The crystal structure of methanol monohydrate (CD3OD·D2O) at 160K from powder neutron diffraction

Fortes, A. Dominic

doi:10.1016/j.cplett.2006.09.077

Cited by 11 publications

(6 citation statements)

References 16 publications

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“…shortest d-spacing data) available. We had found previously (Fortes, 2006) that the early stages of structure refinement using the FOX output required the application of hard constraints on atomic coordinate and displacement parameter shifts, as well as stiff bond distance and angle restraints. In this instance, however, the refinement converged very smoothly without any bond restraints, proceeding quickly to the point at which all atoms could be refined with anisotropic displacement parameters.…”

Section: Indexing and Structure Solutionmentioning

confidence: 99%

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The crystal structure of perdeuterated methanol monoammoniate (CD₃OD·ND₃) determined from neutron powder diffraction data at 4.2 and 180 K

2009

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The crystal structure of perdeuterated methanol monoammoniate, CD3OD·ND3, has been solved from neutron powder diffraction data collected at 4.2 and 180 K. The crystal structure is orthorhombic, space group Pbca (Z = 8), with unit‐cell dimensions a = 11.02320 (7), b = 7.66074 (6), c = 7.59129 (6) Å, V = 641.053 (5) Å3 [ρcalc = 1162.782 (9) kg m−3] at 4.2 K, and a = 11.21169 (5), b = 7.74663 (4), c = 7.68077 (5) Å, V = 667.097 (4) Å3 [ρcalc = 1117.386 (7) kg m−3] at 180 K. The crystal structure was determined by ab initio methods from the powder data; atomic coordinates and anisotropic displacement parameters were subsequently refined by the Rietveld method to Rp < 3% at both temperatures. The crystal comprises a sheet‐like structure in the bc crystallographic plane, consisting of strongly hydrogen bonded elements; these sheets are stacked along the a axis, and adjacent sheets are linked by what may be comparatively weak C—D...O hydrogen bonds. Within the strongly bonded sheet structure, ND3 molecules are tetrahedrally coordinated by the hydroxy moieties of the methanol molecule, accepting one hydrogen bond (O—D...N) of length ∼1.75 Å, and donating three hydrogen bonds (N—D...O) of length 2.15–2.25 Å. Two of the methyl deuterons appear to participate in weak interlayer hydrogen bonds (C—D...O) of length 2.7–2.8 Å. The hydrogen bonds are ordered at both 4.2 and 180 K. The relative volume change on warming from 4.2 to 180 K, ΔV/V, is +4.06%, which is comparable to, but more nearly isotropic (as determined from the relative change in axial lengths, e.g.Δa/a) than, that observed in deuterated methanol monohydrate.

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Section: Indexing and Structure Solutionmentioning

confidence: 99%

“…References: (a) this work; (b)Fortes, Wood & Knight (2009); (c) our unpublished work (seeFortes, 2006; ISIS experimental report RB610064); (d )Torrie et al (1989Torrie et al ( , 2002; (e) Hewat & Riekel(1979); ( f ) Fortes et al (2008); (g) Fortes et al (2003); (h) our unpublished work.…”

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confidence: 96%

The crystal structure of perdeuterated methanol monoammoniate (CD₃OD·ND₃) determined from neutron powder diffraction data at 4.2 and 180 K

2009

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“…Haghighi et al (2009), Vuillard andSanchez (1961), and Miller and Carpenter (1964), and adapted from Kargel (1992), Ott et al (1979), and Takaizumi and Wakabayashi (1997). The hydrated solid phase is methanol monohydrate (Fortes, 2006;Fortes et al, 2011). On Enceladus, the observations of water-rich plumes (Dougherty et al, 2006;Hansen et al, 2011;Hsu et al, 2015;Porco et al, 2006;Waite et al, 2009) reveal either the presence of a liquid reservoir or highly active melting. The hydrated solid phase is methanol monohydrate (Fortes, 2006;Fortes et al, 2011). On Enceladus, the observations of water-rich plumes (Dougherty et al, 2006;Hansen et al, 2011;Hsu et al, 2015;Porco et al, 2006;Waite et al, 2009) reveal either the presence of a liquid reservoir or highly active melting.…”

Section: Introductionmentioning

confidence: 99%

“…Phases are solid unless indicated otherwise. The hydrated solid phase is methanol monohydrate (Fortes, 2006;Fortes et al, 2011). On Enceladus, the observations of water-rich plumes (Dougherty et al, 2006;Hansen et al, 2011;Hsu et al, 2015;Porco et al, 2006;Waite et al, 2009) reveal either the presence of a liquid reservoir or highly active melting. The composition of the plumes suggests a liquid reservoir (Hsu et al, 2015;Postberg et al, 2011), and the measured libration is consistent with a global subsurface ocean, rather than a localized reservoir (Thomas et al, 2016).…”

Section: Introductionmentioning

confidence: 99%

The Liquidus Temperature for Methanol‐Water Mixtures at High Pressure and Low Temperature, With Application to Titan

et al. 2018

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Methanol is a potentially important impurity in subsurface oceans on Titan and Enceladus. We report measurements of the freezing of methanol‐water samples at pressures up to 350 MPa using a volumetric cell with sapphire windows. For low concentrations of methanol, the liquidus temperature is typically a few degrees below the corresponding ice freezing point, while at high concentrations it follows the pure methanol trend. In the Ice‐III regime, we observe several long‐lived metastable states. The results suggest that methanol is a more effective antifreeze than previously estimated and might have played an important role in the development of Titan's subsurface ocean.

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“…The NMR spectra exhibit a central line component above 140 K due to the onset of dynamic reorientation of water molecules in the structure. The structure of perdeuterated methanol monohydrate was established from neutron powder diffraction at 160 K (Fortes 2006). The crystal is actually orthorhombic, space-group Cmc2 1 (Z = 4) ρ calc = 1265.55(2) kg m −3 at 4.2 K, but coincidentally passes through a state of metric tetragonality at ∼80 K, the temperature of the earlier X-ray study, by virtue of its anisotropic thermal expansion.…”

Section: The Methanol-water Binary Systemmentioning

confidence: 99%

Phase Behaviour of Ices and Hydrates

Fortes¹,

Choukroun

2010

Space Sci Rev

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The primary volatile 'rock-forming' minerals in the icy satellites of the outer solar system include water-ice and various hydrated crystals of methane and ammonia. The rich polymorphism of these substances as a function of pressure and temperature are described in this chapter. This polymorphism has a fundamental influence on the exchange of mass and energy between the core and the surface of icy satellites. We describe the current stateof-the-art in our understanding of the high pressure phase behaviour and the measurements of thermoelastic and transport properties of these substances. In addition we describe the structures and properties of hydrated phases of methanol, sulfuric acid, and various sulfate salts.

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The crystal structure of methanol monohydrate (CD3OD·D2O) at 160K from powder neutron diffraction

Cited by 11 publications

References 16 publications

The crystal structure of perdeuterated methanol monoammoniate (CD₃OD·ND₃) determined from neutron powder diffraction data at 4.2 and 180 K

The crystal structure of perdeuterated methanol monoammoniate (CD₃OD·ND₃) determined from neutron powder diffraction data at 4.2 and 180 K

The Liquidus Temperature for Methanol‐Water Mixtures at High Pressure and Low Temperature, With Application to Titan

Phase Behaviour of Ices and Hydrates

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The crystal structure of methanol monohydrate (CD3OD·D2O) at 160K from powder neutron diffraction

Cited by 11 publications

References 16 publications

The crystal structure of perdeuterated methanol monoammoniate (CD3OD·ND3) determined from neutron powder diffraction data at 4.2 and 180 K

The crystal structure of perdeuterated methanol monoammoniate (CD3OD·ND3) determined from neutron powder diffraction data at 4.2 and 180 K

The Liquidus Temperature for Methanol‐Water Mixtures at High Pressure and Low Temperature, With Application to Titan

Phase Behaviour of Ices and Hydrates

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Product

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The crystal structure of perdeuterated methanol monoammoniate (CD₃OD·ND₃) determined from neutron powder diffraction data at 4.2 and 180 K

The crystal structure of perdeuterated methanol monoammoniate (CD₃OD·ND₃) determined from neutron powder diffraction data at 4.2 and 180 K