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71.
72.
Single Crystal Investigations on Fluoroperovskites MPdF3 (M = Rb, K) and PdF2 Single crystal investigations on PdF2 (violet) confirm the tetragonale rutile structure [1, 2] with a = 495.44(3) pm, c = 338.48(3) pm, Z = 2, space group P42/mnm-D (No. 136) (xF = 0.3058(8)). RbPdF3 and KPdF3 have been obtained. RbPdF3 and KPdF3 both ruby-red single crystals crystallize cubic (perovskite-structure), space group Pm3m-O (No. 221) with a = 429.41(8) pm (RbPdF3) respectively a = 424.30(4) pm (KPdF3). 相似文献
73.
Reaction of tBuPLi2 with Carbodiimides The reaction of bis(cyclohexyl)carbodiimide with tBuPLi2 in THF at 20 °C leads to the tetranuclear Li‐complex [Li4(THF)2{tBuP([cHexN]2C)2}2] ( 1 ). No addition on the carbodiimide but a silyl transfer was observed under similar conditions during the treatment of bis(trimethylsilyl)carbodiimide with tBuPLi2 to give the lithium salts tBuP(SiMe3)Li and [Li(THF)(Me3SiN‐C≡N)]n ( 2 ). 1 was characterized by NMR, IR and RE spectroscopy, mass spectrometry and X‐ray analyses. Theoretical calculations were performed for 1 . According to the structural investigations 1 consists ofa central centrosymmetrical twelve‐membered Li2N4C4P2 ring adjacent by two six‐membered LiN2C2P rings. The peripheric Li+ cations posssess coordination number (cn) 3 buildt‐up by two N atoms and a THF ligand, while the two central Li+ cations possess only cn 2. However, the theoretical calculations have shown no relevant bonding Li···Li or Li···P interaction. 相似文献
74.
Bernd G. Müller 《Journal of fluorine chemistry》1982,20(3):291-299
Single crystals of CaPdF4 (purple) and CdPdF4 (dark blue) have been obtained by heating CaF2 (CdF2) with PdF2 at 820°C (900°C) for ca. 20–30 d in sealed Pd (Pt) tubes. CaPdF4 crystallizes tetragonal (KBrF4-Type) with a = 5.521, c = 10.570 Å (space group I4/mcm ? D184h, No. 140) Z = 4, 283 unique reflexions, R = 0.083; Rw = 0.079, CdPdF4 cubic (CaF2-variant) with a = 5.403 Å (space group Pa3 ? T6h, No. 205) Z = 4, 165 unique reflexions, R = 0.047, Rw = 0.032. The high pressure modification of PdF2, obtained by heating PdF2 in closed Pt-tubes under a pressure of ≈ 60 kbar and ‘HgPdF4’, both black, a = 5.327 Å and a = 5.43 Å are isotypic. CaPdF4 is diamagnetic, CdPdF4 and HPPdF2 are antiferromegnetic. 相似文献
75.
The free NH3 molecule and the [Zn(NH3)4]2+ ion were studied by the kinematic coupling approach. The pure effects of this coupling were found to be small, and some modifications had to be introduced in order to get a reasonable force field. The force constants deduced for the skeletal vibrations are comparable with those of a quasi-exact force field. Calculated frequencies for [68Zn(NH3)4]2+ and [64Zn(ND3)4]2+ are reported in addition to those of [64Zn(NH3)4]2+. Mean amplitudes of vibration for [64Zn(NH3)4]2+ are given. 相似文献
76.
B. W. Wenclawiak Torsten Hees Corinna E. Z?ller Hans-Peter Kabus 《Fresenius' Journal of Analytical Chemistry》1997,358(4):471-474
An on-line system of supercritical fluid extraction (SFE) and high performance liquid chromatography (HPLC) via solid phase
extraction (SPE) is described for the determination of palladium and rhodium 2,2,6,6-tetramethyl-3,5-heptanedione-(thd) as
well as rhodium-acetylacetonate-(acac) and benzylacetonate-(bzac) chelates. The chelates were extracted with supercritical
CO2 from sand and humic acid, concentrated on SPE cartridges and analysed with HPLC. Two cartridge materials were tested and
compared to off-line trapping. The percentage of the breakthrough and cartridge retained material were measured in liquid
dichloromethane. The SFE conditions could be optimized to separate metal chelates during the extraction. The supercritical
fluid (SF) behaviour of different ligands on rhodium were investigated.
Received: 19 July 1996/Revised: 11 December 1996/Accepted: 14 December 1996 相似文献
77.
N.M.R. Investigation of Methylphosphonium Chloride The n.m.r. spectra of [CH3PH3]Cl in aqueous hydrochloric acid as solvent and of [OP(CH3) (OCH2CH2Cl)OCH2? ]2 in C6D6 und CD2Cl2 are described. 31P n.m.r. resonances with a line width at half height of 55 Hz are found for the H2O? HCl solutions of [CH3PH3]Cl in the solid state at 183 K. 相似文献
78.
The photoelectron(PE)spectrum of tricyclo[3.1.0.02,6] hex-2-ene(benzvalene 1) has been recorded. The first four bands in the PE spectrum of 1 can be assigned to transitions to 2B2, 2A1, 2A2 and 2B1 states of 11. This assignment is discussed in terms of the results of semiempirical and ab initio calculations on 1. Furthermore the highest occupied MO's of 1 are derived qualitatively from an interaction diagram between a distorted bicyclobutane and an ethylene moiety. 相似文献
79.
Horst Müller 《Fresenius' Journal of Analytical Chemistry》1962,189(4):336-339
Zusammenfassung Es wurde die ionophoretische Trennung von ReCl6
2–, ReBr6
2– und ReO4
– unter Verwendung verschiedener Papiersorten untersucht. Am geeignetsten erwies sich das Papier 2045 b Gl von Schl. & Sch.
Herrn Prof. G. Brauer danke ich für Förderung. Für die Überlassung von Rheniumverbindungen bin ich der Fa. W. C. Heraeus, Hanau, verpflichtet. Die Neutronenaktivierung wurde freundlicherweise von den Herren Dr. Marth und Dr. Köhler von der Reaktorstation in Garching bei München vorgenommen. Das Bundesministerium für Atomkernenergie und Wasserwirtschaft unterstützte die Untersuchung durch eine Sachbeihilfe. 相似文献
Summary The ionophoretic separation of ReCl6 2–, ReBr6 2–, and ReO4 – has been examined using different kinds of paper. Best results have been obtained with the paper 2045 b Gl from Schleicher & Schüll.
Herrn Prof. G. Brauer danke ich für Förderung. Für die Überlassung von Rheniumverbindungen bin ich der Fa. W. C. Heraeus, Hanau, verpflichtet. Die Neutronenaktivierung wurde freundlicherweise von den Herren Dr. Marth und Dr. Köhler von der Reaktorstation in Garching bei München vorgenommen. Das Bundesministerium für Atomkernenergie und Wasserwirtschaft unterstützte die Untersuchung durch eine Sachbeihilfe. 相似文献
80.
Heinz Falk Gabriele Streßler Norbert Müller 《Monatshefte für Chemie / Chemical Monthly》1988,119(4):505-508
Using a specific force field model, relative stabilities of 2,2-bipyrrole and 2,2-furylpyrrole conformers as well as of prodigiosene tautomers, configurations, and conformations, are studied. 2,2-Bipyrrole adopts anantiperiplanar conformation in accord with other theoretical calculations and experimental findings. Its rotational barrier calculated by this method compares favourably to the one derived by other means. For the parent prodigiosene the (Z)sp,sp arrangement is found to be the most stable one. The two possible tautomers within its dipyrrin fragment do not show a significant energy difference. 相似文献