A crystal chemical investigation of a natural specimen of whitlockite, ideally Ca9Mg(PO4)(6)[PO3(OH)], from Palermo Mine (USA), was achieved by means of a combination of electron microprobe analysis (EMPA) in WDS mode, single-crystal neutron diffraction probe (NDP) and single-crystal X-ray diffraction (XRD), and Fourier transform infrared (FTIR) spectroscopy. The crystal-chemical characterization resulted in the empirical formula (Ca8.682Na0.274Sr0.045)(sigma 9.000)(Ca-0.034(0.996))(sigma 1.000)(Mg0.533Fe0.3422+Mn0.0622+Al0.046)(sigma 0.983)(P1.006O4)(6)[PO3(OH0.968F0.032)(sigma 1.000)]. Crystal-structure refinement, in the space group R3c, converged to R1 = 7.12% using 3273 unique reflections from NDP data and to R1 = 2.43% using 2687 unique reflections from XRD data. Unit cell parameters from NDP are a = 10.357(3) angstrom, c = 37.095(15) angstrom and V = 3446(2) angstrom(3), and from XRD, the parameters are a = 10.3685(4) angstrom, c = 37.1444(13) angstrom and V = 3458.2(3) angstrom(3). NDP results allowed a deeper definition of the hydrogen-bond system and its relation with the structural unit [PO3(OH)]. The FTIR spectrum is very similar to that of synthetic tricalcium phosphate Ca-3(PO4)(2) and displays minor band shifts due to slightly different P-O bond lengths and to the presence of additional elements in the structure. A comparison between whitlockite, isotypic phases from the largest merrillite group, and its synthetic counterpart Ca-3(PO4)(2) is provided, based on the XRD/NDP and FTIR results.

Capitelli, F., Bosi, F., Capelli, S.C., Radica, F., Della Ventura, G. (2021). Neutron and xrd single‐crystal diffraction study and vibrational properties of whitlockite, the natural counterpart of synthetic tricalcium phosphate. CRYSTALS, 11(3), 1-19 [10.3390/cryst11030225].

Neutron and xrd single‐crystal diffraction study and vibrational properties of whitlockite, the natural counterpart of synthetic tricalcium phosphate

Radica F.;Della Ventura G.
2021-01-01

Abstract

A crystal chemical investigation of a natural specimen of whitlockite, ideally Ca9Mg(PO4)(6)[PO3(OH)], from Palermo Mine (USA), was achieved by means of a combination of electron microprobe analysis (EMPA) in WDS mode, single-crystal neutron diffraction probe (NDP) and single-crystal X-ray diffraction (XRD), and Fourier transform infrared (FTIR) spectroscopy. The crystal-chemical characterization resulted in the empirical formula (Ca8.682Na0.274Sr0.045)(sigma 9.000)(Ca-0.034(0.996))(sigma 1.000)(Mg0.533Fe0.3422+Mn0.0622+Al0.046)(sigma 0.983)(P1.006O4)(6)[PO3(OH0.968F0.032)(sigma 1.000)]. Crystal-structure refinement, in the space group R3c, converged to R1 = 7.12% using 3273 unique reflections from NDP data and to R1 = 2.43% using 2687 unique reflections from XRD data. Unit cell parameters from NDP are a = 10.357(3) angstrom, c = 37.095(15) angstrom and V = 3446(2) angstrom(3), and from XRD, the parameters are a = 10.3685(4) angstrom, c = 37.1444(13) angstrom and V = 3458.2(3) angstrom(3). NDP results allowed a deeper definition of the hydrogen-bond system and its relation with the structural unit [PO3(OH)]. The FTIR spectrum is very similar to that of synthetic tricalcium phosphate Ca-3(PO4)(2) and displays minor band shifts due to slightly different P-O bond lengths and to the presence of additional elements in the structure. A comparison between whitlockite, isotypic phases from the largest merrillite group, and its synthetic counterpart Ca-3(PO4)(2) is provided, based on the XRD/NDP and FTIR results.
Capitelli, F., Bosi, F., Capelli, S.C., Radica, F., Della Ventura, G. (2021). Neutron and xrd single‐crystal diffraction study and vibrational properties of whitlockite, the natural counterpart of synthetic tricalcium phosphate. CRYSTALS, 11(3), 1-19 [10.3390/cryst11030225].
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Utilizza questo identificativo per citare o creare un link a questo documento: https://hdl.handle.net/11590/424530
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