TY  - JOUR
A1  - Beske, Maurice
A1  - Cronje, Stephanie
A1  - Schmidt, Martin U.
A1  - Tapmeyer, Lukas
T1  - Disordered sodium alkoxides from powder data: crystal structures of sodium ethoxide, propoxide, butoxide and pentoxide, and some of their solvates
T2  - Acta crystallographica / Section B
N2  - The crystal structures of sodium ethoxide (sodium ethano­late, NaOEt), sodium n-propoxide (sodium n-propano­late, NaOnPr), sodium n-butoxide (sodium n-butano­late, NaOnBu) and sodium n-pentoxide (sodium n-amylate, NaOnAm) were determined from powder X-ray diffraction data. NaOEt crystallizes in space group P421m, with Z = 2, and the other alkoxides crystallize in P4/nmm, with Z = 2. To resolve space-group ambiguities, a Bärnighausen tree was set up, and Rietveld refinements were performed with different models. In all structures, the Na and O atoms form a quadratic net, with the alkyl groups pointing outwards on both sides (anti-PbO type). The alkyl groups are disordered. The disorder becomes even more pronounced with increasing chain length. Recrystallization from the corresponding alcohols yielded four sodium alkoxide solvates: sodium ethoxide ethanol disolvate (NaOEt·2EtOH), sodium n-propoxide n-propanol disolvate (NaOnPr·2nPrOH), sodium isopropoxide iso­propanol pentasolvate (NaOiPr·5iPrOH) and sodium tert-amylate tert-amyl alcohol monosolvate (NaOtAm·tAmOH, tAm = 2-methyl-2-butyl). Their crystal structures were determined by single-crystal X-ray diffraction. All these solvates form chain structures consisting of Na+, –O− and –OH groups, encased by alkyl groups. The hydrogen-bond networks diverge widely among the solvate structures. The hydrogen-bond topology of the iPrOH network in NaOiPr·5iPrOH shows branched hydrogen bonds and differs considerably from the networks in pure crystalline iPrOH.
KW  - sodium alkoxide
KW  - powder data
KW  - solvate
KW  - isopropanol
KW  - Bärnighausen tree
KW  - PXRD
Y1  - 2021
UR  - http://publikationen.ub.uni-frankfurt.de/frontdoor/index/index/docId/63876
UR  - https://nbn-resolving.org/urn:nbn:de:hebis:30:3-638764
SN  - 2052-5206
N1  - Open access funding enabled and organized by Projekt DEAL.
VL  - 77
IS  - 1
SP  - 68
EP  - 82
PB  - Wiley-Blackwell
CY  - Oxford [u.a.]
ER  -