| | 61 | Author
| R. Nagel3, M. Botovab, G. Pracht3, E. Suchanek3, M. Manevab, H. D. Lutz3 ', Herrn | Requires cookie* | | | Title
| Kristallstruktur, Infrarot-und Ramanspektren sowie thermische Zersetzung von Magnesiumtetrahydrogendimesoperiodat, MgH4I2O10 * 6H20 Crystal Structure, Infrared and Raman Spectra and Thermal Decomposition of Magnesium Tetrahydrogen Dimesoperiodate, MgH4I2O ,0 * 6H20  | | | | Abstract
| Crystal structure, DRIFT, infrared and Raman spectra, and the results of thermal analyses of the hitherto wrongly as Mg(H4I 0 6)2 • 4H20 and M g(I04) • 8H20 described dimesoperiodate MgH4I2O l0 • 6H20 and of the isostructural zinc compound are presented. The compounds crystallize in the monoclinic space group P2, (Z = 2) with a = 1071.0(2), b = 547.0(1), c = 1194.9(2) pm, and ß = 112.58(3)° and a = 1073.3(3), b = 545.3(2), c = 1188.3(5) pm, and ß = 112.52(3)°, respectively. The structure, which was refined from X-ray single crystal data of the magnesium compound (R 1 = 2.72%, 3824 independet reflections}, is built up from isolated distorted M(H20) 62+ octahedra and dimesoperiodate ions H4I2O 10 -connected by a network of hydrogen bonds formed by the H4I2O 10"~ ions and six crystallographically different hydrate H20 molecules. The strength of the hydrogen bonds ranges from unusually weak bonds corresponding to uncoupled (isotopically dilute samples) OD stretching modes of > 2600 cm-1 and ver^ strong ones (uOD: < 2200 cm-1). The IO stretching modes of the trans-configurated H4I2O l0~-ions are assigned to terminal 1-0 groups (816 cm-1), I-OH groups (746 and 762 cm' 1) and bridging 1-0 groups (618 and 647 cm-1). On heating, MgH4I2O |0 • 6H20 undergoes dehydration in the range of 373 -485 K (Differential Scanning Calorimetry) to two different polymorphs of magnesium metaperiodate (H4I2O |02-—» ■ 2 I0 4-+ 2H20). Anhydrous M g(I04)2 is instable. Above 423 K (high-temperature Raman data), it decomposes to magnesium iodates. | | | |
Reference
| Z. Naturforsch. 54b, 999—1008 (1999); eingegangen am 16. April 1999 | | | |
Published
| 1999 | | | |
Keywords
| Magnesium Periodate Hydrate, Zinc Periodate Hydrate, Dimesoperiodate Ions, Crystal Structure, Raman Data | | | |
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| default:Reihe_B/54/ZNB-1999-54b-0999.pdf | | | | Identifier
| ZNB-1999-54b-0999 | | | | Volume
| 54 | |
| 62 | Author
| A. Rto, M. Aaninena, R. Ené, T. B. Oeré, Tristram Chivers0, M. Asood Parvezc | Requires cookie* | | | Title
| Preparation and X-Ray Structure of 4-N,N'-Bis(trimethylsilyl)- amino-3,5-diisopropylphenylselenium Trichloride | | | | Abstract
| The reaction of SeCU or SeCF with /V,/V'-bis(trimethylsilyl)-2,6-diisopropylaniline occurs not at the nitrogen atom but by electrophilic aromatic substitution at C-4 of the phenyl ring to give [(CH3)3Si]2NC6 H2('Pr:)SeCl3, which crystallizes as the chloro-bridged dimer in the triclinic system, space group P i, a -10.2598(17), b = 13.665(3), c = 9.7838(10) A, a = 90.056(13), ß = 102.439(11), 7 = 70.922(14)°, V = 1262.3(4) A \ Z = 1. The dimer contains an essentially planar CUSe^-Cl^SeCU unit, with trans apical (Me3SihNC6H2('Pr)2 groups, resulting in approximately square pyramidal geometry at Se. The bridging Se-Cl distances are unequal at 2.587(2) and 2.749(2) A. | | | |
Reference
| Z. Naturforsch. 54b, 1170—1174 (1999); received April 22 1999 | | | |
Published
| 1999 | | | |
Keywords
| Crystal Structure, 2, 6-Diisopropylaniline, Aryl Selenium Trichloride, Bridging Chloride, NMR Data | | | |
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| default:Reihe_B/54/ZNB-1999-54b-1170.pdf | | | | Identifier
| ZNB-1999-54b-1170 | | | | Volume
| 54 | |
| 64 | Author
| A. Baumann, J. Beck, T. Hilbert | Requires cookie* | | | Title
| Octachalcogen Cations Te82+, Se82+, and Mixed (Te8.JC SeJC )82+ Stabilized by Chlorometallates of Bi, Zr, and Hf: Synthesis and Crystal Structures of Se8[Bi4Cli4] and E8[MC16] (E = Se, Te; M = Zr, Hf) | | | | Abstract
| The title compounds were obtained by the reaction of elemental chalcogens E (E = Se, Te) with the respective tetrachlorides ECU and the Lewis acidic metal halides ZrCL, HfCU, and BiCfi. An alternative way, particularly for the preparation of mixed Se/Te-species, is the enlargement of smaller cationic rings in E4MC16] (M = Zr, Hf) by adding the respec tive complementary chalcogen. All reactions were carried out in sealed, evacuated glass am poules at temperatures between 120 °C and 220 °C, and yielded black crystals of SegfBijClu], (Te5.oSe3.o)[HfCl6], (Te5.3Se2.7)[ZrCl6], (Teft.sSei.sMZrCU] and Te8[HfCl6], which have been identified by crystal structure analyses. All five compounds contain eight-membered chalcogen rings in an endo-exo-conformation which are isostructural to the known octachalcogen dica tions E82+ (E = S, Se, Te). While in (Te5.0Se3.o)[HfCl6], (Te5.3Se2.7)[ZrCl6], (Te6.5Se,.5)[ZrCl6 _] and TesfHfClft] the molecular polycations are surrounded by discrete, octahedral [MClö]"-counterions, Se4 [Bi4CZT14] contains a two-dimensional polymeric anion ([Bi-jCl^ ] 2)" built of a variety of vertex and edge-sharing BiClv-polyhedra (x = 6 , 7). The Bi-Cl bond lengths are spread over a wide range between 250 and 350 pm. | | | |
Reference
| Z. Naturforsch. 54b, 1253—1259 (1999); received July 15 1999 | | | |
Published
| 1999 | | | |
Keywords
| Octaselenium(2+), Octatellurium(2+), Chalcogen Polycations, Halogenobismutates(III), Crystal Structure | | | |
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| default:Reihe_B/54/ZNB-1999-54b-1253.pdf | | | | Identifier
| ZNB-1999-54b-1253 | | | | Volume
| 54 | |
| 65 | Author
| D. Blaschette, PeterG. Jones | Requires cookie* | | | Title
| Polysulfonylamine, CXVII [1] | | | | Abstract
| Wasserstoffbrücken in kristallinen Onium-dimesylamiden: Sechs systematisch variierte s££.-Ammonium-dimesylamide mit sechs verschiedenen null-, ein-oder zweidimensionalen Wasserstoffbrückenmustern Polysulfonylamines, C X V II [1] H ydrogen B onding in Crystalline O n iu m Dimesylamides: Six Systematically Varied sec. -A m m onium Dimesylamides Exhibiting Six D ifferent Zero-, One-, or Two-Dimensional Hydrogen B onding Patterns O liver Moers, Karna W ijaya, D agm ar Henschel, A rm a n In order to examine packing preferences and hydrogen bond patterns in secondary ammo nium salts, low-temperature X-ray analyses were conducted for six compounds of general formula R^N H ^M eSO ^hN ", where R 2NH2 = Me2NH2 (1, triclinic, space group P I), | | | |
Reference
| Z. Naturforsch. 54b, 1420—1430 (1999); eingegangen am 13. Juli 1999 | | | |
Published
| 1999 | | | |
Keywords
| Di(methanesulfonyl)amide, Secondary Ammonium Cation, Crystal Structure, Hydrogen Bonding, Crystal Engineering | | | |
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| default:Reihe_B/54/ZNB-1999-54b-1420.pdf | | | | Identifier
| ZNB-1999-54b-1420 | | | | Volume
| 54 | |
| 66 | Author
| Dagmar Henschel, Oliver Moers, Karna Wijaya, Blaschette Arm, PeterG. Jones | Requires cookie* | | | Title
| Wasserstoffbrücken in kristallinen Onium-dimesylamiden: Drei prim. -Ammonium-dimesylamide mit zwei-oder dreidimensionalen Wasserstoffbrückenmustern Polysulfonylamines, CXVIII [1] Hydrogen Bonding in Crystalline Onium Dimesylamides: Three prim. -Ammonium Dimesylamides Exhibiting Two-or Three-Dimensional Hydrogen Bond Patterns | | | | Abstract
| In order to study hydrogen bonding patterns in primary ammonium salts and the hydrogen bond acceptor potential of the dimesylamide anion, low-temperature X-ray structures have been determ ined for the 1:1 salts R N H ^M eSC ^^N -, where R = Et (1, monoclinic, space | | | |
Reference
| Z. Naturforsch. 54b, 1431—1440 (1999); eingegangen am 13. Juli 1999 | | | |
Published
| 1999 | | | |
Keywords
| Di(methanesulfonyl)amide, Primary Ammonium Cation, Crystal Structure, Hydrogen Bonding, Ionic Self-Clathrate | | | |
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| default:Reihe_B/54/ZNB-1999-54b-1431.pdf | | | | Identifier
| ZNB-1999-54b-1431 | | | | Volume
| 54 | |
| 67 | Author
| K. Am, Wijaya, Oliver Moers, A. Rm, Blaschette, PeterG. Jones | Requires cookie* | | | Title
| Wasserstoffbrücken in kristallinen Onium-dimesylamiden: Ein antidromes Achtringmuster als robustes supramolekulares Synthon - Drei prototypische Strukturen Polysulfonylamines, CXIX [1, 2] Hydrogen Bonding in Crystalline Onium Dimesylamides: An Antidromic Eight-M embered Ring Pattern as a Robust Supramolecular Synthon - Three Prototypical Structures | | | | Abstract
| Syntheses and low-temperature X-ray structures are reported for three ionic solids of gen eral formula BH +(M eS 0 2)2N_, where B H + is 3,4,6,7,8,9-hexahydro-2//-pyrimido[l,2-tf]pyri-midinium (1, monoclinic, space group P 2 1/c), N,N'-diphenylformamidinium (2, monoclinic, P2xlc), or 2-phenylaminopyridinium (3, triclinic, P I, two independent formula units). As a common feature, the onium cations in question exhibit a difunctional hydrogen-bond donor sequence H -N -C (s p 2) -N -H geometrically complementary to an O -S -N fragment of the anion. Consequently, the three crystal packings consist of discrete cation-anion pairs (for mula units) assembled by an N -H --N and an N -H ---0 hydrogen bond. In both independ ent ion pairs of 3, the N -H ---N bond originates from the pyridinium centre and the N-H-O bond from the amino group. The eight-membered ring [graph set N2 = R2(8), antidromic] that results in all these prototypical structures has potential as a new and robust supramolecular synthon. In each case, short C-H-O contacts with H -O < 260pm and C-H-O ^ 140° are present; in 2, two Car-H ---0 hydrogen bonds are assisted by a C(formyl)-H -O contact and a n -n interaction to create a centrosymmetric formula unit dimer. | | | |
Reference
| Z. Naturforsch. 54b, 1441—1449 (1999); eingegangen am 13. Juli 1999 | | | |
Published
| 1999 | | | |
Keywords
| Di(methanesulfonyl)amide, Onium Cation, Crystal Structure, Hydrogen Bonding, Molecular Recognition, Supramolecular Synthon | | | |
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| default:Reihe_B/54/ZNB-1999-54b-1441.pdf | | | | Identifier
| ZNB-1999-54b-1441 | | | | Volume
| 54 | |
| 68 | Author
| G. Ernot, Heckm Ann3, Stefan Planka, Ekke Hard Fluckb, Dashti-M Anahita, Bernhard Ommertzc, Neumüllerc | Requires cookie* | | | Title
| 6-Pyridyl-l-aza-2A5,4/.5-diphosphinin - ein 2,2'-Bipyridin-Analogon 6-Pyridyl-l-aza-2/l5,4/l5-diphosphinine - a 2,2'-Bipyridine Analogue | | | | Abstract
| -Tetrakis(dimethylamino)-lA5,3A5-diphos-phete, (1), reacts with 2-cyano-pyridine to yield 6-pyridyl-l-aza-2/l5,4A5-diphosphinine (3). 3 is cha racterized by its 'H , 31P, and 13C NMR, mass, and IR spectra as well as the results of the X-ray struc ture analysis. | | | |
Reference
| Z. Naturforsch. 54b, 1478—1481 (1999); eingegangen am 23. August 1999 | | | |
Published
| 1999 | | | |
Keywords
| A5-Diphosphete, l-Aza-2A5, 4A5-diphosphinine, NMR D ata, Crystal Structure l, l, 3, 3 | | | |
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| default:Reihe_B/54/ZNB-1999-54b-1478_n.pdf | | | | Identifier
| ZNB-1999-54b-1478_n | | | | Volume
| 54 | |
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