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  • Articles  (5,023)
  • Springer  (5,023)
  • 2020-2020
  • 1970-1974  (5,023)
  • 1945-1949
  • 1974  (2,372)
  • 1973  (2,651)
  • Geosciences  (4,723)
  • Nature of Science, Research, Systems of Higher Education, Museum Science  (300)
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  • Articles  (5,023)
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  • 2020-2020
  • 1970-1974  (5,023)
  • 1945-1949
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  • 1
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    Journal of chemical crystallography 3 (1973), S. 3-13 
    ISSN: 1572-8854
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract An X-ray diffraction study of nupharidine hydrobromide has been carried out in order to obtain an unequivocal solution to the question of the N-oxide configuration. Nupharidine hydrobromide (C15H24BrNO2) crystals are orthorhombic, space groupP212121 withz = 4. The unit cell constants at 22 ± 3 ° area = 13·419(2),b = 13·668(4),c = 8·731(2) Å (CuKα1, λ = 1·54051 Å). Three-dimensional intensity data, to the limit 2θ = 145 ° for CuKα1, were measured on a GE XRD-490 automatic diffractometer equipped with Ni-Co balanced filters for monochromatization. The crystal structure was solved by the heavy-atom method and refined by least squares to anR of 0·06 for 1960 reflections. X-ray analysis clearly established that (a) the quinolizidine N-oxide system is built of twocis-fused chairs, (b) the methyl and the furan substituents occupy the equatorial position and (c) the absolute configuration indicated by the chemical methods is in agreement with the X-ray work. The stereochemical aspects of the Polonovski elimination reaction in the conversion of (+) nupharidine to Δ6-dehydrodeoxynupharidine has been studied in the light of these X-ray results.
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  • 2
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    Journal of chemical crystallography 3 (1973), S. 15-23 
    ISSN: 1572-8854
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract β-ethylenediaminetetraacetic acid crystallizes in the monoclinic system:a = 13·273(4),b = 5·575(7),c = 16·110(6) Å, β = 96·26(3),Z = 4,C2/c. The structure has been determined by direct methods with CuKα diffractometer data, and refined by full-matrix least squares toR = 0·057 for 755 observed reflexions. The molecule exists in acis conformation and possesses two-fold symmetry, the diad axis passing through the central C—C bond. The nitrogen atom is protonated, and takes part in a bifurcated intramolecular hydrogen bond. A short (2·46 Å) hydrogen bond links the oxygen atoms of adjacent molecules.
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  • 3
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    Journal of chemical crystallography 3 (1973), S. 25-35 
    ISSN: 1572-8854
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The structure of 3,3′-dibromobenzophenone has been reinvestigated using new three-dimensional data. Crystals of 3,3′-dibromobenzophenone are orthorhombic:a = 4·05,b = 11·74,c = 24·80 Å,Z = 4, space groupPbcn. The structure has been refined by three-dimensional methods, including anisotropic full-matrix least squares, to anR index 0·104. The conformation of isolated molecules of benzophenone,pp′-dimethoxy benzophenone and 3,3′-dibromobenzophenone have been calculated by semi-empirical methods, and the results are compared with those obtained from X-ray crystallographic investigations on these compounds. It has been found that the calculated geometries of isolated molecules of benzophenone and its derivatives are different from those observed in the crystal structures of these compounds.
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  • 4
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    Journal of chemical crystallography 3 (1973), S. 47-54 
    ISSN: 1572-8854
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    Topics: Geosciences , Physics
    Notes: Abstract The crystal and molecular structure of chloro(2,2′,2″-terpyridine)palladium(II)-chloride dihydrate, C15H15Cl2N3O2Pd, has been determined by single crystal X-ray diffraction techniques. The crystals are orthorhombic: space groupPna21,a = 17·217(9),b = 14·026(8),c = 6·801(5) Å,Z = 4. Least-squares refinement of 2064 non-zero manually gathered diffractometer reflexions was carried out to a conventional unweightedR of 0·069. The molecule consists of a basically planar 4-coordinate [Pd(terpy)Cl]+ cation and a Cl− anion. The molecules are packed in a layer structure in which the average separation is about 3·4 Å, the closest approach being 3·13 Å between a palladium atom and one of the nitrogen atoms of a neighboring molecule. Bond distances are within acceptable limits of predicted values. Deviations from planarity in the coordinated terpyridine ligand are presumably due to its steric limitations and are similar to those found in other terpyridine complexes.
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  • 5
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    Journal of chemical crystallography 3 (1973), S. 37-45 
    ISSN: 1572-8854
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Yohimbine (C21H26N2O3) is an important indole alkaloid found in the Indian snake rootrauwolfia serpentina, and is very closely related to reserpine. Yohimbine hydrochloride (C21H27ClN2O3) is orthorhombic:P212121,a = 11·54,b = 24·88,c = 7·00 Å,Z = 4. X-ray diffraction data to a Bragg angle of 80 ° were collected on a G.E. diffractometer using CuKα radiation. The structure was solved by direct methods, and refined to a reliability index of 9·9 % by the block-diagonal least-squares method. Yohimbine has a ring system very similar to that of reserpine, though the conformations of the ringsC andD about the C—N bond are different in the two molecules. The absolute configuration of the molecule, determined by X-ray anomalous scattering, confirms the 3α, 15α, 20β configuration assigned earlier by conformational analysis.
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  • 6
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    Journal of chemical crystallography 3 (1973), S. 65-68 
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  • 7
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    Journal of chemical crystallography 3 (1973), S. 55-64 
    ISSN: 1572-8854
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    Topics: Geosciences , Physics
    Notes: Abstract The crystal structure ofo-chlorobenzylidenemalononitrile, C10H5ClN2, has been determined by X-ray crystallographic analysis. The compound crystallizes in the monoclinic space groupP21/c, with unit cell dimensionsa = 3·971,b = 21·140,c = 10·747 Å, β = 95·29 °;Z = 4. The structure was solved by matching an assumed molecular shape to the near-origin peaks of a sharpened vector map, the detail being established by Fourier syntheses. Refinement by full-matrix least squares converged to an indexR of 0·097 for 1729 reflections from CuKα Weissenberg photographs. The molecular components, the phenyl and malononitrile groups, are individually planar but mutually tilted with a dihedral angle of 12·7 °. The deviation from planarity is related to steric hindrance between the malononitrile group and theortho-hydrogen of the phenyl ring.
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  • 8
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    Journal of chemical crystallography 3 (1973), S. 79-86 
    ISSN: 1572-8854
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract The alkaloid porantherine, C15H23N, has been isolated fromPoranthera corymbosa Brogn. (family Euphorbiaceae). It forms a stable hydrobromide which crystallizes in the orthorhombic space groupP212121, with cell dimensionsa=11·689,b = 15·190 andc = 7·721 Å. Its structure has been solved by the heavy-atom method and refined to anR of 0·063. The molecular skeleton has the form of a tertiary amine, with three fused six-membered rings centred on the nitrogen atom and a two-carbon atom bridge which holds the whole molecule rigid. The absolute configuration has been determined from the differences between Bijvoet pairs of reflexions.
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  • 9
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    Journal of chemical crystallography 3 (1973), S. 71-78 
    ISSN: 1572-8854
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    Topics: Geosciences , Physics
    Notes: Abstract Oxidation of acetone-4-p-bromophenylsemicarbazone with lead tetraacetate yields only one isomer of 5,5-dimethyl-2-p-bromophenylimino-Δ3-1,3,4-oxadiazoline, C10H10BrN3O. Crystals of this compound are triclinic, space groupP¯1,a = 5·91(1),b = 9·52(1),c = 11·59(2) Å, α =114·1(1) °, β = 93·5(1) ° and γ = 108·8(1) °;z = 2 and the chemical composition is C10H10BrN3O. Of 2306 independent reflexions examined, 877 were strong enough to be measured with integrated precession photographs using MoKα radiation. The structure was refined using a full-matrix least-squares program to a finalR value of 0·064. The structure consists of planar phenyl and oxadiazoline rings, with a van der Waals interaction between a phenyl hydrogen atom and oxygen atom of the five member ring preventing the two rings from being co-planar; the H(13)-O(1) separation is 2·47 Å. TheZ-configuration of the product suggests a specific mechanism for the ring closure involving an organolead intermediate.
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  • 10
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    Journal of chemical crystallography 3 (1973), S. 87-93 
    ISSN: 1572-8854
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Crystals of the hydrobromide of the alkaloid designated porantheridine, C15H27NO, isolated from the plantPoranthera corymbosa Brogn. (family Euphorbiacaea), belong to the space groupP212121, with cell dimensionsa= 10·059,b = 16·704 andc = 9·629 Å. The crystal structure was solved by the heavy-atom method and refined with 624 reflexions to a residual of 0·078. The molecule consists of three six-membered rings fused on to a common central nitrogen atom; one ring contains an oxygen atom with ann-propyl group and a methyl group substituted on the vicinal carbon atoms. The rings have thechair conformation, two being fusedtrans to each other andcis to the third. The absolute configuration was determined using the anomalous scattering power of the bromine atom.
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  • 11
    ISSN: 1572-8854
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    Topics: Geosciences , Physics
    Notes: Abstract The crystal structure of dichloro-(N,N,N′,N′-tetramethylethylenediamine)zinc(II), C6H16Cl2N2Zn, has been determined from 1684 reflexions measured on a Siemens four-circle diffractometer (A.E.D.) using the ω/2θ-scan technique and CuKα radiation. The crystals are monoclinic, space groupP21/c,a = 7·716(3),b = 13·335(9),c =11·545(5) Å, β = 105·59(6) ° andZ = 4. The structure was solved by Fourier methods, and refined by full-matrix least squares to a finalR (conventional) of 6·7 %. Anisotropic thermal parameters were evaluated for the non-hydrogen atoms, but the hydrogen atoms were assigned the equivalent isotropic thermal parameters of the carbon atoms to which they were bonded. The geometry around the zinc atom is distorted tetrahedral, with the Zn-Cl and Zn-N average bond lengths of 2·207(4) and 2·08(1) Å respectively.
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  • 12
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    Journal of chemical crystallography 3 (1973), S. 103-114 
    ISSN: 1572-8854
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    Topics: Geosciences , Physics
    Notes: Abstract 10,10′-(5H,5′H)-spirobiphenophosphazinium chloride is one of the few examples of a spirophosphonium salt reported in the literature. This compound crystallized in space groupP21/c witha = 12·293(7),b = 13·279(8),c = 17·56(1) Å, β = 130·43(3) ° andZ = 4. The finalR index was 0·057. The results of the X-ray analysis indicated that this phosphorus heterocycle may indeed possess aromatic character. This contention was supported in solution by a31 P nmr study.
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  • 13
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    Journal of chemical crystallography 3 (1973), S. 115-123 
    ISSN: 1572-8854
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    Topics: Geosciences , Physics
    Notes: Abstract The crystal and molecular structure of 2,5-dimethyl-3,4-diacetylfuran has been determined by direct methods using CuKα. photographic data. Refinement by full-matrix least-squares methods gave a finalR factor of 0·097. The crystals are monoclinic: space groupP21/c,a =14·92(2),b = 4·09(1),c =16·68(3) Å and β = 109·7(5) °;Z = 4. The furan ring of the molecule is planar, and the exocyclic atoms bound to the atoms of the ring lie close to the ring plane. The planes of the acetyl groups are tilted by 16 ° and 47 ° with respect to the ring plane. The exocyclic bond angles of this compound are significantly different from the equivalent angles in furan.
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  • 14
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    Journal of chemical crystallography 3 (1973), S. 127-137 
    ISSN: 1572-8854
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    Topics: Geosciences , Physics
    Notes: Abstract An X-ray crystallographic study of 2,5-dimethyl-3,4-diacetylpyrrole showed that the crystals are monoclinic, space groupP21/n,a = 10·01(3),b = 12·93(3),c = 7·41(2) Å and β = 91·5(5) °. The crystal structure was solved by direct methods and refined by least squares to a finalR factor of 0·13. The values determined for the bond distances and angles of the pyrrole ring are in good agreement with the values reported in the literature. However, there are significant changes in the exocyclic bond angles of the atoms of the ring. The planes of the acetyl groups are tilted with respect to the ring plane, forming dihedral angles of 22 ° and 40 °.
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  • 15
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    Journal of chemical crystallography 3 (1973), S. 139-146 
    ISSN: 1572-8854
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    Topics: Geosciences , Physics
    Notes: Abstract Crystals of the hydrobromide of poranthericine, C15H27NO, an alkaloid isolated from the plantPoranthera corymbosa Brogn. (family Euphorbiaceae) were found to belong to the orthorhombic space groupP212121, with unit cell dimensionsa = 12·761,b = 15·144 andc = 8·030 Å, andZ = 4. The structure was solved by the heavy-atom method and refined with 1276 reflections to a residual of 0·091 The molecule was found to consist of three saturated six-membered rings fused on to a common central nitrogen atom, with methyl, ethyl and hydroxyl groups attached to the periphery. All rings had thechair conformation and were fusedtrans to one another. The absolute configuration was determined using the anomalous scattering power of the bromine atom.
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  • 16
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    Journal of chemical crystallography 3 (1973), S. 147-155 
    ISSN: 1572-8854
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    Notes: Abstract The crystal structure of 4,4′-diaminodiphenylsulphide, C12H12N2S, has been determined by three-dimensional X-ray methods. The crystals are orthorhombic, with space-groupP212121,a = 9·874(6),b = 19·445(9),c = 5·876(6) andZ= 4. The structure was solved by the heavy-atom method and refined by full-matrix least squares to anR value of 0·074. The molecules are held together by hydrogen bonds of the N-H ⋯ N type, and form chains parallel to theb axis.
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  • 17
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    Journal of chemical crystallography 3 (1973), S. 157-169 
    ISSN: 1572-8854
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    Notes: Abstract The crystal structure of bis-tetraphenylarsonium-tris-(cis-1,2-dicyano-1,2-ethylenedithiolato)Fe(IV), [(C6H5)3As]2Fe[S2C2(CN)2]3, has been determined using 3154 independent, non-zero reflexions collected by counter techniques. The substance crystallizes in the monoclinic system: space groupI2/a,a = 20·153(8),b = 13·411(5),c = 21·497(8) Å and β = 95·28(8) °;D m = 1·41(2),D c = 1·43 g cm−3 andZ = 4. The structure consists of Ph4As+ cations in general positions and tris-(cis-1,2-dicyano-1,2-ethylenediothiolato)Fe(IV) anions on two-fold axes. Although the coordination around the arsenic atom is tetrahedral, the overall symmetry of the cation is 1 (C 1), probably because the phenyl rings are rotated to accommodate the requirements of packing. The coordination of the six sulphur atoms about the iron atom is trigonal antiprismatic, approximating closely to an octahedron: for any pair oftrans sulphur atoms, the S-Fe-S angle is about 171 °.
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  • 18
    ISSN: 1572-8854
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    Notes: Abstract Crystals of the title compound, C12H18O8, are orthorhombic:P212121,a = 7·260(5),b = 9·483(6),c = 20·199(6) Å,Z = 4. The structure has been solved from the Patterson synthesis, and refined to anR-factor of 8·4% by full-matrix least-squares methods. The 6-membered rings are each in thechair conformation and arecis-fused at the 4a, 8a ring-junction. The structure led to an explanation of an unusually large chemical shift in the nmr signal from one of the methylenic hydrogen atoms on C(7).
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  • 19
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    Journal of chemical crystallography 3 (1973), S. 181-191 
    ISSN: 1572-8854
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    Notes: Abstract The title compound, Ni(C5H7O2)2· (C2H5OH)2, crystallizes in the triclinic system with unit cell dimensionsa = 8·923,b = 5·283,c = 9·522 Å, α = 81·4, β = 106·1 and γ = 103·3 °;Z= 1, space groupP¯1. The structure was solved by Fourier methods, and the 1557 three-dimensional counter diffraction intensity data (CuKα) were used in a least-squares refinement to a conventional unweightedR of 0·053. The nickel atom is surrounded by the four oxygen atoms of the two acetylacetone ligands and the two oxygen atoms of the ethanol molecules, forming a tetragonally-distorted octahedron with acetylacetone oxygen atoms at 1·997 and 2·026 Å and ethanol oxygen atoms at 2·140 Å. Parallel molecules are linked into columns along theb-axis by hydrogen bonds between the ethanol oxygen atom of one molecule and an acetylacetone oxygen atom of a neighboring molecule.
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  • 20
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    Journal of chemical crystallography 3 (1973), S. 193-199 
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    Notes: Abstract The crystal structure of diglycollic acid has been determined by X-ray diffraction techniques and refined by full-matrix least squares, with three-dimensional counter data. The crystals are monoclinic:C2/c,a = 9·708(4),b = 3·938(3),c = 15·685(6) Å, β = 112·01(3) °, andZ = 4. The finalR-factor for 673 observed reflections is 0·050. The carboxyl groups are related by a two-fold axis, parallel tob, passing through the central oxygen atom of the molecule. Polymeric chains of molecules are formed by hydrogen bonding. The intermolecular O—O separation is 2·668 Å, and is consistent with the observed infrared spectrum of solid diglycollic acid.
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  • 21
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    Journal of chemical crystallography 3 (1973), S. 201-207 
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    Notes: Abstract The structure of crystals of the composition Zn[Cl2Ti(C5H5)2]2·2C6H6 has been determined from Patterson and Fourier syntheses of two projections, and refined toR = 0·117 by full-matrix three-dimensional least-squares methods. The crystals are orthorhombic:Pbcn,a = 18·45(5),b = 15·40(6),c = 11·35(3) Å,Z= 4. The complex consists of a central distorted ZnCl 4 2− tetrahedron linked along the Cl—Cl edges to two distorted TiCl2(C5H5)2 + tetrahedra in such a way that their centres are nearly collinear The two C6H6 molecules in the formulae unit may be regarded as benzene of crystallization.
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  • 22
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    Journal of chemical crystallography 3 (1973), S. 209-219 
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    Notes: Abstract The crystal structure of methyl β-D-hamameloside has been determined by direct methods. The trigonal crystals have the space groupR3. Referred to hexagonal axes, there are nine molecules in the non-primitive unit cell witha =b = 18·08(2),c = 7·22(2)Å. The molecule exists in the 1C-trans-chair conformation, with the mean C-C and C-O bond lengths being 1·531 and 1·428Å respectively. The mean value for the carbon bond angle is 110·2 °. The crystal structure is composed of columns of molecules hydrogen-bonded about 32 axes, and with van der Waals forces holding these columns together around the 31 and 3-fold axes.
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  • 23
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    Notes: Abstract The crystal and molecular structures of the title compounds have been determined by three-dimensional single-crystal X-ray techniques. All crystallographic details are fully reported. The major chemical conclusion for the pair, [Rh(NH3)5Cl]Cl2 and [Rh(NH3)Br]Br2, is that neither Cl nor Br exert a static intramoleculartrans effect. Furthermore, the two halogens have the same static electronic structural effect on the [RhIII(NH3)5] fragment. The conclusions shed much light on spectroscopic, thermodynamic and kinetic data of other compounds.
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  • 24
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    Journal of chemical crystallography 3 (1973), S. 221-233 
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    Notes: Abstract Crystals of bis(tropolonato)-dioxo(ethanol)uranium(VI) are orthorhombic:a = 12·495(8),b = 8·817(7),c = 15·459(9) Å,Z = 4, space groupPnam. The structure was determined with MoKα diffractometer data by standard Patterson and Fourier methods, and was refined by full-matrix least-squares methods toR = 0·049 for 1289 observed reflexions. The coordination plane consists of the four tropolonato oxygen atoms and the oxygen from the ethanol ligand; the uranyl group is perpendicular to it. The molecule lies across the mirror plane, consistent with a boat conformation for the tropolone rings; the dihedral angle between the plane of tropolone ring and the coordination plane is 22·5 °. The deviations of the tropolonato oxygen atoms from the tropolonato plane are 0·08 Å (above) and 0·16 Å (below). It is almost certain that the ethyl group of the ethanol ligand does not lie in the symmetry plane; C(8) is about 0·3 Å on one side of this plane and C(9) is about the same distance on the other, within a satisfactory bonding scheme.
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  • 25
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    Journal of chemical crystallography 3 (1973), S. 249-258 
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    Notes: Abstract The crystal structure of the charge-transfer complex of iodine with 9-cyclohexyladenine, C11H15I2N5, has been determined, and refined by three-dimensional least-squares techniques. The crystals are monoclinic:P21/c,Z = 4,a = 9·1728(7),b = 12·289(1),c = 13·596(1) Å, β = 99·564 °(6). The finalR value for 3629 reflexions is 0·039. The iodine forms a charge-transfer bond with N(1) of the adeninering, with an N—I bond length of 2·520(3) Å. The I—I—N(1) arrangement is approximately linear (bond angle, 177·1 °). The I—I molecule makes an angle of 21·5 ° with the plane of the adenine ring.
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  • 26
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    Journal of chemical crystallography 3 (1973), S. 259-270 
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    Notes: Abstract Tetragonal and monoclinic forms of crystalline pentachloropyridine are described. Both forms may be regarded as layer structures. The basic layer common to the two structures has neighbouring molecules in the same orientation. The tetragonal form has a repeat unit of four layers, whereas the monoclinic form has a repeat unit of two layers. The packing of adjacent layers is essentially the same for both forms. Examples have been found in which the stacking sequences are interrupted, producing faults, twins and diphasic crystals.
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  • 27
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    Journal of chemical crystallography 3 (1973), S. 271-275 
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    Notes: Abstract The crystal structure of 2-diethylaminoethyl-p-nitrobenzoate hydrochloride (C13H18N2O4, HCl) been has determined from three-dimensional diffractometer data. A detailed discussion of the molecular structure is presented, together with a comparison to other similar local anesthetic structures.
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    Journal of chemical crystallography 3 (1973), S. 277-283 
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    Notes: Abstract The crystal and molecular structure of bicyclo[2,2,1]hept-5-ene-2,3-endo-dicarboxylic acid, C9H10O4, has been determined by single-crystal X-ray diffraction techniques. The crystals are monoclinic:P21/c,a = 11·009(5),b = 7·394(5),c = 10·479(5) Å, β = 98 ° 22′(3) andZ = 4. The least-squares refinement of 1826 diffractometer reflexions resulted in a conventionalR of 0·074. Bond distances and angles of the bicyclo [2,2, 1]hept-5-ene ring system agree well with other recently published structures of this type, including similar asymmetry of bond distances. Hydrogen bonding of the acid groups occurs between the molecules so as to form infinite chains in the direction of thea-axis. Large anisotropic thermal motions of the oxygen atoms of one carboxylic acid group are, presumably, the result of differences in hydrogen-bonding geometry.
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    Journal of chemical crystallography 3 (1973), S. 299-307 
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    Notes: Abstract The crystal and molecular structure of the phthalide isoquinoline alkaloid bicuculline, C20H17NO6, has been determined by X-ray diffraction methods. The compound crystallizes in the orthorhombic space groupP212121 (No. 19) witha = 14·49,b = 10·90 andc = 10·43 Å. The atomic parameters were refined by least squares to give a conventionalR-factor of 0·0437 for 1557 symmetry independent reflections. The bicuculline molecule consists of two approximate planes of atoms with a dihedral angle of 14·3 ° between them. The two planes are joined by the bond . The torsion angle is 164·1 ° in the crystal, but in the liquid state there would be partial free rotation about the bond . The structure of bicuculline is of current pharmacological interest as it is a relatively selective antagonist of γ-aminobutyric acid at various sites of the nervous system.
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    Journal of chemical crystallography 3 (1973), S. 285-297 
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    Notes: Abstract The crystal and molecular structures of trimethyltin(IV) acetate and trimethyltin(IV) trifluoroacetate have been determined from three-dimensional X-ray data collected by counter methods using MoKα radiation. Both compounds crystallize in the orthorhombic space groupPnma withZ = 4. The acetate hasa = 10·516,b = 8·013,c = 9·706 Å and the trifluoroacetate hasa = 10·567,b = 9·237,c = 9·985 Å. ConventionalR-factors for the two compounds following least squares refinement are, for the acetate, 0·018 (for 731 reflexions) and, for the trifluoroacetate, 0·055 (for 460 reflexions) respectively. The compounds are isostructural and are polymeric with tin atoms linked by carboxylate bridges which are exactly planar. The tin atoms are in five-fold trigonal bipyramidal coordination with the methyl groups in the basal plane and oxygen atoms at the apices. Sn-O interatomic distances are, for the acetate, 2·205(3) and 2·391(4) Å, and for the trifluoroacetate, 2·18(1) and 2·46(2) Å.
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    Journal of chemical crystallography 3 (1973), S. 309-321 
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    Notes: Abstract Normal vibration analysis of the mono-, di-, tri- and tetra-glycines has been carried out employing the Urey-Bradley force field. The results show that the oligomers possess the planar zig-zag structure of polyglycine-I in the solid state.
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    Journal of chemical crystallography 3 (1973), S. 331-336 
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    Notes: Abstract On the assumption that, in certain molecules, nitrogen does not use its lone pair electrons for bonding to sulphur, an S to N bond length-bond order correlation has been established using currently available crystal structure data.
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    Journal of chemical crystallography 3 (1973), S. 323-327 
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    Journal of chemical crystallography 3 (1973), S. 337-342 
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    Notes: Abstract The crystal and molecular structure of diphenylthiosulphodiimide, C12H10N2S3, has been solved by the symbolic addition procedure using three-dimensional CuKα diffractometer data. The system is monoclinic,a = 30·41(3),b = 5·601(5),c = 7·792(8) Å, β= 108·77(1) °, space groupC2/c andZ = 4. The structure was refined by full-matrix least-squares methods toR = 0·096 for 926 observed reflexions. All hydrogen positions have been determined. The molecule possesses a crystallographic diad axis through the central sulphur atom. The planes of the phenyl rings make an angle of 30·8 ° with the closely coplanar central five atoms.
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    Journal of chemical crystallography 3 (1973), S. 343-348 
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    Notes: Abstract The crystal structure of bis(morpholino)-disulphide C8H16N2O2S2, has been solved by the symbolic addition procedure using three-dimensional CuKα diffractometer data. The system is monoclinic,a = 5·717(4),b = 8·880(7),c = 23·080(20) Å, β = 107·8(1) ° andZ = 4. The structure was refined by fullmatrix least-squares methods to a conventional, unweightedR of 0·039 for 1441 observed reflexions. All hydrogen positions have been determined. The molecule possesses a pseudo-diad axis, the morpholine rings being in the chair conformation. Bonds at nitrogen are distorted pyramidal with the attached sulphur equatorial.
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    Journal of chemical crystallography 3 (1973), S. 349-356 
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    Notes: Abstract The crystal and molecular structure of hexahydro-cis-(1-H,4a-H)-1-p-bromophenyl-1H,3H-pyrido[1,2-c][1,3]oxazine, (C14H18BrNO), has been determined from three-dimensional diffractometer data. The space group isP21/c; the unit cell has dimensionsa = 10·682(1),b = 21·606(2),c = 5·856(1) Å, β = 90·0 ° (at 20 °C) and contains four molecules. The structure has been refined to a residual (R) of 0·056 using least-squares methods on 1240 independent non-zero reflexions. The molecular geometry and conformation of the bicyclic ring is discussed.
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    Journal of chemical crystallography 3 (1973), S. 357-365 
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    Notes: Abstract The crystal and molecular structure of hexahydro-cis-(1-H,4a-H)-1-p-bromophenyl-1H,3H-pyrido[1,2-c][1,3]thiazine, (C14H18BrNS), has been determined from three-dimensional diffractometer data. The space group isI41/cd and the unit cell has dimensionsa = 22·906(4),b = 22·906(4),c = 10·646(2) Å withZ = 16. The structure has been refined to a residual of 0·065 using least-squares methods on 1235 independent non-zero reflexions. The molecular geometry and conformation of the bicyclic ring is discussed and compared with the related oxazine compound.
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    Journal of chemical crystallography 3 (1973), S. 367-375 
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    Notes: Abstract The alkaloid, 4-methyl-6-(2′-benzoyloxypentyl)-quinolizidme, C22H33NO2, which has been isolated from the plantPoranthera corymbosa Brogn. (family Euphorbiaceae), forms a stable hydrobromide which crystallizes in the orthorhombic space groupP2121 witha = 7·611,b = 31·007 andc = 9·453 Å. Its structure has been solved by the heavy-atom technique and refined to anR of 0·070. The molecule consists of two six-membered ringstrans-fused with methyl andn-pentyl side chains, a benzoate group being esterified to the latter. The absolute configuration has been determined from the differences between Bijvoet pairs of reflexions.
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    Notes: Abstract Bis(4-formyl-2-methoxyphenolato)bis(pyridine)copper(II) monohydrate crystallizes in the triclinic system:a = 10·432,b = 9·342,c = 13·799 Å, α = 103·75, β = 100·53, γ = 100·81 °,Z = 2, space groupP¯1. The structure was determined by Fourier methods with Cukα diffractometer data, and refined by a combination of block-diagonal and full-matrix least squares toR = 0·068 for 2430 observed reflexions. The copper atoms occupy the special positions 0, 0, 0 and 0,1/2, 1/2; hence, both molecules are centrosymmetric. Both the methoxy and phenolic oxygen atoms of the phenolate ions coordinate to the metal. These, together with coordinated nitrogen atoms from the pyridine molecules, give the copper atoms a six-fold coordination. Hydrogen bonding between a water molecule and the phenolic oxygen atoms of adjacent molecules results in chains of molecules linked approximately along [011].
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    Journal of chemical crystallography 4 (1974), S. 23-29 
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    Notes: Abstract The infrared and laser Raman spectra of dibenzyl and poly-p-xylylene in the 20–650 cm−1 region are compared with each other. New laser Raman data for poly-p-xylylene below 200 cm−1 have been obtained using an argon-ion laser (4880 Å) and photon counting detection techniques.
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    Journal of chemical crystallography 4 (1974), S. 1-14 
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    Notes: Abstract The crystal and molecular structure of bis(protonated thiamine) tetrachlorodioxouranium(VI), [C12H18ClN4OS]2 UO2Cl4, has been determined from three-dimensional X-ray diffractometer data. The crystals are monoclinic:P21/n,a = 11.199,b = 6.968,c = 23.675 Å, β = 97.50°,Z = 2. The structure was determined by Fourier methods and refined by least squares toR = 0.062, using 1675 observed reflections. The structure contains octahedral [UO2 Cl4]2−ions with average U-Cl and U-O distances of 2.67(1) and 1.78(1) Å, respectively. The organic portion of the molecule resembles that of previously reported thiamine structures. The failure to find the hydrogen atoms no doubt prevented our determining either which nitrogen atom is protonated or, with certainty, the hydrogen-bonding distribution.
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    Journal of chemical crystallography 4 (1974), S. 31-42 
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    Notes: Abstract The crystal and molecular structure of the thermodynamically more stable isomer of 24,25-dibromolanost-8-en-3β-yl acetate, the ‘A’ form, has been solved by the heavy-atom method and refined by full-matrix least-squares methods to a finalR-value of 0.153 for 2354 reflections. The crystals are orthorhombic:P212121,a = 40.889,b = 9.990,c = 7.839Å,Z = 4. Some difficulties were encountered owing to both radiation damage and the unusual positions of the bromine atoms. The analysis shows the configuration at C(24) to be 24S, and the rest of the structure does not reveal any unexpected features.
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    Journal of chemical crystallography 4 (1974), S. i 
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    Journal of chemical crystallography 4 (1974), S. 187-191 
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    Journal of chemical crystallography 4 (1974), S. I 
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    Journal of chemical crystallography 4 (1974), S. 193-198 
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    Notes: Abstract The proton magnetic resonance spectrum of phenylacetylene dissolved in a nematic phase has been recorded, and analysed in terms of dipolar coupling and chemical shifts. The spectrum is particularly well resolved, and accurate relative interproton distances are derived. The results have been compared with those of a previous study.
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    Journal of chemical crystallography 4 (1974), S. 213-225 
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    Notes: Abstract The crystal and molecular structure of the benzylisoquinoline alkaloid papaverine hydrochloride, C20H21NO4. HCl, has been determined with CuKα diffractometer data by direct methods. The compound crystallizes in the monoclinic space groupP21/c (No. 14) witha= 13.059(3),b = 15.620(3),c = 9.130(2) Å and β = 92.14(1) °. The structure was refined by full-matrix least-squares methods toR = 0.052 using all 2652 reflections. The nitrogen atoms is protonated and forms a strong hydrogen bond with the chloride ion, the N ... Cl distance being 3.01 Å. The isoquinoline ring is slightly non-planar but the benzene ring is planar within experimental error. The dihedral angle between the benzene ring and the best plane through the isoquinoline group is 109 °. The molecular structure of papaverine is of interest in gaining a better understanding of its pharmacological action on smooth muscle.
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    Journal of chemical crystallography 4 (1974), S. 199-212 
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    Notes: Abstract The crystal structure of 2,4-di-p-methoxyphenylcyclobutadiene-1,3-quinone has been been determined using three-dimensional X-ray data collected by means of a Picker FACS-1 four-circle diffractometer. The crystal used was one of four modifications of this compound, two low density (1.38 g cm−3) and two high density (1.54 g cm−3) forms, obtained by us, depending on crystallization conditions. The space group isP¯1, with unit cell dimensionsa = 3.89,b = 10.80,c = 9.03 Å, α = 77.88, β = 74.12, γ = 85.15 °D m = 1.38 g cm−3 andZ = 1. A least-squares refinement of the positional and anisotropic thermal parameters gave a finalR-value of 6.0% for 364 reflections and 121 variables. The zwitter-ionic nature of the molecule can be seen in both the partial delocalization of the bonds in the 4-membered ring (which is square-planar) and the bonds joining thep-phenylene and 4-membered rings. The nearly planarp-phenylene rings themselves are quinone-like in structure and are parallel, but not coplanar. The columnar packing of the molecules resembles that of graphite, and observed interplanar spacing is 3.64 Å.
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    Journal of chemical crystallography 4 (1974), S. 227-242 
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    Notes: Abstract A simple application of theB3,0 formula is described. This formula is used mainly to avoid inconsistent Σ2-interactions in standard symbolic-addition or multiple-solution techniques. Computer time is reduced by a reflection selection procedure based upon the use of theB2,0 formula. The solution of a centrosymmetric structure is described. This compound, a photodimerization product ofo-distyrylbenzene, is 5,6,11,12-tetraphenyl-dibenzo[2–3,8–9] tricyclo[8,2,0,04,7] dodecadiene-2,8, C44H36. The compound crystallizes in the monoclinic space groupC2/c, with unit cell parametersa = 28.047,b = 9.504,c= 12.600 Å and β = 103.4 °. A rather poor set of data was collected by an automatic diffractometer. Structural parameters were refined by full-matrix least-squares methods to anR-value of 0.06 for 970 non-zero reflections. The molecule is situated on a twofold rotation axis. It containscis-, trans-, cis-substituted puckered cyclobutane rings. The dihedral angle between the benzo-groups is 61.5 °.
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    Journal of chemical crystallography 4 (1974), S. 243-252 
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    Notes: Abstract The crystal and molecular structure of dichlorobis(pyridine-1-oxide) copper(II), C10H10N2O2Cl2Cu, has been determined from 3931 reflections measured on a Picker four-circle diffractometer, using the θ/2θ scan technique and MoKα radiation. The crystals are monoclinic, space groupP21/c,a = 6.900(4),b = 15.065(7),c = 12.065(5) Å, β = 97.00(4) ° andZ = 4. The structure was solved by Fourier methods and refined by full-matrix least-squares. The final conventionalR-factor was 0.033. The compound is dimeric, and the units of the dimer are held together by oxygen bridges. The coordination polyhedron for Cu is a tetragonal pyramid, with two bridging oxygens and two chlorines in the basal plane. The apical position is occupied by oxygen in the non-bridging ligand. The Cu−Cu distance in the dimer is 3.306(1) Å.
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    Journal of chemical crystallography 4 (1974), S. 253-262 
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    Notes: Abstract The compound bis(acetylcholine)tetrabromodioxouranium(VI), [C7H16-NO2]2 UO2 Br4, has been prepared and its physicochemical properties studied. No influence of the uranyl-bromide system on the muscarinic conformation of acetylcholine in the adduct was inferred on the basis of biological activity measurements. This lack of effect on the acetylcholine molecule by [UO2Br4]2− anion is confirmed by X-ray structure determination. The crystals are orthorhombic, space groupPnma,Z = 4,a =13.60(2),b = 20.94(3),c = 9.22(2) Å. The conventional discrepancy index is 0.087 for 1822 diffractometer data. Some disorder is observed in the acetylcholine molecule.
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    Journal of chemical crystallography 4 (1974), S. 305-311 
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    Notes: Abstract Crystals of 4-cyanopyridine-N-oxide crystallize in space groupP21/c (No. 14). There are four molecules per unit cell, witha = 7.88(2),b = 6.10(2),c =11.61(3) Å and β =101.4(4) °. Data for 838 unique reflections were recorded using the multiple-film technique and visually estimated intensities. A three-dimensional least-squares refinement of the structure was carried out to a final conventionalR of 0.098. It was found that the molecule was planar, as expected, and that the centrosymmetric pairs were stacked parallel to each other, as viewed down thea-axis. Bond distances and angles are in agreement with those from comparable molecules.
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    Notes: Abstract α-Edta is monoclinic:C2/c,a= 11.812,b = 9.647,c = 12.970 Å, β = 113.23 ° andZ = 4. The structure has been determined by direct methods with CuKα diffractometer data, and refined by full-matrix least squares toR = 7.2% for 737 observed reflexions. The molecule exists as a zwitter ion in acis conformation, and possesses crystallographic two-fold symmetry. The nitrogen atom is protonated and takes part in hydrogen bonding. α-Edta is hydrated, in this specimen, refinement indicated a value of 0.39 H2O per molecule of edta. A short (2.47 Å) hydrogen bond links oxygen atoms in adjacent molecules. Infrared spectra are reported for both α-edta and β-edta; the results are discussed in terms of the crystal structures. The formulation of α-edta with 0.39 mole H2O is explained.
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    Journal of chemical crystallography 4 (1974), S. 269-285 
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    Notes: Abstract The crystal and molecular structures of diphenyl sulphone (A), 4,4′-difluorodiphenyl sulphone (B) and 3,3′-dinitro-4,4′-difluorodiphenyl sulphone (C) have been determined from three-dimensional MoKα diffractometer data. Each molecule crystallizes in the monoclinic space groupP21/c with cell dimensionsa = 12.225(4),b = 7.830(2),c = 11.328(2) Å, β = 98 °19′(2);a = 8.255(3),b= 13.062(3),c = 10.135(2) Å, β = 99 ° 31′(2) anda = 14.736 (4),b = 8.145(2),c= 14.626(3) Å, β= 129°8′(2), respectively. The structures were solved by Patterson and Fourier techniques and refined by the method of least squares toR-factors of 3.8% over 1798 reflections, 6.3% over 1834 reflections and 5.4% over 2185 reflections forA,B andC, respectively. The dimensions of the sulphone group are similar in each molecule; the S—C bond lengths range from 1.764(3) to 1.775(3) Å, and the S—O bond lengths from 1.432(3) to 1.439(3) Å. The dihedral angles between the aromatic rings and the S—S—C planes lie between 72,6 and 88.9 °, compared with the value of 90 ° predicted for maximum conjugation between the sulphone group and the aromatic ring. Intermolecular H―O contacts of 2.37 Å suggest possible C—H—O type hydrogen bonds joining the molecules of 4,4′-difluorodiphenyl sulphone into dimers and the molecules of 3,3′-dinitro-4,4′-difluorodiphenyl sulphone into chains.
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    Journal of chemical crystallography 4 (1974), S. 287-303 
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    Notes: Abstract The crystal and molecular structure of 4,4′-dichloro-diphenyl sulphone (A), 4,4′-dibromodiphenyl sulphone (B) and 4,4′-diiododiphenyl sulphone (C) have been determined from three-dimensional MoKα. diffractometer data. These structures are isomorphous in the monoclinic space groupI2/a, with four molecules per unit-cell. The cell dimensions ofA,B andC area = 20.216 (4),b = 5.004(1),c = 12.248(2) Å, β = 90 °34′(1);a = 20.813(10),b = 5.055(3),c = 12.421(9) Å, β = 92 °46′(2) anda = 19.762(8),b = 4.947(2),c = 14.480(5) Å, β =103 ° 18′(1), respectively. Least-squares refinements converged toR-factors of 6.0% over 925 reflections, 6.8% over 1273 reflections and 3.8% over 995 reflections forA,B andC, respectively. The S—O bond lengths are 1.432(3), 1.453(5) and 1.445(7) Å and the S—C bond lengths 1.766(4), 1.764(6) and 1.756(7) Å inA,B andC, respectively. The C—Cl, C—Br and H—-I bond lengths are 1.748(5), 1.905(6) and 2.103(7) Å, respectively. The dihedral angle between the plane of each aromatic ring and the C—S—C plane is 84.6 ° inA, 83.8 ° inB and 86.9 ° inC. Intermolecular Br―Br and I―I contacts of 3.65 and 3.90 Å are considerably shorter than the van der Waals contacts given by Pauling.
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    Journal of chemical crystallography 4 (1974), S. 357-360 
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    Journal of chemical crystallography 4 (1974), S. 411-418 
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    Notes: Abstract The structure of acetylacetonatodicarbonylrhodium(I), Rh(acac)(CO)2, has been refined from three-dimensional X-ray diffractometer data. The complex crystallises in the triclinic space groupP¯1 with two molecules in a unit cell of dimensionsa = 6.5189(5),b = 7.7614(8),c = 9.2049(12)Å, α = 106.04(1), β = 91.15(1), γ = 100.21(1) °. Full-matrix least-squares refinement, using 1456 independent reflections, has reachedR = 0.038. The rhodium atom has a square-planar coordination with two Rh-O(acac) distances of 2.040 and 2.044Å, and two Rh-C(carbonyl) distances both equal to 1.831Å, the O-Rh-O angle is 90.8 ° and the C-Rh-C angle is 88.9 °. All twelve non-hydrogen atoms are closely planar, with an average deviation of 0.003Å, and a maximum deviation of 0.006Å, from the least-squares plane through the molecule. A second non-crystallographic plane of symmetry bisects the molecule, which therefore has essentiallymm2 (C 2v ) point symmetry. The molecules stack in such a way that the rhodium atoms of neighbouring molecules occupy the two remaining pseudo-octahedral positions, with Rh...Rh distances of 3.253 and 3.271Å.
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    Journal of chemical crystallography 4 (1974), S. 419-432 
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    Notes: Abstract Histidine dihydrochloride crystallizes in the orthorhombic system, space groupP212121, with unit-cell dataa = 6.970(4),b = 16.165(7),c = 8.964(6)Å,V c = 1010.0Å3 andZ = 4. Intensities for 1360 independent reflections were collected on an automated diffractometer. The structure was solved by standard heavy-atom methods and refined by full-matrix least squares, based onF, to anR-value of 0.027. The final weightedR-value and goodness-of-fit are 0.029 and 1.9, respectively. The histidine residue exists in the crystal as the carboxylic acid with protonation of the primary amine nitrogen and the imidazole ring. The overall conformation of the molecule is extended, similar to that observed inL-histidine,DL-histidine hydrochloride dihydrate, and one of the two independent molecules in the structure ofL-N-acetylhistidine. There is an extensive array of hydrogen bonds formed in the crystal, which, presumedly, together with the observed electrostatic interactions, account for the adopted molecular conformation.
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    Journal of chemical crystallography 4 (1974), S. I 
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    Journal of chemical crystallography 4 (1974), S. 327-334 
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    Notes: Abstract The crystal and molecular structure of dichlorotetrakis(propanol-2)titanium (III) chloride, C12H32Cl3O4Ti, has been determined by X-ray methods. The complex crystallizes in the monoclinic system:a = 15.968(4),b = 11.610(5),c = 11.90(5) Å, β = 94.15(2) °, space groupC2/c andZ = 4. The positions of all non-hydrogen atoms have been refined by least squares to giveR = 0.126 for 1211 observed structure factors. The crystal structure consists of {TiCl2(HOCH(CH3)2)4}+ cations and Cl− anions. From the space-group symmetry, it follows that the complex cation has 2(C 2) symmetry. The 2 chlorine and 4 oxygen atoms of the inner coordination sphere are arranged in the form of a distorted octahedron around the central Ti atom. Two chlorine atoms, with the interatomic distance Ti—Cl of 2.32 Å, are in acis-conformation. The interatomic distances Ti—O, two oxygen atoms opposite to the chlorine atoms, are 2.10 Å. The pair oftrans-oriented oxygen atoms are at distances Ti—O= 2.09 Å. The Cl− ions occupy positions at symmetry centres. Each of them is in contact with four oxygen atoms, the paired Cl—O distances being 3.04 Å and 3.12 Å.
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    Journal of chemical crystallography 4 (1974), S. 87-96 
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    Notes: Abstract Cis-mesityl(phenylsulphonyl)sulphine, C16H16O3S2, crystallizes in the tri-clinic system: space groupP¯1,a = 9.209(2),b = 11.106(2),c = 7.626(1) Å, α = 92.53(1), β = 98.53(3), γ = 89.82(2) °. The structure has been determined by Patterson and direct methods and refined by full-matrix least squares toR = 0.057 for 2724 observed reflections. The sulphine moiety has bond lengths 1.622(2) Å for C-S, 1.466(3) Å for S-O and a C-S-O angle of 115.2(2) °, indicating sp2 hybridization on the sulphur atom. All other bond distances and angles are close to normal values. The molecules are held together by van der Waals forces.
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    Journal of chemical crystallography 4 (1974), S. II 
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    Journal of chemical crystallography 4 (1974), S. i 
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    Journal of chemical crystallography 4 (1974), S. 15-21 
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    Notes: Abstract The crystal structure of acetylcholine perchlorate has been determined from three-dimensional X-ray diffractometer data. The molecular geometry of this compound differs from that observed for acetylcholine bromide but is structurally similar to that observed for acetylcholine chloride.
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    Journal of chemical crystallography 4 (1974), S. 43-54 
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    Notes: Abstract The structure of the title compound has been determined by X-ray analysis. It is monoclinic:a = 10.147,b = 10.081,c = 38.627 Å, β = 102.27 °,Z = 4,P21/c. The structure was solved by standard methods and refined by least squares to a (conventional)R-factor of 4.7%. The Ru atom is in square-pyramidal configuration: the Ru-S distances (2.286, 2.336Å) are significantly different, but the Ru-P distances average to 2.389 Å. Comparisons are made with the violet isomer.
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    Journal of chemical crystallography 4 (1974), S. 55-61 
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    Notes: Abstract The structure of dimethanolbis(salicylaldehydato)cobalt(II) has been determined by three-dimensional X-ray diffraction methods. The crystals are monoclinic, space groupP21/c,a = 5.099(7),b = 19.446(9),c = 8.889(7) Å, β = 111.85(10) °, andZ = 2. The structure consists of discrete centro-symmetric molecules of C16H18CoO6 in which the oxygen atoms form a distorted octahedron about the cobalt atom, with cobalt-oxygen distances of 2.010(4), 2.076(4) Å (salicylaldehyde) and 2.115(4) Å (methanol). The molecules are linked together along thea-axis by intermolecular hydrogen bonds from the hydrogen atoms of the methanol groups to phenolic oxygen atoms of neighboring molecules. The final conventionalR-factor for 1232 observed reflections is 0.058.
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    Journal of chemical crystallography 4 (1974), S. 63-75 
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    Notes: Abstract 2′-nitro-4-aminobiphenyl (5), C12H10N2O2, crystallizes in the monoclinic space groupP21/c:a = 6.043(2),b =15.795(3),c = 11.577(2) Å, β = 103.42(8) °;D c = 1.324 g cm−3 forZ = 4. 2-amino-7-nitrofluorene (3), C13H10N2O2, crystallizes in the monoclinic space groupP21 n:a = 10.765(2),b = 7.454(4),c = 12.959(2) Å, β = 95.44(1) °;D c = 1.451 g cm−3 forZ = 4. Three-dimensional CuKα intensity data were measured with a computer-controlled diffractometer, and the initial phases were obtained by direct methods. The two structures were refined by the full-matrix least-squares method, which gave finalR values for 5 and 3 of 0.045 and 0.043, respectively. Bond lengths in the compounds are normal, apart from slight shortening of the phenyl-phenyl C-C bond and some distortion of the phenyl rings caused by the amino and nitro groups. In 5, the two phenyl rings are twisted by 57.1 °, and the nitro group is twisted by 34.6 ° from the plane of its phenyl group. The carbon backbone of 3 is nearly planar with the two phenyl groups tilted by 4.0 ° to each other. The nitro group in 3 is twisted 5.7 ° from the plane of its phenyl group. There is amino hydrogen to nitro oxygen intermolecular hydrogen bonding in each structure.
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    Journal of chemical crystallography 4 (1974), S. 77-85 
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    Notes: Abstract The crystal structure of the title compound has been determined from single-crystal X-ray diffractometer data. The crystals are orthorhombic with unit-cell dimensionsa =17.147(3),b = 18.147(3),c = 13.860(3) Å, space groupPbca andZ = 8. Full-matrix least-squares refinement, using 2215 independent reflections, has reachedR = 0.040. The structure contains tetrahedral benzy IPPh3 cations and free chloride ions. The three P-C(phenyl) distances are in the range 1.785(3)-1.796(3) Å, with a mean of 1.790 Å, while the P-C(benzyl) distance is fractionally larger at 1.811(3) Å. The tetrahedral angles at the phosphorus atom range from 108.0 to 111.6 °. There are indications that one of the phenyl rings may be slightly disordered.
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    Journal of chemical crystallography 4 (1974), S. i 
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    Notes: Abstract The crystal structure of dibromo-(N,N,N′N′-tetramethylethylenediamine) cadmium(II), C6H16Br2CdN2, has been determined from 1890 reflections measured on a Siemens four-circle diffractometer using the ω/2θ scan technique and CuKα. radiation. The crystals are monoclinic:P21/c,a = 7.532(2),b = 10.689(6),c = 14.674(7) Å, β = 91.91(7) β andZ = 4. The structure was solved by Fourier methods and refined by full-matrix least squares to a finalR (conventional) of 6.1%. Anisotropic thermal parameters were evaluated for the non-hydrogen atoms, but the hydrogen atoms were assigned the average isotropic thermal parameter of the carbon atoms. Each cadmium atom is octahedrally coordinated by two pairs of bromine atoms, giving average Cd-Br bond lengths of 2.753(2) and 2.844(2) Å, and a pair of nitrogen atoms in thecis configuration with respect to cadmium, with an average Cd-N bond length of 2.46(1) Å. The average Br-Cd-Br and N-Cd-Br angles are 88.1 and 90.6 ° respectively. The bromine atoms provide bridges to the metal atoms, resulting in a chain-like structure with the chain direction approximately parallel to thex-axis.
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    Journal of chemical crystallography 4 (1974), S. 121-127 
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    Notes: Abstract The molecular structure of 5α-bromo-8β,9α-dimethylhydrindane-1,4-dione (C11H15BrO2) has been confirmed using three-dimensional X-ray data collected by means of a Picker FACS-1 four-circle diffractometer. The compound crystallized in the space groupC2/c with unit cell constantsa = 26.56(5),b = 6.68(1),c = 12.32(2) Å and β = 90.6(1) °; the density was 1.55 g cm−3 andZ = 8. Least-squares refinement of the positional and anistropic thermal parameters gave a finalR 1 value of 0.083 for 793 significant reflections.
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    Journal of chemical crystallography 4 (1974), S. 107-120 
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    Notes: Abstract The calculation of general three-dimensional heavy-atom phases, without assumption of heavy-atom sites, using the tangent formula is investigated. Phases obtained in this way have an average difference of 27 ° as compared with phases calculated for the known heavy-atom constellation in the K2PtCl6 derivative of ribonuclease in space groupP21. Five out of eight of the phase sets produce the correct heavy atom positions by calculation of Δ.E maps.
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    Journal of chemical crystallography 4 (1974), S. 129-140 
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    Notes: Abstract Crystals of 1,3-diphenyl-4-p-chlorobenzal-5-pyrazolone, C22H15ClNN2O, are triclinic:a = 13.96,b = 12.94,c = 7.29 Å, α = 93.0 ° β = 100.1 °, γ = 135.6 °,Z = 2, space groupP¯1. The structure has been determined from Weissenberg X-ray data by direct methods, and refined by full-matrix least squares toR = 0.098 for 1949 observed reflexions. The molecular conformation of the double bond at chlorobenzal is of type Z. The phenyl rings make angles of 9.2 ° and 47.7 ° and thep-chlorophenyl group an angle of 4.2 ° all with the plane of the pyrazolone moiety, thus allowing extended conjugation. Comparisons of bond distances and angles with those of similar molecules are made. Close molecular packing is afforded by layers of molecules approximately parallel to (¯110).
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    Journal of chemical crystallography 4 (1974), S. 141-148 
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    Notes: Abstract Crystals of N,O-diacetyl-5-p-chloranilino-4-hydroxypenta-2,4-dienal, the degradation product from a Stenhouse salt, belong to the monoclinic space groupP21/c witha = 10.845,b = 17.607,c = 8.056 Å, β = 95.87 ° andZ = 4. The structure was solved by the heavy-atom method from intensity data measured out to 1.14 Å−1 with CuKα radiation. Hydrogen atoms were not located. A finalR of 0.098 for the 549 observed terms was attained. The molecule is in thetrans-trans conformation, and the non-hydrogen atoms in the pentadienal chain and N-acetyl group are almost co-planar. Thep-chloraniline and O-acetyl groups lie on the same side of the pentadienal skeleton, and their respective planes are approximately parallel and at right angles to the plane of the chain. The molecules in the crystal structure are held together by van der Waals' interactions.
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    Journal of chemical crystallography 4 (1974), S. 165-171 
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    Notes: Abstract Far-infrared (50–400 cm−1) and Raman spectra of complexes HgX 2py2 (X = Cl, Br or I) have been studied. Previous infrared bands attributed to the chloride have been shown to arise from HgCl2py as impurity. The correct spectral data show that the true description of the structure of HgCl2py2 is one involving infinite planar chains [HgCl2py2] n and not the previously described alternative of HgCl2 molecules with loosely-held pyridine of crystallization. Contrary to previous reports, HgBr2py2 contains tetrahedrally coordinated mercury atoms, as does HgI2py2.
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    Journal of chemical crystallography 4 (1974), S. 149-164 
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    Notes: Abstract The crystal structures of CsCrO3Cl and RbCrO3Cl have been determined from MoKα1diffractometer data and refined anisotropically toR = 0.029 andR = 0.033 respectively for 769 and 590 statistically significant reflections. CsCrO3Cl, which has a structure of the BaSO4 type, crystallizes in the orthorhombic space groupPnma, witha = 9.928,b = 6.043,c = 8.712 Å andZ = 4. RbCrO3Cl is isostructural with KCrO3C1 and NH4CrO3Cl and crystallizes in the monoclinic space groupP21/c witha = 7.857,b = 7.711,c = 8.055 Å, β = 90.43 ° andZ = 4. The geometry of the approximately tetrahedral CrO3Cl− groups is very similar in both structures, and the Cr-Cl and average Cr-O bond distances, corrected for thermal vibration of the terminal atoms, are 2.197 and 1.612 Å in CsCrO3Cl and 2.194 and 1.606 Å in RbCrO3Cl. Caesium ions are in 12-fold coordination and rubidium ions in irregular 11-fold coordination to chlorine and oxygen.
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    Journal of chemical crystallography 4 (1974), S. 173-185 
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    Notes: Abstract Bis(N,N′-diethyldithiocarbamato)diphenylstannane crystallises in the mono-clinic system:a = 14.98(3),b = 9.44(2),c = 18.30(3) Å, β = 90.5(1) °,Z = 4,P21/c. The structure has been solved using visually estimated three-dimensional intensity data collected with a precession camera and MoKα. radiation, and refined by full-matrix least squares toR = 0.08 for 1724 non-zero reflections. The molecule contains two bidentate dithiocarbamato ligands resulting in a distortedcis octahedral geometry around the tin atom; the phenyl groups subtend an angle of 101.4(6) ° at this atom.
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    Journal of chemical crystallography 4 (1974), S. i 
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    Notes: Abstract The crystal structure of bis(tiethylphosphine)(hexakis(trifluoromethyl)benzene) platimum, C24H30F18P2Pt, has been determined. The crystals are monoclinic: space groupP21/n,a = 9.937(6),b = 30.89(1),c= 11.398(8) Å, β = 117.15(3) ° andZ = 4. X-ray data were collected by counter methods using MoKα radiation, and least-squares refinement led toR = 0.057 for the 2154 independent reflexions for which ¦F 0¦2〉 3σ(¦F 0¦2). The molecule has a 1,2-hapto structure, with the platinum atom bonded to only two carbon atoms of the hexakis(trifluoromethyl)benzene ring. The planarity of this ring is destroyed as a result of the coordination and there is an alternation of long and short bonds around the ring. The mean Pt—C bond length is 2.14(2) Å.
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    Notes: Abstract The crystal structure of a nickelahexakis(trifluoromethyl)cycloheptatriene, C18H18F18NiO6P2 has been determined. The compound crystallizes in the orthorhombic space groupPbcn, witha = 17.355(5),b = 11.014(3),c = 15.026(5) Å andZ = 4. The molecular symmetry is 2(C 2). X-ray intensity data were collected by counter methods, using MoKα radiation, and least-squares refinement led toR = 0.050 for the 804 reflexions for which. ¦F 0¦2 〉2σ(¦F 0¦2). The [C2(CF3)2]3 ligand is attached to the nickel atom by σ-bonds from the two terminal carbon atoms (Ni—C = 1.96 Å) and by a η-bond from the two central (double-bonded) carbon atoms (Ni—C = 2.04 Å). This is the first example of the coordination to a transition metal of an olefinic group which is also part of a chelate.
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    Journal of chemical crystallography 4 (1974), S. 383-389 
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    Journal of chemical crystallography 4 (1974), S. 373-381 
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    Notes: Abstract E-mesityl(phenylsulphinyl)sulphine, C16H16O2S2, crystallizes in the monoclinic system: space groupP21/c,a = 8.310(2),b = 14.141(3),c = 14.873(4)Å, β = 116.67(4) ° andz = 4. The structure has been determined by direct methods and refined by full-matrix least squares toR = 0.060 for 1834 non-zero reflections. The sulphine moiety has bond lengths 1.628(5)Å for C-S, 1.470(5)Å for S-O and a C-S-O angle of 113.8(2) °, values which are consistent with a cumulated double-bond system and sp2 hybridization on the sulphur atom. All other bond distances and angles are close to those usually found for such functional groups.
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    Journal of chemical crystallography 4 (1974), S. 361-371 
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    Notes: Abstract The crystal and molecular structure of the charge-transfer complex formed between 2,4,7-trinitrofluorenone and hexamethylbenzene has been determined by single-crystal X-ray diffraction techniques. The complex crystallizes with four charge-transfer pairs in a monoclinic cell (P21/c) of dimensionsa = 9.533(1),b = 14.944(2),c= 17.470(2) Å and β = 113.18(1) °. The structure was solved by direct methods. The orderly packing of donor and acceptor molecules in parallel crystalline planes made the determination a severe test of direct methods techniques. The 2294 statistically significant reflections were refined to a final value ofR = 0.063. Estimated standard deviations were 0.004 Å in bond distances and 0.5 ° in bond angles among the non-hydrogen atoms. The acceptor and donor molecules lie in alternate (212) planes with a separation of 3.25 Å between the planes.
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    Journal of chemical crystallography 4 (1974), S. 391-402 
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    Notes: Abstract The crystal and molecular structure of 5-anilinopentadienylidenanilinium bromide has been solved by X-ray diffraction methods. The crystals of this compound are monoclinic, space groupC2/c (No. 15), with unit cell data:a = 14.63,b = 12.68,c= 17.77 Å and β = 104.8 °,D m = 1.39 g cm−3,Z = 8,D c = 1.37 g cm−3 and μ = 38.4 cm−1 (CuKα radiation). The structure has been refined to anR-value of 0.049, using diffractometer intensity data for 2014 reflexions. The bond angles in the pentamethene chain are widened by about 3.8 ° from the expected value of 120 °, owing to the repulsion of hydrogen atoms in the chain. Steric hindrances from the hydrogen atoms cause the phenyl rings to be twisted by approximately 20.7 and 16.5 ° in the opposite directions with respect to the pentamethene chain. The nitrogen atoms take part in hydrogen bonds with the neighbouring bromine atoms (N ...; Br = 3.35 Å).
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    Journal of chemical crystallography 4 (1974), S. 403-410 
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    Notes: Abstract The visible and ultraviolet absorption spectra of crystalline 5-anilinopenta-dienylidenaniliniumbromide have been measured with a microreflexion spectrometer, using polarized light. The (110) crystal plane shows exceptional dichroism, which is interpreted from the results of X-ray structure analysis as being due to the approximately parallel arrangement of the molecular oscillators.
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    Rock mechanics and rock engineering 5 (1973), S. 21-41 
    ISSN: 1434-453X
    Keywords: soil mechanics ; rock mechanics ; hydrofracture ; permeation grouting ; seepage force ; fracture initiation ; fracture propagation ; energy balance
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    Topics: Architecture, Civil Engineering, Surveying , Geosciences
    Description / Table of Contents: Zusammenfassung Brucherscheinungen im Fels bei Verpreβarbeiten. In der Arbeit wird der grundlegende Mechanismus untersucht, welcher bei Verpreßarbeiten in Fels und geschichtetem Boden zur Einleitung und Ausbreitung von Brüchen führt. Frühere Untersuchungen des Bruchbeginns stützten sich im wesentlichen auf vereinfachte Modelle, in denen der Untergrund als undurchlässiges Kontinuum angesehen wird, das entweder elastisch ist oder der Mohr-Coulombschen Bruchbedingung genügt. Die neue Methode berücksichtigt dagegen eine Porosität oder Klüftung des Untergrundes durch Ansatz der vom strömenden Medium auf das Gebirge ausgeübten Belastung. Diese Belastung wird aufgeteilt in einen Druckverlust an der Bohrlochwand (gleich ParameterN mal Verpreßdruck) und die entsprechende, über den gesamten durchströmten Bereich verteilte Belastung. Die Untersuchung der Bruchausbreitung geht von der Spannungsermittlung um ein Bohrloch in einem elastischen Kontinuum aus, wobei in der sich ausbreitenden Bruchzone um das Bohrloch herum nichtelastisches Material angenommen wird, das dem Mohr-Coulombschen Bruchkriterium genügt. Zur Ergänzung dient eine Energie-Betrachtung, bei der die von der Injektionspumpe abgegebene Energie gleichgesetzt wird der im Untergrund gespeicherten Energie und der aufgewendeten Brucharbeit.
    Abstract: Résumé Les mécanismes de la fracturation hydraulique dans les roches pendant les injections sous pression. Le mémoire examine les mécanismes fondamentaux qui gouvernent l'initiation des ruptures dans les roches et les sols stratifiés, au cours des injections et leur propagation dans les massifs. Les analyses antérieures de l'initiation de la rupture, se sont concentrées sur des modèles simplifiés où l'on considérait la roche comme un milieu élastique et imperméable, ou comme un milieu de Mohr-Coulomb. La présente méthode admet que le massif est poreux ou fissuré, en considérant l'action des forces de percolation engendrées par le gradient de pression interstitielle. Cette action est quantifiée par un paramètreN, tel que le rapport de la force du liquide employée à dilater le forage d'injection, à celle employée pour forcer le coulis à travers les vides soitN/(1—N). L'analyse de la propagation des ruptures se base sur l'analyse des contraintes autour d'un forage dans un milieu élastique, alors que la zone de la rupture qui se propage autour du forage est représentée par un milieu non-élastique admettant le critère de rupture de Mohr-Coulomb. Cette analyse est complétée par une approche énergétique, où l'énergie qui est fournie au massif par la pompe d'injection est égalée à l'énergie emmagasinée dans la roche et à l'énergie de rupture.
    Notes: Summary Hydrofracture Mechanisms in Rock During Pressure Grouting. The paper examines the basic meachnisms controlling the initiation of fractures in rocks and layered soils during pressure grouting, and their subsequent propagation into the ground mass. Previous analyses of fracture initiation have tended to concentrate on simplified models in which the ground is treated as an impervious elastic or Mohr-Coulomb continuum. The present method allows for the porous or fissured nature of the ground by considering the effect of seepage forces induced by the pore pressure gradient. The effect is quantified by use of a parameterN such that the ratio of fluid force used in expanding the injection hole, to that used in forcing fluid through void spaces, isN to (1—N). Analysis of hydrofracture propagation is based on stress analysis of a borehole in an elastic continuum, the propagating fracture zone around the borehole being represented as a non-elastic material governed by the Mohr-Coulomb failure criterion. This is supplemented by an energy approach which equates the energy supplied to the ground from the injection pump, with the energy stored in the ground and the energy necessary to fracture it.
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    Rock mechanics and rock engineering 5 (1973), S. 188-188 
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    Rock mechanics and rock engineering 5 (1973), S. 163-187 
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    Description / Table of Contents: Zusammenfassung Über den Ursprung von Plattenklüften Obwohl die tiefliegenden, ungefähr zur Geländeoberfläche parallel verlaufenden, als Plattenklüfte bezeichneten Brüche verschiedentlich der Sonneneinstrahlung u. ä., weitgehend aber der Entlastung durch Erosion allein zugeschrieben werden, liegt eine Reihe von Argumenten vor, die Zweifel an dieser Hypothese aufkommen lassen. Es gibt für die Annahme einer Druckentlastung als Ursache für diese Entscheidung keinen mechanisch verständlichen Grund. Plattenklüfte sind deutlich in Gesteinen ausgebildet, die nie eine größere Überlagerung hatten. Domartige Inselberge oder Bornhardts, bei denen Plattenklüftung weit verbreitet und gut entwickelt ist, scheinen ihre Formresistenz dadurch zu sichern, daß ihre Klüftung unter Kompression stand. Dies widerspricht einer Erklärung als Effekt einer radialen Ausdehnung oder einer Dehnungsspannung. Einige Inselberge sind von Gesteinen unterlagert, die eine Plattenklüftung aufweisen, welche nicht parallel zum Bergprofil verläuft, sondern gegen die Hänge des Inselberges einfällt. Vieles deutet darauf hin, daß die Plattenklüftung nicht als Folge einer Druckentlastung, sondern als Folge einer Druckbelastung zu deuten ist. Plattenklüfte und druckbedingte Verwerfungen treten häufig zusammen auf. Messungen geben Zeugnis von hoher Druckbelastung in Bergwerken und Steinbrüchen. Druckbelastung scheint ein physikalischer Parameter für die Ausbildung von Plattenklüftung zu sein. Auch viele morphologische Merkmale, die mit Plattenklüftung verbunden sind, weisen auf Kompression hin. Eine solche macht insbesondere die Formresistenz der Inselberge verständlich.
    Abstract: Résumé Sur l'origine des joints en nappe L'origine des fractures profondes, dites joints en nappe, qui sont à peu près parallèles à la surface de la terre, a été attribuée à plusieurs causes, dont l'insolation, l'altération chimique, l'injection plutonique, l'expansion métasomatique et le soulèvement vertical. Ces idées peuvent fournir des explications partielles, ou bien elles peuvent éclaircir des cas particuliers, mais en tant qu'explications générales elles ne sont pas acceptables. La présence des joints en nappe est attribuée le plus souvent à l'allègement par l'érosion uniquement, au point que certains géologues les désignent sous le nom de joints d'allègement. Toutefois de nombreux témoignages et discussions mettent cette hypothèse en doute. Aucune raison mécanique valable ne mène normalement au développement des fractures par suite de la décompression. Les joints en nappe se montrent aussi bien dans des couches qui n'ont jamais été profondément enfouies. Les inselbergs à dôme ou bornhardts, sur lesquels les joints en nappe se manifestent amplement, paraissent subsister en raison de la compression de leurs joints; il s'ensuit que le développement de ces joints en nappe ne peut pas être attribuable à l'expansion radiale ou au travail à la tension. Quelques-uns des inselbergs ont pour base des roches qui ont été soumises à l'influence des joints en nappe qui ne sont pas parallèles au profil de la colline mais qui, au contraire, s'inclinent jusque dans les pentes des résiduels. D'autre part, divers témoignages et discussions font croire que les joints en nappe ont pu évoluer par la suite du travail à la compression. Certaines failles sont causées par la compression, et d'ordinaire les failles et les joints en nappe se produisent dans des conditions uniformes; il existe des observations de mesures de compression très considérable dans beaucoup de mines et carrières; le travail à la compression paraît matériellement capable de produire ces joints; de nombreuses caractéristiques morphologiques associées aux joints en nappe se rapportent à la compression. Ce qui s'explique surtout, c'est la conservation des inselbergs à dôme. Cette hypothèse propose donc que les joints en nappe déterminent les configurations de la surface terrestre, et non vice versa.
    Notes: Summary On the Origin of Sheet Jointing Although the deep-seated fractures which run approximately parallel to the land surface and are known as sheeting joints are widely attributed to erosional offloading alone, there is much evidence and argument which casts doubt on this hypothesis. There is no sound mechanical reason why fractures should normally develop as a result of decompression. Sheet jointing is well developed in strata which have never been deeply buried. The domed inselbergs on which sheet jointing is commonly displayed appear to survive by virtue of their joints being compressed, which is inconsistent with the sheet jointing developing through radial expansion or tensional stress. A few inselbergs are underlain by rocks affected by sheeting joints which are not parallel to the hill profile but on the contrary dip into the slopes of the residuals. These and other types of evidence and lines of argument point to sheeting joints having developed under compressive stress. The joints determine the shape of the land surface and not vice versa.
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    Rock mechanics and rock engineering 5 (1973), S. 249-249 
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    Rock mechanics and rock engineering 6 (1974), S. 1-2 
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    Rock mechanics and rock engineering 6 (1974), S. 3-13 
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    Description / Table of Contents: Summary Excavation in Rock — Examples from Switzerland Subject of the contribution are two large building excavations in rock, both situated on a slope. This created fairly long and high cuts along the mountain side which had to be stabilized by pretensioned rock anchors. Nevertheless a surprisingly large extension of the remaining rock mass was noticed. In one case the cut in soft micaceous schist standing vertically was 200 m long and as an average 25 m high. Excavation was done by explosive but with limited charges controlled continuously by measuring the vibrations in the adjoining buildings. No damages therefore could be traced back to blasting operations. On the other hand the concrete lining of the vertical cut showed an inward movement up to about 60 mm in the central part. As a result the buildings founded on the same rock above the cut were caused to crack from the bottom, especially the walls standing cross to the cut. By means of additional and longer anchors the deformation could successfully be limited. A profile of five borehole extensometers was placed and the deformations inside the rock mass checked; there was a distinct zone of maximum strain inclined at an angle of about 30°. The other pit had a similar size but only 17 m depth. It is situated in a sequence of soft sandstone, siltstone and marl with the layers inclined at an angle of about 20°. As a measure to improve the stability of the cut, rock anchors were placed but nevertheless a horizontal deformation of the cut by more than 50 mm was measured causing excitement about the safety of a nearby clock tower. Finally it was found that a larger part of the deformation was created by the grout used for the anchors and injected at too high a pressure. According to our calculations the rest could be attributed to the elastic extension of the rock mass adjoining the cut.
    Abstract: Résumé Excavation de roche à ciel ouvert — exemples de la Suisse L'article traite l'excavation et le blindage de deux grandes fouilles pour des buildings commerciaux, situées à une pente, tellement qu'amont une tranchée longue et haute dans la roche s'est produite. Il s'y agissait moins de la stabilité de l'excavation, qui était soutenue appropriéement par de l'ancrage, que des déformations résultant de la détente de la masse rocheuse, qui par son étendue ont surpris et alarmé les intéressés. En un cas l'excavation dans la mica-schiste mou, orienté vertical, avait 200 m de longeur et en moyenne 25 m de hauteur. L'excavation avait exécuté par explosion, pourtant limitée par des contrôles rigoureux des perturbations à une dimension de charge qui n'est pas nuisible pour les voisins. La paroi amont fut soutenu par des ancres précontraintes de 20 à 30 m de longueur. Quant même des mouvements se passaient, qui se manifestaient dans les maisons se trouvant audessus du chantier en forme de fissures, spécialement dans les murs situées en travers de la fouille. Ce phénomène pouvait être combattu avec succès par l'installation des ancres additionelles et plus longues. L'installation d'extensomètres donnait l'occasion de suivre les mouvements aussi vers l'intérieur de la montagne; on trouvait un plan de dilatation maximum, incliné avec 30° vers la fouille. Dans une fouille de grandeur semblable de 17 m de profondeur dans la molasse les couches pendent avec 20° vers l'excavation. Pour amender la résistance au glissement on a appliqué des ancres précontraintes; quand même des mouvements latéraux de 50 mm et plus ont été constatés. L'examination plus exacte des points fixes et des ancres de mesurage a montré, que la plupart de ces déformations était causée par le coulis d'injection des ancres, qui ont été injectées avec une pression trop forte. Le reste était à peu près conforme à la détente élastique du massif rocheux résultant d'une calculation comparative.
    Notes: zusammenfassung Felsabtrag über Tag — Beispiele aus der Schweiz Es handelt sich um den Aushub und die Sicherung zweier großer Baugruben für Geschäftshäuser, beide Male an einem Berghang gelegen, so daß auf der Bergseite jeweils ein langer und hoher Felsanschnitt entstand. Dabei ging es weniger um die Stabilität des Anschnittes — dieser wurde durch Felsanker sachgemäß gesichert — als um die aus der Entspannung des Gebirges entstehenden Deformationen, welche in ihrem Ausmaß die Beteiligten überraschte und beunruhigte. Im einen Fall war der Anschnitt in weichem, senkrecht gestelltem Glimmerschiefer 200 m lang und im Mittel 25 m hoch. Der Abtrag erfolgte durch Sprengen, das aber durch strenge Erschütterungskontrollen auf ein für die Nachbarn unschädliches Ladungsmaß beschränkt war. Die bergseitige Wand wurde laufend durch 20–30 m lange Spannanker gesichert. Trotzdem traten Bewegungen auf, die sich in den oberhalb der Baustelle stehenden Häusern in Form von Rissen äußerten, namentlich in den quer zur Baugrube stehenden Wänden. Durch Einbau zusätzlicher und längerer Anker wurde diese Erscheinung mit gutem Erfolg bekämpft. Der Einbau von Extensometern gab Gelegenheit, die Bewegungen auch im Berginneren zu verfolgen; es zeigte sich eine Ebene der größten Dehnung, die mit etwa 30° gegen die Baugrube einfiel. Bei einer ähnlich großen Baugrube von 17 m Tiefe in der Molasse fallen die Schichten mit 20° gegen den Abtrag ein. Zur Verbesserung der Gleitsicherheit wurden Spannanker eingesetzt, jedoch trotzdem seitliche Bewegungen von 50 mm und mehr festgestellt. Die genaue Untersuchung der Fixpunkte und Meßanker zeigte, daß der größere Teil dieser Deformationen durch das Injektionsgut der Felsanker verursacht wurde, das mit zu großem Druck eingepreßt worden war. Der Rest entsprach etwa der elastischen Entspannung des Gebirges, die sich aus einer Vergleichsrechnung ergab.
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    Rock mechanics and rock engineering 6 (1974), S. 53-64 
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    Keywords: Stress Determinations ; In-Situ Stresses ; Triaxial Strain Cell ; Stress Tensor
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    Description / Table of Contents: Zusammenfassung Druckspannungsmessungen in Kanada Druckspannungsmessungen mit der biachsialen (Doorstopper) und der dreiachsialen Dehnungszelle des C. S. I. R., Pretoria, Süd-Afrika, werden beschrieben und zeigen, daß das dreiachsiale Gerät das wünschenswertere ist, falls die Gesteinseigenschaften ausreichend gut sind. Druckspannungen in Kanada besitzen ähnliche Werte wie andere Teile der Erdkruste und zeigen, daß die vertikale Komponente mit dem Überlagerungsdruck zunimmt und daß der vorwiegende Zuwachs der Horizontalkomponente mit der Tiefe 0,407 kg/cm2/m beträgt. Zusätzliche Messungen der Horizontalkomponente in Tiefen größer als 800 m sind notwendig, um allgemeine Schlüsse zu erlauben. Ein Beispiel wird beschrieben, in dem die Vorhersage von Druckspannungsrichtungen aufgrund einer tektonischen Analyse durch Druckmessungen überprüft wurde.
    Abstract: Résumé Déterminations de compression de terre au Canada Essais de compression avec le “strain cell” biaxial et triaxial du C. S. I. R., Afrique du Sud, sont discutés et démontrent que le “strain cell” triaxial est l'instrument le plus desirable si lorsque la roche est en bonne condition. Des compilations composants des compressions verticales determinées et des compressions horizontales moyennes des parties de l'écorce terrestre sont presentées et demontrent que des compressions verticales sont une fonction du poids de la couverture et que les compressions horizontales moyennes augmentent en général à raison de 0,407 kg/cm2/m. Des données additionelles sont réquises pour pouvoir prédire le compression horizontale moyenne au-delà de 800 m de profondeur. L'exemple presenté décrit les déterminations des compressions et donne une analyse tectonique demontrant que l'interpretation de l'histoire géologique des deformations permet une prédiction quant aux directions de la compression principale. Cependant, les incertitudes alliées, dues aux lacunes existantes dans la documentation, requièrent une épreuve par détermination des compressions.
    Notes: Summary Ground Stress Determinations in Canada Stress determinations with the biaxial (Doorstopper) and the triaxial strain cell of the C. S. I. R., South Africa, are discussed and show that the triaxial cell is the more desirable instrument if good rock conditions exist. Vertical and average horizontal stresses in Canada are similar in magnitude to those from other parts of the earth's crust and show that vertical stresses are related to weight of overburden and average horizontal stresses increase in most of the cases with 0.407 kg/cm2 per metre of depth. More data are necessary to make any prediction for the average horizontal stress beyond a depth of 800 m. Stress determinations and a tectonic analysis show that the unravelling of the geological stress-strain history allows some prediction of principal stress directions, but the attached uncertainties due to gaps in documentation require proof by stress determinations.
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    Rock mechanics and rock engineering 6 (1974), S. 123-128 
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    Rock mechanics and rock engineering 6 (1974), S. 141-166 
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    Description / Table of Contents: Zusammenfassung Bestimmung des Ursprunges seismischer Vorgänge mit Hilfe eines untertägigen Geophon-Netzwerkes Ein Verfahren zur Bestimmung seismischer Vorgänge mit Hilfe einer dreidimensionalen Seismometeranordnung wird vorgeschlagen. In dem beschriebenen Verfahren wird vorausgesetzt, daß die „beste Lage“ des Ursprunges von seismischen Vorgängen durch Minimieren der Summe der Quadrate der Restabweichungen erhalten wird. Als Restabweichung ist der Unterschied der gemessenen und berechneten Wege vom geschätzten Fokus des seismischen Vorganges zu einem der Seismometer zu verstehen. Ein System von drei nichtlinearen Gleichungen führt zur Bestimmung der gesuchten Koordinaten. Die endgültige Lösung wird mit Hilfe eines Iterationsvorganges erhalten, wobei die erste Näherungslösung quasi auf einer Methode der kleinsten Quadrate beruht. Die vorliegende Analyse führt zu einer Reihe von interessanten Punkten im Hinblick auf den Entwurf von seismischen Netzwerken. Fallen zum Beispiel alle Seismometer in einem Netzwerk auf den Mantel eines Normalkegels, dann sind die erhaltenen Angaben unzureichend, um einen seismischen Vorgang in der Nähe der Kegelspitze zu erfassen. Um eine derartige „blinde Stelle“ zu vermeiden, muß ein Netzwerk mindestens sieben sachdienlich angeordnete Seismometer enthalten. Im Fall eines Oberflächennetzwerkes werden blinde Stellen unterhalb des Netzwerkes vermieden, wenn wenigstens sechs Seismometer nicht auf einem Kegelschnitt liegen.
    Abstract: Résumé Localisation numérique des foyers d'événements sismiques au moyen des temps d'arrivée des ondes “P” Il est postulé que la meilleure estimation pour la localisation des foyers d'événements sismiques, en milieu homogène isotrope, s'obtient en rendant minimale la somme des carrées des résidus. Le résidu est défini comme étant la différence entre les chemins, calculés ou mesurés, partant du foyer présumé et aboutissant à l'un des sismomètres. Un système de trois équations non linéaires doit être résolu pour déterminer les coordonnées demandées. La solution est obtenue par itération à partir d'une première approximation établie par la méthode des moindres carrées. Lorsque tous les sismomètres d'un réseau sont situés sur la surface d'un cône circulaire droit, l'information obtenue ne permet pas de localiser les événements près du sommet. Afin d'éviter ces points “invisibles” le réseau doit posséder au moins sept géophones placés judicieusement. Un reseau situé à la surface doit contenir un minimum de six sismomètres qui ne font pas partie d'une même section conique.
    Notes: Summary Digital Location of Seismic Events by an Underground Network of Seismometers using the Arrival Times of Compressional Waves It is postulated that the ‘best’ estimate of the location of the foci of events in homogeneous isotropic ground is obtained by minimizing the sum of the squares of the residuals. The residual is defined as the difference between the computed and the measured paths from the estimated focus of one of the seismometers. A set of three non-linear equations is used to determine the required co-ordinates. The solution is obtained by a process of iteration, the first approximation for which is produced through a ‘quasi-least-squares’ method. If all seismometers of a network fall on one of the sheets of a right circular cone then the information obtained will be insufficient to allow the location of an event occurring at or in the neighbourhood of the apex to be determined. If such a ‘blind spot’ is to be avoided, the network must contain at least seven appropriately-placed geophones. If at least six seismometers of a network on the ground surface are not all on a conic section then there will be no blind spots in the half-space beneath the instruments.
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    Rock mechanics and rock engineering 6 (1974), S. 247-253 
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    Description / Table of Contents: Zusammenfassung Geotechnische Eigenschaften des Kalksteins im Niltal, Ägypten Es werden die Ergebnisse einer geotechnischen Studie des ägyptischen Kalksteins entlang des Niltales gezeigt. Diagramme, die die Zusammenhänge zwischen Druck und Porosität als auch von Druck und Raumgewicht darstellen, zeigen eine deutliche Abnahme des Druckes bei steigender Porosität und einen Anstieg bei zunehmendem Raumgewicht. Ferner wurden empirische Gleichungen, die die Abhängigkeit dieser Werte voneinander erfassen, aufgestellt.
    Abstract: Résumé Propriétés géotechniques des calcaires de la vallée du Nil, Egypte Résultats d'une étude géotechnique des calcaires Egyptiens le long de la vallée du Nil. Représentation graphique montrant les rélations entre la compression et la porosité, respectivement le poids volumetrique. Les graphiques montrant clairement la diminuition de la compression lorsque la porosité augmente; par contre on constate un croissance de la compression lorsque le poids volumetrique augmente. Des équations empiriques montrant l'interdépendence des valeurs messurées.
    Notes: Summary Geotechnical Properties of the Limestones Exposed Along the Nile Valley, Egypt The results of a geotechnical study of the Egyptian limestones exposed along the Nile Valley are represented. Graphs representing the relations between compressive strength and both porosity and volumetric weight show clearly the decrease of the compressive strength with the increase in the porosity as well as its increase with an increasing volumetric weight. Empirical equations representing the interdependence of these values have been also derived.
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    Rock mechanics and rock engineering 5 (1973), S. 1-19 
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    Description / Table of Contents: Zusammenfassung Spannungsverteilung und Bruchzonen in Firste und Ulmen von Strebbauen. Eine zweidimensionale Spannungsanalyse mittels der Finite-Element-Methode wurde benützt, um die Spannungsverteilung und die Entwicklung von Bruchbildungsvorgängen im Firstgestein am Streb einer Kohlengrube zu studieren. Bei der Ermittlung von Untergrundverschiebungen und der Anwendung einer „Inverse Approximation“-Technik wurden anstelle von Laborversuchsmessungen effektive Materialeigenschaften verwendet. Die Ausgangsspannungen im Fels um die Öffnung herum wurde ausfindig gemacht und drei Ansätze der Mohr-Coulombschen Bruchtheorie wurden zur Errechnung der entsprechenden Sicherheitsfaktoren benützt. Entsprechend den Druck- und Zugfestigkeiten wurden vier Zonen von Progressiven Brüchen festgestellt. Die wirksamen Elastizitätsmoduli für diese Zonen wurden mittels eines Verfahrens zur Bestimmung der Restelastizität errechnet. Schließlich wurden Kriterien für die Festigkeit von gebrochenem Gestein eingeführt und die Standsicherheitsfaktoren für den unmittelbaren Firstbereich errechnet. Aufgrund der Hauptspannungsrichtungen in den Zonen größter Schubspannungen wurden die Richtungen der Bruchlinien ermittelt.
    Abstract: Résumé Distribution des contraintes et zones de fracture en roche autour de la cavité d'une longue taille. Une analyse des contraintes par la méthode des éléments finis a été faite pour étudier la distribution des contraintes et le développement du processus de fracturation du toit rocheux d'une longue taille dans une mine de charbon. Les propriétés effectives du matériau furent utilisées au lieu de celles qu'on mesure par des essais de laboratoire. Elles furent obtenues à partir des enregistrements des déplacements souterrains et par une technique d'approximation inverse. Les contraintes initiales autour des cavités ont été trouvées et trois variantes de la théorie de la rupture de Mohr-Coulomb furent utilisées pour calculer les coefficients de sécurité correspondants. Quatre zones de rupture progressives furent définies d'après le rapport résistance à la compression/résistance à la traction. Le module élastique effectif de ces zones fut calculé au moyen d'une approche par résidu élastique. Finalement le critère de stabilité des roches rompues fut introduit et les facteurs de stabilité furent calculés pour la zone immédiate du toit. Les directions des lignes de fracture du toit furent prévues à partir des directions des contraintes principales dans la zone de cisaillement maximal.
    Notes: Summary Stress Distribution and Rock Fracture Zones in the Roof of Longwell Face in a Coal Mine. A two-dimensional finite element method of stress analysis was used to study the stress distribution and development of the fracturing process within the roof rock of a longwall face in a coal mine. Effective material properties were used instead of those measured in laboratory tests by employing underground displacement data and an inverse approximation technique. Initial stresses in the rock around the opening were found and three variations of the Mohr-Coulomb failure theory were used to calculate the corresponding safety factors. Four zones of progressive failure were established according to compressive-tensile stress proportions. The effective elastic moduli for these zones were calculated by means of a residual elasticity approach. Finally, the fractured rock stability criteria were introduced and the stability factors were calculated for the immediate roof area. Directions of fracture lines in the roof were found using the principal stress directions in the maximum shear stress zone.
    Type of Medium: Electronic Resource
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  • 100
    Electronic Resource
    Electronic Resource
    Springer
    Rock mechanics and rock engineering 5 (1973), S. 121-124 
    ISSN: 1434-453X
    Source: Springer Online Journal Archives 1860-2000
    Topics: Architecture, Civil Engineering, Surveying , Geosciences
    Type of Medium: Electronic Resource
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