| | 41 | Author
| Abdel-Fattah Shihada, Frank Wellerb | Requires cookie* | | | Title
| Synthesis, Spectroscopic Studies, and Crystal Structure of Diethylchlorotin Dimethylphosphinate Et2C lSn02PMe2  | | | | Abstract
| Diethylchlorotin dimethylphosphinate has been synthesized by treating (E tiC lS n^O with H02PMe2 in toluene. Single crystal X-ray analysis shows that Ü 2PM e2 groups behave as bidentate bridge ligands between Et2ClSn units leading to a polymeric chain structure in which the tin atoms exhibit a distorted trigonal bipyramidal geometry with the oxygen atoms in the axial positions. The S n-C l bond lies on a C2 axis of symmetry in the (C2V) OCClSnCO unit. Et2ClSn02PMe2 crystallizes in the monoclinic space group C2/c (a = 877.9 (2), b = 1907.8 (4), c = 695.5 (1) pm, /5 = 106.72 (2)°, Z = 4 and R = 0.043). The characteristic IR bands of Et2ClSn0 2 PMe2 are assigned and the mass spectrum is reported and discussed. | | | |
Reference
| Z. Naturforsch. 53b, 699—703 (1998); received December 29 1997 | | | |
Published
| 1998 | | | |
Keywords
| Crystal Structure, IR Data, Mass Spectroscopic Data, Diethylchlorotin Dimethylphosphinate | | | |
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| default:Reihe_B/53/ZNB-1998-53b-0699.pdf | | | | Identifier
| ZNB-1998-53b-0699 | | | | Volume
| 53 | |
| 42 | Author
| H. Ans Bock, N.Orbert Nagel, Professor Heinz | Requires cookie* | | | Title
| Wechselwirkungen in Molekülkristallen, 143 [1]. ortho-Benzol-Derivate mit ineinander verzahnten Chlormethyl-und Methylamino-Substituenten: Strukturen und Rotationsenthalpie-Hyperflächen | | | | Abstract
| Interactions in M olecular Crystals, 143 [1]. orr/io-B enzene Derivatives w ith M eshed C ogw heel C hlorom ethyl and M ethylam ino Substituents: Structures and R otation Enthalpy H ypersurfaces Facets of molecular dynamics in organic compounds such as coupled rotations of adjacent substituents are advantageously discussed based on structural data. Within this context, crystal structures of spatially overcrowded ortho-disubstituted benzene derivatives with chloromethyl or methylamino groups are presented together with semiempirical enthalpy hypersurfaces for the substituent rotation. Both compounds, 1 -trichloromethyl-2-dichloromethyl-benzene as well as l-trimethylammonium-2-dimethylamino-benzene exhibit comparable steric overcrowding and their preferred dynamics are predicted to be dominated by the rotation of the threefold substituted group during an approximate standstill of the twofold substituted, mirror-symmetric one. According to known solid state NMR measurements as well as to atom/atom-potential model calculations for the pentachloro orf/zo-xylene derivative, this molecular dynamic mode is still active in the crystal. Dreizählige molekulare Zahnrad-Systeme Bei der zahnradartigen, | | | |
Reference
| Z. Naturforsch. 53b, 792—804 (1998); eingegangen am 10. März 1998 | | | |
Published
| 1998 | | | |
Keywords
| ortho-Benzene Derivatives, Meshed Cogwheel Substituents, Crystal Structure, Rotation Enthalpy Hypersurfaces | | | |
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| default:Reihe_B/53/ZNB-1998-53b-0792.pdf | | | | Identifier
| ZNB-1998-53b-0792 | | | | Volume
| 53 | |
| 43 | Author
| Hans Bock, Norbert Nagel, Professor Heinz | Requires cookie* | | | Title
| Wechselwirkungen in Molekülkristallen, 144 [1]. ortho-Benzol-Derivate mit ineinander verzahnten Trimethylsilyl- Substituenten: Strukturvergleich mit Benzol-l,2-disulfonat-Salzen und Rotationsenthalpie-Hyperflächen Interactions in Molecular Crystals, 144 [ 1], orr/zo-Benzene Derivatives with Meshed Cogwheel Trimethylsilyl Substituents: Structural Comparison with Benzene-1,2-disulfonate Salts and Rotation Enthalpy Hypersurfaces | | | | Abstract
| orr/zo-Benzene derivatives with adjacent bulky propeller substituents are well-suited mo del compounds to investigate their potentially coupled rotations. To approach the molecular dynamics of l,2-bis(trimethylsilyl)benzene, a liquid at room temperature and containing hete roelement substituents, an advantageous starting point are the crystal structures of the stereo-chemically correspondent benzene-1,2-disulfonate dianion salts. For both the rotations of the synperiplanar three-bladed rotor-groups -S 0 3e and -Si(CH3)3, PM3-enthalpy hypersurfaces are presented, which suggest only weak interdentate interaction and, concomitantly, only partly coupled intermolecular substituent rotation dynamics. Additional data from the Cambridge Structural Database for silicon organic compounds fit into the contour lines of the enthalpy surface calculated for l,2-bis(trimethylsilyl)benzene, and the structure correlation with varying distances Si • • • Si between the heteroelement centers can be discussed in more general terms of the substituent propeller blade length vs. thickness ratio. Dreizählige molekulare Zahnrad-Systeme mit Heteroelement-Substituenten | | | |
Reference
| Z. Naturforsch. 53b, 805—815 (1998); eingegangen am 10. März 1998 | | | |
Published
| 1998 | | | |
Keywords
| orf/zo-Benzene Derivatives, Meshed Cogwheel Substituents, Crystal Structure, Rotation Enthalpy Hypersurfaces | | | |
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| default:Reihe_B/53/ZNB-1998-53b-0805.pdf | | | | Identifier
| ZNB-1998-53b-0805 | | | | Volume
| 53 | |
| 45 | Author
| Frank Leßmann3, Lothar Beyer3, Rainer Richter3, Reinhard Meusingerb | Requires cookie* | | | Title
| N-Benzoylthiocarbamoyl Amino Acid Ethyl Esters as Chelate Ligands for Transition Metal Ions | | | | Abstract
| The reactions of benzoyl isothiocyanate with amino acid ethyl esters (N-butyl glycine ethyl ester, (S)-(-)-proline ethyl ester) give N-benzoylthiocarbamoyl amino acid ethyl esters. Apart from the expected N-benzoylthiocarbamoyl (S)-(-)-proline ethyl ester the racemic N-benzoyl thiocarbamoyl (/?)/(S)-proline ethyl ester is formed because of base catalyzed racemization of the educt (5')-(-)-proline ethyl ester during the reaction of (S)-(-)-proline ethyl ester hy drochloride with triethylamine. The structures of both compounds were established by X-ray crystal structure analysis and specific optical rotation measurements. The ligands yield neutral 2:1 chelates with Ni , Cu11, Pd11 and Pt11. The carboxylic oxygen atoms are not involved in the chelation. The ligands and the resultant complexes show configurational E/Z isomerism. In the case of the chelates of the racemic N-benzoylthiocarbamoyl (/?)/(5)-proline ethyl ester, additional R/S isomerism is observed as shown by | | | |
Reference
| Z. Naturforsch. 53b, 981—990 (1998); received November 11 1997 | | | |
Published
| 1998 | | | |
Keywords
| Thioureas, Amino Acid Ethyl Esters, Chelates, NMR Data, Crystal Structure | | | |
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| default:Reihe_B/53/ZNB-1998-53b-0981.pdf | | | | Identifier
| ZNB-1998-53b-0981 | | | | Volume
| 53 | |
| 46 | Author
| Stephanie Janeda, Dietrich Mootz, Herrn | Requires 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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| default:Reihe_B/53/ZNB-1998-53b-1197.pdf | | | | Identifier
| ZNB-1998-53b-1197 | | | | Volume
| 53 | |
| 47 | Author
| Jones | Requires cookie* | | | Title
| Polysulfonylamine, CV [1] Die ersten N,N-disulfonylierten Sulfinsäureamide: Synthese und Kristallstrukturen von R S ( 0 )-N (S 0 2Me)2 (R = Me, CC13) | | | | Abstract
| P o ly su lfo n y lam in es, C V [1] T h e F irst N ,N -D isu lfo n y lated S ulfinic A m id es: S y nthesis a n d C ry sta l S tru c tu re s o f R S (0) -N (S 0 2M e)2 (R = M e, CC13) M a rtin a N äv e k e, A rm a n d B lasc h ette* , P e te r G. The novel sulfinamides R S (0) -N (S 0 2M e)2, where R = Me (la) or CC13 (lb), were ob tained by treating the corresponding sulfinyl chlorides with Me3S iN (S 02Me)2 or AgN-(S 0 2Me)2, respectively. A presumedly ionic 1:1 adduct of lb with 4-dimethylaminopyridine was isolated and analytically characterized. In the crystals of la (monoclinic, space group P2\!ri) and lb (monoclinic, P l j c) , the molecules feature approximately planar NS3 moieties, unusually long S (0) -N bonds and, in the case of lb, an extremely long S (0) -C bond [for la and lb, in order: sum of bond angles at nitrogen 359.5 and 357.1°, S (0) -N 178.2(2) and 173.6(2) pm, S (0) -C 178.8(2) and 194.1(2) pm]. In both molecular structures, an attractive S (0) --0 1,4-interaction leads to a 7.3° discrepancy in the S (0) -N -S 0 2 angles. The crystal packing of la displays a tape (double-chain) motif generated by two prominent intermolecu-lar C -H -O interactions involving one M e S 0 2 group and the sulfinyl oxygen atoms of two adjacent molecules, whereas in lb the molecules are associated into parallel chains via a bonding C l-"0(sulfonyl) interaction. | | | |
Reference
| Z. Naturforsch. 53b, 734—741 (1998); eingegangen am 6. April 1998 | | | |
Published
| 1998 | | | |
Keywords
| N, N-Bis(organosulfonyl)sulfinamides, Synthesis, Crystal Structure, Long S ( 0 ) -N Bond | | | |
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| default:Reihe_B/53/ZNB-1998-53b-0734.pdf | | | | Identifier
| ZNB-1998-53b-0734 | | | | Volume
| 53 | |
| 48 | Author
| Hiromitsu Terao, Masao Hashimoto\, Tsutomu Okuda, Alarich Weiss | Requires cookie* | | | Title
| Phase Transitions and Crystal Structure of Dimethylammonium Tribromomercurate(II), (CH 3 ) 2 NH 2 HgBr 3 , as Studied by 81 Br NQR and Single Crystal X-ray Diffraction | | | | Abstract
| The temperature dependence of the 81 Br NQR frequencies of the title compound has revealed the presence of three phases (I, II and III, in the order of decreasing temperature): T cl (II -1) = (318 ± 10) K and T c2 (III -II) = (202 ± 1) K. The transitions were confirmed by thermal analysis (DTA). Both of the II-I and I-II transitions exhibited strong hysteresis (/. e., superheating and supercooling, respectively). The crystal data, determined by single crystal X-ray diffraction, are: monoclinic, space group P2/a, a = 1384.8(3), b = 934.7(4), c = 1452.0(2) pm, ß = 104.10(1)°, Z= 8, R = 0.076. The crystal has two crystallographically independent cations (CH 3) 2 NH 2 + and an infinite chain of anions almost in the c-direction. The anion chain is considered to consist of a HgBr 2 molecule and two different HgBr 4 2 ~ anions which are interconnected via weak intermolecular Hg-Br bonds. The splitting patterns of the 8 'Br NQR spectra indicate that rearrangements of the Hg-Br bonds are slight at the III-II transition but serious at the II-I transition. Some of the 81 Br NQR lines show anomalous temperature coefficients, attributable probably to thermal motions of cations. | | | |
Reference
| Z. Naturforsch. 53a, 559—567 (1998); received January 26 1998 | | | |
Published
| 1998 | | | |
Keywords
| (CH 3 ) 2 NH 2 HgBr 3, X-Ray Analysis, NQR, Phase Transition, Crystal Structure | | | |
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| default:Reihe_A/53/ZNA-1998-53a-0559.pdf | | | | Identifier
| ZNA-1998-53a-0559 | | | | Volume
| 53 | |
| 49 | Author
| J. Seemann, W. Preetz | Requires cookie* | | | Title
| Schwingungsspektren und Normalkoordinatenanalyse von Hexathiocyanatoplatinat(IV), Kristallstruktur von [Py2CH2][Pt(SCN)6] Vibrational Spectra and Normal Coordinate Analysis of Hexathiocyanatoplatinate(IV), Crystal Structure of [Py2CH2][Pt(SCN)6] | | | | Abstract
| By treatment of [PtCl6]2-with an excess of SCN~ in aqueous solution [Pt(SCN)6]2~ is formed. The X-ray structure determination on a single crystal of [Py2CH2][Pt(SCN)6] (orthor-hombic, space group Pna21? a = 15.5084(9), b = 11.8444(11), c = 13.2830(9)A, Z = 4) shows, that the thiocyanate groups are exclusively S-coordinated with average Pt-S distances of 2.378 A and Pt-S-C angles in the range from 103.1° to 108.1°. Based on the molecular parameters of the X-ray determination the low temperature (10 K) IR and Raman spectra have been assigned by normal coordinate analysis. The valence force constant is fd(PtS) = 1.62 mdyn/A. | | | |
Reference
| (Z. Naturforsch. 53b, 13—16 [1998]; eingegangen am 15. Oktober 1997) | | | |
Published
| 1998 | | | |
Keywords
| Hexathiocyanatoplatinate(IV), IR Spectra, Raman Spectra, Normal Coordinate Analysis, Crystal Structure | | | |
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| default:Reihe_B/53/ZNB-1998-53b-0013.pdf | | | | Identifier
| ZNB-1998-53b-0013 | | | | Volume
| 53 | |
| 50 | Author
| Rainer Niewa3, GrigoriV. Vajenine3, FrancisJ. Disalvo, Haihua Luob, WilliamB. Yelonb | Requires cookie* | | | Title
| Unusual Bonding in Ternary Nitrides: Preparation, Structure and Properties of Ce2MnN3 | | | | Abstract
| CeiMnNj was prepared by reaction of cerium nitride and manganese with nitrogen gas at 900 °C. It crystallizes isotypic to AC2MN3 (Ac = U, Th; M = Cr, Mn) and Ce^CrN^, space group Immm (No. 71), a = 3.74994(6) A, b = 3.44450(6) A and c = 12.4601(2) A. The manganese atoms are coordinated in a nearly square planar fashion by four nitrogen atoms. These corner-connected MnN* units form infinite J. [MnN2N2/ 2 ] chains, which run parallel to each other along the crystallographic a-axis, forming the motif of hexagonal rod packing. Cerium atoms connect the chains into a three-dimensional network. The results of measurements of the magnetic susceptibility, as well as of the electrical resistivity suggest metallic behavior. Electronic effects leading to shorter bonds between manganese and bridging nitrogen atoms than between manganese and terminal nitrogen atoms in the J. [MnN2N2/ 2 ] chains were investigated through extended Hiickel and LMTO band structure calculations. Issues pertaining to stability of this and some other nitridometallate structures are discussed. | | | |
Reference
| (Z. Naturforsch. 53b, 63—74 [1998]; received September 17 1997) | | | |
Published
| 1998 | | | |
Keywords
| Ternary Nitride, Crystal Structure, Magnetic Susceptibility, Electrical Resistivity, Extended Hiickel Method | | | |
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| default:Reihe_B/53/ZNB-1998-53b-0063.pdf | | | | Identifier
| ZNB-1998-53b-0063 | | | | Volume
| 53 | |
| 51 | Author
| K. Dallmann, W. Preetz | Requires cookie* | | | Title
| | | | | Abstract
| Normalkoordinatenanalyse von [Os(acac)3] Synthesis, Crystal Structure, Vibrational Spectra, and Normal Coordinate Analysis o f [Os(acac)3] In the reaction o f K 2[O sCl6] with boiling water/acetylacetone (1:1) a mixture o f different chloro-acetylacetonato complexes is formed, from which [Os(acac)3] can be isolated by column chromatography with dichloromethane on silica gel. The crystal structure o f [Os(acac)3] (m o noclinic, space group P2,/c,a = 13.968(5), b = l . 517(5), c = 16.455(5) A ,ß = 98.939(5)°, Z = 4) has been determined by single crystal X-ray diffraction analysis. High resolution IR and Raman spectra were measured at low temperature (10 K). Based on the molecular parameters o f the X-ray structure determination a normal coordinate analysis has been performed and the normal modes o f vibration have been assigned. With a set o f 32 force constants, taking into account the intraligand vibrations, a good agreement between observed and calculated frequencies has been achieved. The valence force constants are fd(OsO) = 3.19 and fd(O C) = 6.74 mdyn/A. | | | |
Reference
| Z. Naturforsch. 53b, 232—238 (1998); eingegangen am 26. November 1997 | | | |
Published
| 1998 | | | |
Keywords
| Tris(acetylacetonato)osmium(III), Crystal Structure, IR Data, Raman Data, Normal Coordinate Analysis | | | |
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| default:Reihe_B/53/ZNB-1998-53b-0232.pdf | | | | Identifier
| ZNB-1998-53b-0232 | | | | Volume
| 53 | |
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