Abstract:Indium arsenate(V) monohydrate, InAsO4.H2O, (I), crystallizes in the structure type of MnMoO4.H2O. The structure is built of In2O8(H2O)2 dimers (mean In-O=2.150 A) corner-linked to slightly distorted AsO4 tetrahedra (mean As-O=1.686 A). The linkage results in a three-dimensional framework, with small voids into which the apical water ligand of the InO5(H2O) octahedron points. The hydrogen bonds in (I) are of medium strength. Lead(II) indium arsenate(V) hydrogen arsenate(V), PbIn(AsO4)(AsO3OH), (II), represents… Show more
“…Octahedral-tetrahedral framework structures in which all linkages are via octahedral-tetrahedral corner-sharing appear to be quite rare. Besides Pb 3 Fe 2 (PO 4 ) 4 (H 2 O) [and Pb 3 Cr 2 (PO 4 ) 4 ], the only example that we are aware of is that of PbIn(AsO 4 )(AsO 3 OH) (Kolitsch & Schwendtner, 2005). The octahedra in both structure types share each of their six vertices with tetrahedra and the tetrahedra share three of their four vertices with octahedra.…”
A new lead iron(III) hydrated phosphate, Pb 3 Fe 2 (PO 4 ) 4 (H 2 O), has been synthesised hydrothermally in Teflon-lined stainless steel autoclaves at 220 C for 7 days, with an initial pH of 1.5. It is the first example of a synthetic hydrous Pb-Fe 3þ phosphate. Crystals are small, colourless to white prisms, uniaxial (þ) and non-pleochroic. The calculated refractive index for white light is n ¼ 1.95. Single-crystal structure determination (R(F) ¼ 0.0457) shows Pb 3 Fe 2 (PO 4 ) 4 (H 2 O) to be tetragonal, space group P4 1 2 1 2 (no. 92), with a ¼ 9.0440(10), c ¼ 16.766(3) A ˚, V ¼ 1371.4(3) A ˚3 and Z ¼ 4. Pb 3 Fe 2 (PO 4 ) 4 (H 2 O) has a structure type which is based on a tetrahedral-octahedral framework of FeO 6 octahedra sharing corners with PO 4 tetrahedra, with Pb atoms and H 2 O molecules occupying voids in the framework. Pb 3 Fe 2 (PO 4 ) 4 (H 2 O) is homeotypic with synthetic Pb 3 Cr 2 (PO 4 ) 4 ; both compounds share the same heteropolyhedral topology and the same space group, but only Pb 3 Fe 2 (PO 4 ) 4 (H 2 O) contains an additional position occupied by a water molecule. The octahedral-tetrahedral chain of Pb 3 Fe 2 (PO 4 ) 4 (H 2 O) is topologically similar to double-strand chains found in the structures of hannayite, galliskiite, kapundaite, PbIn(AsO 4 )(AsO 3 OH) and Na 2.88 Fe(PO 4 ) 2 . Infrared spectroscopy is used to describe the vibrational properties of Pb 3 Fe 2 (PO 4 ) 4 (H 2 O).
“…Octahedral-tetrahedral framework structures in which all linkages are via octahedral-tetrahedral corner-sharing appear to be quite rare. Besides Pb 3 Fe 2 (PO 4 ) 4 (H 2 O) [and Pb 3 Cr 2 (PO 4 ) 4 ], the only example that we are aware of is that of PbIn(AsO 4 )(AsO 3 OH) (Kolitsch & Schwendtner, 2005). The octahedra in both structure types share each of their six vertices with tetrahedra and the tetrahedra share three of their four vertices with octahedra.…”
A new lead iron(III) hydrated phosphate, Pb 3 Fe 2 (PO 4 ) 4 (H 2 O), has been synthesised hydrothermally in Teflon-lined stainless steel autoclaves at 220 C for 7 days, with an initial pH of 1.5. It is the first example of a synthetic hydrous Pb-Fe 3þ phosphate. Crystals are small, colourless to white prisms, uniaxial (þ) and non-pleochroic. The calculated refractive index for white light is n ¼ 1.95. Single-crystal structure determination (R(F) ¼ 0.0457) shows Pb 3 Fe 2 (PO 4 ) 4 (H 2 O) to be tetragonal, space group P4 1 2 1 2 (no. 92), with a ¼ 9.0440(10), c ¼ 16.766(3) A ˚, V ¼ 1371.4(3) A ˚3 and Z ¼ 4. Pb 3 Fe 2 (PO 4 ) 4 (H 2 O) has a structure type which is based on a tetrahedral-octahedral framework of FeO 6 octahedra sharing corners with PO 4 tetrahedra, with Pb atoms and H 2 O molecules occupying voids in the framework. Pb 3 Fe 2 (PO 4 ) 4 (H 2 O) is homeotypic with synthetic Pb 3 Cr 2 (PO 4 ) 4 ; both compounds share the same heteropolyhedral topology and the same space group, but only Pb 3 Fe 2 (PO 4 ) 4 (H 2 O) contains an additional position occupied by a water molecule. The octahedral-tetrahedral chain of Pb 3 Fe 2 (PO 4 ) 4 (H 2 O) is topologically similar to double-strand chains found in the structures of hannayite, galliskiite, kapundaite, PbIn(AsO 4 )(AsO 3 OH) and Na 2.88 Fe(PO 4 ) 2 . Infrared spectroscopy is used to describe the vibrational properties of Pb 3 Fe 2 (PO 4 ) 4 (H 2 O).
“…It is topologically identical to the chain in hannayite, Mg 3 (NH 4 ) 2 (PO 3 OH) 4 ⋅8H 2 O (Catti and Franchini-Angela, 1976), while the chains in galliskiite, Ca 4 Al 2 (PO 4 ) 2 F 8 ⋅5H 2 O (Kampf et al , 2010), kapundaite, (Na,Ca) 2 Fe 3+ 4 (PO 4 ) 4 (OH) 3 ⋅5H 2 O (Mills et al , 2010a) and synthetic Pb 3 Fe 2 (PO 4 ) 4 (H 2 O) (Mills et al , 2010b) are geometrical isomers. The octahedral–tetrahedral double-strand chains in synthetic PbIn(AsO 4 )(AsO 3 OH) (Kolitsch and Schwendtner, 2005) and synthetic Na 3 Fe(PO 4 ) 2 (Hatert, 2007) differ topologically from those in the aforementioned structures in that their octahedra share three corners of the same octahedral face with tetrahedra, while in all of the other chains, the octahedra share three equatorial corners with tetrahedra. Fig.…”
“…This contribution is part of a comprehensive study of the synthesis, crystallography, and properties of arsenate (V) compounds in the system M 1+ -M 3+ -As-O-H (M 1+ = Li, Na, K, Rb, Cs, Tl, Ag, NH 4 ; M 3+ = B, Al, Ga, In, Sc, Cr, Fe) [6,[13][14][15][16][17][18][19]. The present paper reports the hydrothermal synthesis and crystal structure determination of three new, isotypic In-diarsenates of monovalent cations, and demonstrates that more novel structure types are still being found among arsenates.…”
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