title: Structure determination of a partially ordered layered silicate material with an NMR crystallography approach.
abstract: Structure determination of layered materials can present challenges for conventional diffraction methods due to the fact that such materials often lack full three-dimensional periodicity since adjacent layers may not stack in an orderly and regular fashion. In such cases, NMR crystallography strategies involving a combination of solid-state NMR spectroscopy, powder X-ray diffraction, and computational chemistry methods can often reveal structural details that cannot be acquired from diffraction alone. We present here the structure determination of a surfactant-templated layered silicate material that lacks full three-dimensional crystallinity using such an NMR crystallography approach. Through a combination of powder X-ray diffraction and advanced29Si solid-state NMR spectroscopy, it is revealed that the structure of the silicate layer of this layered silicate material templated with cetyltrimethylammonium surfactant cations is isostructural with the silicate layer of a previously reported material referred to as ilerite, octosilicate, or RUB-18. High-field1H NMR spectroscopy reveals differences between the materials in terms of the ordering of silanol groups on the surfaces of the layers, as well as the contents of the inter-layer space.
authors.affiliation: Department of Chemistry, Redeemer University College, 777 Garner Road East, Ancaster, ON, L9K 1J4, Canada.
authors.forename: Darren Henry
authors.initials: DH
authors.lastname: Brouwer
authors.affiliation: Institut des Matériaux Jean Rouxel, 2 rue de la Houssinire, Nantes, France.
authors.forename: Sylvian
authors.initials: S
authors.lastname: Cadars
authors.affiliation: Department of Chemistry, Redeemer University College, 777 Garner Road East, Ancaster, ON, L9K 1J4, Canada.
authors.forename: Kathryn
authors.initials: K
authors.lastname: Hotke
authors.affiliation: Department of Chemistry, Redeemer University College, 777 Garner Road East, Ancaster, ON, L9K 1J4, Canada.
authors.forename: Jared
authors.initials: J
authors.lastname: Van Huizen
authors.affiliation: Department of Chemistry, Redeemer University College, 777 Garner Road East, Ancaster, ON, L9K 1J4, Canada.
authors.forename: Nicholas
authors.initials: N
authors.lastname: Van Huizen
keywords: NMR crystallography; computational chemistry; disordered materials; layered silicates; powder X-ray diffraction; solid-state NMR