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1992[X]
41Author    W. S. Sheldrick, C. M. ArtinRequires cookie*
 Title    Darstellung und Kristallstrukturen von Chloro-und Bromophenylantimonaten(III) [Ph2SbX2]~ und [Ph2Sb2X7]3-(X=C1, Br) Preparation and Crystal Structures of Chloro-and Brom ophenylantim onates(III) [Ph2SbX2]~ and [Ph2Sb2X 7]3-(X=C1, Br)  
 Abstract    The halophenylantim onates(III) [ P h ^ P h ^ b C l J (1), [Ph4P][Ph2SbBr2] (2), [Me3N H ]3[Ph2Sb2Cl7] (3) and [Me3N H ]3[Ph2Sb2Br7] (4) have been prepared and their structures established by single crystal X-ray diffraction. The anions [Ph2SbCl2]" and [PhjSbBrJ-display ^-trigonal bipyramidal geometries with axial halogen atoms. S b -C l [2.618(4), 2.601(4)Ä] and S b -B r distances [2.779(3), 2.794(2)Ä] are very similar to one another in the individual anions of 1 and 2. The anions [Ph2Sb2Cl7]3~ and [Ph2Sb2Br7]3~ both contain two square pyramidal coordination polyhedra which are vertex-linked to one another via S b -X -S b (X = C1, Br) an­ gles o f respectively 152.9(1) and 152.3(1)°; the latter anion displays crystallographic C2-sym-metry. trans-Sited S b -C l or S b -Br bond distances in 3 and 4 are structurally correlated to one another. 
  Reference    Z. Naturforsch. 47b, 919—924 (1992); eingegangen am 21. November 1991 
  Published    1992 
  Keywords    Chlorophenylantim onates(III), Bromophenylantimonates(III), Crystal Structure, Structural Correlation 
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 Identifier    ZNB-1992-47b-0919 
 Volume    47 
42Author    W. S. Sheldrick, J. KieferRequires cookie*
 Title    Trioktaedrische Halogenoarsenate(III) [As3X12]3 (X = Br, I) mit Ecken-und Flächenverknüpfung. Strukturkorrelation für Iodoarsenate(III) Trioctahedral H aloarsenates(III) [As3X 12]3 (X = Br, I) with Vertex and Face Sharing. Structural Correlation for Iodoarsenates(III)  
 Abstract    The haloarsenates(III) [Et3N H ]3[As3Brl2] (1) and [M e3N H ]3[As3Il2] (2) have been prepared and their structures established by X-ray analysis. Both trioctahedral anions display a novel structure in which a central A sX 6 octahedron shares tw o faces with a com m on vertex with two terminal A sX 6 octahedra. The bridging A s-X -b o n d s in the latter building units are markedly longer than the opposite terminal A s-X -b o n d s in both anions. For example, the former A s -I -bonds in [As3I12]3~ lie in the range 3 .1 5 4 (1)-3 .4 0 0 (1)A , the latter A s-I-b o n d s between 2.581(1) and 2.656(1)Ä . The distortion o f the central A sX 6 octahedron is less marked for both anions, e.g. the A s -1 distances in [As3I 12]3~ lie in this central polyhedron between 2.706(1) and 3.048(1) A. U sing the results for (2) and for other characterised anions, a structural correlation is presented for 28 rraws-sited A s -1 bond distances in iodoarsenates(III). 
  Reference    Z. Naturforsch. 47b, 1079—1084 (1992); eingegangen am 12. Februar 1992 
  Published    1992 
  Keywords    Bromoarsenates(III), Iodoarsenates(III), Crystal Structure, Structural Correlation 
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 Identifier    ZNB-1992-47b-1079 
 Volume    47 
43Author    SvenM. Jessen, H. Orst Küppers, DeanC. LuehrsRequires cookie*
 Title    Hydrogen Bonding in Acid Li-, Ni-, Tetrabutylammonium, and Ammonium Salts of Benzene-1,2,4,5-tetracarboxylic Acid (Pyromellitic Acid)  
 Abstract    Four acid salts o f pyromellitic acid (benzene-1,2,4,5-tetracarboxylic acid) have been syn­ thesized and studied by X-ray diffraction and IR spectroscopy. (1) Dilithium dihydrogen py-romellitate pentahydrate, Li2[C6H 2(COO)4H 2] • 5 H zO; monoclinic, P 2 1/m, a = 6.214(2), b = 19.647(7), c = 6.592(2)Ä , ß = 115.90(2)°, Z = 2, R = 0.068, Rw = 0.067. (2) Hexaaquanickel dihydrogen pyromellitate, [N i(H 20) 6][C6H 2(C 0 0) 4H2]; monoclinic, P2/m, a = 6.528(1), b = 9.927(2), c = 6.472(1)Ä , ß = 115.57(1)°, Z = 1, R = 0.044, /?w = 0.039. (3) Tetrabutylammoni­ um trihydrogen pyromellitate, [(C4H 9)4N][C6H-,(COO)4H 3]; monoclinic, P 2 ,/c, a = 9.719(4), b = 18.823(8), c = 15.795(5) Ä, ß = 107.42(3)°, Z = 4, R = 0.059, Rw = 0.039. (4) Diam m onium dihydrogen pyromellitate, [N H 4],[C6H ,(CO O)4H2]; monoclinic, P 2 l/c\ a = 4.7665(6), b = 11.681(3), c = 10.149(2) Ä, ß = 102'. 19(2)°, Z = 2, R = 0.045, Rw = 0.039. Com pounds 1, 2, and 3 show very short intramolecular hydrogen bonds between adjacent carboxylic groups (O -O distances 2.384(6), 2.386(5), 2 . 3 8 7 (3) respectively). Com pound 4 forms intermolecular hy­ drogen bonds (O -O distance 2.642(2) A). The different hydrogen bonding modes are also evi­ dent in the IR spectra. 
  Reference    Z. Naturforsch. 47b, 1141—1153 (1992); received October 1 1991 /March 27 1992 
  Published    1992 
  Keywords    Pyromellitates, Hydrogen Bonds, Crystal Structure, Acid Pyromellitates, IR Spectra 
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 TEI-XML for    default:Reihe_B/47/ZNB-1992-47b-1141.pdf 
 Identifier    ZNB-1992-47b-1141 
 Volume    47 
44Author    M. Athias, O. Senge, M. Aria Da, GragaH. Vicente, SeanR. Parkin, H. Äkon, Hope, KevinM. SmithRequires cookie*
 Title    Structural Investigations on Mono-and Di-Acrolein Substituted Ni(II) Porphyrins and a Ni(II) Benzochlorin. Model Compounds for Photosensitizers in Photodynamic Therapy  
 Abstract    The structures o f four N i complexes and a free base related to tetrapentanoporphyrin (TC7P) and octaethylporphyrin (OEP) have been determined by X-ray crystallograpic m eth­ ods. The N i(II) complexes exhibit considerable S4-ruffling induced by coordination hole con ­ traction due to the low spin Ni(II). The degree o f conform ational distortion is enhanced by one or tw o additional acrolein substituents at the meso positions. The steric strain im posed by interaction o f the meso substituent with the neighboring /?-pyrrole substituents leads to a sig­ nificant displacement from the mean plane o f the molecule o f the meso carbon(s) involved. Increasing non-planarity o f the macrocycles is correlated with shifts to longer wavelenghts in the absorption spectra. Ring closures o f the acrolein group to afford benzochlorin type pig­ ments results in further bathochromic shifts and a very non-planar m olecular conform ation. Long wavelength absorbing pigments such as benzochlorins are useful photosensitizers for photodynam ic therapy and thus one criterion for a good photosensitizer might be its confor­ m ational distortion. Crystal data -3. C40H46N 4 • C H 2C12, M r = 667.7, triclinic, P I , a ~ 7.776(5)Ä , b = 8.556(4)Ä, c = 14.509(8)Ä, a = 73.96(1)°, ß = 82.04(2)°, y = 82.58(2)°, V = 914.5(9)Ä 3, Z = 1, D x = 1.212 M g/m 3, (M oK a) X = 0.71069Ä , fi = 0.209 m m "1, F(000) = 356, 130 K, R = 0.082_for 2217 reflections with I > 1.5<r(I). Ni4. C ^ H ^ N i O • CH 2C12, M r = 770.4, triclinic, P I, a = 11.283(3)Ä, b = 11.800(4)Ä, c = 15.871 (7)Ä , a = 79.28(3)°, ß = 88.95(2)°, y = 62.41(1)°, V = 1838.8(11)Ä 3, Z = 2, D v = 1.391 M g/m 3, (M o K a), n = 0.715 m m '1, F(000) = 804, 130 K, R = 0.072 for 5309 reflections with I > 2.0cr(I). Ni5. C46H 28N 4N i 0 2 CH2Cl2, M r = 812.4, triclinic, P I, a = 8.959(4)Ä, b = 14.420(7)A, c = 15.471 (5)Ä , a = 102.73(4)°, ß = 101.83(4)°, y = 92.01(5)°, V = 1901,3(14)Ä 3, Z = 2, D t = 1.419 M g/m 3, (M oK a), n = 0.679 m m '1, F(000) = 836, 130 K, R = 0.059 for 4197 reflections with I > 1.75<t(I). Ni7. C43H 45N 4N i 0 2 • C H 2C12, M r = 793.5, triclinic, P I , a = 8.948(3)Ä, b= 13.855(3)Ä , c = 15.451(3)A, a = 8 2 .4 3 (2)°,£ = 78.79(2)°, y = 81.24(2)°, V = 1846.7(8)Ä 3, Z = 2, D v = 1.427 M g/m 3, (C uK a) X = 1.54178Ä ,// = 2.448 m m -', F(000) = 834, 126 K, R = 0.09 for 4039 reflections with I > 2.0er(I). Ni8. C42H4gN 4N iO , M r = 683.6, monoclinic, P 2,/n, a = 15.168(6)Ä, b = 14.796(3) k ,c = 15.983(4)Ä, ß = 97.17(3)°, V = 3552(2)Ä 3, Z = 4, Dx = 1.278 M g/m 3, (M oK a), n = 0.584 m m -1, F(000) = 1456, 130 K, R = 0.042 for 5904 reflections with I > 2.5er(I). 
  Reference    Z. Naturforsch. 47b, 1189—1202 (1992); received February 4 1992 
  Published    1992 
  Keywords    Crystal Structure, Tetrapentanoporphyrin, Ring Conform ation, Benzochlorins, P hotodynam ic Therapy 
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 Identifier    ZNB-1992-47b-1189 
 Volume    47 
45Author    M. Artina Andratschke, Klaus-Jürgen Range, Heinz Haase, Ulrich KlementRequires cookie*
 Title    Die Kristallstruktur von a-K Z nP04 The Crystal Structure o f a  
  Reference    Z. Naturforsch. 47b, 1249—1254 (1992); eingegangen am 21. Februar 1992 
  Published    1992 
  Keywords    Potassium Zinc O rthophosphate, Low-Temperature M odification, Synthesis, Crystal Structure 
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 Identifier    ZNB-1992-47b-1249 
 Volume    47 
46Author    AxelG. Udat, Rüdiger Kniep, Joachim MaierRequires cookie*
 Title    LiBa4 [Mo2 N7| * BaCl2: Dimere Anionen [Mo2 N7 ] 9 durch Kondensationsreaktion von Ba3 [MoN4] in LiCl-Schmelzen LiBa4[M o2N 7] * BaCl2: Dimeric Anions [Mo2N 7]9" by Condensation Reaction o f Ba3[M oN4] in LiCl Melts  
 Abstract    Pale yellow crystals o f LiBa4[M o2N 7] • BaCl2 (m onoclinic, P2,/m ; a = 1113.5(3), b = 605.8(1), c = 1122.7(3) pm; ß = 95.65(2)°; Z = 2) were grown from the melt (L iC l/Ba3[M oN 4], m olar ratio 3:1, Tmax = 1050 °C) by cooling (5°C/h). The crystal structure contains dimeric units [M o2N 7]9" (eclipsed conformation; N -M o -N : 173.7°; M o —N (term): 182.7(5)-186.1(8) pm; M o -N (brid 190.6(8) and 192.3(8) pm). 
  Reference    Z. Naturforsch. 47b, 1363—1366 (1992); eingegangen am 30. März 1992 
  Published    1992 
  Keywords    Nitridom olybdate(V I), Dimeric Anions, Preparation, Crystal Structure 
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 Identifier    ZNB-1992-47b-1363 
 Volume    47 
47Author    Klaus-Jürgen Range, Peter Rögner, A. Nton, M. Heyns, LindaC. PrinslooRequires cookie*
 Title    An X-Ray, Raman and IR Study of a-C sR e04, the High-Temperature Modification of Cesium Perrhenate  
 Abstract    Cesium perrhenate undergoes a reversible phase transition from the orthorhom bic room-temperature phase (/?-CsRe04, space group Pnma) to a tetragonal high-temperature phase (a -C sR e 0 4). The space group o f a -C sR e 0 4 was unam biguously confirmed by high-tempera-ture X-ray diffraction to be 14 Jamd in contrast to the earlier literature, in which space group 14 Ja (and hence, a scheelite type structure) was assumed for a -C sR e 0 4. From a data set ob­ tained at 468 K the crystal structure o f a -C sR e 0 4 (a = 5.9607(4), c = 14.446(1)Ä, Z = 4) was refined to R = 0.032, Rw = 0.029 using anisotropic displacement factors. In the vibrational spectra not all o f the predicted com ponents for /?-C sR e04 could be con­ firmed by the experiments, but for a -C sR e 0 4 very good agreement was obtained between the predicted and observed bands. The fact that v2 at ~ 3 0 0 cm "' is not observed in the IR spectra o f a -C sR e 0 4 confirms the space group 14Jamd, since, under 14,/a symmetry, this band is allowed. The structure o f a -C sR e 0 4 consists o f isolated R e 0 4 tetrahedra which are linked together by cesium atoms. The relationships between the scheelite, a -C sR e 0 4 and /?-C sR e04 structural types are discussed. 
  Reference    Z. Naturforsch. 47b, 1513—1520 (1992); received June 15 1992 
  Published    1992 
  Keywords    Cesium Perrhenate, High-Temperature M odification, Crystal Structure, Vibrational Spectra 
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 Identifier    ZNB-1992-47b-1513 
 Volume    47 
48Author    Gary Wulfsberg, Debra Jackson, William Ilsley, Shi-Qi Dou, Alarich Weiss, John GagliardiRequires cookie*
 Title    Coordination of OrfÄö-Chlorines in Copper (I) and Silver (I) 2,6-Di-and 2,4,6-Trichlorophenolates Crystal Structure of (2,4,6 -Trichlorophenolato-O, CI) bis (triphenylphosphine) silver (I)  
 Abstract    The crystal structure of (Ph 3 P) 2 AgOC 6 H 2 Cl 3 (I) is reported along with the syntheses and 35 C1 and 63 Cu NQR spectra of I and several related silver (I) and copper (I) 2,6-di-and 2,4,6-trichlorophe-nolates containing phosphines, phosphites, and pyridine as co-ligands. I crystallizes in space group P2 Jc with a= 16.692(4) Ä, b= 17.942 (4) A, c= 12.857 (3) Ä, /? = 97.60 (1)°, F = 3816.68 Ä 3 , and Z = 4. The final R (F) = 0.0475 and R (W) = 0.0396. Ag is coordinated in a trigonal planar geometry by the P atoms of the two triphenylphosphine ligands and the O atom of the chlorophenolate; Ag is then capped by one ortho-chlorine of the trichlorophenolate ligand at a distance of 3.160 (2) Ä. In the 35 C1 NQR spectrum of this compound the two orf/io-chlorines of the trichlorophenolate ligand have a large frequency difference of 1.500 MHz, indicating that one ortho-chlorine is coordinated to the silver; 35 C1 NQR spectra of related complexes are also presented and discussed. The 35 C1 NQR frequency differences of coordinated and non-coordinated orr/io-chlorines in metal chlorophenolates correlate well with the metal-chlorine distances but not with the metal-chlorine-carbon bond angles. A different correlation is found for the silver complexes of dichloroalkanes; possible reasons for this are discussed. 
  Reference    Z. Naturforsch. 47a, 75—84 (1992); received July 15 1991 
  Published    1992 
  Keywords    Nuclear quadrupole resonance, Chlorophenolates, Crystal structure, Chlorocarbons as ligands, Silver(I) complexes 
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 Identifier    ZNA-1992-47a-0075 
 Volume    47 
49Author    Masao Hashimoto, Takahiro Isono, Noriko Yomesaka, Haruo Niki, Hiroshi Kyan, Takeshi HamagawaRequires cookie*
 Title    Reorientation of the CC1 3 Group in Chloral 4-Chlorobenzyl- hemiacetal. A Pulsed 35 C1 NQR and X-ray Study  
 Abstract    The crystal structure of the title compound was determined at 291 K: monoclinic, space group C^h-P21/n, Z = 4, a = 1693.2(1), 6 = 579.3(1), c = 1232.5(1) pm, and ß = 107.21 (1)°, R = 0.0415. A sharp decrease of of Cl NQR found at T> 270 K for the CC13 group is attributed to the reorientation of the group over a potential barrier of ca. 50 kJ/mol. Intermolecular interactions between the CC13 and the neighboring atoms seem to dominate the magnitude of the potential barrier. T{~ 1 of the 35 C1 NQR of the Cl atom on the benzene ring obeyed the T 2 law well in the range 80 < T/K <270, while at T>280 K it deviated from the T 2 law. 
  Reference    Z. Naturforsch. 47a, 293—298 (1992); received July 25 1991 
  Published    1992 
  Keywords    Crystal structure, Hydrogen bond, Chlorine NQR, Spin lattice relaxation, Atom-atom potential method 
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 Identifier    ZNA-1992-47a-0293 
 Volume    47 
50Author    Dieter LentzRequires cookie*
 Title    Cycloadditionsreaktion von Trifluorm ethylisocyanid an Diphenylethin Cycloaddition Reaction o f Trifluoromethyl Isocyanide to Diphenyl Ethyne  
  Reference    Z. Naturforsch. 47b, 148—150 (1992); eingegangen am 8. Juli 1991 
  Published    1992 
  Keywords    Trifluoromethyl Isocyanide, Cycloaddition Reaction, l, 2-Diphenyl-3, 4-bis(trifluoromethylimino)-cyclo-butene Crystal Structure 
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 Identifier    ZNB-1992-47b-0148_n 
 Volume    47 
51Author    Dietrich Mootz, Dieter StäbenRequires cookie*
 Title    Clathrathydrate von Tetramethylammoniumhydroxid: Neue Phasen und Kristallstrukturen [1] C lathrate Hydrates of Tetramethylammonium Hydroxide: New Phases and Crystal Structures [1]  
 Abstract    The melting diagram o f the system tetramethylammonium hydroxide-water has been re­ investigated in the region o f 6 6 .6 7 -100 mol% H 20 , using D T A , DSC and temperature-depend-ent X-ray powder diffraction. This was done as correction and supplementation o f a previous study in the same laboratory (D. M ootz, R. Seidel, J. Incl. Phenom. 8 , 139 (1990)). The system is now considered to contain as many as eight stable hydrates, three o f them dimorphic with a low-temperature a and a high-temperature ß form. The com positions are Me4N 0 H -x H 20 with x = 2 (a and ß), 4, 4.6 (a and ß), 5 (a and ß), 6.67, 7.5, 8.75 and 10. A second 7.5-hydrate, called 7 .5 a in the previous study, is now regarded as metastable. -Structure determinations have been performed for the new phases with x = 4.6 (a), 6.67 and 8.75. The 4.6a-hydrate, transforming to 4.6ß at 32 °C, is cubic with space group Pa 3 and Z = 40 formula units per unit cell. The lattice constant is a = 21.493Ä at -1 6 0 °C. The 6.67-hydrate, melting with decom ­ position at 13 °C, is monoclinic with space group P 2 ,/w and Z = 6 . It was studied as the O-deuterated isotype with unit-cell dimensions a -11.874, b = 20.019, c = 8.272 Ä and ß = 103.84° at 3 °C. The 8.75-hydrate, melting with decom position at -3 °C, is cubic with space group 143 d, Z = 16 and a -18.38(2) Ä at -2 0 °C. The three structures, as most others o f the higher hydrates o f the system studied previously, are those o f polyhedral clathrate hydrates. For the hydrates 4 .6 a and 6.67 deviations o f the anionic, i.e. proton-deficient, new water structures from being fully four-connected are described in detail. The 8.75-hydrate is isostruc-tural with the hitherto unparalleled 9.75-hydrate o f /-butyl amine. -The phase identity and structure o f the 4.6/?-hydrate were recognized as those attributed to an erroneously assumed 5/?-phase in the previous study. 5 ß now denotes the room-temperature form o f the penta-hydrate, previously called 5 a. The present 5 a is another o f the new phases and the only one o f the system with its structure still undetermined. 
  Reference    Z. Naturforsch. 47b, 263—2 (1992); eingegangen am 8. Juli 1991 
  Published    1992 
  Keywords    Clathrate Hydrates, Crystal Structures, Hydrogen Bonding, M elting Diagram, Tetramethylammonium Hydroxide 
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 Identifier    ZNB-1992-47b-0263 
 Volume    47 
52Author    Peter Willershausen, Andrea Höfner, Jürgen Allwohn, M. Onika Pilz, W. Erner Massa, Armin BerndtRequires cookie*
 Title    Zum Einfluß von Substituenten auf o— ^--Wechselwirkung: Winkelverzerrungen in C-Borylmethylenboranen Effect of Substituents on <r-7r-Interaction: D istortion of Angles in C-Borylmethyleneboranes  
 Abstract    C -Borylmethyleneboranes with one or two O-Aryl substituents in the boryl group, 3 a and 4b, are obtained by cleavage o f B -C single bonds in the presence o f a B -C double bond. The duryl(methyl)borylmethyleneborane 7 is formed by thermal rearrangement o f the vinylborane 
  Reference    Z. Naturforsch. 47b, 983—9 (1992); eingegangen am 30. Oktober 1991/6. Februar 1992 
  Published    1992 
  Keywords    Synthesis, Crystal Structure, "B N M R Spectra, l3C N M R Spectra 
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 Identifier    ZNB-1992-47b-0983 
 Volume    47 
53Author    Thomas Strelow, Jürgen Voss, Gunadi AdiwidjajaRequires cookie*
 Title    Preparation and Structure of Ethyl 4-Bromo-2-(diphenylmethyIene)- 3-oxo-5,5-diphenyl-4-pentenoate  
  Reference    Z. Naturforsch. 47b, 1007—7 (1992); eingegangen am 23. Dezember 1991 
  Published    1992 
  Keywords    2, 4-D im ethylene-l, 3-cyclobutandione, D ouble-bond Splitting, Crystal Structure 
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 Identifier    ZNB-1992-47b-1007 
 Volume    47 
54Author    Albert Stützer, Peter Bissinger, Hubert SchmidbaurRequires cookie*
 Title    Gold Chains and Gold Pairs in the Layer Structure of 1,191 -T ris[chloro-gold(I)-dimethylphosphanylmethyl]ethane  
 Abstract    The title com pound, l,l,l-tris[chloro-gold(I)-dim ethylphosphanylm ethyl]ethane (1) has been prepared from the tripodal tertiary phosphine ligand and three equivalents o f chloro(dim ethylsulfide)gold(I) in good yield. The complex has been characterized by means o f its 'H, l3C, and 31P N M R , and l97Au M ößbauer spectra, by elemental analysis, and by a single crystal X-ray structure analysis. The crystals have a layer structure. In each o f the crystallo-graphically equivalent individual molecules two o f the gold(I) centers are associated via a short /«rramolecular A u -A u contact [3.077(2) A]. These pairs o f gold atom s are aligned in chains through mrermolecular A u --Au contacts o f similar distances [3.084(2) Ä], According to this structural principle, strings o f complex molecules are formed. The third Au(I) center o f each o f these m olecules is associated with a similar unit o f a neighbouring chain through interstrand A u --A u contacts [3.179(3) A], thus crosslinking the chains to give a layer structure. The Au • • • Au contacts are recognized to be the main structure-determining force for the conform a­ tion o f the m olecules and their packing in this solid phase. 
  Reference    Z. Naturforsch. 47b, 1261—1266 (1992); received May 11 1992 
  Published    1992 
  Keywords    G old(I) C om plexes, Phosphine Gold Complexes, Gold G old Contacts, Crystal Structure 
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 Identifier    ZNB-1992-47b-1261 
 Volume    47 
55Author    Thom As, K. Aukorat, PeterG. Jones, Reinhard SchmutzlerRequires cookie*
 Title    Das 7,8-Benzo-5-chloro-1,4,4-trimethyl-l-aza-4-azonia-6,9-dioxa-5 A5-phospha- spiro[4.4]nonanyl-Kation: Röntgenstrukturanalyse und temperaturabhängige ^ -N M R -Spektren4]nonanyl Cation: X-Ray Crystal Structure Determination and Variable 'H NMR Spectra  
 Abstract    The 7,8-Benzo-5-chloro-1,4,4-trimethyl-1 -aza-4-azonia-6,9-dioxa-5/l5-phosphaspiro[4. The 'H N M R spectrum o f the spirophosphorane 3 at room temperature indicates dynamic behaviour o f the cation. The low-temperature 'H N M R spectra o f 3 exhibit two sets o f dou­ blets for the protons o f the diastereotopic N (C H 3)2 groups. The free enthalpy o f activation for the dynamic process was determined (58.6 KJ/mole). In the reaction o f 3 with sodium tetra-phenylborate the crystalline com pound, 4, involving the non-coordinating anion, [B(C6H 5)4]~, was obtained. The X-ray crystal structure analysis o f 4 reveals the presence o f a five-membered ring, formally as a result o f intramolecular donor-acceptor interaction between the nitrogen atom o f the N (C H 3)2 group and phosphorus. The geometry at phosphorus deviates som ewhat from ideal trigonal bipyramidal. 
  Reference    Z. Naturforsch. 47b, 755 (1992); eingegangen am 9. September 1991 
  Published    1992 
  Keywords    N, N', N'-Trim ethylethylenediam ine, A zonium Salt, Donor-Acceptor-Interaction, Temperature-Dependent N M R Spectra, X-Ray Crystal Structure 
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 Identifier    ZNB-1992-47b-0755 
 Volume    47 
56Author    H. Hillebrecht, G. Thiele, P. Hollm, Ann, W. PreetzRequires cookie*
 Title    Darstellung, Charakterisierung und Normalkoordinatenanalyse von gemischtvalentem Dodekabromotriplatinat(IV,II,IV) [Pt3Br12]2~ und Kristallstruktur von (Ph3P =N =P P h3)2[Pt3Br12] * 2 CH2C12 Preparation, Characterization and Norm al Coordinate Analysis o f the Mixed Valence Dodecabrom otriplatinat(IV ,II,IV ) [Pt3Br12]2~ and Crystal Structure of (Ph3P = N = PPh3)2[Pt3Br 12] * 2 C H 2C12  
 Abstract    Heating a mixture (2:1) o f the tetrabutylammonium salts (TBA^JPtBrJ and (T B A)2[PtBr4] with trifluoroacetic acid leads to the mixed valence dodecabromotriplatinate(IV,II,IV) (T B A)2[Pt3Br12], The X-ray structure determination o f (Ph3P = N = PPh3)2[Pt3Br12] • 2C H 2C12 (triclinic, P 1, Z = 1) shows trinuclear groups with nearly D 2h symmetry for the anions, formed o f two PtBr6 octahedra and one planar PtBr4 group sharing edges. U sing the structural data a normal coordinate analysis based on a general valence force field for [Pt3Br12]2-has been per­ formed, which gives good agreement o f the calculated frequencies with the bands observed in the IR and Raman spectra. 
  Reference    Z. Naturforsch. 47b, 1099—1104 (1992); eingegangen am 10. Februar 1992 
  Published    1992 
  Keywords    Dodecabrom otriplatinate(IV, II, IV), M ixed-Valence C om pound, Synthesis, Crystal Structure, Raman Spectra 
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 Identifier    ZNB-1992-47b-1099 
 Volume    47 
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