| | 2 | Author
| Brigitte Eisenmann, Roland Zagler | Requires cookie* | | | Title
| Selenoantimonate  | | | | Abstract
| (V): Darstellung und Struktur von Na3SbSe4, K3SbSe4 und [Ba(en)4]2[Ba(en)3](SbSe4)2 Selenoantim onates(V): Preparation and Crystal Structure of N a3SbSe4, K3SbSe4 and [Ba(en)4]2[Ba(en)3](SbSe4) 2 The crystal structures of N a 3SbSe4, K3SbSe4 and [B a(en)4]2[B a(en)3](SbSe4)2 contain isolated tetrahedral anions SbSe43 -, which are the first exam ples o f selenoantim onates(V). Na3SbSe4 | | | |
Reference
| Z. Naturforsch. 44b, 249 (1989); eingegangen am 24. Oktober 1988 | | | |
Published
| 1989 | | | |
Keywords
| Selenoantim onates, Preparation, Crystal Structure | | | |
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| default:Reihe_B/44/ZNB-1989-44b-0249.pdf | | | | Identifier
| ZNB-1989-44b-0249 | | | | Volume
| 44 | |
| 3 | Author
| HansG. Eorg Stammler, Johannes Weiss | Requires cookie* | | | Title
| Synthese | | | | Abstract
| und Kristallstruktur von (S4N3)2Se2Cl10, (S4N3)2Se2CI6 und [(S4N3)SeCl5]n Synthesis and Crystal Structure of (S4N3)2Se2C l10, (S4N3)2Se2Cl6, and [(S4N 3)SeCl5]" (S4N 3)2S e2C l10, (S4N 3)2Se2Clft and [(S4N 3)SeC l5]" are formed by the reaction o f S4N 4, Se2Cl2, and SO C l2. The structures o f the three com pounds where determ ined by X-ray diffraction. The yellow crystals o f (S4N 3)2Se2C l10 are monoclinic, space group P 2,/a, a = 817.5(2) pm , b = 1790.4(5) pm, c = 843.1(6) pm, ß = 104.31(4)°, Z = 2. The Se2C l102~ anion consists o f 2 Cl-bridged distorted octahedra. (S4N 3)2Se2Cl6 forms red m onoclinic crystals, space group P2,/c, a = 1036.5(3) pm , b = 1376.5(5) pm , c = 1400.4(4) pm ,/3 = 100.65(2)°, Z = 4. In the Se2Cl62" anion the Se atoms have a square planar environm ent. The yellow crystals o f (S4N 3)SeC l5 are orthorhom bic, space group P 2 12 12 1, a = 734.2(3) pm , b — 989.4(4) pm , c = 1627.4(6) pm , Z = 4. In the SeC l5_ anion the Se atom has an octahedral environm ent o f chlorine atom s, thus forming a polym eric structure. | | | |
Reference
| Z. Naturforsch. 44b, 1483 (1989); eingegangen am 5. Mai 1989 | | | |
Published
| 1989 | | | |
Keywords
| Thiotrithiazyl-chloroselenates, Synthesis, Crystal Structure | | | |
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| default:Reihe_B/44/ZNB-1989-44b-1483.pdf | | | | Identifier
| ZNB-1989-44b-1483 | | | | Volume
| 44 | |
| 4 | Author
| Dieter Schmidt-Bäse, Uwe Klingebiel | Requires cookie* | | | Title
| Von 1,5-funktionelIen Trisiloxanen zu (SiO)4-, [Si(OSiN)2Si]-und [0 (S i0 S i)2N]-Ringen From 1,5-Functional Trisiloxanes to (SiO)4-, [Si(OSiN)2Si]-, and [0(Si0Si)2N]-Rings | | | | Abstract
| C om pounds of the general formula (CM e3)2Si(R)O H , (R = Cl, O H . N H :) react with «-C 4H,,Li or Na to give the alkali silanolates 1—5 .1 —5 serve as starting materials in the reactionsw ithchlorosilanes for the synthesis o f siloxanes (6—12). Ring closure reactions of dilithiated 9 ,1 1 , and 12 occur with SiCl4 (13) and C l,SiM e, (15, 16). 13 contains an (SiO)4. 15 an Si(O SiN),Si. and 16 an 0 (S i0 S i) ,N eight-m em bered ring. Hydrolysis o f 13 leads to the formation o f the hydroxy-substituted eight-m em bered ring 14. The crystal structures of (C M e3),S i(O H) —O —SiM e, —Ö —(H ,N)S i(C M e3), (11) and M e,Si[O Si(C M e3),N H ],S iM e, (15) are reported and discussed. | | | |
Reference
| Z. Naturforsch. 44b, 395 (1989); eingegangen am 16. D ezem ber 1988/23. Januar 1989 | | | |
Published
| 1989 | | | |
Keywords
| Silanolates, Siloxanes, Am inosiloxanol Eight-M embered Rings, Crystal Structure | | | |
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| default:Reihe_B/44/ZNB-1989-44b-0395.pdf | | | | Identifier
| ZNB-1989-44b-0395 | | | | Volume
| 44 | |
| 5 | Author
| Gabriele Rebera, Jürgen Riede3, Nils Wibergb, Gerhard Wagnerb, Gerhard Müller | Requires cookie* | | | Title
| Silaheterocyclen: Molekülstruktur eines 3-Oxa-2 | | | | Abstract
| ,4,6,7-tetrasiIabicycIo[3.1.1]heptans Silaheterocycles: Molecular Structure of a 3-Oxa-2,4,6,7-tetrasilabicyclo[3.1.l]heptane A ccording to an X-ray structure analysis l,5-b is(di-rm -butylrnethylsilyl)-2,2.4.4,6.6,7,7-octa-m ethyl-3-oxa-2,4,6,7-tetrasilabicyclo[3.1. l]heptane (1) is a rigid bicyclic m olecule consisting o f a 1,3-disilacyclobutane ring whose 2,4 positions are bridged by a M e:Si —O —SiM e: fragment. The four-m em bered ring is non-planar with a dihedral angle o f 33.8° along the C —C axis. The intraring valence angles at carbon are significantly smaller than those at silicon leading to a transannular Si • • • Si distance o f only 2.558(1) Ä (triclinic, space group P I with a = 9.125(2), b = 12.668(2), c = 15.499(3) Ä , a = 101.25(1), ß = 87.87(1), y = 96.88(1)°. V = 1744.4 Ä 3, R (w R) = 0 .0 4 4 (0 .0 5 1) for 316 refined parameters and 5156 observables). | | | |
Reference
| Z. Naturforsch. 44b, 796—799 (1989); eingegangen am 17. März 1989 | | | |
Published
| 1989 | | | |
Keywords
| Crystal Structure Cyclic D isiloxane, 1, 3-Disilacyclobutane | | | |
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| default:Reihe_B/44/ZNB-1989-44b-0796.pdf | | | | Identifier
| ZNB-1989-44b-0796 | | | | Volume
| 44 | |
| 7 | Author
| Hans Hartl, Irene Brüdgam | Requires cookie* | | | Title
| Synthese und Strukturuntersuchungen von Iodocupraten(I) | | | | Abstract
| X . [Co(cp)2]2[CuI3] und [Co(cp)2][Cu2I3] = l/9{[Co(cp)2]9[Cu6Iu Ji [(Cn6I8)2]} [ 1 ] Syntheses and Structure Analyses of Iodocuprates(I) X. [Co(cp)2]2[CuI3] and [Co(cp)2][Cu2I3] = l/9{[Co(cp)2]9[Cu6I n]2[(Cu6I8)2]} [1] Bis-(cobalticenium)triiodocuprate(I), [ C o (c p) 2]2[ C u I , ] s (l) and cobalticenium-triiodo-dicuprate(I), [Co(cp)2][Cu2I,]=l/9{[Co(cp)2]9[Cu6I u ] 2 [(Cu6I8)2]}==(2) were obtained by reacting [Co(cp)2]I with Cul in acetone 1 and acetonitrile 2, respectively. The crystal structure of 1 exists of cobalticenium cations and mononuclear planar anions C u l,2". The crystal structure of 2 contains cobalticenium cations and two different types of iodocuprate(I) anions: an isolated hexa-nuclear ion Cu6I n5-built up by 6 edge sharing C ul4 tetrahedra and polymeric layers 2 [CuftI8]2-. In the latter anion Cu6I n components are two-dimensionally connected via 3 common edges and Cu(I) ions are distributed over two kinds of tetrahedral sites. | | | |
Reference
| Z. Naturforsch. 44b, 936—941 (1989); eingegangen am 10. März/28. April 1989 | | | |
Published
| 1989 | | | |
Keywords
| Iodocuprate(I), Cobalticenium Cation, Crystal Structure, Synthesis | | | |
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| default:Reihe_B/44/ZNB-1989-44b-0936.pdf | | | | Identifier
| ZNB-1989-44b-0936 | | | | Volume
| 44 | |
| 8 | Author
| Tetraphenylphosphonium Hexachlorodizincate, Hexachlorodicadmate, JörgH. Ubertus, Wilhelm, Ulrich Müller | Requires cookie* | | | Title
| Tetraphenylphosphonium-hexachlorodizinkat und -hexachlorodicadmat, (PPh4)2Zn2CI6 und (PPh4)2Cd2Cl6 | | | | Abstract
| The title com pounds were obtained by the reactions of PPh4Cl. HC1 and ZnS or CdS in C H 2C12. Their crystal structures were determ ined by X-ray diffraction. (PPh4),Z n,C l6: a = 973.6(1), b = 982.6(2), c = 1296.7(3) pm, a = 107.93(2), ß = 94.50(2), y = 100.91(2)°, R = 0.036 for 2237 unique observed reflexions. (PPh4)2Cd2Cl6: a = 977.1(2), b = 997.5(3). c = 1306.6(3) pm. a = 108.81(2), ß = 94.18(2), y = 100.24(2)°, R = 0.050 for 1921 reflexions. Both com pounds are isotypic in the triclinic space group P I and consist of PPh4 ions and dimeric, centrosymm etric M2Clg-ions in which the tetrahedrally coordinated metal atoms are linked via chloro bridges. Synthese von (PPh4)2Zn2Cl6 und (PPh4)2Cd2CI6 | | | |
Reference
| Z. Naturforsch. 44b, 1037—1040 (1989); eingegangen am 26. April 1989 | | | |
Published
| 1989 | | | |
Keywords
| H exachlorodizincate, H exachlorodicadm ate, Synthesis, Crystal Structure | | | |
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| default:Reihe_B/44/ZNB-1989-44b-1037.pdf | | | | Identifier
| ZNB-1989-44b-1037 | | | | Volume
| 44 | |
| 9 | Author
| Z. Naturforsch | Requires cookie* | | | Title
| Stereoselective Synthesis o f a Phenylphosphido-Bridged Dimetallic Complex: Crystal and Molecular Structure of [(R * ,R * ),(R * )]-(± )-[(i/5-C5H 5){l,2 -C 6H 4(PM ePh)2}FePH Ph{Cr(CO )5}]- 2 H20 * 0.5 CH2C12 * 0.5 C4H 80 | | | | Abstract
| D eprotonation of (R * ,R *)-(±)-[(^ -C 5H 5){l,2-C 6H 4(PM ePh)2}Fe(PH 2Ph)]PF6 with «-BuLi in tetrahydrofuran at 20 °C, followed by treatm ent of the interm ediate phenylphosphido-iron complex with [Cr(CO)5(NM e3)] produces a separable 3 :2 mixture of the diastereom ers [(R* ,R*),(R*)]-and [(R*,R*),(S*)]-(±)-'[(/75-C5H 5){ l,2 -C 6H 4(PM ePh)2} F e -P H (P h) -*■ C r(C O)5], The m ajor com po nent of the mixture crystallizes from dichlorom ethane-tetrahydrofuran in the atm osphere as the mixed solvate [(R *,R *),(R *)]-(±)-[(/75-C5H 5){ l,2 -C 6H 4(PM ePh)2} F e -P H (P h) -* C r(C O)5]-2 H 20 0.5C H iC l2-0.5 C 4H 80 in the triclinic space group P I with two formula units in the unit cell; the lattice constants are a = 10.933(2) Ä , b = 13.161(4) Ä ,c = 15.249(3) A, a = 76.83(1)°, 0 = 75.62(3)°, and y = 79.31(1)°. In the structure, the pyram idal phenylphosphido group bridges the dissimilar metals via relatively long m etal-phosphorus bonds, v iz., Fe —P = 2.285(5) Ä, C r—P = 2.511(4) Ä. | | | |
Reference
| Z. Naturforsch. 44b, 1041 (1989); received M arch 29 1989 | | | |
Published
| 1989 | | | |
Keywords
| Stereoselective Synthesis, Dimetallic, Bridging Phenylphosphido, Crystal Structure | | | |
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| default:Reihe_B/44/ZNB-1989-44b-1041.pdf | | | | Identifier
| ZNB-1989-44b-1041 | | | | Volume
| 44 | |
| 10 | Author
| Reiner Figge, Claus Friebel, U. Te Patt-Siebel, Ulrich Müller, Kurt Dehnicke | Requires cookie* | | | Title
| Nitridokomplexe von Molybdän(V); Synthesen, IR-und EPR-Spektren. Die Kristallstruktur von [Na(15-Krone-5)Na(THF)]2[MoNCI3 THF]4-2THF Nitrido Complexes of M olybdenum (V ); Syntheses, IR , and EPR Spectra. Crystal Structure of [N a(15-Crow n-5)N a(TH F)]2[MoNCl3-THF]4-2T H F | | | | Abstract
| Nitrido C om plexes o f M olyb denu m (V), | | | |
Reference
| Z. Naturforsch. 44b, 1377—1384 (1989); eingegangen am 30. Mai 1989 | | | |
Published
| 1989 | | | |
Keywords
| Syntheses, IR Spectra, EPR Spectra, Crystal Structure | | | |
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| default:Reihe_B/44/ZNB-1989-44b-1377.pdf | | | | Identifier
| ZNB-1989-44b-1377 | | | | Volume
| 44 | |
| 11 | Author
| W. S. Sheldrick, H. G. Braunbeck | Requires cookie* | | | Title
| Preparation and Crystal Structure of Cs4Se16 | | | | Abstract
| The cesium polyselenide Cs4 S e 16 has been prepared by the m ethanolotherm al reaction o f Cs2 C 0 3 and Se at 160 °C and 13 bar. [S e16]4-fragments may be regarded as containing an Se6 ring with Cs symmetry and two Se5 chains related by the crystallographic mirror plane. S e4 o f the six-m em bered ring, which displays a square planar geom etry, participates in two relatively long S e 4 —Se5 bonds [2.989(4) A ] to individual chains. The /rans-sited S e 4 —Se3 bonds [2.425(4) Ä] are markedly longer than the remaining S e -S e bonds in the Se6 ring [2.344(4), 2.356(4) Ä ]. Further Se —Se interactions o f length 3.132(4) and 3.346(4) Ä are observed betw een individual [Sel6]4~ fragments. | | | |
Reference
| Z. Naturforsch. 44b, 1397—1401 (1989); eingegangen am 26. Mai 1989 | | | |
Published
| 1989 | | | |
Keywords
| Cesium P olyselenide, M ethanolotherm al Synthesis, Crystal Structure | | | |
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| default:Reihe_B/44/ZNB-1989-44b-1397.pdf | | | | Identifier
| ZNB-1989-44b-1397 | | | | Volume
| 44 | |
| 12 | Author
| R. Oland Boese, D. Ieter Bläser, M. Bolatiana Andrianarison, Uwe Klingebiel | Requires cookie* | | | Title
| Lithio-di-terf-butylfluorsilyl-te/t-butylphosphan — Kristallstruktur und Reaktionen Lithio-di-terf-butylfluorosilyl-ferr-butylphosphane — Crystal Structure and Reactions | | | | Abstract
| Di-/er/-butylfluorosilyl-fe/7-butylphosphane (1) reacts with «-C 4H gLi to give the lithium salt (C M e3)2S iF —PLi(TFIF)3CM e3 (2) and butane. The crystal structure o f 2 has been determ ined. Fluorosilylphosphanes of the type (C M e3)2SiFP(R)C M e3 [R = SiM e3 (5), SiCl2Me (6). SiCl3 (7), SiF2CA H 5 (8), B F N (SiM e3)2 (9), SiClM eP(CM e3)SiF(CM e3)2 (10)] are obtained in the reaction of 2 with halogenosilanes and -borane. 6 and 7 undergo rearrangement via chloro-fluoro exchange reaction to give (C M e3)2S iC l-P (S iC lR F)C M e3 [R = Cl (11), Me (12)]. | | | |
Reference
| Z. Naturforsch. 44b, 265 (1989); eingegangen am 7. N ovem ber 1988 | | | |
Published
| 1989 | | | |
Keywords
| F luorosilylphosphanes, Lithium Salt, Crystal Structure Phosphasilene, Fluoro-C hloro Exchange | | | |
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| default:Reihe_B/44/ZNB-1989-44b-0265.pdf | | | | Identifier
| ZNB-1989-44b-0265 | | | | Volume
| 44 | |
| 13 | Author
| JörnM. Üller, Corinna Hänsch, Joachim Pickardt | Requires cookie* | | | Title
| ;r-01efin-Iridium-Komplexe, XV [1] Kationische Bis(2.3-dimethylbutadien)iridium-L-Verbindungen mit verschiedenen Donorliganden L jr-Olefin Iridium Complexes, XV [1] Cationic Bis(2.3-dim ethylbutadiene)iridium-L Compounds with Various D onor Ligands L | | | | Abstract
| (dm b)2IrCH , (dm b = 2.3-dim ethylbuta-l,3-diene) reacts with Ph,CBF4 in C H 2C12 to form the | | | |
Reference
| Z. Naturforsch. 44b, 278 (1989); eingegangen am 10. Oktober 1988 | | | |
Published
| 1989 | | | |
Keywords
| Synthesis, IR Spectra, NM R Spectra, Mass Spectra, Crystal Structure | | | |
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| default:Reihe_B/44/ZNB-1989-44b-0278.pdf | | | | Identifier
| ZNB-1989-44b-0278 | | | | Volume
| 44 | |
| 14 | Author
| Karl-Friedrich Tebbe, N. Orbert Krauß | Requires cookie* | | | Title
| Untersuchungen an Polypseudohalogeniden, VI [1] Darstellung und Kristallstruktur des Natriumdicyanoiodat(I)-dihydrats, Na[I(CN)2] * 2 H20 Studies on the Polypseudohalides, VI [1] Preparation and Crystal Structure of N a[I(CN )2] -2 H 20 | | | | Abstract
| The new com pound N a[I(C N)2] • 2 H 20 can be prepared by addition o f iodine to a concentrated aqueous solution of sodium cyanide. It crystallizes in the monoclinic space group P 2,/c with a — 1044.0(2), b — 480.2(2), c = 730.2(2) pm , ß — 95.94(2)° and Z = 2. The crystal structure has been refined to Rf = 0.027 for 692 reflections. The structure may be described as a layer-like package o f cations N a+, water m olecules and trihalide-analogous anions [I(C N)2]~. The anion is strictly linear at the I atom and nearly linear at the C atom s with cp(l—C —N) = 176.2° and d(I —C) = 231.1, d (C —N) = 110.6 pm. The cation is surrounded by a slightly distorted octahedron o f nitrogen and oxygen atoms with d(N a--N) = 263.8, d(N a--O) = 242.0, 242.8 pm. | | | |
Reference
| Z. Naturforsch. 44b, 637 (1989); eingegangen am 27. Januar 1989 | | | |
Published
| 1989 | | | |
Keywords
| Sodium dicyanoiodate, C yanogen Com pound, Polypseudohalide, Pseudotrihalide, Crystal Structure | | | |
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| default:Reihe_B/44/ZNB-1989-44b-0637.pdf | | | | Identifier
| ZNB-1989-44b-0637 | | | | Volume
| 44 | |
| 15 | Author
| Georg Beuter, Joachim Strähle | Requires cookie* | | | Title
| Clusteraufbau durch Photolyse von R3PAuN3 | | | | Abstract
| , III [1] Synthese von [(Ph3PAu)5Fe(CO)3]PF6 und Ru3(CO)10(jM-AuPPh3)(/i-NCO) Cluster Synthesis by Photolysis of R3PA uN 3, III [1] Synthesis of [(Ph3PA u)5Fe(C O)3]PF6 and R u3(C O)10(«-A uPPh3)(w-NCO) Photolysis of a mixture of Ph3P A u N 3 with F e(C O)5, Fe2(C O)9 or Fe3(C O),2 in TH F yields [(Ph3P A u)5F e(C O)3]+ (1) which crystallizes with PF6" as counterion as air stable, yellow platelets in the space group P2,/c: a = 2230.0(7), b = 1655.0(6), c = 2462.7(8) pm, ß = 94.04(5)°, Z = 4. The cationic A u5Fe cluster forms a bicapped F eA u 3 tetrahedron with almost equal Fe — A u dis tances o f 259.0 to 265.1 pm to all five A u atoms. D ue to the local symmetry C3|, o f the F e(C O)3 group two v(CO) at 1880 and 1930 c m ' 1 are observed. C o-photolysis of R u3(C O),2 and Ph3P A uN 3 does not result in a cleavage of the R u3 cluster. Bridging ,w-AuPPh3 and /^-NCO groups substitute two CO ligands to form Ru3(C O)10 («-A uPP h3)(u-N C O) (2). | | | |
Reference
| Z. Naturforsch. 44b, 647 (1989); eingegangen am 26. Januar 1989 | | | |
Published
| 1989 | | | |
Keywords
| Pentagold Iron Cluster, Synthesis, Crystal Structure, Triruthenium M onogold Cluster | | | |
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| default:Reihe_B/44/ZNB-1989-44b-0647.pdf | | | | Identifier
| ZNB-1989-44b-0647 | | | | Volume
| 44 | |
| 16 | Author
| Kurt Merzweiler, D. Ieter Fenske, Eva Hartm, Ann, Kurt Dehnicke | Requires cookie* | | | Title
| Synthese und Kristallstruktur des Imidokomplexes {TaCl4NC(Ph)[N(SiM e3)2]}2 * 2 C H 2C 12 Synthesis and Crystal Structure of the Imido Complex {TaCl4NC(Ph)[N(SiM e3)2]}2 * 2 C H 2C12 | | | | Abstract
| The title com pound has been prepared by the reaction of N ,N,N '-tris(trim ethylsilyl)benz-amidine with tantalum pentachloride in C H 2CL suspension, forming am ber-coloured, moisture-sensitive crystals, which were characterized by an X-ray structure determ ination. Space group P 2,In, Z = 2, 4895 observed independent reflexions, R = 0.059. Lattice dimensions (— 65 °C): a — 1165.2(6), b -1335.4(6), c = 1629.0(7) pm, ß -93.23(4)°. The complex forms centrosymmetric molecules dimerized via chloro bridges TaCLTa with TaCl bond lengths of 247.2(2) and 277.1(2) pm, the longer one being in frarcs-position to the imido group, which can be formulated a sT * a= $ = C < *M (bond len g th sT a= N = 183.5(8), C = N = 134(1) pm. bond angle TaNC = Ph 162.7(7)°). | | | |
Reference
| Z. Naturforsch. 44b, 1003 (1989); eingegangen am 8. Mai 1989 | | | |
Published
| 1989 | | | |
Keywords
| Imido Complex of Tantalum, Synthesis, IR Spectra, Crystal Structure | | | |
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| default:Reihe_B/44/ZNB-1989-44b-1003.pdf | | | | Identifier
| ZNB-1989-44b-1003 | | | | Volume
| 44 | |
| 18 | Author
| EvaH. Artm Ann, Kurt Dehnicke, D. Ieter Fenske, Helm Ut Goesmann, G.Erhard Baum | Requires cookie* | | | Title
| [Na-15-Krone-5]2[ZrF2Cl4] und (PPh4)2[ZrCI6] * 2 CH2CI2; Synthesen, IR-Spektren und Kristallstrukturen [Na-15-Crown-5]2[ZrF:Cl4] and (PPh4)2[ZrCl6] * 2 C H 2C12; Syntheses, IR Spectra, and Crystal Structures | | | | Abstract
| [Na-15-crown-5]: [Z rF2Cl4] has been prepared by the reaction of the amidinato complex [Ph—C(NSiM e3)2Z rC l3]2 with sodium fluoride in acetonitrile suspension, as well as by the reaction ° f Z rC l4 in acetonitrile, both in the presence of 15-crown-5. On an analogous route (PPh4)2[ZrCl6] • 2 CH2C12 has been prepared by the reaction of [P h -C (N S iM e3)2Z rC l3]2 with PPh4Cl in C H 2C12 solution, as well as by the reaction of ZrC l4 with PPh4Cl in C H 2C12. The compounds are characterized by their IR spectra and by crystal structure determ inations. [Na-15-crown-5]2[ZrF2Cl4]: Space group P 2 1/a, Z = 4, 6589 observed independent reflexions, R = 0.069. Lattice dimensions at 20 °C: a = 1705.0(9), b = 1092.4(6), c = 1906.5(10) pm , ß = 113.14(3) . [Na-15-crown-5]2[ZrF2Cl4] forms ion triples, in which both sodium ions are seven-coordinate by five oxygen atoms of the crown ether molecules, as well as by a fluorine and a chlorine atom of the c/s-[ZrF2Cl4]2~ unit. (PPh4)2[ZrCl6] -2 C H 2C12: Space group P I , Z = 1, 4831 observed independent reflexions, R = 0.041. Lattice dimensions at 20 °C: a = 1030.1(5), b = 1124.8(6), c = 1245.6(6) pm, a = 70.81(3), ß = 80.61(4), y = 80.39(4)°. The com pound has an ionic structure with Z rC l62^ ions of symmetry Cr | | | |
Reference
| Z. Naturforsch. 44b, 1155 (1989); eingegangen am 21. Juni 1989 | | | |
Published
| 1989 | | | |
Keywords
| H alogeno-Zirconates(IV ), Syntheses, IR Spectra, Crystal Structure | | | |
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| default:Reihe_B/44/ZNB-1989-44b-1155.pdf | | | | Identifier
| ZNB-1989-44b-1155 | | | | Volume
| 44 | |
| 19 | Author
| Klaus Hosier, Frank Weller, Kurt Dehnicke | Requires cookie* | | | Title
| Kristallstruktur von [MoC12(N S N )-2TH F]2; einem Metallaheterocyclus mit der NSN4 -Einheit Crystal Structure of [MoC12(N S N )-2T H F ]2; a M etallaheterocycle with the NSN4-Unit | | | | Abstract
| The chlorothionitrene complex [Cl4M o(NSCl)]2 reacts with N ,N,N '-tris(trim ethylsilyl)benzam idine in T H F solution to form the heterocyclic complex [MoC12(NSN) ■ 2T H F ]2, which contains the [NSN]4-unit. The com pound is characterized by IR spectro scopy and by an X-ray structure determ ination (Space group P2,/c, Z = 2, 1504 observed unique re flexions, R = 0.044. Lattice dim ensions at 19 °C: a = 1176.0(1), b = 1108.6(4), c = 1227.3(3) pm, ß = 118.25(1)°). The com pound forms centrosym m etric molecules [(TH F)2C12M o(NSN)2MoC12(T H F)2], in which the molybdenum atoms are members of a nearly planar M o(NSN)2Mo eight-m em bered ring with bond lengths MoN 180.2 and 175.2 pm; NS 157.5 and 160.6 pm; the bond angle NSN is 108.3°, corresponding to a NSN4-unit. | | | |
Reference
| Z. Naturforsch. 44b, 1325—1328 (1989); eingegangen am 5. Juni 1989 | | | |
Published
| 1989 | | | |
Keywords
| M etallaheterocycle with NSN4~ U nit, Synthesis, IR Spectra, Crystal Structure | | | |
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| default:Reihe_B/44/ZNB-1989-44b-1325_n.pdf | | | | Identifier
| ZNB-1989-44b-1325_n | | | | Volume
| 44 | |
| 20 | Author
| FrankW. Eller, Harald Borgholte, H. Arald Stenger, Stefan Vogler, Kurt Dehnicke | Requires cookie* | | | Title
| Synthesen und Kristallstrukturen der Kronenether-Komplexe (18-Krone-6) * 2 CH3CN, [Na-15-Krone-5][Re04] CH3CN und [Na-15-Krone-5]PF6 Syntheses and Crystal Structures of the Crown E ther Complexes (18-C row n-6)-2C H 3CN, [N a-15-Crow n-5][Re04] * C H 3CN, and [Na-15-Crown-5]PF6 | | | | Abstract
| Single crystals o f (18-crow n -6)-2C H 3CN were obtained by cooling a solution o f 18-crown-6 in acetonitrile to 4 °C. Space group P 2 x/n, Z = 2, 629 observed independent reflexions, R = 0.062. Lattice dim ensions at 19 °C: a = 911.7(1), b = 852.0(1), c = 1370.0(2) pm; ß — 104.61(1)°. The com pound forms a m olecular structure with approximate D 3d symmetry o f the crown ether m olecule, and C —H -O interactions of the acetonitrile m olecules with the crown ether, the H ---0 distances being 243, 253, and 267 pm , respectively. [N a-15-crow n-5][R e04] • C H 3CN is formed as a by-product o f the reaction o f R eN C l4 with sodium fluoride in acetonitrile in the presence o f 15-crown-5 and traces o f water. Space group P 1, Z = 2, 3107 observed independent reflexions, R = 0.045. Lattice dim ensions at 19 °C: a — 823.4(1), b = 1078.8(1), c = 1204.0(1) pm; a = 112.40(1)°, ß = 94.35(1)°, y = 104.63(1)°. The com pound forms ion pairs, in which the sodium atom is sixfold coordinated by the five oxygen atoms o f the crown ether m olecule, as well as by one oxygen atom o f the R e 0 4~ ion, which is only slightly distorted. The bond length Na — 0 R e 0 3 is 237.8(8) pm , the bond angle N aO R e is 164.3(5)°. [Na-15-crown-5]PF6 is formed in the reaction o f [R eC l3(N SC l)2 • PO C l3] with sodium fluoride in acetonitrile solution in the presence o f 15-crown-5. Space group P na2,, Z = 4, 1130 observed independent reflexions, R = 0.123. The high R value is due to disorder of the skeletal atoms of the crown ether m olecule. The com pound forms ion pairs, in which the sodium atom is sevenfold coordinated by the five oxygen atom s o f the crown ether m olecule, as well as by two fluorine atom s o f the PF6~ ion with N a —F bond lengths o f 240(2), and 246(2) pm, respectively. | | | |
Reference
| Z. Naturforsch. 44b, 1524 (1989); eingegangen am 25. Juli/5. September 1989 | | | |
Published
| 1989 | | | |
Keywords
| Crown Ether C om plexes, Syntheses, IR Spectra, Crystal Structure | | | |
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| default:Reihe_B/44/ZNB-1989-44b-1524.pdf | | | | Identifier
| ZNB-1989-44b-1524 | | | | Volume
| 44 | |
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