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21Author    Stefan Horstmann, Wolfgang SchnickRequires cookie*
 Title    Synthese, Kristallstruktur und Eigenschaften von Tetraaminophosphoniumiodid [P(NH2)4]I Synthesis, Crystal Structure, and Properties of Tetraaminophosphonium Iodide [P(NH2)4]I  
 Abstract    The title compound has been prepared starting from phosphorothionic triamide SP(N H 2)3 by methylation of the sulfur atom and subsequent ammonolysis reaction in dry acetonitrile and dichloromethane, respectively, both at room temperature. Suitable single crystals are obtained from an acetonitrile solution in a temperature gradient between 70 °C and room temperature. The crystal structure o f [P(N H 2)4]I has been determined by single crystal X-ray methods (P 4!nbm\ a = 842.6(2), c = 486.7(2) pm, Z = 2). In the solid [P(NH2)4]+-and I~-ions are found with significant N -H -I -h y d r o g e n bonding interactions between anions and cations (H —I: 276.4 pm). The P -N -b o n d length in the cation (160.7(2) pm) represents the shortest P -N H 2 bond distance reported to date indicating a significant electrostatic strengthening. The condensation behaviour of [P(N H 2)4]I in solution and in the solid has been investigated. 
  Reference    Z. Naturforsch. 49b, 1381—1386 (1994); eingegangen am 5. Mai 1994 
  Published    1994 
  Keywords    Tetraaminophosphonium Salt, Synthesis, Crystal Structure, Hydrogen Bonding, Condensation Reactions 
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 TEI-XML for    default:Reihe_B/49/ZNB-1994-49b-1381.pdf 
 Identifier    ZNB-1994-49b-1381 
 Volume    49 
22Author    DietrichK. Breitinger, Roman BreiterRequires cookie*
 Abstract    ?ram-(NH4)2[R u (S 0 3)2(N H 3)4]-4 H 20 (1) (m onoclinic, P l x!n\ a = 629.8(3), b = 1000.6(2), c = 1345.7(5) pm, ß = 112.25(4)°, Z = 2; R = 0.021; R w = 0.017) is obtained as pale greenish-yellow crystals by reaction of /ra « s-[R u (S 0 3H)2(N H 3)4] (2) with aqueous ammonia, and crys­ tallization at +5 °C. The compound, when isolated, is stable at room temperature for only a few days even under inert gas, but persists under the mother liquor. In the centrosymmetric anion frö/?s-[Ru(S03)2(N H 3)4]2~ the bonds Ru-S = 230.5(1) pm are significantly longer than in the neutral complex 2 (227.6(1) pm), whereas the Ru-N bonds are the same in both com ­ plexes within experimental error (averages 214.1 and 214.0 pm). Hence, the mutual trans-influence of the sulfite ligands is weakened on protonation; the bonding of the co-ligands in c/s-position is not affected. The internal structure o f the sulfite ligand in 1 with long S-O bonds (average 151.2(5) pm) and small angles O-S-O (average 106.1(6)°) and the weakened Ru-S bond are a good match. The structure of 1 is held together by a complex network of hydrogen bonds, in which all potential hydrogen-bond donors (O H 2, N H 4+, N H 3) and accep­ tors (H 20 , S 0 3) are involved. The structural findings are reflected in the vibrational spectra. 
  Reference    Z. Naturforsch. 51b, 517 (1996); received August 25 1995 
  Published    1996 
  Keywords    Ruthenium(II) Sulfito Complex, Crystal Structure, m ws-Influence, Hydrogen Bonding 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0517.pdf 
 Identifier    ZNB-1996-51b-0517 
 Volume    51 
23Author    Thomas Dahlems, Dietrich Mootz, Michaela SchillingRequires cookie*
 Title    Zweidimensionales Eis und H50 2+-Ionen. Zur Bildung und Struktur tiefschmelzender molekularer und ionischer Hemi-bis Hexahydrate halogenierter Essigsäuren CCl"F3."COOH (n = 1 bis 3) [1] Two-Dimensional Ice and H 50 2+ Ions. On Formation and Structure of Low-Melting Molecular and Ionic Hemi-through Hexahydrates of Haloacetic Acids CCl"F3."COOH (n = 1 to 3) [1]  
 Abstract    Hydrate formation o f haloacetic acids CCl"F3_"COOH (n = 1, 2, 3) has been studied by D TA and tem perature-dependent X-ray powder diffraction, and evidence obtained for five phases, all melting at temperatures below ambient. The hydrates have been confirmed and further characterized by their crystal structures at -1 5 0 °C. Three lower hydrates, CC12F C O O H 0.5H -> 0 (space group P2,/c and Z = 8 formula unites per unit cell), CC1F2C 0 0 H H 20 (P2,/c, Z = 4), and CC1F2C 0 0 H -4 H 20 (P I, Z = 2), have molecular structures with the acid and water m olecules hydrogen-bonded in two-dimensional arrays. The structures of the remaining hydrates, CCl2F C O O H -6H 20 and CC13C 0 0 H -6 H 20 (sim i­ lar, but not isotypic, both P 1 and Z = 2), are ionic, as (H s0 2+)(C X 3C 0 Ö) -4 H 20 , and three-dimensional. The neutral water molecules are hydrogen-bonded in ice-like layers rare in crystal chemistry. A lso, CCl2FCOOH is established only as the second acid o f which a lower hydrate is molecular and a higher one ionic. 
  Reference    Z. Naturforsch. 51b, 536 (1996); eingegangen am 16. Oktober 1995 
  Published    1996 
  Keywords    Crystal Structure, Haloacetic Acid Hydrate, Hydrogen Bonding, Melting Diagram 
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 TEI-XML for    default:Reihe_B/51/ZNB-1996-51b-0536.pdf 
 Identifier    ZNB-1996-51b-0536 
 Volume    51 
24Author    Antje Albert, D. Ietrich, M. OotzRequires cookie*
 Title    Formation and Crystal Structures of the Hydrates of 18-Crown-6 [1]  
 Abstract    The melting diagram of the system 18-crown-6/water has been set up and the existence of four binary hydrates confirmed. Crystal structures have been determined for three of these, in addition to that for the hexahydrate already published. The hydrates are monoclinic, a tetrahydrate (previously reported as a 4.5-hydrate) with space group P2|/c and Z = 2 formula units per unit cell, an octahydrate with I2/a and Z = 4, and a dodecahydrate with P2i/n and Z= 2. In each structure the crown ether molecule has the (pseudo) D.^ conformation common for many of its complexes, and is immediately hydrogen-bonded by a group of four water molecules in a similar, characteristic pattern. In the tetrahydrate, with one of the waters disordered, the total connectivity is that of a 1D chain, while the overall structures of the octa-and dodecahydrate are 3D networks. Four of the six independent water molecules in the dodecahydrate are linked with each other into a rare 2D ice-like layer. 
  Reference    Z. Naturforsch. 52b, 615—619 (1997); received January 15 1997 
  Published    1997 
  Keywords    Crown Ether, Crystal Structure, Hydrate, Hydrogen Bonding, Melting Diagram 
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 TEI-XML for    default:Reihe_B/52/ZNB-1997-52b-0615.pdf 
 Identifier    ZNB-1997-52b-0615 
 Volume    52 
25Author    Stephanie Janeda, Dietrich Mootz, HerrnRequires cookie*
 Title    Niedere Hydrate aliphatischer primärer Amine. Neue Untersuchungen zu Bildung und Struktur [1] Lower Hydrates of Aliphatic Primary Amines. New Studies of Formation and Structure [1]  
 Abstract    After earlier work in this laboratory on lower hydrates of amines, the melting diagram of the system 1 ,8-diaminooctane/water and six new crystal structures of hemi-and monohydrates of terminal primary n-alkylamines and diamines have been determined. In the hydrates 1 -PrNH2 • 0.5 H20 (space group C 2/m with Z = 4 formula units per unit cell), l-HexNH2 • 0.5 H20 (PI, Z = 2) and H2N(CH2)nNH2 • H20 with n = 4, 6, 8 (P 2x/c, Z = 4), the O and N atoms are hydrogen-bonded into a two-dimensional array analogous to the mutual coordination of cations and anions in the Cdl2 structure type: [ON6/3] ~ [CdI6/3]. In the hydrate H2N(CH2)2NH2 • H20 (C 2/c, Z = 4), the H20/N H 2 partial structure is three-dimensional but can be reduced, by neglecting the longest H bond, to an array which is again just two-dimensional and related now to the red Hgl2 structure type: [ON4y2] ~ [HgI4/2], In all the monohydrates, the arrays as defined are crosslinked by the alkylene cnains of the bifunctional amine molecules. 
  Reference    Z. Naturforsch. 53b, 1197—1202 (1998); eingegangen am 22. Mai 1998 
  Published    1998 
  Keywords    Amine Hydrates, Hydrates, Melting Diagram, Crystal Structure, Hydrogen Bonding 
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 TEI-XML for    default:Reihe_B/53/ZNB-1998-53b-1197.pdf 
 Identifier    ZNB-1998-53b-1197 
 Volume    53 
26Author    Di, Stephanie Janeda, Dietrich MootzRequires cookie*
 Title    Di-bis Pentahydrate von fünf Alkylendiaminen. Eine Fallstudie zu ein-und zweidimensionalen Wasserpolymeren in Festkörpern [1]-to Pentahydrates of Five Alkylenediamines. A Case Study of One-and Two-Dimensional Water Polymers in Solids [1]  
 Abstract    The crystal structures of five low-melting hydrates of »-alkane-a,u;-diamines, H2N(CH2)"NH2 • x H20 , for short C" ■ x W, have been determined. As a common feature, the water molecules are mutually linked by hydrogen bonds O-H -O to form low-dimensional polymers. These are a meandering chain in C2 • 2 W (space group I 2la, Z -4 formula units per unit cell), a zig zag chain in C6 • 2 W (P 2,/c, Z = 2), a ribbon of consecutively condensed five-membered rings in C3 • 3 W (P 2,/c, Z = 4) and a layer of condensed and spiro-linked rings of varying size each in C7 • 3 W (P i, Z = 4) and C4 • 5 W (C 21c, Z = 4). Further hydrogen bonding, between the water polymers and the bifunctional amine molecules, leads to overall connectivities which are three-dimensional in each structure. 
  Reference    (Z. Naturforsch. 54b, 103—108 [1999]; eingegangen am 7. September 1998) 
  Published    1999 
  Keywords    Amine Hydrates, Hydrates, Melting Diagram, Water Polymers, Hydrogen Bonding 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0103.pdf 
 Identifier    ZNB-1999-54b-0103 
 Volume    54 
27Author    M. Athias, O. SengeRequires cookie*
 Title    Fixation o f Neutral M olecules in the Binding Cavity of Nonplanar Porphyrins -A Third Dodeca- phenylporphyrin Modification with NH -Solvent Hydrogen Bonding  
 Abstract    Reprint requests to Priv.-Doz. Dr. M. O. Senge. Fax: 0 3 0 -8 3 8 -4 2 4 8 . E-mail: mosenge@chemie.fu-berlin.de A third crystalline modification of dodecaphe-nylporphyrin is described in which the pyrrole ni­ trogen atoms are hydrogen-bonded to two etha­ nol molecules. This is the first crystallographic proof for the accessibility of nitrogen atoms in saddle-distorted free base porphyrins for hy­ drogen bonding. N o such coordination is possible in either planar or ruffled porphyrins. Thus, the possibility exists to utilize conformationally dis­ torted porphyrins for the binding of neutral m ole­ cules. 
  Reference    Z. Naturforsch. 54b, 821 (1999); received March 2 1999 
  Published    1999 
  Keywords    Porphyrins, Steric Strain, Conformational Flexi­ bility, Crystal Structure, Hydrogen Bonding 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0821_n.pdf 
 Identifier    ZNB-1999-54b-0821_n 
 Volume    54 
28Author    Christoph Mockenhaupt, Ralf Eßmanna, HeinzDieter LutzRequires cookie*
 Title    [Ni(NH3 )6]S0 4 : Kristallstruktur und Infrarotspektren [Ni(NH3)6]S 0 4: Crystal Structure and Infrared Spectra  
 Abstract    The crystal structure of [Ni(NH3)6]S 0 4 has been determined by single-crystal X-ray dif­ fraction (P2,/c; Z = 4; a = 705.0(1), b = 1195.2(2), c = 1180.0(2) pm, ß = 96.14(3)°; 2271 reflections; R x = 3.94%). In the hitherto unknown structure type, both the [Ni(NH3)6]2+ and the S 0 42-ions form chains along [100], The six crystallographically different ammine ligands of the distorted [Ni(NH3)6]2+ octahedra are involved in hydrogen bonds to six crystallographically equivalent S 0 42-ions (site symmetry C |). The strength of the hydrogen bonds differs strongly (i'od ° f matrix isolated N H 2D molecules: 2378 -2494 cm -1 , N -O distances: 272 -340 pm). The temperature evolution of the IR bands reveals the decrease of the dynamic orientational disorder of the N H 3 molecules with decreasing temperature. 
  Reference    Z. Naturforsch. 54b, 843—848 (1999); eingegangen am 8. März 1999 
  Published    1999 
  Keywords    Hexammine Nickel Sulfate, Ammoniates, Crystal Structure, IR Data, Hydrogen Bonding 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0843.pdf 
 Identifier    ZNB-1999-54b-0843 
 Volume    54 
29Author    Michael Schur, Astrid Gruhl, Christian Näther, Inke Jeß, Wolfgang BenschRequires cookie*
 Title    (CH3NH3)2Sb2S4, a New Thioantimonate(III) with Building Groups Stabilized by Hydrogen Bonds  
 Abstract    (CH3NH3)2Sb2S4 has been isolated from the reaction of antimony with sulfur in the presence of manganese in an ethanolic solution of methylamine under solvothermal conditions. Two pyramidal SbS? units are linked via common S-S edges to give dimeric Sb2S42-anions, which are joined via secondary Sb --S contacts of 3.074(2) and 2.975(2) A forming infinite 1 [SbS2]-^n chains consisting of edge-linked xp-SbS4 trigonal bipyramids. The cis configuration o? the Sb2S42-anions in the title compound is observed for the first time. A specific hydrogen-bonding pattern between the amino-hydrogen and the sulfur atoms stabilizes this configuration and gives rise to anionic layers separated by the methyl groups. 
  Reference    Z. Naturforsch. 54b, 1524—1528 (1999); received July 21 1999 
  Published    1999 
  Keywords    Thioantimonates, Solvothermal Synthesis, Crystal Structure, Hydrogen Bonding, Polymerie Anions 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-1524.pdf 
 Identifier    ZNB-1999-54b-1524 
 Volume    54 
30Author    Dietrich Mootz, Angelika Merschenz-QuackRequires cookie*
 Title    Zur Kenntnis der höchsten Hydrate der Schwefelsäure: Bildung und Struktur von H2S 0 4*6,5 H20 und H2S 0 4-8 H20 [1] On the Highest Hydrates of Sulfuric Acid: Formation and Structure of H 2S 0 4 -6.5 H 20 and H 2S 0 4-8 H 20 [1]  
 Abstract    The phase diagram of the system sulfuric acid-water in the range 80—100 mol % H20 was reinvestigated by low-temperature DTA and X-ray powder diffraction. The results are compared with other studies in the literature. The crystal structures of the hydrates H2S 0 4 • 6.5 H20 , melting incongruently at —54 °C, and H2S 0 4-8 H 20 (metastable) were determined to be those of oxonium salts, (H50 2)(H 70 3)S 0 4-1.5 H20 and (H50 2)2S 0 4-4 H20 , respectively. 
  Reference    Z. Naturforsch. 42b, 1231 (1987); eingegangen am 1. Juni 1987 
  Published    1987 
  Keywords    System H2S 0 4—H20, Sulfuric Acid, Hydrate Structures, Hydrogen Bonding, Oxonium Salts 
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 TEI-XML for    default:Reihe_B/42/ZNB-1987-42b-1231.pdf 
 Identifier    ZNB-1987-42b-1231 
 Volume    42 
31Author    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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 TEI-XML for    default:Reihe_B/47/ZNB-1992-47b-0263.pdf 
 Identifier    ZNB-1992-47b-0263 
 Volume    47 
32Author    C. Hristian, Robl, Stephanie HentschelRequires cookie*
 Title    Unendliche Y2(H2O)10[C6(COO)6]-Ketten in Y2[C6(COO)6] * 14H20  
 Abstract    Infinite Chains o f Y2(H2O)10[C6(COO)6] in Y 2[C6(COO)6] • 14H20 Colourless monoclinic single crystals of Y ^C ^C O O)^ • 14H20 were grown in aqueous silica gel (space group P 2 Jn, a = 847.5(1), b = 923.4(2), c = 1632.0(3) pm, ß = 100.33(1)°, Z = 2, 223 param eters, 1784 reflections, Rg = 0.0357). Y 3+ is coordinated by 5 water molecules and 3 oxygen atom s o f the mellitate anion in a dodecahedral fashion. Y 3+ and [C6(COO)6]6-ions are linked by coordinative bonds, yielding infinite chains o f com position Y 2(H 2O)10[C6(COO)6] extending parallel to [100], Hydrogen bonds connect adjacent chains. 
  Reference    Z. Naturforsch. 47b, 1561—15 (1992); eingegangen am 5. M ärz 1992 
  Published    1992 
  Keywords    Y ttrium Mellitate, X-Ray, Chain Structure, Hydrogen Bonding, Differential Thermal Analysis 
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 TEI-XML for    default:Reihe_B/47/ZNB-1992-47b-1561.pdf 
 Identifier    ZNB-1992-47b-1561 
 Volume    47 
33Author    Tetramethylammoniumfluorid Bildung, Wasserstoffbrückenbindung Struktur, Dieter Stäben, Dietrich MootzRequires cookie*
 Title    Die kristallinen Hydrate  
 Abstract    The melting diagram of the system M e4N F -H 20 in the region 50-100 mol% H zO has been investigated for the first time, using D T A , D SC and tem perature-dependent X-ray powder diffraction. Four crystalline hydrates M e4N F\*H 20 were found, with x = 1 ,2 .3 3 ,4 and 5, which decom pose irreversibly above ca. 160 °C and m elt incongruently at 36 °C, congruently at 46 °C and again incongruently at 10 °C, respectively. The crystal structure o f each hydrate, except the already known one of the tetrahydrate, has b een determ ined with M oK a diffractom eter data. The monohydrate is rhombohedral with space group R3m and Z = 6 formula units per unit cell (hexagonal axes), the 2.33-hydrate m onoclinic with P2j/n and Z = 12, and the pen-tahydrate tetragonal with 142 m and Z = 2. The hydrogen-bonded H 20/F ~ structure is an iso­ lated centrosymmetric [F2(H 20) 2]2_ four-m em bered ring in the m onohydrate, a rather open three-dim ensional network in the 2.33-hydrate and a corrugated dense layer o f fused five-mem bered rings in the pentahydrate. 
  Reference    Z. Naturforsch. 48b, 1057—57 (1993); eingegangen am 5. April 1993 
  Published    1993 
  Keywords    Tetramethylamm onium Fluoride, Fluoride Hydrates, M elting Diagram, Crystal Structure, Hydrogen Bonding 
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 TEI-XML for    default:Reihe_B/48/ZNB-1993-48b-1057.pdf 
 Identifier    ZNB-1993-48b-1057 
 Volume    48 
34Author    Michael Born, Dietrich Mootz, Sigrid SchaefgenRequires cookie*
 Title    Tautomere Wasserschichten. Bildung und Struktur tiefschmelzender Trihydrate von Triethylamin und 4-Methylpyridin [1] Tautomeric Water Layers. Formation and Structure of Low-Melting Trihydrates of Triethylamine and 4-Methylpyridine [1]  
 Abstract    Low-melting trihydrates of triethylamine (E t3N) and 4-methylpyridine (4-M ePy) have been confirmed and detected by phase analysis and the crystal structures determined. Both are monoclinic with space group P 2!/c and Z = 4 formula units per unit cell. The lattice parameters are a = 13.606, b = 6.291, c = 12.412 A , and ß = 99.47° at -1 0 0 °C for Et3N -3 H 20 , and a = 9.982, b = 6.877, c = 12.958 Ä , and ß = 103.50° at -9 0 °C for 4-M eP y-3 H20 . The water m olecules in the two structures are hydrogen-bonded in condensed four-, five-, and six-membered rings with 1:2:1 ratio, thus forming characteristic layers parallel (1 0 0) of identical topology and tautomeric to each other. The amine m olecules are linked to both sides of the layers by O -H — N bonds from different O atoms. 
  Reference    (Z. Naturforsch. 50b, 101—105 [1995]; eingegangen am 11. August 1994) 
  Published    1995 
  Keywords    Am ine Hydrates, Crystal Structure, Hydrates, Hydrogen Bonding, M elting Diagram, Water Layers 
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 TEI-XML for    default:Reihe_B/50/ZNB-1995-50b-0101.pdf 
 Identifier    ZNB-1995-50b-0101 
 Volume    50 
35Author    Saalfrank, JochenN. Achtrab, Stephan Reck, Frank HampelRequires cookie*
 Title    Synthese und Aggregatbildung eines 5-Hydroxy-2,5-dihydropyrrols. Enantiomerenreine, eindimensionale Stränge durch Wasserstoff- brückenbindungen und chiroselektive Selbstorganisation [1]  
 Abstract    Synthesis and A ggregation o f a 5-H ydroxy-2,5-dihydropyrrole. E nantiom erically Pure, O ne-dim ensional Strands via Hydrogen Bonds and Chiroselective S eif O rganization [ 1 ] R olf W. Reaction of dimethyl 1,3-acetonedicarboxylate 8 with oxalylchloride 2 and magnesium chlo­ ride as catalyst yielded 2,3-dioxo-2,3-dihydrofuran 9, which is in equilibrium with tautomer 10 (9:10 = 1:2). Addition of thionyl chloride to a mixture of 9/10 afforded 3-chloro-2(5H)-furanone 11. The structure of 11 was unequivocally established by X-ray diffraction, which indirectly pro­ ved the structure of 10 as well. Ring opening of 11 by nucleophilic attack with benzylamine 14 in C2-position and subsequent recyclization led to racemic 3-chloro-5-hydroxy-2-oxo-2,5-di-hydropyrrole 15. According to a single crystal X-ray analysis, 15 aggregates via stereospecific self selection through hydrogen bonds to give chiroselectively the one-dimensional strands 1 1(S)-15] and I [(R)-1SI 
  Reference    Z. Naturforsch. 54b, 179—186 (1999); eingegangen am 28. September 1998 
  Published    1999 
  Keywords    2(5H)-Furanones, Hydrogen-Bonding, Chiral Recognition, One-Dimensional Strand, Crystal Structure 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0179.pdf 
 Identifier    ZNB-1999-54b-0179 
 Volume    54 
36Author    Biing-Chiau Tzeng, Johann Zank, Annette Schier, Hubert SchmidbaurRequires cookie*
 Title    The Structural Chemistry of GoId(I) Quinoline-2-thiolate and Iodide Complexes of Polytertiary Phosphines  
 Abstract    Treatment of (chloro)gold(I) complexes of di-and tetra-tertiary phosphines with equivalent quantities of sodium quinoline-2-thiolate in methanol / dichloromethane affords the correspond­ ing (phosphine)gold(I) quinoline-2-thiolates in high yields. The di-and tetranuclear complexes, respectively, of a,u>bis(diphenylphosphino)-propane (1), -butane (2) and -pentane (3) and of tris(2-diphenylphosphino-ethyl)phosphine (4) have been obtained as crystalline solids, and the structures of 2 and 4 have been determined by single crystal X-ray diffraction studies. Un­ expectedly, the molecules of 2 are loosely aggregated into strings via weak intermolecular gold-sulfur, not via Au-Au interactions. Compound 4 is a monomeric tetranuclear cluster in the solid state with two intramolecular gold-gold bonds. Bis(2-diphenylphosphino-ethyl)-phenylphosphine (PPP) forms trinuclear complexes with gold(I) chloride, bromide and iodide (5a -c). The iodide complex features a chain structure through intermolecular Au -Au contacts between the two terminal P-Au-I units. The closest contacts between the chains are determined by Au-I and I -I interactions of the central P-Au-I unit. 
  Reference    Z. Naturforsch. 54b, 825—831 (1999); received April 19 1999 
  Published    1999 
  Keywords    Gold(I) Complexes, Thiolate Complexes, Aurophilicity, Hydrogen Bonding, Polytertiary Phos-phine Complexes 
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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-0825.pdf 
 Identifier    ZNB-1999-54b-0825 
 Volume    54 
37Author    D. Blaschette, PeterG. JonesRequires 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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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-1420.pdf 
 Identifier    ZNB-1999-54b-1420 
 Volume    54 
38Author    Dagmar Henschel, Oliver Moers, Karna Wijaya, Blaschette Arm, PeterG. JonesRequires 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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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-1431.pdf 
 Identifier    ZNB-1999-54b-1431 
 Volume    54 
39Author    K. Am, Wijaya, Oliver Moers, A. Rm, Blaschette, PeterG. JonesRequires 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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 TEI-XML for    default:Reihe_B/54/ZNB-1999-54b-1441.pdf 
 Identifier    ZNB-1999-54b-1441 
 Volume    54