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Title: The synthesis and structural characterization of novel transition metal fluorides

Technical Report ·
DOI:https://doi.org/10.2172/7017272· OSTI ID:7017272

High purity KMF[sub 6] and K[sub 2]MF[sub 6] salts (M = Mo,Re, Ru, Os, Ir, Pt) are obtained from reduction hexafluorides. A rhombohedral unit cell is observed for KReF[sub 6]. Fluoride ion capture by Lewis acids from the hexafluorometallate (IV) salts affords high purity tetrafluorides for M = Mo, Re, Ru, Os, and Pd. The structure of RuF[sub 4] is determined from X-ray synchrotron and neutron powder data. Unit cells based on theorthorhombic PdF[sub 4] type cell are derived from X-ray powder data for ReF[sub 4] and OsF[sub 4]. Fluoride ion capture from KAgF[sub 4] provides the thermally unstable trifluoride as a bright, red, diamagnetic solid. The structure solution of AgF[sub 3] and redetermination of the AuF[sub 3] structure from X-ray synchrotron and neutron powder data demonstrate that the two are isostnictural. Thermal decomposition product of AgF[sub 3] is the mixed valence compound Ag[sup II]Ag[sub 2][sup III]F[sub 8]. Several new salts containing the (Ag - F)[sub n][sup n+] chain cation are prepared. The first linear (Ag - F)[sub n][sup n+] chain is observed in AgF[sup +]BF[sub 4 [sup [minus]]] which crystallizes in a tetragonal unit. AgFAuF[sub 4] has a triclinic unit cell and is isostructural with CuFAuF[sub 4]. AgFAuF[sub 6] has an orthorhombic unit cell and appears to be isostructural with AgFAsF[sub 6]. A second mixed valence silver fluoride, Ag[sup II]Ag[sup III]F[sub 5], is prepared, which magnetic measurements indicate is probably an AgF[sup +] salt. Magnetic data for all of the AgF[sup +] salts exhibit low magnitude, temperature independent paramagnetism characteristic of metallic systems. Cationic AG(II) in acidic AHF solutions is a powerful oxidizer, capable of oxidizing Xe to Xe(II) and O[sub 2] to O[sub 2][sup +]. Reactions with C[sub 6]F[sub 6] and C[sub 3]F[sub 6] suggest an electron capture mechanism for cationic AG(II) oxidations.

Research Organization:
Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)
Sponsoring Organization:
USDOE; USDOE, Washington, DC (United States)
DOE Contract Number:
AC03-76SF00098
OSTI ID:
7017272
Report Number(s):
LBL-32892; ON: DE93002551
Resource Relation:
Other Information: Thesis (Ph.D.)
Country of Publication:
United States
Language:
English