abständen Co—Au zwischen 250,4(1) und 254,0(2) pm und Au—Au zwischen 279,5(1) pm und 285,1(1) pm auf. v(CO) treten bei 1963, 1905 und 1891 cm-1 auf. Reaktion von 2 mit [(Ph3PAu)4Co(CO)3]+ führt unter Clusterkondensation zu [(Ph3PAu)6AuCo2(CO)6]+.
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  • 46
    ISSN: 0044-2313
    Keywords: Amalgams ; sodium-rich amalgams ; phase transitions ; crystal structure ; DTA measurements ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Temperature Dependent Phase Transitions of Sodium-rich AmalgamsStarting from thermoanalytical measurements the temperature dependent phase transitions of the microcrystalline, sodium rich amalgams Na8Hg3 (= Na2.67Hg) and Na3Hg are investigated using a fast, position sensitive X-Ray detector in combination with a modified counter Guinier system. Near the melting point (64°C) Na8Hg3 shows two phase transitions.At 54°C α-Na8Hg3 forms a slightly distorted monoclinic defect variant of the cubic Li3Bi-structure (β-Na8Hg3). At 62°C this modification transforms into the corresponding undistorted cubic phase (γ-Na8Hg3). The increase of symmetry results mainly from the fact, that small deviations of the mercury atoms from the positions of an ideal close packing vanish due to strong thermal vibrations.The “literature-melting point” of Na3Hg (33°C) corresponds to a phase transition from α-Na3Hg (hexagonal, modified Na3As type) into β-Na3Hg (monoclinic distorted Li3Bi type, corresponding to β-Na8Hg3). The actual melting point of Na3Hg is 59°C.
    Notes: Ausgehend von thermoanalytischen Messungen werden die temperaturabhängigen Phasenumwandlungen der mikrokristallinen natriumreichen Amalgame Na8Hg3 (Na2.67Hg) und Na3Hg mit einem schnellen, ortsempfindlichen Röntgendetektor in Kombination mit einer modifizierten Zählrohr-Guinierkamera untersucht. Na8H3 zeigt dicht unter dem Schmelzpunkt (64°C) zwei Phasenumwandlungen: Bei 54°C wandelt sich α-Na8Hg3 zunächst in eine monoklin verzerrte Defektvariante (β-Na8Hg3) der kubischen Li3Bi-Struktur um. Daraus entsteht bei 62°C die entsprechende unverzerrte kubische Phase (γ-Na8Hg3). Die Symmetrieerhöhung resultiert aus der Aufhebung geringfügiger Abweichungen der Hg-Atompositionen von einer dichtesten Kugelpackung infolge starker thermischer Schwingung.Der „Literaturschmelzpunkt“ von Na3Hg (33°C) entspricht einer Phasenumwandlung von α-Na3Hg (hexagonal, modifizierte Na3As-Struktur) in β-Na3Hg (monoklin verzerrter Li3Bi-Typ, entsprechend β-Na8Hg3). Der Schmelzpunkt der Verbindung Na3Hg liegt dagegen tatsächlich bei 59°C.
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  • 47
    ISSN: 0044-2313
    Keywords: Ytterbium nitrates ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Molecular and Crystal Structure of Ytterbium(III)-triaqua-trinitrate, Yb(H2O)3(NO3)3Yb(H2O)3(NO3)3 crystallizes from a concentrated solution of Yb2O3 in nitric acid in a vacuum desiccator at ambient temperature as colourless single crystals. The crystal structure was determined from single crystal four-circle diffractometer data (R3, Z = 6, a = 1175.5(1), c = 1117.7(2) pm, Vm = 134.25 cm3/mol, R = 3.0%, Rw = 2.9%). The structure may be viewed at as a heavily compressed packing of [Yb(H2O)3(NO3)3] molecules. Yb3+ is coordinated by three bidentate nitrate ligands and three water molecules so that a tricapped trigonal prism (C.N. 9) of oxygen atoms results as the coordination polyhedron.
    Notes: Yb(H2O)3(NO3)3 kristallisiert aus einer konzentrierten Lösung von Yb2O3 in Salpetersäure im Vakuumexsikkator bei Raumtemperatur in Form farbloser Einkristalle aus. Die Kristallstruktur wurde aus Einkristall-Vierkreis-Diffraktometer-Daten bestimmt (R3, Z = 6, a = 1175,5(1), c = 1117,7(2) pm, Vm = 134,25 cm3/mol, R = 3,0%, Rw = 2,9%). Sie kann als stark gestauchte Kugelpackung von [Yb(H2O)3(NO3)3]- Molekülen aufgefaßt werden. In diesen ist Yb3+ von drei zweizähnigen Nitratliganden und drei Wassermolekülen in Form eines dreifach bekappten trigonalen Prismas (C. N. 9) von Sauerstoffatomen umgeben.
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  • 48
    ISSN: 0044-2313
    Keywords: Alkaline earth lanthanoide iron (cobalt) oxide ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of Ba4.5Ca1.5La2Fe4O15, Ba5CaEu2Fe4O15 and Ba5CaNd2Co4O15The compounds (I) Ba4.5Ca1.5La2Fe4O15, (II) Ba5CaEu2Fe4O15 and (III) Ba5CaNd2Co4O15 were prepared and investigated by single crystal X-Ray technique. They belong to the Ba6Nd2Al4O15 typ, space group C6v4—P63mc, (I): a = 11.677, c = 6.959 Å; (II): a = 11.570, c = 6.892 Å; (III): a = 11.604, c = 6.839 Å, Z = 2. The crystal chemistry of these substances will be discussed.
    Notes: Die Verbindungen (I) Ba4,5Ca1,5La2Fe4O15, (II) Ba5CaEu2Fe4O15 und (III) Ba5CaNd2Co4O15 wurden einkristallin dargestellt und röntgenographisch untersucht. Sie kristallisieren im Ba6Nd2Al4O15-Typ, Raumgruppe C6v4—P63mc mit (I): a = 11,677, c = 6,959 Å; (II): a = 11,570, c = 6,892 Å; (III): a = 11,604, c = 6,839 Å, Z = 2. Die Kristallchemie dieser Stoffe wird diskutiert.
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  • 49
    ISSN: 0044-2313
    Keywords: Silicon ; addition compounds ; N-trimethylsilyl-N′-methylimidazolium ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure Determination of N-Trimethylsilyl-N′-Methylimidazolium BromideThe reaction of Trimethylbromosilane and N-Methylimidazole (NMI) led to a 1:1 compound stable at room temperature. The reaction was carried out at room temperature and colorless single crystals were obtained by sublimation. The addition compound crystallizes in the orthorhombic space group Pbnb (No. 56) with lattice constants a = 1218.3(2)pm, b = 1333.6(1)pm, c = 1360.2(2)pm, Z = 8, Dcalc = 1.414 g/cm3. For 1506 independent reflections, measured at 21°C the structure could be refined to R = 0.067 and Rw = 0.062.
    Notes: Die Reaktion von Trimethylbromsilan und N-Methylimidazol (NMI) führt zu einer bei Raumtemperatur stabilen 1:1 Verbindung. Die Umsetzung wurde bei Raumtemperatur durchgeführt und durch Sublimation ließen sich farblose Einkristalle der Verbindung erhalten. Die Additionsverbindung kristallisiert in der orthorhombischen Raumgruppe Pbnb (Nr. 56) mit den Gitterkonstanten a = 1218,3(2) pm, b = 1333,6(1) pm, c = 1360,2(2) pm, Z = 8 und Dcalc = 1,414 g/cm3. Unter Verwendung von 1506 symmetrieunabhängigen Reflexen konnte die Struktur, gemessen bei 21°C, bis auf R = 0,067 und Rw = 0,062 verfeinert werden.
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  • 50
    ISSN: 0044-2313
    Keywords: 3-Diethylamino-5-phenyl-1,2,4-diselenazolium-tetrachloroniccolate(II) ; 1,2,4-diselenazolium salt ; selenaheterocyclic cation ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: 3-Diethylamino-5-phenyl-1,2,4-diselenazolium-tetrachloroniccolate(II)  -  Synthesis and StructureBis-(N′, N′-diethyl-N-benzoylselenoureato)nickel(II) reacts with diphosgene in benzene to 3-diethylamino-5-phenyl-1,2,4-diselenazolium-tetrachloroniccolate(II). Its structure is confirmed by RKSA and ESCA. The compound consists of cations, which are planar fivemembered rings and of tetrahedral tetrachloroniccolate(II) anions. The complex is isomorphic with 3-diethylamino-5-phenyl-1,2,4-dithiazolium-tetrachloroniccolate(II).
    Notes: Bis-(N′, N′-diethyl-N-benzoylselenoureato)nickel(II) reagiert mit Diphosgen in Benzen zu 3-Diethylamino-5-phenyl-1,2,4-diselenazolium-tetrachloroniccolat(II), dessen Röntgenkristallstrukturanalyse und Röntgenphotoelektronenspektrum vorgestellt und interpretiert werden. Die Verbindung besteht aus 1,2,4-Diselenazolium-Kationen, die als planare Fünfringe vorliegen und aus tetraedrischen Tetrachloroniccolat(II)-Anionen. Sie ist zu 3-Diethylamino-5-phenyl-1,2,4-dithiazolium-tetrachloroniccolat(II) isomorph.
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  • 51
    ISSN: 0044-2313
    Keywords: Strontium manganate, Sr7Mn4O15 ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Compound Sr7Mn4O15 and Structure Relations to Sr2MnO4 and α-SrMnO3The “compound” hitherto described as a α modification of Sr2MnO4 is shown to consist of a mixture of SrO and the new monoclinic compound Sr7Mn4O15 crystallizing in the space group P 21/c, a = 681.78(6), b = 962.24(8), c = 1038.0(1) pm, β = 91.886(7)°, Z = 2. Up to 0.3 mm long black crystals were grown from prereacted Sr7Mn4O15, SrO, and SrCl2 at 1350°C in a sealed platinum tube under argon. Its structure is related to α-SrMnO3. It contains layers of cornershared double octahedra [O2/2OMnO3MnO2O1/2]7- parallel to (100). Above 100 K the magnetism of Sr7Mn4O15 follows the Curie Weiss law with Θ ∼ -426 K and a moment μeff = 3.62 μB corresponding Mn4+.
    Notes: Die bisher als α-Modifikation von Sr2MnO4 beschriebene Substanz stellt ein Gemenge aus SrO und Sr7Mn4O15 dar. Bis zu 0,3 mm lange schwarze Einkristalle wurden durch Erhitzen von vorreagiertem Sr7Mn4O15, SrO und SrCl2 in einer unter Argon zugeschmolzenen Platinampulle auf 1350°C erhalten. Die neue Verbindung kristallisiert monoklin in der Raumgruppe P 21/c mit den Gitterkonstanten a = 681,78(6), b = 962,24(8), c = 1038,0(1)pm, β = 91,886(7)° und Z = 2 in einem neuen Strukturtyp, der mit α-SrMnO3 verwandt ist. Charakteristisch für die Struktur von Sr7Mn4O15 sind Schichten eckenverknüpfter Doppeloktaeder[O2/2OMnO3MnO2O1/2]7- parallel zur (100). Oberhalb 100K folgt der Magnetismus von Sr7Mn4O15 dem Curie-Weiss-Gesetz mit Θ ∼ -426K und einem Moment μeff = 3,62μB pro Mn entsprechend Mn4+.
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  • 52
    ISSN: 0044-2313
    Keywords: Bis(7-isopropyl-8-quinolinato)nickel(II) ; crystal structure ; association of nickel 8-quinolates ; steric hindrance ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Chelates of 8-Quinolinol Derivatives. XII. Crystal and Molecular Structure of Bis(7-isopropyl-8-quinolinato)nickel(II)The crystal and molecular structure of bis(7-isopropyl-8-quinolinato)nickel(II) was determined by X-ray diffraction. The structure is monoclinic with the space group P21/n (Z = 2, 1403 observed independent reflections, R = 0.049. Lattice dimensions at 20°C: a = 1328.3(5) pm, b = 632.8(2) pm, c = 1330.0(5) pm, β = 112.99(3)°). The coordination of the nickel atom is planar with the quinoline rings in trans position.
    Notes: Die Kristallstruktur von Bis(7-isopropylchinolin-8-olato)nickel(II) wurde durch eine Röntgenkristallstrukturuntersuchung bestimmt. Es liegt ein monoklines Kristallsystem mit der Raumgruppe P21/n vor (Z = 2, beobachtete unabhängige Reflexe 1403, R = 4,9%, Gitterabmessungen bei 20°C: a = 1328,3(5) pm, b = 632,8(2) pm, c = 1330,0(5) pm, β = 112,99(3)°). Das Nickelatom ist planar koordiniert mit den beiden Chinolinringen in trans-Stellung.
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  • 53
    ISSN: 0044-2313
    Keywords: Zirconocene-phosphido complexes ; (tricyclohexyltriphosphane-1,3-diyl)zirconocene(IV) ; preparation ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of meso-(1,2,3-Tricyclohexyltriphosphane-1,3-diyl)zirconocene(IV), Cp2(Cp = η5-C5H5, Cy = C6H11)Cp2ZrCl2 reacts with Li(THF)2PHCy (Cy = C6H11) to yield the metallacyclic compound Cp2 1., The 31P{1H} NMR spectrum of 1, shows a coupling pattern for an A2X system, indicating the presence of only the meso-forms in solution, which are also present in the solid state. 1, crystallizes in the monoclinic space group P21/n (No. 14) with a = 12.984(8), b = 9.241(7), c = 23.05(1) Å, β = 93.48(4)°, V = 2760.1 Å3 and four formula units in the unit cell (2718 independent observed reflections, R = 7.3%). The central ZrP3 ring in 1, is almost planar. The Zr—P bond lengths of 2.618(4) and 2.628(4) Å are nearly identical.
    Notes: Cp2ZrCl2 setzt sich mit Li(THF)2PHCy (Cy = C6H11) zu der metallacyclischen Verbindung Cp2 1, um. Im 31P{1H}-NMR-Spektrum von 1, tritt das für ein A2X-System zu erwartende Aufspaltungsmuster auf, was auf das Vorliegen der meso-Formen in Lösung hinweist. Auch im Festkörper liegen nur die meso-Formen vor. 1, kristallisiert monoklin in der Raumgruppe P21/n (Nr. 14) mit a = 12,984(8), b = 9,241(7), c = 23,05(1) Å, β = 93,48(4)°, V = 2760,1 Å3 und vier Formeleinheiten pro Elementarzelle (2718 unabhängige beobachtete Reflexe, R = 7,3%). Der zentrale ZrP3-Ring in 1, ist angenähert planar. Die Zr—P-Bindungslängen sind mit 2,618(4) und 2,628(4) Å fast gleich.
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  • 54
    ISSN: 0044-2313
    Keywords: CeIII double decker complex ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Reaction of Macrocycles with Lanthanoids. I. The Crystal Structure of [Li(thf)][(C22H22N4)2Ce] · THFIn THF CeBr3 forms with [(TMTAA)Li2] the paramagnetic doubledecker complex [Li(thf)][(TMTAA)2Ce]. The complex crystallizes with 1 Mol THF per formula unit. The structure was characterized by X-ray single crystal structure analysis (space group C2 (No. 5), z = 6, a = 1741.8(2) pm, b = 1622.1(2) pm, c = 2540.4(3) pm, β = 104.72(1)°). The sandwich-like arrangement of the heterocyclic ligands leads to a quadratic-prismatic coordination of the Ce3+ ion. One macrocyclic ligand is additionally coordinated by a [Li(thf)]+ fragment. The coordination of the Li ion is square pyramidal.
    Notes: CeBr3 reagiert mit [(TMTAA)Li2] in THF zu dem paramagnetischen Doppeldeckerkomplex [Li(thf)][(TMTAA)2Ce], der mit 1 Mol THF pro Formeleinheit kristallisiert. Der Aufbau konnte durch eine Kristallstrukturanalyse aufgeklärt werden (Raumgruppe C2 (Nr. 5), Z = 6, a = 1741,8(2) pm, b = 1622,1(2) pm, c = 2540,4(3) pm, β = 104,72(1)°). Durch die sandwichartige Anordnung der TMTAA-Liganden erhält das Ce3+-Ion eine quadratisch-prismatische Koordination. An einen der makrozyklischen Liganden koordiniert zusätzlich ein [Li(thf)]+-Fragment. Das Li-Ion besitzt tetragonal-pyramidale Umgebung.
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  • 55
    ISSN: 0044-2313
    Keywords: SmIII polynuclear complex ; CoII complex ; synthesis ; crystal structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Reaction of Macrocycles with Lanthanoids. II. The Crystal Structures of [K(thf)3]2[(C22H28N4)2Sm2] · 4 THF and [(C22H22N4)Co] · DMEIn a complicated redox reaction [(TMTAA)K2] and [SmI2(thf)2] form the polynuclear metal complex [K(thf)3]2[(TMTAT)2Sm2]. This complex crystallizes with four molecules THF per formula unit and its structure was determined by single crystal X-ray investigation (spacegroup P21/c (No. 14), z = 4, a = 998.0(2) pm, = b = 2618.3(6) pm, c = 1619.4(3) pm, β = 96.52(2)°). In the dimeric unit [(TMTAT)2Sm2]2- the Sm3+ ions are bonded to the four N atoms of the macrocyclic ligand and one C6H4 ring of the second ligand is attached η6 like to one metal ion. Additionally two [K(thf)3]+ fragments are bonded to this central unit, and therefor coordination number seven results for the K+ ion. [TMTAA]2- is not reduced by [Cp2Co] in a similar reaction. The monomeric paramagnetic complex [(TMTAA)Co] (μeff = 2,76 μB) is formed instead. The structure reveils a square planar coordination of the Co atom by the four N atoms of the TMTAA ligand (spacegroup C2/c (No. 15), z = 4, a = 1945.1(4) pm, b = 1165.6(2) pm, c = 1144.7(2) pm, β = 116.38(1)°).
    Notes: [(TMTAA)K2] und [SmI2(thf)2] reagieren in einer unübersichtlichen Redoxreaktion zu dem mehrkernigen Metallkomplex [K(thf)3]2[(TMTAT)2Sm2]. Der Aufbau dieser mit vier Molekülen THF pro Formeleinheit kristallisierenden Verbindung konnte durch eine Röntgenstrukturanalyse aufgeklärt werden (Raumgruppe P21/c (Nr. 14), Z = 4, a = 998,0(2) pm, b = 2618,3(6) pm, c = 1619,4(3) pm, β = 96,52(2)°). In der dimeren Einheit [(TMTAT)2Sm2]2- sind die Sm3+-Ionen außer an die vier N-Atome eines makrozyklischen Liganden auch η6-artig an einen C6H4-Ring des zweiten Liganden gebunden. Zusätzlich koordinieren an die zentrale Einheit zwei [K(thf)3]+-Fragmente. Dies führt zu einer Koordinationszahl von 7 für das K+-Ion. [TMTAA]2- wird in einer analogen Reaktion mit [Cp2Co] nicht reduziert. Statt dessen bildet sich der monomere paramagnetische Komplex [(TMTAA)Co] (μeff = 2,76 μB). Nach der Kristallstrukturanalyse ist das Co-Atom quadratisch planar von den vier N-Atomen des TMTAA-Liganden koordiniert (Raumgruppe C2/c (Nr. 15), Z = 4, a = 1945,1(4) pm, b = 1165,6(2) pm, c = 1144,7(2) pm, β = 116,38(1)°).
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  • 56
    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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  • 57
    ISSN: 0044-2313
    Keywords: Phosphorane iminato complex of tantalum ; synthesis ; IR spectrum ; crystal structure ; ab initio calculation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Tetrakis(triphenylphosphane-iminato)tantalonium hexachlorotantalate, [Ta(NPPh3)4]TaCl6. Synthesis, IR Spectrum, Crystal Structure, and ab initio Calculations of the [Ta(NPH3)4]+ IonThe title compound has been prepared by the reaction of tantalum pentachloride with Me3SiNPPh3 in acetonitrile, forming colourless moisture sensitive crystals, which were characterized by IR spectroscopy and by an X-ray structure determination (Space group P1, Z = 4, 6479 observed unique reflections, R = 0.053. Lattice dimensions at 20°C: a = 1268.4(3), b = 2361.0(6), c = 2400.0(6) pm, α = 85.81(2)°, β = 87.47(3)°, γ = 87.27(3)°). The compound consists of two symmetry-independent cations [Ta(NPPh3)4]+ and anions TaCl6-, respectively. In the cations the tantalum atoms are surrounded in a distorted tetrahedral fashion by the four nitrogen atoms of the phosphane-iminato ligands. The TaN and PN bond lengths in both individuals correspond well with double bonds. According to twisting phenomena of the phenyl rings the TaNP bond angles are different in the two cation species. The investigation is supplemented by ab initio calculations of the [Ta(NPH3)4]+ ion.
    Notes: Die Titelverbindung entsteht aus Tantalpentachlorid und Me3SiNPPh3 in Acetonitril in Form farbloser, feuchtigkeitsempfindlicher Kristalle, die durch das IR-Spektrum und eine röntgenographische Strukturanalyse charakterisiert werden (Raumgruppe P1, Z = 4, 6479 beobachtete unabhängige Reflexe, R = 5,3%. Gitterkonstanten bei 20°C: a = 1268,4(3); b = 2361,0(6); c = 2400,0(6) pm, α = 85,81(2