| | 1 | Author
| Norbert Kuhn3, Riad Fawzi3, M. Anfred Steimann3, Jörg Wiethoff3, D. Ieter Bläserb, Roland Boeseb | Requires cookie* | | | Title
| Synthese und Struktur von 2-Imino-l,3-dimethylimidazolin [1] Synthesis and Structure of 2-Imino-l,3-dimethylimidazoline [1]  | | | | Abstract
| Deprotonation of the 2-amino-1,3-dimethylimidazolium salt 5 (obtained through methyla-tion of 2-am ino-l-m ethylim idazole (4)) by KH gives 2-im ino-l,3-dim ethylim idazoline 6. The trimethylsilylimino compound 14 is formed on the reaction of 6 with chlorotrimethylsilane in the ratio 2:1. Further reaction with chlorotrimethylsilane gives the silylated aminoimidazo-lium salt 15. The X-ray structures o f 5 and 6 are reported. | | | |
Reference
| Z. Naturforsch. 50b, 1779—1784 (1995); eingegangen am 23. Mai 1995 | | | |
Published
| 1995 | | | |
Keywords
| Imidazole, Imine, X-Ray | | | |
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| default:Reihe_B/50/ZNB-1995-50b-1779.pdf | | | | Identifier
| ZNB-1995-50b-1779 | | | | Volume
| 50 | |
| 2 | Author
| Bernd Wrackmeyer, Udo Dörfler, Wolfgang Milius, Max Herberhold | Requires cookie* | | | Title
| Triferrocenylborane -Molecular Structure in Solution and in the Solid State | | | | Abstract
| According to a single crystal X-ray structure determination all three ferrocenyl substituents of triferrocenylborane (1) adopt the same orientation with respect to the BC3-plane [P 2 Jc\ monoclinic; Z = 4; a = 1353.5(3), b = 1695.6(3), c = 1056.4(2) pm, ß = 109.27(3)°]. The simu lated X-ray powder pattern of the single crystal is identical with the powder diagram o f a macroscopic sample, indicating the presence of a single diastereomer (l a) in the solid state. How ever, at low temperature (< -9 5 °C) in solution, the 13C NM R spectra suggest the pres ence of the second diastereomer (lb) in which one ferrocenyl group is oriented opposite to the other two with respect to the central BC3-plane. | | | |
Reference
| Z. Naturforsch. 50b, 201—2 (1995); received July 25 1994 | | | |
Published
| 1995 | | | |
Keywords
| Triferrocenylborane, 13C NMR Spectra, Dynamic Processes, X-Ray | | | |
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| default:Reihe_B/50/ZNB-1995-50b-0201.pdf | | | | Identifier
| ZNB-1995-50b-0201 | | | | Volume
| 50 | |
| 3 | Author
| Thomas Schmidt, Stephan Neis, Richard Goddard | Requires cookie* | | | Title
| Synthesis, Structure, and Properties of Homoleptic l-Oxa-l,3-diene Molybdenum and Tungsten Complexes | | | | Abstract
| Homoleptic tris(l-oxa-l,3-diene)m olybdenum and tungsten complexes are formed as yel low, crystalline compounds in 54-80% isolated yield on treatm ent of the corresponding /3-unsubstituted a,/3-unsaturated ketones with W (CO)3(CH 3CH 2CN)3 or (y6-C6H 6)M o(CO)3 in refluxing hexane. Reaction of these oxadienes with (^6-C6H 5CH3)2Mo in tetrahydrofuran or /7-hexane provides a new high yield route to homoleptic molybdenum complexes that are otherwise difficult to prepare. X-ray crystal structure analyses of two air-stable, isomeric tungsten complexes reveal a significant contribution of a cr2,?/2-bonding mode in the coordi nated oxadiene moieties. U nder reaction conditions that allow the platinum catalyzed hydro genation of phenyl substituents in these ligands, the coordinated oxadiene fragments are inert, thus demonstrating an unprecedented chemoselectivity in the hydrogenation of aryl-substituted enones. On the other hand, the complexes are labile enough to catalyze the cyclotrimerization of alkynes such as methyl propiolate. | | | |
Reference
| Z. Naturforsch. 50b, 315—325 (1995); received September 7 1994 | | | |
Published
| 1995 | | | |
Keywords
| Oxadiene Complex, Molybdenum, Tungsten, X-Ray, Selective Hydrogenation | | | |
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| default:Reihe_B/50/ZNB-1995-50b-0315.pdf | | | | Identifier
| ZNB-1995-50b-0315 | | | | Volume
| 50 | |
| 4 | Author
| B. Gabor, R. Goddard, S. Holle, P. W. Jolly, C. Krüger, R. Mynott, W. Wisniewski | Requires cookie* | | | Title
| T h e R eaction o f D ien es with [F e (P r z2P ( C H 2) /IP P r /2) ] Species | | | | Abstract
| D ed ica ted to Prof. D r. Dr. h.c. m u lt G ü n th e r W ilk e o n the o cca sio n o f his 70th birthday The structure of the compounds formed upon reacting Fe(Pr'2P(C H 2)"PPr'2)Cl2 (n = 1-3) and active-Mg with acyclic and cyclic 1,3-, 1,4-and 1,5-dienes depends upon the nature of the diene and upon the length of the methylene-chain bridging the two P-atoms of the biden-tate ligand. For example, isoprene reacts to give either (774-isoprene)2FePPr'2C2H4PPr'2 or (^4-isoprene)Fe(Pr'2PC3H6PPr'2) while the products of the reaction with 1,5-hexadiene are (?75-l-methylpentadienyl)Fe(Pr'2PC2H 4PPr'2)H or (//2,?/2-l,5-hexadiene)Fe(Pr'2PC3H6PPr'2). The crystal structures of the last two compounds have been established by X-ray diffraction. The penultimate species catalyses the linear dimerization of 1,5-hexadiene. | | | |
Reference
| Z. Naturforsch. 50b, 503—513 (1995); received September 15 1994 | | | |
Published
| 1995 | | | |
Keywords
| Iron-Organo Complex, Diene Pentadienyl, X-Ray | | | |
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| default:Reihe_B/50/ZNB-1995-50b-0503.pdf | | | | Identifier
| ZNB-1995-50b-0503 | | | | Volume
| 50 | |
| 5 | Author
| K. Polborn, W. Steglich, J. D. Connolly, S. Huneck, To Prof, G. Antonio, Gonzalez | Requires cookie* | | | Title
| Structure of the Macrocyclic Bis-lactone Lepranthin from the Lichen Arthonia im polita; an X-Ray Analysis celebrating his half-century of involvement with natural products chemistry | | | | Abstract
| The structure and relative stereochemistry o f lepranthin from the lichen Arthonia impolita has been elucidated as 1 by NM R spectroscopy and X-ray analysis. | | | |
Reference
| Z. Naturforsch. 50b, 1111—1114 (1995); received February 20 1995 | | | |
Published
| 1995 | | | |
Keywords
| Lepranthin, Macrocyclic Bis-lactone, X-Ray, Lichen | | | |
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| default:Reihe_B/50/ZNB-1995-50b-1111.pdf | | | | Identifier
| ZNB-1995-50b-1111 | | | | Volume
| 50 | |
| 6 | Author
| R. Ainer Pöttgen | Requires cookie* | | | Title
| EuPdGe -a New Germanide with EuNiGe Type Structure | | | | Abstract
| The title compound was prepared from the elem ental com ponents in a tantalum tube at 1070 K and investigated by X-ray diffraction of both powder as well as single crystals. The crystal structure was refined from four-circle diffractometer data: P 2 xln, a = 618.1(1), b = 613.6(1), c = 743.9(1) pm, ß = 109.40(1)°, V = 0.2661(1) nm3, Z = 4 ,w R 2 = 0.0536 for 1564 F2 values and 29 variables. EuPdGe crystallizes with the E uN iG e type structure. Both Pd and G e atom s in EuPdGe have three germanium or palladium neighbors, respectively. They form two-dim ensionally infinite [PdGe] polyanions which consist o f corrugated 4.82 nets. These polyanions are separated by the europium atoms. | | | |
Reference
| Z. Naturforsch. 50b, 1181—1184 (1995); received March 1 1995 | | | |
Published
| 1995 | | | |
Keywords
| Germanide, Crystal Structure, X-Ray, Europium | | | |
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| default:Reihe_B/50/ZNB-1995-50b-1181.pdf | | | | Identifier
| ZNB-1995-50b-1181 | | | | Volume
| 50 | |
| 7 | Author
| Wolfgang Pohl, Ingo-Peter Lorenz, Heinrich Nöth, Martin Schmidt | Requires cookie* | | | Title
| Offene und geschlossene Triferriophosphonium-Salze und Triferriophosphane O pen and Closed Triferriophosphonium Salts and Triferriophosphines | | | | Abstract
| The reaction of P(SiM e3)3 with an excess of C pFe(CO)2X (X = Cl, Br) through the action o f water gives the triferriophosphonium salt [{CpFe(CO)2}3PH]2FeX4 together with ferrocene as by-product. The cation of the salt can be deprotonated by D B U to afford the unstable triferriophosphine {CpFe(CO)2}3P. Its subsequent realkylation with RX (R = Me, CH2Ph; X = I, Br) leads to alkyltriferriophosphonium salts [{CpFe(CO)2}3PR]X. Photolysis of [{CpFe(CO)2}3PH]2FeX 4 induces the elimination of one CO group, and the CO-bridged and partly closed complex [{//-CO(CpFeCO)2}{CpFe(CO)2}PH]2FeX 4 is formed, the cation of which can also be deprotonated to give the corresponding m onobridged phosphine (w-CO(CpFeCO)2}{CpFe(CO)2}P. Both PH-phosphonium salts undergo a hydrogen-chlorine exchange reaction to give the P -C l analogues [{CpFe(CO)2}3PCl]2FeX4 and [{//-CO (CpFeCO)2}{CpFe(CO)2}PCl]2FeX 4. The IR and NM R spectra of all species as well as the X-ray structure analyses of the open and closed P -H functional com plexes are reported and discussed. | | | |
Reference
| Z. Naturforsch. 50b, 1485—1493 (1995); eingegangen am 30. März 1995 | | | |
Published
| 1995 | | | |
Keywords
| Iron, Tristrimethylsilylphosphine, Hydrogen Chlorine Exchange, X-Ray, Decarbonylation | | | |
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| default:Reihe_B/50/ZNB-1995-50b-1485.pdf | | | | Identifier
| ZNB-1995-50b-1485 | | | | Volume
| 50 | |
| 8 | Author
| YalcinE. Lerm Ana+, MehmetK. Abaka, Ingrid Svobodab, H. Artm Ut Fuessb-, KlausG. Riesarc, WolfgangH. Aasec | Requires cookie* | | | Title
| X-Ray Structure and Magnetic Properties of the Tetracupferronato-bis(//-methoxy)-diiron(III) Complex | | | | Abstract
| The tetracupferronato-bis(w-methoxy)-diiron(III) complex has been synthesized in aceto nitrile and its crystal structure determined. C i6H->6N80 1(>Fe2, monoclinic, space group C2/c, a =18.425(3), b = 12.999(2), c = 15.046(3) A, ß = 12 4 .6 6 (2)°,> = 2964(1) A , Z = 4, wR(2) = 0.097 from 1491 reflections (F2). Two iron(III) atoms are at special positions in six-fold co ordination, bridged by O with a F e -O -F e angle of 102.4(1)° and a distance between two iron(III) centers of 3.075(1) A. Temperature-dependent magnetic susceptibility measure ments reveal a antiferromagnetic exchange interaction (J = -1 4 cm -1) betw een the iron(III) centers. | | | |
Reference
| Z. Naturforsch. 50b, 1587—1590 (1995); received January 11 1995 | | | |
Published
| 1995 | | | |
Keywords
| X -Ray, Magnetic Properties, Antiferromagnetic Coupling | | | |
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| default:Reihe_B/50/ZNB-1995-50b-1587.pdf | | | | Identifier
| ZNB-1995-50b-1587 | | | | Volume
| 50 | |
| 9 | Author
| Dagmar Holthenrich, Imre Sóvágó, G. Erd Fusch, Andrea Erxleben, EddaC. Fusch, Ingo Rombeck, B.Ernhard Lippert | Requires cookie* | | | Title
| Heteronuclear Nucleobase Complexes as Tools for the Isolation of the Minor Rotamer of the Parent Compound: Synthesis and Crystal Structure Determination of H ead-H ead and H ead-Tail Forms of rrfl«5-[(CH3NH2)2Pt(l-MeC-Ar J)2]2+ (1-MeC = 1-methylcytosine) | | | | Abstract
| The two rotamers (head-tail, 1, and head-head, 2) of the bis(l-m ethylcytosine)com plex of f/ww-(CH3N H 2)2Pt(II), have been crystallized as C104-(1, 2a) and PF6-(2b) salts and characterized by X-ray crystal structure analysis and 'H and 19:iPt NMR spectroscopy. In aqueous solution, 1 is preferred over 2 by 70:30. Upon slow crystallization from H 2Ö, 1 is obtained as the only product. Isolation of 2a and 2b has now been accomplished via forma tion of the heteronuclear derivative rrans-[(CH3N H 2)2Pt(l-MeCv/V3,./W)2Hg]2+, in which the deprotonated 1-methylcytosinato ligands (1 -M eC) are oriented head-head, precipitation of Hg(II) by thiourea, and rapid crystallization of the parent compound. The solid state struc tures of 1 and 2b differ markedly in a number o f aspects. Isolation of pure 1 and 2 permits a detailed study of the kinetics and thermodynamics of the interconversion of the two rotam ers. From comparison with the behavior of 1 and 2 in H20 on the one hand and DM SO and DM F on the other a clear solvent effect on the rotamer distribution is seen which most likely relates to differences in H bonding between solvent and solute. | | | |
Reference
| Z. Naturforsch. 50b, 1767—1775 (1995); received May 15 1995 | | | |
Published
| 1995 | | | |
Keywords
| Transplatin, Nucleobase, 1-Methylcytosine, R otation, X-Ray | | | |
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| default:Reihe_B/50/ZNB-1995-50b-1767.pdf | | | | Identifier
| ZNB-1995-50b-1767 | | | | Volume
| 50 | |
| 10 | Author
| Volker Lorenz3, Bernhard Neumiillerb, Karl-Heinz Thiele3 | Requires cookie* | | | Title
| Synthese und Kristallstrukturen von Diazadien-Komplexen der Erdalkalimetalle Syntheses and Crystal Structures of Diazadiene Complexes of the Alkaline Earth Metals | | | | Abstract
| [C aN R -CPh=CPh-N R (D M E)2] 1 (R = C6H4-4 -C H 3; D M E = dim ethoxyethane) was pre pared by reaction of calcium with N R = C P h -C P h = N R in D M E solution. The compound forms orange, moisture sensitive crystals, which were characterized by an X-ray structure determination [space group orthorhombic, P 2 i2 12 1, Z = 4, 4634 observed unique reflections, R = 0.046; lattice dimensions at -7 0 °C: a = 1340.2(3), b = 1528.1(3), c = 1609.1(3) pm]. The calcium atom is coordinated by the four oxygen atoms of two chelating D M E molecules and two nitrogen atoms of the diazadiene ligand, bonded in its enediam ide form. [Ba2(D M E)3(N P h -C P h = C P h -N P h)2 DM E] 3 was obtained from barium metal and N Ph=C Ph-C Ph=N Ph in D M E solution as red crystals [space group monoclinic, P2!/c, Z = 4, 4000 observed unique reflections, R = 0.166; lattice dim ensions at -7 0 °C: a = 1704.5(3), b = 1786.1(4), c = 2177.4(4) pm, ß = 105.98(3)°]. The two barium atoms are bridged by two differently bonded diazadiene ligands (/<2-N ,N ';/i-N ,a -N '). Additionally, one of the barium atoms is coordinated to two DM E m olecules and the other one to only one of the ether molecules. A further DM E molecule is a constituent of the crystal lattice. | | | |
Reference
| (Z. Naturforsch. 50b, 71—7 [1995]; eingegangen am 13. Juli 1994) | | | |
Published
| 1995 | | | |
Keywords
| Alkaline Earth Metal Complexes, Diazadiene Ligands, Enediamide Structure, X-Ray | | | |
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| default:Reihe_B/50/ZNB-1995-50b-0071.pdf | | | | Identifier
| ZNB-1995-50b-0071 | | | | Volume
| 50 | |
| 11 | Author
| A. Chrissafidou, J. Fuchs, H. Hartl, R. Palm | Requires cookie* | | | Title
| Kristallisation und Strukturuntersuchung von Alkali-Parawolframaten Crystallization and Structure Determ ination of Alkaline M etal-Paratungstates | | | | Abstract
| The syntheses and crystal structures of the following paratungstates-Z with different alka line cations are reported and discussed: N a10[H2W 120 42]-2 0 H 20 (I), N a10[H2W 12O 42]-2 7 H 20 (II), N a10[H2W 12O47] -2 8 FLO (III), K10[H2W 120 42] 1 0 H 20 (IV), K6Na4[H ,W 120 42]-1 3 H 20 (V), Cs6Na4[H?W P0 42] • 16IÜO (VI), Cs8N a2[H2W 120 42]-1 0 H 20 (VII), Cs8Na2[H2W 120 42] • 12 H20 (VIII), K3N a7[H2W 120 42] -24H 20 (IX) and KsNa2[H2W 120 42] • 12H20 (X). Priority has been set on the description of the coordination of the cations with the oxygen ligands H2W 12O 4210_ and h 2o . | | | |
Reference
| Z. Naturforsch. 50b, 217 (1995); eingegangen am 22. Juli 1994 | | | |
Published
| 1995 | | | |
Keywords
| Paratungstates-Z, Synthesis, Structure Determination, X-Ray, Cation Coordination | | | |
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| default:Reihe_B/50/ZNB-1995-50b-0217.pdf | | | | Identifier
| ZNB-1995-50b-0217 | | | | Volume
| 50 | |
| 12 | Author
| Anne Utzolino, Karsten Bluhm | Requires cookie* | | | Title
| Cox 5Ti0 5(B 0 3) 0 and Co! 5Zro.5(B 0 3) 0 | | | | Abstract
| Single crystals of Co15Tio.5(B 0 3)0 (I) and Coj 5Zr0 5(BO3)O (I I) were obtained by a B20 3 flux technique. Both compounds crystallize with orthorhombic symmetry, space group D -Pnma (Nr. 62), I a = 928.1; b = 311.1; c = 940.1 pm; Z = 4 and I I a = 949.5; b = 323.42; c = 934.7 pm; Z = 4. The compounds are isotypic to the mineral warwickite. All metal ions are octahedrally coordinated by oxygen ions. The structure contains isolated, trigonal planar B 0 3 units and oxygen that is not coordinated to boron. Die Synthese und Kristallstruktur von cobalthaltigen Boratoxiden: Coi^Tio,5(B03)0 und C o i?5Zr<),5(B03)0 | | | |
Reference
| Z. Naturforsch. 50b, 1653—1657 (1995); eingegangen am 4. Mai 1995 | | | |
Published
| 1995 | | | |
Keywords
| Cobalt, Titanium, Zirconium, Borate Oxide, Crystal Structure, X-Ray | | | |
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| default:Reihe_B/50/ZNB-1995-50b-1653.pdf | | | | Identifier
| ZNB-1995-50b-1653 | | | | Volume
| 50 | |
| 14 | Author
| Bernd Wrackmeyer, HeidiE. Maisel, Wolfgang Milius | Requires cookie* | | | Title
| 2-Stannylpyridine-Borane Adducts -Multinuclear Magnetic Resonance Study and X-Ray Structure Determination of a l,4-Dihydro-4 a,l,4-azastannabora-naphthalene Derivative | | | | Abstract
| The adduct formation between 2-trimethylstannyl-pyridine (1) and triethylborane, leading to 2a, and 9-borabicyclo[3.3.1]nonane, leading to 2b, was studied by 'H, " B, 13C, 15N and 119Sn NMR in solution. Changes in the magnitude of the coupling constants 7(119Sn, 13C), with respect to the data for 1, were analysed. The absolute signs have been determined [all coupling constants " /(119Sn,13C) to methyl and pyridine carbon atoms in 1 to 3 possess a negative sign and the same is true for "y(119Sn,*H) of the pyridine hydrogen atoms] by various two-dimensional NMR experiments, and attributed to the influence of the lone pair of electrons at the nitrogen atom in 1. The NMR spectroscopic results for the 1,4-dihydro-4a,l,4-azastannabora-naphthalene derivative 3, in which structural fragments are present analogous to those in the borane adducts 2, correspond to those for 1 and 2a,b. The molecu lar structure of 3 has been determined by X-ray analysis [orthor' nombic; P 2 i2121; a = 713.9(2), b = 1566.0(2), c -1578.4(2) pm]. Solid-state 13C and 119Sn CP/MAS NM R spectra prove that the molecular structures of 3 in the solid state and in solution are very similar. | | | |
Reference
| Z. Naturforsch. 50b, 809—815 (1995); received | | | |
Published
| 1995 | | | |
Keywords
| O ctober 28, 1994 2-Trimethylstannyl-pyridine, Borane Adducts, Heterobicycle, X-Ray, NM R Spectra | | | |
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| default:Reihe_B/50/ZNB-1995-50b-0809.pdf | | | | Identifier
| ZNB-1995-50b-0809 | | | | Volume
| 50 | |
| 15 | Author
| LutzD. Ahlenburg, A.Lexander Wolski | Requires cookie* | | | Title
| Oligophosphan-Liganden, XXXIX* | | | | Abstract
| (lS,2S)-fraw s-C yclopentan-l,2-diyl-bis(phosphan), C5H 8(P H 2)2? durch Reduktion eines diastereomerenreinen Cyclopentandiyl-bis(dioxaphospholans) O ligophosphine Ligands, X X X IX . (1 5,25')-rra/t5-C yclopentane-l,2-diyl-bis(phosphine), C5FI8(P H 2)2, by R eduction of a D iastereom erically Pure C yclopentanediyl-bis(dioxaphospholane) C hristine E ckert, The title compound (S, S)-2, has been obtained by reduction with Li[A lH 4] o f the cyclopen-tane-l,2-diyl-bis(l',3',2'-dioxaphospholane) (1 5 ,2 S)-frans-C5H 8[P (0 C H (C 0 2Pr-/)-(/ ?) -)2]2, (S, 5")-l, which itself was isolated in diastereomerically pure form (X-ray structure analysis) from the reaction between rac, /rfl«s-CsH8(PCl2)2 and (2 /? ,3 /?)-(+)-d iiso p ro p y l tartrate. C l e a v a g e o f (S ,.S)-1 w i t h P C U y i e l d e d a n u n s e p a r a b l e m i x t u r e o f (1 S , 2 S W r a n s -C 5 H 8(P C l 2) 2 a n d (4 R .5 R) -C l P [ 0 C H (C 0 2P r -t) -]2. | | | |
Reference
| Z. Naturforsch. 50b, 1004—1008 (1995); eingegangen am 30. N ovem ber 1994 | | | |
Published
| 1995 | | | |
Keywords
| Chiral Bis(phosphine) Reduction of P -O, X-Ray, Mass Spectra, NM R Spectra | | | |
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| default:Reihe_B/50/ZNB-1995-50b-1004.pdf | | | | Identifier
| ZNB-1995-50b-1004 | | | | Volume
| 50 | |
| 16 | Author
| Neda, Michael Farkens, Holger Thönnessen, PeterG. Jones, Reinhard Schmutzler | Requires cookie* | | | Title
| Zur Chemie der l,3,5-Triaza-2-phosphorinan-4,6-dione. Teil X*. Umsetzungen von 2-Hydro | | | | Abstract
| l,3,5-trimethyl-l,3,5-triaza-2-oxo-2A4-phosphorinan-4,6-dion mit Triazin-Derivaten sowie mit einigen Aldehyden Chemistry of the l,3,5-Triaza-2-phosphorinan-4,6-diones. Part X*. Reactions of 2-H ydro-1,3,5-trim ethyl-1,3,5-triaza-2-oxo-2A4-phosphorinan-4,6-dione with Triazine Derivatives and with Some Aldehydes Ion | | | |
Reference
| Z. Naturforsch. 50b, 1833—1 (1995); eingegangen am 8. Mai 1995 | | | |
Published
| 1995 | | | |
Keywords
| 1, 3, 5-Trimethyl-Substituted l, 3, 5-Triaza-2A 4 -phosphorinan-4, 6-diones, NM R Spectra, Mass Spectra, X-Ray | | | |
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| default:Reihe_B/50/ZNB-1995-50b-1833.pdf | | | | Identifier
| ZNB-1995-50b-1833 | | | | Volume
| 50 | |
|
