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Single-crystal neutron diffraction and Raman spectroscopic study of hydroxylherderite, CaBePO4(OH,F)

Published online by Cambridge University Press:  05 July 2018

G. D. Gatta ,
S. D. Jacobsen ,
P. Vignola ,
G. J. McIntyre ,
G. Guastella  and
L. F. Abate
G. D. Gatta*
Affiliation:
Dipartimento di Scienze della Terra, Universitá degli Studi di Milano, Via Botticelli 23, I-20133 Milan, Italy CNR - Istituto di Cristallografia, Sede di Bari, Via G. Amendola 122/o, 70126 Bari, Italy
S. D. Jacobsen
Affiliation:
Department of Earth and Planetary Sciences, Northwestern University, Evanston, IL 60208, USA
P. Vignola
Affiliation:
Dipartimento di Scienze della Terra, Universitá degli Studi di Milano, Via Botticelli 23, I-20133 Milan, Italy CNR-Istituto per la Dinamica dei Processi Ambientali, Milan, Italy
G. J. McIntyre
Affiliation:
Australian Nuclear Science and Technology Organisation, Locked Bag 2001, Kirrawee DC NSW 2232, Australia
G. Guastella
Affiliation:
Agenzia delle Dogane e dei Monopoli, Direzione Regionale per la Lombardia, Laboratorio e Servizi Chimici, Via M. Bruto 14, I-20138 Milan, Italy
L. F. Abate
Affiliation:
Dipartimento di Scienze della Terra, Universitá degli Studi di Milano, Via Botticelli 23, I-20133 Milan, Italy
*
E-mail: [email protected]
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Abstract

The crystal structure, H bonding and chemical composition of hydroxylherderite from the Bennett pegmatite, Buckfield, Oxford County, Maine, USA were investigated by single-crystal X-ray diffraction and neutron Laue diffraction, electron microprobe analysis in wavelength-dispersive mode, inductively coupled plasma-atomic emission spectrometry and polarized Raman spectroscopy [Ca(Na0.01Ca1.01)∑1.02Be(Be0.98Li0.01)∑0.99P(Si0.03P0.98)∑1.01O4(OH0.67F0.33)∑1, Z = 4, a = 9.7856(5), b = 7.6607(5), c = 4.8025(3) Å, β = 90.02(3)°, V = 360.02(4) Å3, space group P21/a]. The neutron-structure refinement converged with fully anisotropic displacement parameters to give a final agreement index R1 = 0.0363 for 85 refined parameters and 1614 unique reflections with Fo >4σ(Fo). The structure refinement was used to determine the H position and geometry of H bonding in the structure. One H site was found on the O5 anion with an O–H interatomic distance, corrected for “riding motion”, of 0.996(2) Å. The H bond of hydroxylherderite is bifurcated with O2 and O4 acceptors forming H bonds with O5⋯O2 = 3.163(1) Å, H⋯O2 = 2.544(2) Åand O5–H⋯O2 = 121.8(1)°; O5⋯O4 = 3.081(1) Å, H⋯O4 = 2.428(2) Å and O5–H⋯O4 = 124.4(1)°. The highly non-linear O–H⋯O hydrogen bonds in hydroxylherderite and in the isotypic datolite [ideally CaBSiO4(OH)] are constrained by the tetrahedral network topology. Two main O–H stretching modes were observed in the Raman spectra at 3565 and 3620 cm–1, which are attributed to the bifurcated H bond. Two additional weak bands at 3575 and 3610 cm–1 are attributed to Si–P disorder in the tetrahedral sites. Results of this study will contribute to the correlation of H-bonding geometry and O–H stretching frequencies of highly non-linear H bonds.

Keywords

hydroxylherderiteelectron microprobe analysis (WDS)inductively coupled plasma-atomic emission spectrometryRaman spectroscopyneutron Laue diffractionhydrogen bonding
Type
Research Article
Information
Mineralogical Magazine , Volume 78 , Issue 3 , June 2014 , pp. 723 - 737
Copyright
Copyright © The Mineralogical Society of Great Britain and Ireland 2014

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