| | 61 | Author
| Joachim Pickardt, Norbert Rautenberg | Requires cookie* | | | Title
| Die Kristallstruktur von Hexa- The Crystal Structure of Hexa-^-chloro-/^- oxo-tetrakis [hexamethylenetetraminecopper- (II)], [Cu4Cl60(C6H12Nl)4], a Copper(II) Complex with a Structure Related to that of Beryllium Oxoacetate  | | | | Abstract
| -tetrakis [hexamethy lentetramin -kupfer(II)], [CU4C160(C6H12N4)4], einem Kupfer(II)-Komplex mit Berylliumoxoace-tat-ähnlicher Struktur By reaction of solutions of CuCl2 • 2H20 and hexamethylenetetramine, C6H12N4, in acetone, a complex [Cu4Cl60(C6Hi2N4)] could be ob-tained as single crystals. An X-ray analysis shows that the complex has a structure related to that of basic beryllium acetate. An oxygen atom is tetrahedrally surrounded by four cop-per atoms which, together with six chlorine atoms, form an adamantane-like core. Each copper atom is bonded via a nitrogen atom to a hexamethylenetetramine molecule. | | | |
Reference
| Z. Naturforsch. 37b, 1355—1357 (1982); eingegangen am 28. Juni 1982 | | | |
Published
| 1982 | | | |
Keywords
| Copper(II) Complexes, Chloro Complexes, Hexamethylenetetramine, X-ray | | | |
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| default:Reihe_B/37/ZNB-1982-37b-1355_n.pdf | | | | Identifier
| ZNB-1982-37b-1355_n | | | | Volume
| 37 | |
| 62 | Author
| Beatrix Milewski-Mahrla, Hubert Schmidbaur | Requires cookie* | | | Title
| Synthese und Kristallstrukturen einiger Tetramethylstibonium-Hydrogendicarboxylate Synthesis and Crystal Structures of Some Tetramethylstibonium Hydrogendicarboxylates | | | | Abstract
| Reactions of pentamethylantimony (CH^sSb with carboxylic acids in the molar ratio 1:2 afford one equivalent of methane and essentially quantitative yields of crystalline tetramethylstibonium hydrogendicarboxylates. Six new compounds of this series have been synthesized using benzoic, o-phthalic, salicylic, 4-ethoxy-salicylic, oxalic, and malic acid, and characterized by analytical and spectroscopic data. An ionic structure with strong hydrogen bonds in the anionic components is proposed. The crystal structures of the hydrogen-dibenzoate (1), hydrogen-ortho-phthalate (2) and 4-ethoxy-hydrogen-salicylate (3) were determined by single crystal X-ray diffraction. The compounds can be described as having ionic lattices with some donor-acceptor inter-actions between the stibonium centers and the carboxylate oxygen atoms. The anions are characterized by strong hydrogen bonds O...H...O. Thus, the (CH^Sb-tetrahedron in 1 is distorted by two benzoate oxygen atoms (at 304(2) and 340(2) pm). The cation in 2 is largely undistorted and the anion has a bydrogenpbthalate hydrogen bond of d(O...H...O) = 232 pm. The cation-anion contact in 3 is as short as d(Sb-O) = 289 pm rendering the Sb atom pentacoordinate. | | | |
Reference
| Z. Naturforsch. 37b, 1393—1401 (1982); eingegangen am 5. Juli 1982 | | | |
Published
| 1982 | | | |
Keywords
| Pentamethylantimony, Tetramethylstibonium Salts, Hydrogendicarboxylates, Hydrogen Bonding, X-ray | | | |
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| default:Reihe_B/37/ZNB-1982-37b-1393.pdf | | | | Identifier
| ZNB-1982-37b-1393 | | | | Volume
| 37 | |
| 63 | Author
| Günter Schmid, Roland Boese | Requires cookie* | | | Title
| Azaborolinyl Complexes, IX [1] The Crystal and Molecular Structures of Two Isomers of Bis(l-ter£-butyl-2-methyl-??-l,2-azaborolinyl)cobalt | | | | Abstract
| The crystal and molecular structures of two isomers of bis(l-£er£-butyl-2-methyl-??-l,2-azaborolinyl)cobalt have been determined by single-crystal X-ray diffraction methods. Isomer 1 shows a clockwise, isomer 2 an anti-clockwise conformation of the azaborolinyl rings. In both compounds the azaborolinyl rings have staggered orientations with opposite positions of the tferi-butyl groups. The rings in 1 and 2 are slipped so that the three ring carbon atoms are closer to the cobalt atom than the BN groups. The staggered orientation of the ligands in 2 is probably due to a packing effect, as in similar sandwich complexes the anti-clockwise conformers show eclipsed orientation. | | | |
Reference
| Z. Naturforsch. 38b, 485—492 (1983); eingegangen am 12. November 1982 | | | |
Published
| 1983 | | | |
Keywords
| Azaborolinyl Sandwich Complexes, Cobalt, Isomers, X-Ray | | | |
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| default:Reihe_B/38/ZNB-1983-38b-0485.pdf | | | | Identifier
| ZNB-1983-38b-0485 | | | | Volume
| 38 | |
| 65 | Author
| Werner Winter, Reinhard Merkel, Udo Kunze | Requires cookie* | | | Title
| Koordinationschemie funktioneller Phosphorylide, V [1] Die Molekülstrukturen der isomorphen Mangan-und Rheniumbromtricarbonyl- komplexe von 2-Methyl-2-(triphenylphosphonio)dithiopropionat Coordination Chemistry of Functional Phosphorus Ylides, V [1] The Molecular Structures of the Isomorphous Manganese and Rhenium Bromotricarbonyl Complexes of 2-Methyl-2-(triphenylphosphonio)dithiopropionate | | | | Abstract
| The isomorphous crystal structures of the manganese and rhenium bromotricarbonyl complexes 2 a, b have been determined at room temperature (Mn) and at —110 °C (Mn, Re; P2x/c, Z — 4). At room temperature, data collection is accompanied by crystal decomposi-tion, and a cleavage of the PPh3 group is suggested by the results as the primary process. The same initial step is thought to be valid for the photodecomposition in solution. The main structural difference between the free and coordinated betaine ligand 1 is the reduced electrostatic interaction of P and S in the complexed form. Einführung | | | |
Reference
| Z. Naturforsch. 38b, 747—751 (1983); eingegangen am 20. März 1983 | | | |
Published
| 1983 | | | |
Keywords
| Manganese, Rhenium, Betaine Complexes, Dithiocarboxylate Complexes, X-Ray | | | |
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| default:Reihe_B/38/ZNB-1983-38b-0747.pdf | | | | Identifier
| ZNB-1983-38b-0747 | | | | Volume
| 38 | |
| 66 | Author
| Klaus Brodersen, Hans-U Hummel | Requires cookie* | | | Title
| Die Kristallstrukturell von CaHg(SCN)4 * /ili20 (n = 2,3). Verwandtschaftsbeziehungen zwischen den Verbindungsklassen der Tetrathiocyanatomercurate(II) von Erdalkaliionen und 3 d-Metallionen The Crystal Structures of CaHg(SCN)4 * MH20 (n = 2, 3). Relations between Tetrathiocyanatomercurates(II) of the Alkaline-Earth-Ions and Ions of the 3 d-Type | | | | Abstract
| CaHg(SCN)4 • nH20 (n — 2(1), n = 3(2)) were isolated from an aqueous solution of Ca(NCS)2 • 4H20 and Hg(SCN)2. 1 is compared with the analogous MgHg(SCN)4 • 2H20 by means of powder patterns. The crystal structure of 2 has been determined. 2 is mono-clinic, space group P2i/c with a = 9.469(4), 6 = 22.781(5), c = 6.587(4) A, 0 = 93.6(3)°, Z = 4, dc = 2.46 g-cm -3 . The structure was refined to .ß=7.42 and i?w = 4.96% for 1224 independent reflec-tions. The species MHg(SCN)4 • 2H20 (M = Mg, Ca, Ni) contain nearly tetrahedral Hg(SCN)4 and octahedral M(OH2)2(NCS)4 groups which are joined by Hg-SCN-M bridges. In contrast the structures of the other compounds MHg(SCN)4 • nH20 (M = Co, n = 0; M = Ca, Sr, n = 3) are based on the diamond net. There is tetrahedral coordination of all the metal atoms, M having 4 N and Hg 4 S nearest neighbours. In the hydrates the H20 molecules are situated additionally at the Ca and Sr atoms [*]. | | | |
Reference
| Z. Naturforsch. 38b, 911—916 (1983); eingegangen am 20. April 1983 | | | |
Published
| 1983 | | | |
Keywords
| Calciumtetrathiocyanatomercurates(II), Dihydrate, Trihydrate, X-Ray | | | |
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| default:Reihe_B/38/ZNB-1983-38b-0911.pdf | | | | Identifier
| ZNB-1983-38b-0911 | | | | Volume
| 38 | |
| 67 | Author
| KurtH. Pilgram, LairdH. Gale, GlennE. Pollard | Requires cookie* | | | Title
| a-hydroxyphostones | | | | Abstract
| The addition-cyclocondensation reactions of three /?-hydroxyketones with four dialkyl phosphites gave 2-alkoxy-3-hydroxy-l,2-oxaphospholane-2-oxides ("a-hydroxyphosto-nes") (7), in moderate yields. In the solid state and in solution, these compounds exist as dimers with hydrogen bonding between the hydroxyl group and the phosphoryl oxygen atom of an adjacent molecule. The crystal and molecular structure of 3-hydroxy-2-methoxy-3,5,5-trimethyl-l,2-oxaphospholane-2-oxide (7 a) has been determined by single-crystal X-ray crystallography: C7H15O4P, monoclinic space group P2-l/n, cell dimensions a = 8.087(1) Ä, b = 13.386(2) A, c = 9.306(1) A, V = 1007.4 Ä 3 , Z = 4, final R = 0.052. The five-membered ring is puckered, with the carbon bearing the OH and CH3 groups lying out of the plane of the remaining four atoms in the ring. The doubly bonded oxygen attached to the phosphorus atom and the hydroxyl oxygen are in a cis-relationship. The 0(l)-0(4) intermolecular bond distance of 2.75 Ä suggests hydrogen bonding. The 0(1)-H(1) intermolecular bond distance of 1.97 Ä is consistent with this conclusion. Thorough synthetic studies have been carried out on intramolecular esters of 3-hydroxyalkane (and alkene) phosphonic and phosphinic acids (phosto-nes [1]). For example, dehydration of 3-hydroxy-alkanephosphonic acids gave phostones of general structure 1 [2] (Table I). Similar phostones, 2 and 3, were obtained from the reactions of 1,3-dihalo-alkanes with phosphonites and phosphinites, re-spectively [3]. At elevated temperature, 3-bromo-alkanephosphonates are converted into phostones 4 [4]. Acyl-lactone rearrangement of a-acetyl-a-diethoxyphosphonylbutyrolactone gave 5 [5]. Unsaturated phostones (8) are obtained by dehydration of the corresponding (3-hydroxy-3-phenyl-prop-2-enyl)phosphonic acids [6]. 3-Hy-droxypropenylphosphonates, prepared by catalytic reduction of 3-hydroxy-l-propynyl-phosphonates, cyclocondense to 9 having potent Cholinesterase inhibitory activity [7]. The reaction of dialkyl 1,2-alkadienylphosphonates with halogens [8-10] and sulfenyl chlorides [12] gave 10. In the reaction of 3-methyl-l,2-butadienephos-phonyl di chloride with halogens, unsaturated tetra-halophostones (11), are formed [13]. The chlorina-tion of 2-methyl-2,3,5-hexatriene-4-phosphonyl di-chloride proceeds similarly in the direction of cyclo-dechlorination to form 12 [14]. | | | |
Reference
| Z. Naturforsch. 38b, 1122—1129 (1983); received May 6 1983 | | | |
Published
| 1983 | | | |
Keywords
| X-Ray, Stereochemistry, Hydrogen Bonding, Dimerization | | | |
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| default:Reihe_B/38/ZNB-1983-38b-1122.pdf | | | | Identifier
| ZNB-1983-38b-1122 | | | | Volume
| 38 | |
| 68 | Author
| Paul Klingelhöfer, Ulrich Müller, HansG. Ünter Hauck, Kurt Dehnicke | Requires cookie* | | | Title
| ReCl5 * OPCl3; IR-Spektrum und Kristallstruktur ReCl5 -O PCl3; IR Spectrum and Crystal Structure | | | | Abstract
| Single crystals of ReCl5 • OPCl3 were obtained by cooling a saturated solution of rheniumpen tachloride in phosphorylchloride. It formes black needles, which are extremely sensitive to mois ture. In the IR spectrum v(PO) is shifted downwards by 140 cm-1 in comparison with liquid POCl3, indicating coordination via oxygen. The crystal structure was solved and refined from X-ray diffraction data (space group Pnma, four formula units per unit cell, a = 1629, b = 790, c = 877 pm, 902 observed, independent reflexions, R = 0.040). The complex forms discrete molecules ReCl5 • OPC1, with symmetry Cs (m). Bond lengths are Re —O — 214 pm and P —O = 146 pm, the angle Re —O —P is 143°. | | | |
Reference
| Z. Naturforsch. 39b, 135 (1984); eingegangen am 8. September 1983 | | | |
Published
| 1984 | | | |
Keywords
| Preparation, IR Spectra, X-Ray, Rheniumpentachloride Phosphorylchloride Adduct | | | |
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| default:Reihe_B/39/ZNB-1984-39b-0135.pdf | | | | Identifier
| ZNB-1984-39b-0135 | | | | Volume
| 39 | |
| 69 | Author
| Joseph Grobe, G. Erald, H. Enkel, B. Ernt Krebs, Nikolaos Voulgarakis | Requires cookie* | | | Title
| Atran-analoge Verbindungen des Typs Me(R)SiSiMe (OCH2CH2)2N I I (I) o | | | | Abstract
| c h 2 Atrane Analogous C om pounds of the Type M e(R)SiSiM e (OCH->CH2)?N I 1 (1) Heterocyclic cage compounds of type I (compounds 8—10) have been prepared by condensa tion reactions of 1,2,2-trifunctional disilanes M e(R)XSiSiM eX2 (R = Me, Ph, OEt; X = NMe2, OEt) with triethanolamine using the "Dilution Principle". The starting compounds are obtained by Si—Me cleavage of Si2Me6 with acetylchloride/AlCl3 followed by either aminolysis with HNMe2 or alcoholysis with EtOH. 'H NMR spectra indicate N—*Si(l) intraction with the more acidic Si | | | |
Reference
| Z. Naturforsch. 39b, 341—351 (1984); eingegangen am 30. August/26. Oktober 1983 | | | |
Published
| 1984 | | | |
Keywords
| Silatranes, Transanular N — * Si-Interactions, NMR Spectra, X-Ray | | | |
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| default:Reihe_B/39/ZNB-1984-39b-0341.pdf | | | | Identifier
| ZNB-1984-39b-0341 | | | | Volume
| 39 | |
| 70 | Author
| Klaus Blechschmitt, Ernst Guggolz, ManfredL. Ziegler | Requires cookie* | | | Title
| Reaktiviät von Metall—Metall-Mehrfachbindungen, II [1] Nukleophile Addition von Methylensulfiden an [CpMo(CO) | | | | Abstract
| 2 ]2 unter Bildung von Cp(CO) 2 Mo(|*-S(CH 2)")Mo(CO) 2 Cp-Spezies; Röntgenstrukturanalyse von Cp(CO) 2 Mo(i n-S(CH 2) 6)Mo(CO) 2 Cp Reactivity of Metal-Metal Multiple Bonds, II [1] Nucleophilic Addition of Methylenesulfides to [CpMo(CO) 2 ]2 with Formation of Cp(CO) 2 Mo(M-S(CH 2)") Mo(CO) 2 Cp Spezies; X-Ray Structure Analysis of Cp(CO) 2 Mo(w-S(CH 2) 6)Mo(CO) 2 Cp The triply Mo-Mo bonded molecule [Cp(CO) 2 Mo] 2 was reacted with the cyclic sulfides S(CH 2)" (n = 4-6). The species Cp(CO) 2 Mo(w-S(CH 2)")Mo(CO) 2 Cp were isolated and charac-terized by their analytical and spectroscopic data. X-Ray structure analysis of the compound Cp(CO) 2 Mo(w-S(CH 2) 6)Mo(CO) 2 Cp proved the cyclic sulfide to act as a bridging ligand. | | | |
Reference
| (Z. Naturforsch. 40b, 85—89 [1985]; eingegangen am 2. August/6. November 1984) | | | |
Published
| 1985 | | | |
Keywords
| Synthesis, Metal-Metal Multiple Bonds, X-Ray | | | |
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| default:Reihe_B/40/ZNB-1985-40b-0085.pdf | | | | Identifier
| ZNB-1985-40b-0085 | | | | Volume
| 40 | |
| 71 | Author
| A. Döhring, P. W. Jolly, C. Krüger, M. J. Romão | Requires cookie* | | | Title
| The Ni(0)—C0 2 System: Structure and Reactions of [Ni(PCy 3 ) 2 (i/ 2 -C0 2 )] | | | | Abstract
| The reactions of a variety of bis(tricyclohexylphosphine)nickel species with C0 2 have been studied. The product of the reaction is solvent dependent: in toluene the known complex [NiL 2 (/7 : -C0 2)]-toluene (L = PCy 3) is formed while in ether or pentane a binuclear complex [(NiL 2) 2 (?;-C0 2)] results through the intermediacy of the solvent free species [NiL 2 (// 2 -C0 2)] the structure of which has been determined by X-ray crystallography. | | | |
Reference
| Z. Naturforsch. 40b, 484—488 (1985); received November 30 1984 | | | |
Published
| 1985 | | | |
Keywords
| Carbon Dioxide Complexes, Nickel, X-Ray | | | |
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| default:Reihe_B/40/ZNB-1985-40b-0484.pdf | | | | Identifier
| ZNB-1985-40b-0484 | | | | Volume
| 40 | |
| 72 | Author
| Ekkehard Lindner, Fritz Zinßer, HermannAugust Mayer, Wolfgang Hiller, Riad Fawzi | Requires cookie* | | | Title
| Darstellung und Eigenschaften von und Reaktionen mit metallhaltigen Heterocyclen, XLVII [1] Einschiebungsreaktionen von phasentransferkatalytisch in situ erzeugten Dihalocarbenen in P-haltige Manganacycloalkane — Struktur und chemisches Verhalten der Reaktionsprodukte Preparation and Properties of and Reactions with Metal-Containing Heterocycles, XLVII [1] Insertion Reactions of Phase-Transfer-Catalytically in situ Generated Dihalocarbenes into P-Containing Manganacycloalkanes — Structure and Chemical Behaviour of the Reaction Products | | | | Abstract
| The phase-transfer-catalytically in situ generated dihalocarbenes CC1 2 and CBr 2 are inserted into a ß-C—H bond of the five-and six-membered phosphamanganacycloalkanes (OC) 4 MnPPh 2 (CH 2)"CH 2 CH 2 (la, b) [n = 1(a), 2(b)] to give the functionalized metallacycles (OC) 4 MnPPh 2 (CH 2)"CH(CHX 2)CH 2 (2a, a', b, b') [X = Cl: n = l(a), 2(b); X = Br: n = l(a'), 2(b')]. 2b crystallizes in the orthorhombic space group Pbca with Z = 8 and has a distorted chair conformation with equatorial position of the CHC1 2 group. The envelope conformation of 2a in solution was elucidated by means of 'H and 13 C{'H} NMR spectroscopic investigations. | | | |
Reference
| Z. Naturforsch. 40b, 615—623 (1985); eingegangen am 20. Dezember 1984 | | | |
Published
| 1985 | | | |
Keywords
| Dihalocarbene Insertion, Manganacycloalkanes, X-Ray, NMR Spectra | | | |
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| default:Reihe_B/40/ZNB-1985-40b-0615.pdf | | | | Identifier
| ZNB-1985-40b-0615 | | | | Volume
| 40 | |
| 75 | 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 | |
| 76 | Author
| Gerhard Bremer3, Roland Boeseb, Mustafa Keddoa, Thomas Kruck3 | Requires cookie* | | | Title
| Dialkylchalkogenidverbrückte Carbonylzweikernkomplexe des Typs | | | | Abstract
| [M]2ER2 mit M = {CpMn(CO)2} und {Cr(CO)5}; E = S, Se, Te; R = Me oder R2 = (CH2)3 bzw. (CH2)4; Röntgenstrukturanalyse von [CpMn(CO)2]2S(CH2)3 Dialkylchalcogenide-Bridged Dinuclear Carbonyl Complexes of the Type [M]2ER2 with M = {CpMn(CO)2} and {Cr(CO)5}; E = S, Se, Te; R = Me or R2 = (CH2)3, (CH2)4; X-Ray-Structure Analysis of [CpMn(CO)2]2S(CH2)3 The reaction o f C pM n(C O)2T H F or C r(C O)sT H F with alkylchalcogenides E R 2 (E = S, Se, Te; R = M e or R 2 = (C H 2)3, (C H 2)4) in the molar ratio of 2:1 gives alkylchalcogenide-bridged dinuclear com plexes [C pM n(C O)2]2E R 2 and [C r(C O)5]2E R 2. The heteronuclear com plex C p (C O)2Mn — (u-SM e2) -C r (C O) 5 can be synthesized by reacting C pM n(C O)2SM e2 with C r(C O)5TH F. X-ray structure analysis o f the com pound [CpM n(CO)2]2S(C H 2) 3 dem onstrates the bridging character o f the alkylchalcogenides. | | | |
Reference
| Z. Naturforsch. 41b, 981—986 (1986); eingegangen am 24. Februar/25. April 1986 | | | |
Published
| 1986 | | | |
Keywords
| Synthesis, C halcogenide-Bridged Carbonyl C om plexes, X-Ray | | | |
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| default:Reihe_B/41/ZNB-1986-41b-0981.pdf | | | | Identifier
| ZNB-1986-41b-0981 | | | | Volume
| 41 | |
| 77 | Author
| Richard Neidlein, Dagmar Knecht, Alfred Gieren, Catalina Ruiz-Pérez | Requires cookie* | | | Title
| | | | | Abstract
| The synthesis of 1 by reaction of phenanthro[9,10-c]-l,2,5-selenadiazole with ethylmagnesium-bromide and TeCI 4 is described; the X-ray structure analysis is reported. | | | |
Reference
| (Z. Naturforsch. 42b, 84—90 [1987]; eingegangen am 9. August 1986) | | | |
Published
| 1987 | | | |
Keywords
| Chalkogen-Diimides, 1, 2, 5-Telluradiazole, X-Ray | | | |
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| default:Reihe_B/42/ZNB-1987-42b-0084.pdf | | | | Identifier
| ZNB-1987-42b-0084 | | | | Volume
| 42 | |
| 78 | Author
| W. S. Sheldrick, P. Bell | Requires cookie* | | | Title
| Interaction of Metal Ions with 7-Deaza-8-aza-and 8-Aza-purines Preparation and X-Ray Structural Analysis of Copper(II) Complexes | | | | Abstract
| The reaction of 8-aza-and 7-deaza-8-aza-purines with Cu :+ cations in acid solution has been studied. At a pH value of 2, the 8-azaadenine complex [Cu(H 2 0) 4 (AAdH) 2 ](N0 3) 2 (1), which displays Cu-N9 coordination, may be isolated from solution. The reaction of CuCl 2 with 8-aza-hypoxanthine in concentrated HCl solution leads to ring opening at C 2 of the azapurine with subsequent formation of dichlorobis[(5-amino-4-carboxamide)[l — 3]triazole] copper(II) dihydrate 2, in which the triazole ligands display a chelating function, coordinating the metal via N7 and 06. The results for 1 and 2 suggest that copper coordination of the azapurine base is not a prerequisite for opening of the pyrimidine ring. Respectively N9-and N8-coordinated complexes [CUC13(A11H3)]" 3 and [CuCl 2 (H 2 0)(MAllH)] n (4) of allopurinol (A11H 2) and 9-methylallopurinol (MA11H) may be prepared by the reaction of CuCl 2 with the respective bases in HCl solution. In contrast, with the analogous l-methyl-4-aminopyrazolo[3,4-d]pyrimidine MAPP, only the salt (MAPPH)4(CU2C18) (5) could be isolated under similar conditions, indicating that N8 is less attractive as a binding site in this 7-deaza-8-azaadenine derivative. The structures of 1—5 have been established by X-ray structural analysis. A distorted octahedral [4+2]geometry is found for the copper atoms in 1 and 2. Chlorine bridged polymeric chain structures are adopted by the complexes 3 and 4. An intermediate coordination geometry between trigonal bipyramidal and square-pyrami-dal is observed for the metal atoms in 3, a distorted square-pyramidal geometry in 4. | | | |
Reference
| Z. Naturforsch. 42b, 195—202 (1987); received August 18/October 17 1986 | | | |
Published
| 1987 | | | |
Keywords
| 8-Azapurines, Allopurinol, Copper(II) Complexes, X-Ray | | | |
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| default:Reihe_B/42/ZNB-1987-42b-0195.pdf | | | | Identifier
| ZNB-1987-42b-0195 | | | | Volume
| 42 | |
| 79 | Author
| Wolfgang Hönle, Bernhard Hettich, Arndt Simon | Requires cookie* | | | Title
| Preparation and Crystal Structure of LiGaCLj and LiGaI 4 | | | | Abstract
| The crystal structures of LiGaCl 4 and LiGaI 4 have been determined by single crystal X-ray methods. Both compounds are isotypic with LiAlCl 4 and characterized by LiX 6 octahedra and GaX 4 tetra-hedra. Mean bond lengths are: d(Ga-X) = 217.4 pm (Cl) and 255.9 pm (I); d(Li-X) = 263.9 pm (Cl) and 305.3 pm (I), respec-tively. Common features of the isotypic compounds LiGaX 4 (X -Cl, Br. I) are discussed. | | | |
Reference
| Z. Naturforsch. 42b, 248—250 (1987); eingegangen am 17. Oktober 1986 | | | |
Published
| 1987 | | | |
Keywords
| Crystal Structure, X-Ray, Lithium Compounds | | | |
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| default:Reihe_B/42/ZNB-1987-42b-0248_n.pdf | | | | Identifier
| ZNB-1987-42b-0248_n | | | | Volume
| 42 | |
| 80 | Author
| K. Wieghardt, S. Brodka, K. Peters, E. M. Peters, A. Simon | Requires cookie* | | | Title
| Säure-Base-Eigenschaften des zyklischen Triamins N,N',N"-Trimethyl-l,4,7-triazacyclononan: Die Kristallstruktur seiner monoprotonierten Form [C9H22N3KCIO4) Acid-Base Properties of the Cyclic Triamine N,N\N"-Trimethyl-l,4,7-triazacyclononane and Crystal Structure of its Monoprotonated Form [C 9 H 2 2N 3 ](C10 4 ) | | | | Abstract
| The crystal structure of the monohydroperchlorate of N,N',N"-trimethyl-l,4,7-triazacyclo-nonane, [C 9 H 2 2N3](C10 4), has been determined by single crystal X-ray diffraction. The acidic proton of the cation is bonded to one amine nitrogen and it forms hydrogen bonds to the other two N-atoms in agreement with a proposed model, which has been invoked to interpret successive protonation constants of cyclic triamines. The salt [Me 6 [9]aneN 3 ](BF 4)3 has also been prepared. | | | |
Reference
| Z. Naturforsch. 42b, 279—281 (1987); eingegangen am 8. Oktober/24. November 1986 | | | |
Published
| 1987 | | | |
Keywords
| Macrocyclic Triamine, X-Ray, Acid-Base Properties | | | |
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| default:Reihe_B/42/ZNB-1987-42b-0279.pdf | | | | Identifier
| ZNB-1987-42b-0279 | | | | Volume
| 42 | |
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