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Sinteza in karakterizacija hidroksilamonijevih fluorometalatov titana, cirkonija in hafnija : doktorska disertacijaBan, IrenaV sistemu N▫$H_2$▫OH - HF - Ti▫$F_4$▫ - ▫$H_2$▫O smo v prvi fazi izolirali iz vodne raztopine mikrokristalinično fazo sestave (N▫$H_3$▫OH▫$)_2$▫Ti▫$F_6$▫ in jo karakterizirali s kemijsko, ... rentgenografsko in termično analizo ter IR in Ramansko spektrokopijo. Zadnji dve analizi pokažeta, da vsebuje spojina izolirane [Ti▫$F_6$▫]▫$^{-2}$▫ anione in N▫$H_3$▫O▫$H^+$▫ katione. Pri prekristalizaciji faze (N▫$H_3$▫OH▫$)_2$▫Ti▫$F_6$▫ so nam kasneje izkristalizirali monokristali sestave (N▫$H_3$▫OH▫$)_2$▫Ti▫$F_6$▫x2▫$H_2$▫O. Strukturna analiza dihidrata prav tako pokaže, da vsebuje faza (N▫$H_3$▫OH▫$)_2$▫Ti▫$F_6$▫x2▫$H_2$▫O izolirane [Ti▫$F_6$▫]▫$^{-2}$▫ anoine in N▫$H_3$▫O▫$H^{+}$▫ katione. Koordinacijski polieder je oktaeder. (N▫$H_3$▫OH▫$)_2$▫Ti▫$F_6$▫x2▫$H_2$▫O, ▫$M_r$▫=265.96, monoklinska, P▫$2_1$▫/c(No.:15), a=6.203(1)Å, b=10.057(1)Å, c=7.464(1)Å, ▫$\beta$▫=110.653, V=435.7(1)▫$Å^{3}$▫, Z=2, ▫$D_c$▫=2.027 g▫$cm^{3}$▫, MoK▫$\alpha$▫, ▫$\lambda$▫=0.71069, končni R=0.029, ▫$R_w$▫=0.021 za 1194 opazovanih odbojev. V sistemu N▫$H_2$▫OH - HF - Zr▫$F_4$▫ - ▫$H_2$▫O smo izolirali dve spojini sestave (N▫$H_3$▫OH▫$)_2$▫Zr▫$F_6$▫(1) in (N▫$H_3$▫OH▫$)_3$▫Zr njunih nasičenih vodnih raztopin so izkristalizirali monokristali enake sestave, ki smo jih analizirali s kemijsko, rengenografsko in termično analizo ter IR spektroskopijo. Rezultati strukturne analize pokažejo, da ni strukturne izomerije z zgornjo spojino. Zr ion je v spojinah 1 in 2 koordiniran z osmimi F ioni. Koordinacijski polieder je dodekaeder. V spojini 1 so poliedri povezani v verige, v spojini 2 pa tvorijo dvojne poliedre. (N▫$H_3$▫OH▫$)_2$▫Zr▫$F_6$▫, ▫$M_r$▫=273.29, triklinska, P▫$\bar{1}$▫(No.:2), a=7.400(2)Å, b=7.609(2)Å, c=7.887(2)Å, ▫$\alpha$▫=57.29(3)°, ▫$\beta$▫=62.16(3)°, ▫$\gamma$▫=67.83(2)°, V=325.7(7)▫$Å^{3}$▫, Z=2, ▫$D_c$▫=2.786g▫$cm^{-3}$▫, MoK▫$\alpha$▫, ▫$\lambda$▫=0.7106, končni R=0.018, ▫$R_w$▫=0.015 za 1714 opazovanih odbojev. (N▫$H_3$▫OH▫$)_3$▫Zr▫$F_7▫$, ▫$M_r$▫=326.28, triklinska, P▫$\bar{1}$▫(No.:2), a=7.128(1)Å, b=7.989(1)Å, c=8.888(1)Å, ▫$\alpha$▫=109.72(1)°, ▫$\beta$▫=91.01(1)°, ▫$\gamma$▫=104.27(1)°, V=458.9(1)▫$Å^{3}$▫, Z=2, ▫$D_c$▫=2.361gc▫$m^{-3}$▫, MoK▫$\alpha$▫, ▫$\lambda$▫=0.7106, končni R=0.022, ▫$R_w$▫=0.020 za 2597 opazovanih odbojev. V sistemu N▫$H_2$▫OH - HF - Hf▫$F_4$▫ - ▫$H_2$▫O smo prav tako izolirali dve spojini sestave (N▫$H_3$▫OH▫$)_2$▫Hf▫$F_6$▫(1) in (N▫$H_3$▫OH▫$)_3$▫Hf▫$F_7$▫(2). Strukturne preiskave pokažejo, da sta spojini izomorfni s spojinama(N▫$H_3$▫OH▫$)_2$▫Zr▫$F_6$▫(1) in (N▫$H_3$▫OH▫$)_3$▫Zr▫$F_7$▫(2).Type of material - dissertation ; adult, seriousPublication and manufacture - Maribor : [I. Ban], 1999Language - slovenianCOBISS.SI-ID - 4824342
Author
Ban, Irena
Other authors
Volavšek, Bogdan |
Golič, Ljubo
Topics
anorganska kemija |
sinteze |
kristalokemija |
fluorotitanati |
hidroksilamonijev fluorotitanat (IV) |
rentegenska strukturna analiza |
rentgenska praškovna difrakcija |
termične analize |
inorganic chemistry |
synthesis |
crystallography |
fluorotitanates |
hydroxylammonium fluorotitanate(IV) |
structural X ray analysis |
thermal analysis |
x ray powder diffraction
Library/institution |
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Library of Technical Faculties, Maribor | Maribor | KTFMB |
reading room 1 cop.
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National and University Library, Ljubljana | Ljubljana | NUK |
reading room 1 cop.
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University of Maribor Library | Maribor | UKM |
reading room 1 cop.
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Database name | Field | Year |
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Ban, Irena | 08761 |
Volavšek, Bogdan | 00456 |
Golič, Ljubo | 00842 |
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