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I Hypervalent Tropolonates of 13 Group Metal Ions And RADIOCHEMISTRY, STABLE ISOTOPES, 62 NUCLEAR ANALYTICAL METHODS. GENERAL CHEMISTRY pectation value of orbital radii <r> of the outer- The thin film surface of dioxygenyl hexafluoro- 2 20 most orbitals (nd 3 /2, nds12) for lighter homolo s. antimonate was used to study adsorption of Rn. 22 0 2 24 Due to the unique electron configuration of 1 1 2L+, The Rn (T1 /2=55 s) was obtained from a Ra the 6d 3/2, 6d5 2 and 7s orbitals were considered as generator. Figure shows the gamma spectrum of the outermost. The estimation gives IR=118 pm for dioxygenyl hexafluoroantimonate surface after CN=6. exposition to the 22 0Rn. The peaks in the gamma Table. Ionization potentials and ionic radii of Hg, Xe, Rn and element 112. Hg | Xe Rn 112 Electron configuration of M2 5d | 56p 4 6pd8 7s2 Ist ionization potential fcV] 10.2 12.1 10.8 12.0 2nd ionization potential leV] 18.8 21.0 | 18.0 22.5 Ist + 2nd ionization potential [eV] 29.0 33.1 28.8 34.5 2 Ionic radius of M + [pm) (CN=6) 102 _ . 118 (calc.) l As shown in the Table, the ionization potentials spectrum belong to 2 12Pb and 212 Bi, which are for 1122+ are higher than those for Hg and Rn, also descended from the decay 2 20 Rn. the ionic radius is greater than that for Hg 2 . so we Dioxygenyl hexafluoroantimonate oxidizes Rn can conclude that the reactivity of element 112 and adsorbs the product in the reaction: would lay between those of Xe and Rn, probably Rn + 202 SbF6 -a RnF+Sb2 Fft + 202 closer to Xe. The proposed studies would help us in explain- In this work we studied the chemical properties ing whether the element 112 is similar to its lighter of Rn as an expected homolog of element 112, with 14_ the hope that the results would allow us to plan an experiment on the chemical identification of ele- 12 ment 112. As a model experiment on the chemistry of l element 112 we studied adsorption of Xe and Rn on a thin film surface of dioxygenyl hexafluoroanti- B l monate. The dioxygenyl compounds of hexafluoro- 0 I platinate, heksafluoroarsenate and hexafluoroanti- ,W monate are well known as very effective oxidizing and adsorbing agents for Xe and Rn 31I.We have 2 I synthesized dioxygenyl hexafluoroantimonate in then _ form of thin film surface. One drop of antimony l 20 3 40 WO 6M pentafluoride was placed on a stainless steel disc, Channel and then reacted with fluorine and oxygen from a Fig. TIhe gamma spectrum of O2SbF6 after exposition to the iso- gas mixture according to the following reaction: tope of 220Rn. 2°2F2+ 2bF5hv 20+b, 202 + F2 + 2SbF5 -hv 2O~SbFg congeners in Group 12 as indicates the normal Due to high reactivity of fluorine we used a continuation of the Periodic Table, or to the noble dilute gas mixture. The whole installation was made gases as suggested by the theoretical predictions from Monell alloy, teflon and Pyrex glass. The gases based on the relativistic calculation. were dried before the reaction. After less than one References minute of the contact of the gas mixture with di- oxygenyl hexafluoroantimonate we obtained a white [21. Siekierski S.: Comments Inorg. Chem., 12.,121 (1997). solid film, which was stable at room temperature. 13]. Adloff J.P., Guillaumont R.: Fundamentals of Radiochemistry. The product was highly sensitive for humidity. CRC Press, Boca Raton 1993. p.377. 0an <)) HYPERVALENT TROPOLONATES OF 13 GROUP METAL IONS AND THEIR TOPO ADDUCTS. THE DENSITY FUNCTIONAL STUDIES Jerzy Narhutt, Marian Czerwifiskil/ a Chemistry Institute, Pedagogical University, Czqstochowa, Poland 0L In an earlier communication [1] we reported on ex- of trivalent metal ions of Groups 3 and 13, supple- perimental studies on adduct formation between mented by theoretical calculations of structures, trioctylphosphine oxide (TOPO) and tropolonates energies and charge distribution for the chelates RADIOCHEMISTRY, STABL1E ISOTOPFS, NUCLEAR ANALYTICAL METHIODS, GENERAL, CHEMISTRY 63 and adducts, based on the Density Functional binding of the seventh ligand to the hypervalent Theory (DFT). Both experimental and calculation chelate should additionally decrease the electron results have shown that the 1:1 adducts formed by population on the MOL bonds in the adduct by Group 3 metal chelates are much more stable than 1/7. This has really been observed for In and TI, those formed by Group 13 metal chelates (Table), where the M-O- populations in the TMPO adducts the contribution from the differences in ion radii are by about 13 ±2% less than those in the corres- being less important. We explained the obtained ponding chelates (Table , contrary to the Sc and Y order of increasing stability constants of the adducts, where the M-O - populations remain prac- adducts, In<TI< <Sc<Y, (equivalent to the tically the same as those in the chelates. Therefore, tendency to increase CN of a central metal ion in we suppose that the adducts formed by In and Tl the neutral chelates) in terms of electron structure chelates are also hypercoordinate, with their bond- of the metal ions, in particular in terms of ing MOs formed only from the ns and rip orbitals of hybridization theory. Because of lower energies of the d'11 ions, with no participation of either filled (n-1)d than rid orbitals of an ion, promotion energy (n-1)d or virtual nd orbitals. In contrast, Sc and Y required to transform a p-block metal ion to the chelates form stronger `normal` adducts with seven 2 valence state V6 (nsinp3nd hybridization) was bonding MOs in which the vacant (n-1)d orbitals of expected to be much higher than that for a d-block the metal do participate. Indeed, the analysis of metal ion [(n-1)d 3 nslnp2 ]. Also the promotion charge distribution on the metal ions shows that the energy E6 7, related to the transition V6 - V7, was d-block ions accept some electron density from expected to be much higher for p-block elements TMPO in the adducts, in contrast to the p-block (ns'np3 nd 3 ) than that for the d-block ones metals, which increase their positive charge in the [(n-1)d3 nslnp3], which should be reflected in the adducts [21. Also the analysis of the electron popu- energy of adduct formation. lation of basis metal AOs contributing to bonding The experimental stability constants of the metal (MN-OL) MOs in the chelates betokens a contri- tropolonate - TOPO adducts given in the Table bution from the d orbitals of Sc and Y, but none have been corrected for the effects of tropolone - from those of In and TI. The same has been ob- TOPO association in the organic phase [2]. There is served in the case of the adducts (M-OB bonding). also evidence for formation of some 1:2 adducts. The expansion coefficients of the bonding MOs Also the chelates of Group 3 metals are much more show that the d orbitals of Sc and Y in the adducts stable than those formed by Group 13 metals [21. accept practically the whole charge equal to the Table. Experimental stability constants of the M(trop)3.(T(PO)n adducts 121, calculated Mulliken populations of the M-O bonps in the model M(adik)3 chelates and their TMPO adducts, and average energies (in atomic units; t a.u.=2262 ki mol ) of selected orbitals in the model adducts. Mt Adduct stability constants q(M-OL) Orbital energies lau.l ] 1o09,3,1 og03,2 chelates adductsE(o) E(7) In 0.97 ±0.10 1.86 +0.10 0.177 0.150 -0.027 (15%) -0.4132 -0.2904 T] 1.35 ±0.08 (0.3 ±5.9)a 0.134 0.119 -0.015 (11%) -0.4129 -0.2897 Sc 4.27 ±0.03 -a 0.155 0.159 ( )004 (3%) -0.4099 -0.2936 Y4 4.99 ±0.05 7.39 ±0.08 0.160 0.154 -0.006 (4%) -0.4135 -02943_ a The P3,2 value could not be determined because of either insufficient TOPO concentration in the experiment (Sc) or the antagonistic effect in solvent extraction at higher TOIPO concentration (TI). In this work we have carried out additional DFT difference (ca. 0.03 a.u.) between the Aq values calculations [1,2] of the charge distribution (Mulli- calculated for the adducts of d-block and p-block ken electron population) on the M-O bonds in the metals [2]. model M(adik)3 chelates and their TMPO adducts Rather high electron population on the In-OL (Table), which throw more light on the problem. It bonds (the population on the Tl-OL. bonds is low, may be assumed that less stable both [ML 3] as expected) can be explained in terms of incomp- chelates and [ML 3 .TMPOJ adducts of the dlj ions lete screening from nuclear charge by the filled d (Table) do not necessarily imply that the high-lying shell, which increases the effective charge on the virtual nd orbitals of the (n-l)d ions participate in p-block ion, and also the population of the bonds. bonding. Moreover, general considerations suggest This is in line with the high negative AEdeh and that the use of these distant nd orbitals is unlikely AEint values for In [2]. The lack of unoccupied [3,4J. Molecular orbitals of such a complex with e.g. (n-1)d In orbitals able to accept the electron density six ligands can be formed using only four orbitals of makes the M-O- charge separation in [In(adik)3 J the central ion (s and p) and six ligand orbitals.
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