| 1 | Author
| Willi Buchm, Bernward Engelen, HeinzD. Ieter Lutz | Requires cookie* | | Title
| Kristallstrukturen von NaM g20 H ( S 0 3)2 * H ,(), NaMn20 H ( S 0 3)2 * H20 , N aFe20 H ( S 0 3)2 * H20 , NaCo2O H (S 0 3)2 H 20 und NaZn20 H ( S 0 3)2 H 20 Crystal Structures of NaMg20 H ( S 0 3)2-H 20 , N aM n20 H ( S 0 3)2 * H 20 , N aFe20 H ( S 0 3)2 H 20 , NaCo2OH(SC>3)2 * H 20 , and N aZ n20 H ( S 0 3)2-H 20  | | | Abstract
| The crystal structures of the isotypic hydroxosulfitom etalates N aM 20 H (S 0 3)2-1 H 20 with M = | | |
Reference
| Z. Naturforsch. 41b, 852 (1986); eingegangen am 11. März 1986 | | |
Published
| 1986 | | |
Keywords
| Sulfites, Crystal Structure, Hydroxosulfitom etalates | | |
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| default:Reihe_B/41/ZNB-1986-41b-0852.pdf | | | Identifier
| ZNB-1986-41b-0852 | | | Volume
| 41 | |
3 | Author
| | Requires cookie* | | Title
| On the Nonexistence of a Simple  | | | Abstract
| ^-O xo-diphosphorane Involving two 1,3.5.7-Tetram ethyl-1.3.5.7-tetra-aza-4A''-phospha-spiro[3.3]heptane-2.6-dione Groupings: Preparation and Structure of a A5P —O —A5P D iphosphorane Doubly Bridged with N .N '-D im ethylurea D ietm ar Schomburg3 +, Ulrich W erm uthb und Reinhard Schmutzlerb * a G esellschaft für B iotechnologische Forschung mbH, M ascheroder W eg The reaction between the spiro-chlorophosphorane, [ 0 = C (N M e)2]2PX (X = C l), and the related trimethylsiloxy com pound (X = O SiM e3) was expected to give rise to the formation o f a ^-oxo-bis(spirophosphorane), [ [ 0 = C (N M e)2]2P]20 . Instead, an isom er o f the expected com pound, with two N.N '-dim ethylurea bridges across a A5P —O —A5P bond system was obtained. The identity o f the product was established by spectroscopic means (IR , N M R . mass spectroscopy), and by a single crystal X-ray diffraction study. | | |
Reference
| Z. Naturforsch. 41b, 207 (1986); eingegangen am 8. Juli/17. O ktober 1985 | | |
Published
| 1986 | | |
Keywords
| Penta-co-ordinate Phosphorus, X -R ay, Crystal Structure | | |
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| default:Reihe_B/41/ZNB-1986-41b-0207.pdf | | | Identifier
| ZNB-1986-41b-0207 | | | Volume
| 41 | |
4 | Author
| Klaus Angerm, Borislav Bogdanović, GudrunK. Oppetsch, Carl Krüger, RichardM. Ynott, Manfred Schwickardi, Yi-H Ung Tsay | Requires cookie* | | Title
| Magnesiumorganische Innerkomplexe, Teil I [1] Bis(dialkylaminoalkyl)-und Bis(alkoxybutyl)magnesium-Verbindungen Organomagnesium Inner C om plexes, Part I [1] Bis(dialkylaminoalkyl)-and Bis(alkoxybutyl)m agnesium Compounds  | | | Abstract
| A series of magnesium inner complexes has been prepared by reacting M gH2 (prepared by homogeneous catalysis) with dialkylallyl-and -3-butenylam ines and -3-butenylethers in the p re sence of catalytic amounts of Z rC l4. The m onom eric nature of bis(4-m ethoxybutyl)m agnesium has been confirmed by X-ray diffraction. The analogous syntheses of bis(3-alkoxypropyl)magnesium com pounds failed: cleavage of the allyl ether with elimination of propene occurred. This cleavage reaction is accelerated by catalytic amounts of NiCl2 or ZrC l4. | | |
Reference
| Z. Naturforsch. 41b, 455 (1986); eingegangen am 21. N ovem ber 1985 | | |
Published
| 1986 | | |
Keywords
| Magnesium, Inner Complexes, Crystal Structure, X-Ray | | |
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| default:Reihe_B/41/ZNB-1986-41b-0455.pdf | | | Identifier
| ZNB-1986-41b-0455 | | | Volume
| 41 | |
5 | Author
| Borislav Bogdanović, G. Udrun, K. Oppetsch, Carl Krüger, RichardM. Ynott | Requires cookie* | | Title
| Magnesiumorganische Innerkomplexe, Teil II [1] Ethyl(dialkylaminoalkyl)-und Ethyl(4-alkoxybutyl)magnesium-Verbindungen Organomagnesium Inner Complexes, Part II [1] Ethyl(dialkylam inoalkyl)-and Ethyl(4-alkoxybutyl)magnesium Compounds  | | | Abstract
| The reaction o f bis(dialkylam inoalkyl)-and bis(4-alkoxybutyl)m agnesium inner com plexes with M gEt2 leads to the form ation of ethyl(dialkylam inoalkyl)-and ethyl(4-alkoxybutyl)m agnesium com pounds. The X -ray crystal structures o f ethyl(3-N ,N -dim ethylam inopropyl)m agnesium and ethyl(3-N -cyclohexyl-3-N -m ethylam inopropyl)m agnesium confirm that the com pounds are dim eric with the a-C -atom o f the chelating ligand bridging the magnesium atoms. The difference in reactivity of the M g —Et and M g—C"H2nX bonds (X = NR 'R ", O R) makes itself apparent in the reaction of these com plexes with ethylene: up to six ethylene m olecules are inserted, whereby in the case of the ethyl(4-alkoxybutyl)m agnesium com pounds insertion occurs preferentially into the M g—Et bond w hereas in the case o f the ethyl(dialkylam inoalkyl)m agne-sium com pounds both bonds are equally reactive. | | |
Reference
| Z. Naturforsch. 41b, 617 (1986); eingegangen am 21. N ovem ber 1985 | | |
Published
| 1986 | | |
Keywords
| M agnesium, Inner C om plexes, Crystal Structures | | |
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| default:Reihe_B/41/ZNB-1986-41b-0617.pdf | | | Identifier
| ZNB-1986-41b-0617 | | | Volume
| 41 | |
6 | Author
| HeribertW. Adle, Elke Conradi, Ulrich Müller, Kurt Dehnicke | Requires cookie* | | Title
| Synthese und Kristallstruktur von [W Cl3(N 3S2)(Pyridin)] Synthesis and Crystal Structure of [WCl3(N 3S2)(Pyridine)]  | | | Abstract
| 1,1.1 -T richloro-1 -pyridine-cyclo-1 Ä6-tungsta-3.5-dithia-2,4, | | |
Reference
| Z. Naturforsch. 41b, 796—798 (1986); eingegangen am 14. Februar 1986 | | |
Published
| 1986 | | |
Keywords
| 6-triazine, Synthesis, IR Spectra, Crystal Structure | | |
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| default:Reihe_B/41/ZNB-1986-41b-0796_n.pdf | | | Identifier
| ZNB-1986-41b-0796_n | | | Volume
| 41 | |
7 | Author
| KurtO. Klepp | Requires cookie* | | Title
| Darstellung und Kristallstruktur von TI3AgTe2 Preparation and Crystal Structure of Tl3A gTe2  | | | Abstract
| The new compound Tl3A gTe2 was prepared by the reaction of Tl5T e3, Ag and Te at 550 °C, followed by slow cooling of the melt. It forms black crystals of metallic lustre which decompose by the influence of humidity. Tl3A gTe2 is monoclinic, space group P2,/c, with a = 11.020(5), b = 7.427(2), c = 9.888(3) Ä , ß — 116.62(4)°, Z = 4. The crystal structure was determ ined from four-circle diffractom eter data and refined to a conventional R of 0.083 for 1015 observed reflec tions. Tl3AgTe2 crystallizes with a new structure type, characterized by infinite layers, 2[A gT e2], running along (100), which are separated from each oth er by thallium atom s. The layers are built up by pairs of edge sharing A gTe4-tetrahedra linked together by common Te atoms according to |[A g (T e)T e 3/3]. The crystal structure is based on an arrangem ent of distorted c.p. tellurium layers, stacked along [010] (stacking sequence h2). All octahedral voids are occupied by Tl-atoms, Ag-and Tl-atoms are regularly distributed over the tetrahedral sites. | | |
Reference
| Z. Naturforsch. 41b, 941 (1986); eingegangen am 17. März 1986 | | |
Published
| 1986 | | |
Keywords
| Ternary Chalcogenides, Thallium Silver Telluride, Crystal Structure, Preparation | | |
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| default:Reihe_B/41/ZNB-1986-41b-0941.pdf | | | Identifier
| ZNB-1986-41b-0941 | | | Volume
| 41 | |
8 | Author
| Z. Naturforsch | Requires cookie* | | Title
| Sr3In2P4 und Ca3ln2As4, Zintlphasen mit Bänderanionen aus kanten-und ecken verknüpften InP4-bzw. InAs4-Tetraedern  | | | Abstract
| The new com pounds Sr3In2P4 and Ca3In2A s4 crystallize in the orthorhom bic system , space group Pnnm (N o. 58), with the follow ing lattice constants: Sr3In,P4: a = 1632.3(6), b = 682.8(3), c = 428.9(2); Ca3In2A s4: a = 1621.2(6), b = 659.5(3), c -430.6(2). In the anionic partial lattice InP4 (In A s4) tetrahedra are connected by com m on edges and corners and form (InP21-)" ((In A s23_)") strings o f alternating four-m em bered and eight-m em -bered rings. | | |
Reference
| Z. Naturforsch. 41b, 1416 (1986); eingegangen am 14. Juli 1986 | | |
Published
| 1986 | | |
Keywords
| Interm etallic C om pounds, Zintl Phases, Crystal Structure | | |
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| default:Reihe_B/41/ZNB-1986-41b-1416.pdf | | | Identifier
| ZNB-1986-41b-1416 | | | Volume
| 41 | |
10 | Author
| Z. Naturforsch | Requires cookie* | | Title
| An ESR Study of Structural Phase Transitions o f(N H ,)2Pb|C u(N 02)6|  | | | Abstract
| T etsuo Asaji, Laxm an S hrikrishna P ra b h u m irash i *, and D aiy u N ak a m u ra The structural changes o f (N H 4) 2P b [C u (N 0 2)6] crystals during the phase transitions at 316, 287, and 95 K were studied by means o f a single crystal ESR technique. Anisotropic g values [9 > 9±) were obtained in the lowest temperature phase IV, whereas the ESR spectra recorded in the intermediate phases III and II, in which the crystal is known to be tetragonally compressed along the c axis, could be interpreted by use o f effective g values [g (c) < g (_L c)]. In the highest temperature phase I an isotropic g value was obtained. The phases I, II, and III o f the present complex can be assumed to be very similar to the corresponding phases observed above ~ 250 K for the com pounds R2P b [C u (N 0 2) 6] with R = K, Rb, Cs, and Tl. However, the lowest temperature phase transition transforms the phase III with an antiferrodistortive order o f the elongated [C u (N 0 2)6]4_ octahedra into the phase IV with a ferrodistortive one. This occurs only for the complex with R = N H 4 and is very unusual. The results o f the 14N N Q R experiments already reported for the phases III and IV could be well explained by the present newly proposed model. | | |
Reference
| Z. Naturforsch. 41a, 1154—1158 (1986); received May 3 1986 | | |
Published
| 1986 | | |
Keywords
| Magnetic Resonance (ESR, N Q R ), Phase Transition, Crystal Structure | | |
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| default:Reihe_A/41/ZNA-1986-41a-1154.pdf | | | Identifier
| ZNA-1986-41a-1154 | | | Volume
| 41 | |
11 | Author
| H. Erbert, W. Roesky, Jörg Sundermeyer, Jürgen Schimkowiak, Thomas Gries, M. Athias, N. Oltem Eyer, GeorgeM. Sheldrick | Requires cookie* | | Title
| Reaktionen von l,2,4-Thiadiazol-3,5-dicarbonitril mit Schwefelchloriden: Röntgenstrukturanalyse von S3(CN)4C12* AsF5 und S3(CN)8C12 Reactions of l,2,4-Thiadiazol-3,5-dicarbonitrile with Sulfur Chlorides: X-Ray Crystal Structure Analysis of S3(CN)4C12-A sFs and S3(CN )8C12  | | | Abstract
| The reactions between l,2,4-thiadiazol-3,5-dicarbonitrile, S (C N)4, and sulfur chlorides (SC12 and S2C12) in the presence o f Adogen® 464 (Aldrich) proceeds with formation o f S3(C N)4C12 (1) | | |
Reference
| Z. Naturforsch. 41b, 162 (1986); eingegangen am 18. O ktober 1985 | | |
Published
| 1986 | | |
Keywords
| Crystal Structure, Sulfur-Nitrogen, Catalyst, Lewis Acid A dduct | | |
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| default:Reihe_B/41/ZNB-1986-41b-0162.pdf | | | Identifier
| ZNB-1986-41b-0162 | | | Volume
| 41 | |
12 | Author
| | Requires cookie* | | Title
| Die  | | | Abstract
| Kristallstruktur von [(CH3)4N]2TeCl6 und über die Einschlußverbindung [(CH3)4N]2(CH3CN)TeCl6 The Crystal Structure of [(CH 3)4N]2TeCl6 and the Inclusion Com pound [(CH3)4N]2(CH 3C N)TeCl6 W alter Abriel* Both title com pounds show an antifluorite-like arrangement o f (C H 3)4N + cations and TeC l62~ anions. The remaining octahedral holes in this array can be filled with C H 3CN m olecules forming the inclusion com pound by crystallization from C H 3CN solution. [(C H 3)4N ]2TeC l6 (space group F d 3c with a = 25.791(3) Ä at 265(5) K and Z = 32) contains almost regular TeCl62-octahedra. In contrast, in [(CH 3)4N ]2(C H 3C N)T eC l6 (space group Cmcm with a = 12.765(6), b = 14.349(7), c = 12.716(3) Ä and Z = 4) the anion is statically distorted with the approximate point symmetry 4 mm. A t tem peratures above 320 K the solvent m olecules can be rem oved yielding the F d 3c phase. Finally, structural relationships betw een antifluorite-like phases A 2B X 6 and elpasolites A 2B 'B X 6 considering halogenides and cyanides are discussed. | | |
Reference
| Z. Naturforsch. 41b, 592 (1986); eingegangen am 3. Februar 1986 | | |
Published
| 1986 | | |
Keywords
| Crystal Structure, Tellurates, Inclusion C om pound, Lone Pair Electrons | | |
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| default:Reihe_B/41/ZNB-1986-41b-0592.pdf | | | Identifier
| ZNB-1986-41b-0592 | | | Volume
| 41 | |
13 | Author
| R.Ainer Mattes, AngelaD. Orau | Requires cookie* | | Title
| Kurze inter-und intramolekulare W asserstoffbrückenbindungen in sauren Salzen halogensubstituierter Orthophthalsäuren Short Inter-and Intram olecular Hydrogen Bonds in Acid Salts of Halogen-Substituted o-Phthalic Acids  | | | Abstract
| The hydrogen bonding in several acid salts o f 4,5-dichlorophthalic, 3,6-dichlorophthalic and 3-fluorophthalic acid have been studied by IR spectroscopy and X-ray structure analysis. N H 4H [3,6-C12C8H 204] and KH[3-FCgH 30 4], with 0 ---0 distances o f 247 and 254.1(4) pm, respectively, belong to Speakm an's type B2 of acid salts o f dicarboxylic acids. In N H 4H[4,5-C12C8H 20 4] • H 20 a short hydrogen bond o f 253(1) pm is form ed to the H 20 m olecule. A very short intramolecular hydrogen bond o f only 234.0(10) pm length was found in N (C 4H 9)4H[4,5-C12C8H 20 4], In the [3,6-Cl2C8H 20 4]2_ dianion both carboxylate groups are nearly orthogonal to the phenyl ring. | | |
Reference
| Z. Naturforsch. 41b, 808 (1986); eingegangen am 17. März 1986 | | |
Published
| 1986 | | |
Keywords
| Short Hydrogen Bonds, Acid Salts of o-Phthalic Acids, Crystal Structure | | |
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| default:Reihe_B/41/ZNB-1986-41b-0808.pdf | | | Identifier
| ZNB-1986-41b-0808 | | | Volume
| 41 | |
16 | Author
| H. Erbert, W. Roesky, Jörg Sunderm, M. Athias, N. Oltemeyer, GeorgeM. Sheldrick, Karen Meyer-Bäse, PeterG. Jones | Requires cookie* | | Title
| Darstellung und Struktur des N-Thiobis-N' -(phenylsulfonyl)schwefeldiimids Synthesis and Structure of N-Thiobis-N'-(phenylsulfonyl)sulfurdiimide  | | | Abstract
| The reaction of S4N 4 with P h S 0 2N C l2 proceeds with formation o f (P h S 0 2N S N)2S 2. The main product 2 was characterized by an X-ray structure determination. [P2]/c, a = 996.8(2), b = 1733.0(2), c = 1131.2(1) pm, ß = 114.69(1)°, Z = 4, R — 0.044 for 1911 reflections.] 2 contains a | | |
Reference
| (Z. Naturforsch. 41b, 53—58 [1986]; eingegangen am 27. Septem ber 1985) | | |
Published
| 1986 | | |
Keywords
| Sulfur Nitrogen C om pound, Crystal Structure, cis-trans Configuration, Metal Com plex | | |
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| default:Reihe_B/41/ZNB-1986-41b-0053.pdf | | | Identifier
| ZNB-1986-41b-0053 | | | Volume
| 41 | |
17 | Author
| Karl-Friedrich Tebbe, Magda Fehér | Requires cookie* | | Title
| Beiträge zur Strukturchemie phosphorhaltiger Ketten und Ringe, XIII [1] Die Molekül-und Kristallstruktur von 3 Structural Chemistry of Phosphorus-Containing Chains and Rings, X III [1]  | | | Abstract
| The M olecular and Crystal Structure of 3,4,9,10-Tetraisopropyl-pentacyclo[6.4.0.02-6.0512.07 H]dodecaphosphane, P 12(/-Pr) 4 The structure o f P 12(/-Pr)4, C 12H 28Pi2 , has been determ ined by single crystal X-ray techniques (Rf = 0.026, wRf = 0.029 for 3549 observed reflections with |F0| > 4 a (F 0)). The com pound crystallizes in the triclinic space group P I with a = 879.8, b = 1088.5, c = 1414.1 pm, a — 93.01, ß — 107.61, y = 92.92° and Z = 2. The m olecule contains a polycyclic P 12-unit of nearly C2v symmetry, which represents an essential structural unit o f H itto r fs phosphorus. | | |
Reference
| Z. Naturforsch. 41b, 548 (1986); eingegangen am 14. Januar 1986 | | |
Published
| 1986 | | |
Keywords
| D odecaphosphane, Tetraisopropyl-dodecaphosphane, Phosphorus Cage, Polycyclic O rganophosphane, Crystal Structure | | |
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| default:Reihe_B/41/ZNB-1986-41b-0548.pdf | | | Identifier
| ZNB-1986-41b-0548 | | | Volume
| 41 | |
18 | Author
| Wolfgang Willing, Ulrich Müller, Udo Dem, Kurt Dehnicke | Requires cookie* | | Title
| Synthesen und Kristallstrukturen von PPh4[RuCl4(NO)(NSCl)] und (PPh4)2[RuCl4(NS)]2-4C H 2CI2 Syntheses and Crystal Structures of PPh4[RuCl4(NO)(NSCl)] and (PPh4)2[RuCl4(NS)]2-4 CH 2C12  | | | Abstract
| By reaction o f trithiazylchloride, (NSC1)3, with PPh4[RuCl4(N O)]2 in dichlorom ethane the thiazylchloridenitrosyl com plex PPh4[RuCl4(N O)(N SC l)] is obtained; its vacuum pyrolysis at 2 0 0 -2 2 0 °C yields the thionitrosyl com plex (PPh4)2[RuCl4(N S)]2 which crystallizes from C H 2C12 solution with four m olecules o f CH 2C12. Both com pounds were charaterized by their IR spectra and by X-ray crystal structure determ inations. Crystal data: PPh4[RuCl4(N O)(N S C l)], m on o clinic, space group P 2 xln, Z = 4, a = 982.6, b = 1700.0, c = 1772.3 pm , ß = 104.79° (2548 observed reflexions, R = 0.046); (PPh4)2[RuCl4(N S)]2-4 C H 2C12, triclinic, P I , Z = 1, a = 952.9, b = 1380.0, c — 1458.5 pm , a — 112.91, ß = 106.67, y = 92.61° (3760 observed reflexions, R = 0.053). In the [RuCl4(N O)(N S C l)]e ion the nitrosyl and thiazyl chloride ligands occupy e x positions; bond lengths indicate double bonds in the linear Ru = N -0 group, while the NSC1 m olecule is attached by a donor-acceptor interaction R u -N = S -C l , although with a rather short Ru —N bond o f 198 pm (N = S 144 pm, S —Cl 213 pm). The centrosymm etric [RuC14(N S)]220 ions have chloro bridges and NS ligands in axial positions; the nearly linear R u = N = S group has bond lengths R u = N 175 pm and N = S 147 pm. | | |
Reference
| Z. Naturforsch. 41b, 560 (1986); eingegangen am 29. Januar 1986 | | |
Published
| 1986 | | |
Keywords
| Thionitrosyl and Thiazylchloride C om plexes o f Ruthenium, Syntheses, IR Spectra, Crystal Structure | | |
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| default:Reihe_B/41/ZNB-1986-41b-0560.pdf | | | Identifier
| ZNB-1986-41b-0560 | | | Volume
| 41 | |
19 | Author
| Hans-Günter Hauck, W. Olfgang, Willing, Ulrich Müller, Kurt Dehnicke | Requires cookie* | | Title
| Brom-und Chlorthionitrenkomplexe des Rheniums Die Kristallstruktur von (PPh4)2[ReBr4(N S)(N SBr)] *CH2Br2 Bromo-and Chlorothionitrene Complexes of Rhenium The Crystal Structure of (PPh4)2[ReBr4(NS)(NSBr)] ■ C H 2B r2  | | | Abstract
| The thionitrosyl-halothionitrene com pounds (PPh4)2[R eX 4(N S)(N S X)]-2 C H 2X 2, X = Cl or Br, are obtained by nucleophilic ring cleavage o f the R e(N 2S2) rings o f com plexes [R eX 4(N 2S2)]e with PPh4X in C H 2X 2. (A sP h4)2[R eC l4(N S)(N SC l)] • C H 2C12 can also be obtained by the reaction | | |
Reference
| Z. Naturforsch. 41b, 825 (1986); eingegangen am 7. März 1986 | | |
Published
| 1986 | | |
Keywords
| Bromo- and Chlorothionitrene Complexes of Rhenium, Synthesis, IR Spectra, Crystal Structure | | |
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| default:Reihe_B/41/ZNB-1986-41b-0825.pdf | | | Identifier
| ZNB-1986-41b-0825 | | | Volume
| 41 | |
20 | Author
| Ralf Steudel, Jürgen Steidel, Torsten Sandow | Requires cookie* | | Title
| Preparation and Crystal Structure of £7s-Tetrachlorobis(cycIooctasulfurmonoxide)tin(IV) [1]  | | | Abstract
| Yellow crystals of c/s-[SnCl4(S8 0) 2] containing the homocyclic sulfur oxide S80 have been prepared from the com ponents in carbon disulfide at —35 °C. A n X-ray structural analysis carried out at —105 °C showed the com pound to be monoclinic, space group P2 Jn with Z = 4 in a unit cell of dimensions a = 821.2(2) pm, b = 1331.9(4) pm , c = 2071.7(6) pm and ß -91.82(2)°. The structure was refined to a final agreem ent factor R = 0.038 for 2022 reflections. The tin atom is surrounded by a distorted octahedron of two oxygen atom s in cw-positions and four chlorine atom s in accordance with other oxygen-bonded complexes of SnCl4. The molecular symmetry is approximately C2, and the SS bond lengths in the ligands vary betw een 201 and 218 pm. V ibra tional spectra of [SnCl4 (SH 0) 2] are reported. The title com pound is the second example containing S80 as a ligand. | | |
Reference
| Z. Naturforsch. 41b, 951 (1986); received April 29 1986 | | |
Published
| 1986 | | |
Keywords
| Sulfur Oxides, Tin T etrachloride, Crystal Structure, Complex Form ation, V ibrational Spectra | | |
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| default:Reihe_B/41/ZNB-1986-41b-0951.pdf | | | Identifier
| ZNB-1986-41b-0951 | | | Volume
| 41 | |
|