| 1 | Author
| Siegfried Pohl | Requires cookie* | | Title
| Thioharnstoff-Derivate als Liganden in  | | | Abstract
| Eisen-Komplexen: Synthese und Kristallstrukturen von [FeI2L2l, [Fe2I4L3], (L -L) 2+|FeI4-| 2 (L = (M e2N)2CS) und |Fe2I4(C6H l0(N H -C S -N H M e)2)2| mit einer Notiz zu [FeIL3]+|Fe4S4I3L]-T hiourea D erivatives as Ligands in Iro n Complexes: Syntheses and C rystal Structures o f [F eI2L2], [ F e J 4 L3], (L -L) 2 +[FeI4-] 2 (L = (M e2N)2CS) an d [Fe2I4(C 6H 10(N H -C S -N H M e) 2)2] and a N o te on [F eIL 3]+[F e4S4I3L]~ U lrich Bierbach, W olfgang Saak, D etlev H aase u nd [FeI2L2] (1) and [Fe2I4L3] (2) are obtained from the reaction o f F e l2 and | | |
Reference
| (Z. Naturforsch. 45b, 45 [1990]; eingegangen am 26 Juli / 18. September 1989) | | |
Published
| 1990 | | |
Keywords
| Thiourea Complexes, Iron C om pounds, Synthesis, Crystal Structure | | |
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| default:Reihe_B/45/ZNB-1990-45b-0045.pdf | | | Identifier
| ZNB-1990-45b-0045 | | | Volume
| 45 | |
2 | Author
| Sabine Paashaus, R. Üdiger, K. Niep | Requires cookie* | | Title
|  | | | Abstract
| The pseudobinary systems E T e-E T eH a l (E/H al = A l/I,Br; G a/I.B r,C l; In/I,Br) contain the intermediate phases E3Te3Hal, having incongruent melting behavior (decom position at temperatures between 386 °C and 718 °C). The crystal structures (orthorhombic, Pnma) o f the isotypic ternary phases contain one-dim ensional macrom olecules, in which (Te3 3EInHal)-tetrahedra and (Te3 3G a2nTe3/3) units (staggered conform ation) are linked by com m on T e -T e -edges. The macromolecules can be described in terms o f fragments o f an ETe-crystal structure o f the GaTe structural type. In this way, halogen acts as an oxidizing agent which then satu rates the free valence at the Em positions. Larger fragments o f a respective ETe-crystal struc ture are expected to be present in the crystal structure o f InTeC lv (x ~ 0.16) which is an inter mediate phase (m.p. = 418 °C; incongruent) in the quasibinary system In T e-In T eC l. | | |
Reference
| Z. Naturforsch. 45b, 667—6 (1990); eingegangen am 6. N ovem ber 1989 | | |
Published
| 1990 | | |
Keywords
| Phase Relations, Crystal Structure, Mixed Valency Phases | | |
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| default:Reihe_B/45/ZNB-1990-45b-0667.pdf | | | Identifier
| ZNB-1990-45b-0667 | | | Volume
| 45 | |
4 | Author
| R. J. Schubert, K.-J Range | Requires cookie* | | Title
| T etra-w-butylammoniumdicyanoaurat(I), (/j-C4H9)4N Au(CN)2 Tetra-/7-butylammonium Dicyanoaurate(I), (az-C4H9)4N A u(C N)2  | | | Abstract
| Single crystals o f (/j-C4H9)4N A u (C N) 2 were obtained by crystallization using the tempera ture decreasing method in a newly developed com puter-controlled apparatus. The colourless crystals aor e monoclinic, space group A 2/n, with a = 20.216(2) Ä, b = 13.130(1) A, c = 9.328(1) A, and ß = 109.69(1)°. The measured density is 1.45 g/cm 3, which agrees with the cal culated density o f 1.40 g/cm 3 for Z = 4. The structure was solved by Direct M ethods using 674 independent reflections and refined by least-squares procedures to conventional and weighted R factors o f 0.068 and 0.058, respectively. The nearly linear [A u(C N)2]~-anions form pseudo-hexagonal layers, in which they are arranged parallel to each other. The shortest A u -A u dis tance is 8.05 A. The stacking o f the layers produces pseudo-trigonal channels, occupied by the cations. The tetra-«-butylammonium cation has four ordered trans chains with idealized D 2d symmetry (42 m). | | |
Reference
| Z. Naturforsch. 45b, 1118—1122 (1990); eingegangen am 12. Februar 1990 | | |
Published
| 1990 | | |
Keywords
| Tetra-«-butylammonium Dicyanoaurate(I), Crystal Growth, Crystal Structure | | |
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| default:Reihe_B/45/ZNB-1990-45b-1118.pdf | | | Identifier
| ZNB-1990-45b-1118 | | | Volume
| 45 | |
5 | Author
| Michael Schäfer, Jürgen Pebler, Beatrice Borgsen, Frank Weller, K. Urt Dehnicke | Requires cookie* | | Title
| 21Sb-Mössbauer-spektroskopische und strukturchemische Untersuchungen an Kronenetherkomplexen SbX3(15-Krone-5) mit X = F, Cl, Br, I. Eine Analyse der Orbitalbesetzungszahlen 12lSb-M össbauer-Spectroscopic and Structural Investigations on Crown Ether Complexes SbX3(15-Crown-5) with X = F, Cl, Br, I. A Population Analysis Crown Ether C om plexes SbX3(15-crown-5)  | | | Abstract
| The crown ether complexes SbX3(15-crown-5) with X = F, Cl, Br, and I have been prepared by reactions o f 15-crown-5 with the corresponding antimony trihalides in acetonitrile solu tions. The com pounds were characterized by IR spectroscopy as well as by l21Sb-M össbauer spectroscopy. A m ethod o f orbital population analysis utilizing both M össbauer isomer shifts and quadrupole coupling has been developed for Sb(III) antimony halides and their crown ether com plexes. SbF 3(l 5-crown-5) was also characterized by an X-ray structure determination: Space group P 2 ,/«, Z = 4, 3628 observed unique reflexions, R = 0.032. Lattice dim ensions at 19 °C: a = 891.54(6), b = 1277.26(6), c = 1277.66(7) pm, ß = 95.029(4)3. The com plex has a molecular structure in which the antimony atom is surrounded by three F-atom s with mean bond lengths o f 192.4 pm and by the five oxygen atom s o f the crown ether molecule with mean bond lengths o f 293.9 pm. | | |
Reference
| Z. Naturforsch. 45b, 1243—1250 (1990); eingegangen am 5. März/9. Mai 1990 | | |
Published
| 1990 | | |
Keywords
| Syntheses, IR Spectra, 12lSb-M össbauer Spectra, Crystal Structure | | |
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| default:Reihe_B/45/ZNB-1990-45b-1243.pdf | | | Identifier
| ZNB-1990-45b-1243 | | | Volume
| 45 | |
7 | Author
| Siegfried Pohl, W. Olfgang Saak, R. Ain, Er Lotz, Detlev Haase | Requires cookie* | | Title
| Zur Existenz schwacher Wechselwirkungen zwischen Sb(III) und Phenylgruppen: Sb2 Br6 (SPPh3)2, Sb2 I6 (SePPh3 ) 2 * 2 CH2 C12, Sb4 Br12(SPM e2 Ph) 4 und (Ph4 P)2 Sb2 Br8 * CH3CN  | | | Abstract
| On the Existence o f W eak In teractio n s between Sb(III) and Phenyl G roups: Sb2Br6(SP Ph3)2, Sb2I6(SeP Ph3)2 • 2 C H 2C12, Sb4B r12(SPM e2Ph)4 and (Ph4P)2Sb2Br8 • C H 3CN The com pounds Sb2Br6(SPPh3)2 (1), Sb2I6(SePPh3)2-2 C H 2C12 (2), and Sb4Br12(SPMe2Ph)4 | | |
Reference
| Z. Naturforsch. 45b, 1355 (1990); eingegangen am 6. März 1990 | | |
Published
| 1990 | | |
Keywords
| Sb(III)-Phenyl Interaction, Antimony Trihalides, Crystal Structure | | |
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| default:Reihe_B/45/ZNB-1990-45b-1355.pdf | | | Identifier
| ZNB-1990-45b-1355 | | | Volume
| 45 | |
8 | Author
| H. Einz, Jürgen Beister, K. Arl Syassen, Jürgen Klein | Requires cookie* | | Title
| Phase Transition of N a3As under Pressure  | | | Abstract
| We have investigated the high pressure behaviour of N a3As by powder X-ray diffraction. At 3.6 G Pa the material undergoes a reversible phase transition from the N a3As structure (P 6 3/ mmc, a = 487.4(8) pm, c = 851.5(20) pm, Z = 2, at 3.6 G Pa) to the Li3Bi structure type (Fm 3m , a = 683.5(15) pm, Z = 4, at 3.6 GaP). The equation of states is given for the pressure range up to 26 GPa. Results are discussed with respect to structural properties of related A3BV-compounds. | | |
Reference
| Z. Naturforsch. 45b, 1388—1392 (1990); received M arch 7 1990 | | |
Published
| 1990 | | |
Keywords
| High Pressure, Crystal Structure, Phase Transition | | |
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| default:Reihe_B/45/ZNB-1990-45b-1388.pdf | | | Identifier
| ZNB-1990-45b-1388 | | | Volume
| 45 | |
10 | Author
| Rolf Minkwitz, AndreasK. Ornath, Renate Krause, Hans Preut | Requires cookie* | | Title
| Über die Darstellung der  | | | Abstract
| (Chlorthio)sulfoniumsalze [(CH3)2SSSC l]+SbF6-, I(CH3)2SSCI]+SbF6-und des isomeren [(CH3)(C I)S -S C H 3]+SbCl6-[ l ] On the Preparation o f the (Chlorothio)sulfonium Salts [(CH3):SSSCl]+SbF6-, [(CH3),SSCl]+SbF6-and the Isomer [(CH3)(C l)S -S C H 3]+SbCl6-[1] The preparation o f the stable com pounds [(CH3)2SSCl]+SbF6~ and [(CH3)2SSSCl]+SbF6~ from [(CH3)2SH ]+SbF6~ and SC12 and S2C12, resp., is reported. The isomer [(CH3)(C l)S -S C H 3]+SbCl6" is prepared from [SCl3]+SbCl6~ and CH,SH in the molar ratio 1:2. For this salt a crystal structure analysis was carried out (Space group P 2,2,2,, Z = 4,a = 750.1(4), b = 1133.7(3), c= 1614.8(3) pm). | | |
Reference
| Z. Naturforsch. 45b, 1637—7 (1990); eingegangen am 4. April 1990 | | |
Published
| 1990 | | |
Keywords
| (Chlorothio)sulfonium Salts, Preparation, Crystal Structure | | |
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| default:Reihe_B/45/ZNB-1990-45b-1637.pdf | | | Identifier
| ZNB-1990-45b-1637 | | | Volume
| 45 | |
11 | Author
| Hans-W Alter, Swidersky, K. Urt Dehnicke | Requires cookie* | | Title
|  | | | Abstract
| [OsC14(C H 3C N)2] • 1/2C H 3CN has been pre pared by the reaction o f OsCl5 with acetonitrile in a slow reaction at room temperature, forming red, moisture sensitive crystals. The com pound was characterized by IR spectroscopy as well as by an X-ray structure determination. Space group Pnma, Z = 4, 1281 observed unique reflexions, R = 0.031. Lattice dimensions at 20 °C: a = 1032.5(5), b = 1356.0(7), c = 975.9(5) pm. The complex has a molecular structure, in which the osmium atom is octahedrally coordinated by four chlorine atoms and by two N -atom s o f the cis-coordinated acetonitrile molecules. The included C H 3C N m olecules are disordered in two posi tions. | | |
Reference
| Z. Naturforsch. 45b, 1210—1212 (1990); eingegangen am 26. Februar 1990 | | |
Published
| 1990 | | |
Keywords
| Acetonitrile Solvate o f Osmium Tetrachloride, Synthesis, IR Spectra, Crystal Structure | | |
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| default:Reihe_B/45/ZNB-1990-45b-1210_n.pdf | | | Identifier
| ZNB-1990-45b-1210_n | | | Volume
| 45 | |
12 | Author
| W. Preetz, P. Hollmann, G. Thiele, H. Hillebrecht | Requires cookie* | | Title
| Darstellung, Reaktionen und spektroskopische Charakterisierung von |O s2X8|2", X = Cl, Br, I, und Kristallstruktur von (P P N )2|O s2I8| * 2 CH2C12 Preparation, Reactions and Spectroscopic Characterization of [Os2X 8]2-, X = Cl, Br, I, and Crystal Structure o f (PPN )2[Os2I8] ■ 2 C H 2C12  | | | Abstract
| The triply bonded octahalogenodiosm ate(III) anions [Os2X 8]2-, previously known with X = Cl, Br, have now been extended to include the iodide with two staggered OsI4 units. This com pound was prepared by treating [Os2Cl8]2' with N al at room temperature in acetone solu tion. The structure determination by X-ray diffractometry on single crystals o f (P P N)2[Os2I8] • 2 C H 2C12, reveals crystallization in the m onoclinic system, space group P 2 ,/c with Z = 4. The O s~O s triple bond is with 2.212(1) Ä the longest within the three octahalogenodiosm ates(III). The Raman spectra show v(OsOs) at 285, [Os2Cl8]2-; at 287, [Os2Br8]2_ and for the iodo compound at 270.1 cm ' 1 with up to three overtones. The spectro scopic constants are calculated to be a», = 270.9 cm -1; X u = -0 .5 0 cm "1. The 10 K UV-VIS spectra o f solid [(/7-C4H9)4N ]2[Os2X 8] exhibit ö~n* transitions with maxima at 723, 690 and 643 nm, superimposed by vibrational fine structures with long progressions o f 195, 211 and 183 cm -1 for X = Cl, Br, I, respectively. Oxidation o f [Os2X 8]2~, X = Cl, Br with the corresponding halogen leads to the cleavage o f the O s -O s bond, and the dekahalogenodiosm ates(IV), [Os2X l0]2-, are formed. | | |
Reference
| Z. Naturforsch. 45b, 1416—1424 (1990); eingegangen am 12. März 1990 | | |
Published
| 1990 | | |
Keywords
| O ctaiododiosm ate(III), Synthesis, Crystal Structure, Raman, UV-VIS Spectra | | |
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| default:Reihe_B/45/ZNB-1990-45b-1416.pdf | | | Identifier
| ZNB-1990-45b-1416 | | | Volume
| 45 | |
13 | Author
| Rolf Minkwitz, Volker Gerhard, Hans Preut | Requires cookie* | | Title
| Halogen-Pseudohalogen-Austausch an Bromsulfoniumsalzen. Dimethylthiocyansulfonium-und Dimethylselenocyansulfonium- Hexafluoroarsenat [1] Halide-Pseudohalide Exchange with Bromosulfonium Salts. Dimethylthiocyanosulfonium-and Dim ethylselenocyanosulfonium-Hexafluoroarsenate [1]  | | | Abstract
| The preparation and spectroscopic characterization o f the sulfonium salts (C H 3)-,SSCN+A sF 6~, (C H 3)2SSeCN + A sF 6~ and (C H 3),S N C O +A sF ^ is reported. The com pounds are obtained via halide-pseudohalide exchange reactions with (C H 3)2SBr+A sF 6~ and the corresponding silver pseudohalide. In addition the crystal structure o f (C H 3)2SS C N +A sF 6~ was determined. The salt crystallizes in the orthorhombic space group Pbca with a = 1048.4(9) pm, b -1290.2(6) pm, c = 1405.1(12) pm and Z = 8. | | |
Reference
| Z. Naturforsch. 45b, 1625—1631 (1990); eingegangen am 19. März 1990 | | |
Published
| 1990 | | |
Keywords
| Raman Spectra, N M R Spectra, Crystal Structure, Bromosulfonium Salts, Hexafluoroarsenate | | |
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| default:Reihe_B/45/ZNB-1990-45b-1625.pdf | | | Identifier
| ZNB-1990-45b-1625 | | | Volume
| 45 | |
14 | Author
| R. Castro, M.L D Urán, J.A G Arcía-Vázquez, J. Romero, A. Sousa, A. Castiñeiras, W. Hiller, J. Strähle | Requires cookie* | | Title
| Electrochemical Syntheses of Pyrimidine-2-thiolato Complexes of Nickel(II) Crystal and Molecular Structure of 2,2 -Bipyridine-bis(pyrimidine-2-thiolato)nickel(II) Monohydrate+  | | | Abstract
| The electrochemical oxidation o f nickel in pyrimidine-2-thione (pym tH) solution yields a com pound o f formula [Ni(pymt)-,]. When pyridine (py), 2,2'-bipyridine (bipy) or 1,10-phenan throline (phen) are added to the solution phase, the product obtained is a complex [Ni(pym t)2py2] or [Ni(pym t)2L] (L = bipy or phen). The crystal structure o f [Ni(pym t)2bipy] • H 20 is monoclinic, space group P 2,/c, with a = 726.6(2), b = 1586.2(2), c = | | |
Reference
| Z. Naturforsch. 45b, 1632—2 (1990); received May 14 1990 | | |
Published
| 1990 | | |
Keywords
| Crystal Structure, Nickel(II) Complexes, Pyrimidine-2-thione, Electrochemical Syntheses | | |
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| default:Reihe_B/45/ZNB-1990-45b-1632.pdf | | | Identifier
| ZNB-1990-45b-1632 | | | Volume
| 45 | |
15 | Author
| Á. Vez, C. Rés, M. Isternas, O. Argarita, E. Tero, R. Nrique, U. Lr Ic, Ller | Requires cookie* | | Title
| Syntheses and Electrochemical Properties of |C5M e5Ru]+ Complexes with Polycyclic Arenes. Crystal Structure of |(C5M e5)Ru( //'-chrysene)] PF6 * 0.5 M e2CO  | | | Abstract
| M ononuclear and binuclear com pounds [(C5M e5)Ru(//6-arene)PF6 and [(C5M e5R u)2(//6,/76-arene)](PF6)-, were prepared by reacting (C5M e5)RuCl2, the arene and silver acetate with subsequent addition o f N H 4PF6, for arene = phenanthrene, chrysene, tripheny-lene, fluorene, bifluorene. biphenyl and 4,4'-biphenyl. The mononuclear com pounds were also prepared for arene = naphthalene, anthracene, pyrene and coronene. The 'H and l3C N M R spectra are reported. By cyclic voltammetry all compounds show a first reduction potential that is considerably more positive compared with the free arene. The first cathodic wave is irreversible for a wide range o f scanning speeds. However, the mononuclear coronene and the binuclear phenanthrene com pounds show reversibility. The crystal structure o f [(CsM es)Ru(/76-chrysene)]PF6-0.5 Me^CO was determined by X-ray diffraction (3797 unique observed reflexions, R = 0.098). Crystal data: a = 1689.2(2), b = 1524.0(8), c = 2263.5(3) pm, ß = 107.22(1) , space group P 2,/«, Z = 8. Crystallographically independent, two cations [(C5M e5)Ru(>76-chrysene)]+ and two anions PF6~ are present, but their structures are essentially equal. The [C5M esRu]+ unit is bonded to one o f the terminal benzene rings o f the chrysene in a sandwich manner; the rings bonded to Ru are nearly coplanar. The PF6~ ions and the C5M e5 rings exhibit strong thermal vibrations. | | |
Reference
| Z. Naturforsch. 45b, 658 (1990); received November 18 1989 | | |
Published
| 1990 | | |
Keywords
| Pentamethylcyclopentadienyl-arene-ruthenium Hexafluorophosphates Synthesis, N M R Spectra, Reduction Potentials, Crystal Structure | | |
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| default:Reihe_B/45/ZNB-1990-45b-0658.pdf | | | Identifier
| ZNB-1990-45b-0658 | | | Volume
| 45 | |
17 | Author
| Wolfgang Hönle, Leonhard Walz, Hans Georg, Von Schnering | Requires cookie* | | Title
| Bildung und Kristallstruktur von Ethylendiammonium-hydridotrioxophosphat(2 -) [^ N C F ^ C t^ N F y iP H C ^ p Form ation and Crystal Structure of Ethylenediammonium H ydridotrioxophosphate(2-) [HjNCFUCHoNI-ytPHO,]  | | | Abstract
| Ethylenediammonium H yd ridotrioxophosphate(2-) [HjNCH-jCH-jNHjJITHO:,] is formed by slow oxidation o f white phosphorus by oxygen in ethylendiamine. It crystallizes in the space group Pbca with a = 1570.6(4) pm, b = 676.9(5) pm, c = 1267.8(4) pm and Z = 8 formula units in the unit cell. The structure is built from ethylenediammonium dications and tetra hedral phosphonate dianions, linked by O -H -N bonds (d(O--N) = 275.8 pm). The bond distances are d (P -O) = 151.8 pm, d (P -H) = 136.9 pm, d (N -C) = 148.3 pm and d (C -C) = 151.0 pm. | | |
Reference
| Z. Naturforsch. 45b, 1251—1254 (1990); eingegangen am 13. Februar 1990 | | |
Published
| 1990 | | |
Keywords
| Ethylenediammonium H ydridotrioxophosphate(2-), Crystal Structure, Formation, Phosphonate Dianion, Ethylenediammonium Dication | | |
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| default:Reihe_B/45/ZNB-1990-45b-1251.pdf | | | Identifier
| ZNB-1990-45b-1251 | | | Volume
| 45 | |
18 | Author
| Roswitha Schmidt, Brigitte Eisenmann, Rüdiger Kniep, Jürgen Ensling, Philip Gütlich, Reinhard Seidel | Requires cookie* | | Title
| Zn2(Z n,_;tFe,)Fel" (P 0 4)3 * 2 H 20 : Darstellung, Kristallstruktur und Mößbauer-Untersuchung Zn2(Z n]_ vF ex .)FeIII(P 0 4)3 -2H 20 : Preparation, Crystal Structure and M össbauer Investigation  | | | Abstract
| Single crystals o f the mixed valency phase Zn2(Z n ,_vF eY)F ein(P0 4)3-2 H20 were grown by hydrothermal treatment o f phosphophyllite (Zn2F e (P 0 4)2-4 H 20) at 160 C in 1 M H3P 0 4. The crystal structure (tricl., P i; a = 641.5(4) pm, b = 914.4(4) pm, c = 983.4(4) pm, a = 70.79(5)°, ß = 78.32(5)°, y = 73.69(5)°; Z = 2) contains P 0 4 tetrahedra, connected via vertices shared with coordination polyhedra o f the metal ions. Cation coordination polyhedra (Fem(Op)5Ow octahedra, (Z n|_vFeY)(O p)5Ow octahedra and Zn(Op)5 trigonal bipyramids) are connected to centrosymmetrical six-membered chains by sharing com m on O -edges. These short chains are interconnected by com m on vertices o f Zn(Op)4 tetrahedra to form infinitive ribbons o f cation coordination polyhedra. The x-values observed for the substitutional posi tion (Zn,_A .Fev) varied from .x: = 0.5 (single crystal determ ination) to "y = 1 (Mössbauer investi gation). The M össbauer parameters are consistent with high-spin iron in a slightly distorted octahedral environment and valence states (II) and (III). | | |
Reference
| Z. Naturforsch. 45b, 1255—1261 (1990); eingegangen am 19. April 1990 | | |
Published
| 1990 | | |
Keywords
| Orthophosphate Zn/Fe, Mixed Valency C om pound, Hydrothermal Growth, Crystal Structure, Mössbauer Parameters | | |
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| default:Reihe_B/45/ZNB-1990-45b-1255.pdf | | | Identifier
| ZNB-1990-45b-1255 | | | Volume
| 45 | |
|