dc.contributor.author |
Vongvusharintra, Atita |
|
dc.contributor.other |
Youngstown State University, degree granting institution. |
|
dc.contributor.other |
Youngstown State University. Department of Chemistry. |
|
dc.date.accessioned |
2020-05-18T15:07:51Z |
|
dc.date.available |
2020-05-18T15:07:51Z |
|
dc.date.issued |
1972 |
|
dc.identifier.other |
903505131 |
|
dc.identifier.other |
b1686122 |
|
dc.identifier.uri |
https://jupiter.ysu.edu/record=b1686122 |
|
dc.identifier.uri |
http://hdl.handle.net/1989/15299 |
|
dc.description |
vii, 34 leaves : illustration ; 29 cm
Thesis M.S. Youngstown State University 1972.
Includes bibliographical references (leaves 33-34). |
en_US |
dc.description.abstract |
A fast, efficient, and inexpensive method was developed for the preparation of Nb6Br14
•8H2O. This compound is an important starting material for the preparation of coordination compounds based on hexanuclear (Nb6Br12)n+ central cations and was available previously only in minute quantities. Potassium bromide, niobium pentabromide, and excess niobium metal were conproportionated in Vycor tubes at 720°C to give K4Nb6Br18, which upon extraction with water forms Nb6Br14•8H2o in yields up to 80%.
The new coordination compounds [(Nb6Cl12)Cl2 (CH3CN)4],
[(Nb6Br12)Br2 (CH3CN)4], and [(Nb6Cl12)F2 (C5H5NO)4] have been synthesized. In attempts to prepare the adducts, (Nb6Cl12)F2L4 (L = CH3CN, DMSO, DMF), impure or nonuniform products were obtained.
The new complex, [(Nb6Cl12)Cl2 (CH3CN)4], was used as a starting material for the preparation of a product (Me4N)3 [(Nb6Cl12)Cl6]·3CH3CN with an analysed Cl:Nb ratio of
17.99:6.00. Anionic [(Nb6Cl12)Cl6]n- complexes with Cl:Nb ratios close to the ideal value of 18.00:6.00 are very difficult to obtain with Nb6Cl14•8H2O as -starting material.
Attempts to dehydrate Nb6Cl14•8H20 with thionyl chloride caused its oxidation to (Nb6Cl12)4+containing material. Impure Nb6Cl16 adducts were formed. Reaction of
Nb6Cl14•8H2O with thionyl chloride and acetonitrile did not lead to the adduct Nb6Cl16 •2CH3CN, but yielded impure (Nb6Cl12 )4+-containing materials with approximate Cl:Nb
ratios of 18:6 and 28:6, respectively. |
en_US |
dc.description.sponsorship |
Youngstown State University. Department of Chemistry. |
en_US |
dc.language.iso |
en_US |
en_US |
dc.publisher |
[Youngstown, Ohio] : Youngstown State University, 1972. |
en_US |
dc.relation.ispartofseries |
Master's Theses;no. 0022 |
|
dc.subject |
Niobium compounds. |
en_US |
dc.subject |
Metal complexes. |
en_US |
dc.title |
Synthesis of some hexanuclear niobium halide cluster compounds |
en_US |
dc.type |
Thesis |
en_US |