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NdB6O8(OH)5·H3BO3, triclinic, P 1‾ $\overline{1}$ (no. 2), a = 6.8304(7) Å, b = 7.2004(5) Å, c = 12.707(2) Å, α = 95.479(5)°, β = 98.652(6)°, γ = 101.758(5)°, V = 599.7(2) Å3, Z = 2, R gt(F) = 0.0378, wR ref(F 2) = 0.0826, T = 289(1) K.

Tb3B5O11(OH)2, orthorhombic, Pnna (no. 52), a = 4.4471(1) Å, b = 13.0934(4) Å, c = 13.9055(3) Å, V = 809.68(4) Å3, Z = 4, R gt(F) = 0.0260, wR ref(F 2) = 0.0556, T = 301(1) K.

NdB3.6O7, orthorhombic, Pmn21 (no. 31), a = 10.4169(4) Å, b = 4.4175(2) Å, c = 4.2566(2) Å, V = 195.88(2) Å3, Z = 2, R gt(F) = 0.0179, wR ref(F 2) = 0.0405, T = 153(1) K.

Tm3B12O19(OH)7, monoclinic, C2 (no. 5), a = 23.9849(5) Å, b = 4.4400(1) Å, c = 7.0771(1) Å, β = 94.698(1)°, V = 751.13(3) Å3, Z = 2, R gt(F) = 0.0106, wR ref(F 2) = 0.0247, T = 298(1) K.

A hitherto unknown modification of I2O5 was obtained from high‐pressure/high‐temperature syntheses in a Walker‐type multianvil device at 8 GPa and 250 °C. HP‐I2O5 crystallizes in the monoclinic crystal system with space group P21/c (no. 14) with the unit cell parameters a=12.0612(3) Å, b=4.8613(2) Å, c=6.9585(2) Å, β=100.10(1)° (at 173 K), and four formula units per cell. The single‐crystal structure data are accompanied by powder X‐ray diffraction data at ambient and elevated temperatures. Furthermore, DFT calculations were carried out to investigate the phase transition between the ambient‐pressure polymorph NP‐I2O5 to the newly synthesized high‐pressure phase. [ABSTRACT FROM AUTHOR]

The novel inoborate Ni[B2O2(OH)4] was synthesized under high‐pressure/high‐temperature conditions of 9 GPa and 800 °C. Its structure was determined via single‐crystal X‐ray diffraction analysis. The single‐grain IR‐spectrum of Ni[B2O2(OH)4] supports the existence of O−H bonds. The structural similarities and differences with the mineral vimsite, possessing the sum formula Ca[B2O2(OH)4], as well as with the phylloborate HP−Ni(B2O4) is discussed. The title compound can be described as the structural hydrolysis product of the latter. [ABSTRACT FROM AUTHOR]

The novel inoborate Ni[B2O2(OH)4] was synthesized under high‐pressure/high‐temperature conditions of 9 GPa and 800 °C. Its structure was determined via single‐crystal X‐ray diffraction analysis. The single‐grain IR‐spectrum of Ni[B2O2(OH)4] supports the existence of O−H bonds. The structural similarities and differences with the mineral vimsite, possessing the sum formula Ca[B2O2(OH)4], as well as with the phylloborate HP−Ni(B2O4) is discussed. The title compound can be described as the structural hydrolysis product of the latter. [ABSTRACT FROM AUTHOR]

Orthorhombic Al3BO6 was synthesized in a Walker-type multianvil apparatus under high-pressure/high-temperature conditions of 5 GPa and 1,200 °C, respectively. Its structure has been determined via single-crystal diffraction and is isotypic to M3BO6 (M = Cr, Fe) and homeotypic to the natural mineral norbergite (Mg3SiO4(OH)2). Thereby, we could complement the first report of Al3BO6 by Capponi et al. in 1972 (Capponi, J.-J.; Chenavas, J.; Joubert, J.-C. Eur. J. Mineral.1972, 95, 412–417.) by providing a precise structure description. Al3BO6 crystallizes in the space group Pnma (no. 62) with 4 formula units per unit cell and the lattice parameters a = 9.5060(5), b = 8.1058(4) and c = 4.2899(2) Å. Infrared spectroscopy (powder sample) and high-temperature X-ray powder diffraction further characterize the compound. [ABSTRACT FROM AUTHOR]

A mixed transition metal borate Co5–xVxCoy[B12O26–z(OH)z] was synthesized in a Walker-type module using the high-pressure/high-temperature approach at 12 GPa and 1,300 °C. The product crystallizes in the space group I41/acd. It is isotypic to other 3d metal cation borates of the M5[B12O25(OH)]–M5M[B12O22(OH)4] solid solution series. The title compound features three different metal cation positions; one octahedral site contains a mixture of V and Co, another octahedral site is fully occupied with Co, and a cuboctahedral position that is partially occupied with Co. It is the first compound within this structure type to contain Co, increasing the range of elements that can be incorporated and thus illustrating the adaptability and structural diversity of this anionic borate network. [ABSTRACT FROM AUTHOR]

Explorative high‐pressure/high‐temperature syntheses (7 GPa, 800 °C) starting from Er2O3, CdO, and H3BO3 yielded single‐crystals of the hitherto unknown compound ErCd2B7O13(BO(OH)3). This compound crystallizes trigonally in the non‐centrosymmetric space group R3c with the unit cell parameters a=8.8418(2) Å, c=22.4972(8) Å, and six formula units per cell. The crystal structure is composed of corner‐sharing trigonal planar [BO3] and tetrahedral [BO4] groups, forming a complex three‐dimensional framework. In this article, the structural data and characteristics of ErCd2B7O13(BO(OH)3) are presented in detail. Furthermore, the compound's infrared spectrum is discussed. [ABSTRACT FROM AUTHOR]

AlB4O6N, Al0.97Cr0.03B4O6N, and Al0.83Cr0.17B4O6N are the first representatives of the recently established structure‐family of oxonitridoborates containing Al3+. These compounds are isotypic to CrB4O6N and are synthesized in a multi‐anvil press under high‐pressure/high‐temperature conditions of 7.0 GPa/1350 °C. Structural refinement by single‐crystal X‐ray diffraction shows that they crystallize in the space group P63mc (no. 186) with two formula units per cell. Detailed characterization including high‐temperature X‐ray powder diffraction (HT‐XRD), electron probe microanalysis (EPMA), measurements of second harmonic generation (SHG), hardness, photoluminescence properties, vibrational spectroscopy, and band structure calculations reveal intriguing physicochemical properties that strongly resemble the famous material ruby. [ABSTRACT FROM AUTHOR]

Orthorhombic crystals of the compounds γ-Eu(BO2)3 and γ-Gd(BO2)3 were obtained by high-pressure/high-temperature syntheses at 10.5 GPa and 1100 and 900 °C, respectively. The structures were solved by single-crystal X-ray diffraction methods. The two compounds crystallize with four formula units per cell in the space group Pca21 (no. 29) with the unit cell parameters a = 18.2729(7), b = 4.4076(2), c = 4.2505(1) Å (Ln = Eu), and a = 18.2591(6), b = 4.4055(1), c = 4.2477(1) Å (Ln = Gd). Their infrared spectra and the luminescence spectrum of γ-Eu(BO2)3 are discussed. [ABSTRACT FROM AUTHOR]

This report presents work on the orthorhombic phases Ln2CdB5O11(OH) (Ln = Tm, Lu). The title compounds were synthesized in a Walker-type multianvil device at 7 GPa and 650 °C, and the resulting samples were thoroughly investigated through single-crystal and powder X-ray diffraction methods. Lu2CdB5O11(OH) crystallizes in the space group Pmna (no. 53) with the unit cell parameters a = 12.772(2), b = 4.6017(7), and c = 12.481(2) Å. Similar unit cell parameters are observed for the isotypic Tm analogue compound. The crystals have a layered crystal structure built up by four-, five-, and eight-membered rings of corner-sharing [BO4] tetrahedra. The structural data are accompanied by attenuated total reflection (ATR) infrared spectra and energy-dispersive X-ray spectroscopy (EDX). [ABSTRACT FROM AUTHOR]

Oxyfluorides come in many different structures and are highly adaptable in composition, not least because of their mixed-anionic nature. Slight changes, unless specifically looked for, can easily go unnoticed. In this paper, we present two oxyfluorides, K3Mo2O5.6F3.4 and K3V2O3.3F5.7, synthesized under high-pressure/high-temperature conditions, and demonstrate the importance of careful analysis of composition, oxidation state and O/F anion distribution for an accurate description of oxyfluorides. Their crystal structures were determined by single-crystal X-ray diffraction and the transition metal cation valences analyzed by X-ray photoelectron spectroscopy (XPS). The O/F anion ratio was calculated using the principle of charge neutrality and the local distribution within the crystallographic framework was studied using bond valence (BV) and charge distribution (CHARDI) calculations. Madelung Part of Lattice Energy (MAPLE) calculations and magnetic measurements provide insight into phase stability and corroborate the mixed-valent nature of the compounds. [ABSTRACT FROM AUTHOR]

We report on the synthesis, structure determination, and characterization of a new series of compounds LnCdB6O10(OH)3 (Ln = Sm–Er). Syntheses were carried out in a Walker-type multianvil device at 7 GPa and 650 °C. Structure determinations revealed the coexistence of an orthorhombic and a monoclinic polymorph, depending on the ionic radius of the lanthanoid cation. The orthorhombic structural variants crystallize non-centrosymmetrically in the space group Pna21 (no. 33), while the monoclinic modifications crystallize in space group P21/c (no. 14). Both modifications display a layered crystal structure built up by a repeating [B6O13]8− building block as their main structural feature. [ABSTRACT FROM AUTHOR]

NdB6O8(OH)5·H3BO3, triclinic, P 1 ‾ (no. 2), a = 6.8304(7) Å, b = 7.2004(5) Å, c = 12.707(2) Å, α = 95.479(5)°, β = 98.652(6)°, γ = 101.758(5)°, V = 599.7(2) Å3, Z = 2, Rgt(F) = 0.0378, wRref(F2) = 0.0826, T = 289(1) K. [ABSTRACT FROM AUTHOR]