Ba(BO<sub>2</sub>OH) – A Monoprotonated Monoborate from Hydroflux Showing Intense Second Harmonic Generation

Li, Yuxi; Hegarty, Peter A.; Rüsing, Michael; Eng, Lukas M.; Ruck, Michael

doi:10.1002/zaac.202200193

Cited by 3 publications

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References 64 publications

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“…The work of zur Loye [15,16,[19][20][21][22][23][24][25][26][27][28] and the recent contributions by us [29][30][31][32][33][34][35][36][37][38][39][40][41][42][43][44][45][46][47] give an impression of the potential of the hydroflux method. In just a few years, almost 100 new compounds were found in already extensively explored systems.…”

Section: Introductionmentioning

confidence: 99%

“…[32] Although mainly oxides and hydroxides were targeted, the method is by no means limited to these compound classes. An outlook on the possible applications of the hydroflux is given by the successful syntheses of the optically active borate Ba(BO 2 OH), [47] the oxide iodide Tl 3 OI, [35] the periodato complex K 8 [Rh(IO 6 ) 2 ]OH • 3H 2 O, [42] the tetraselenodiarsenate(II) K 4 (As 2 Se 4 ) • 2H 2 O, [44] or trichalcogenides such as K 2 Te 3 . [41] Hydroflux has several remarkable properties that combine to make it a unique reaction medium.…”

Section: Introductionmentioning

confidence: 99%

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Oxohydroxo‐Tellurates(VI) K₂[TeO₂(OH)₄] and K₂[Fe₂TeO₆(OH)₂] ⋅ 2H₂O from Alkaline Hydroflux

He,

Li,

Albrecht

et al. 2023

Zeitschrift anorg allge chemie

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The ultra‐alkaline conditions of a hydroflux offer the possibility of redox chemistry far from the electrochemical standard potentials. We explored the possibilities of synthesizing tellurium(VI) compounds, using both tellurium(VI) and tellurium(IV) as starting materials. Colorless, block‐shaped crystals of the oxohydroxotellurate(VI) K2[TeO2(OH)4] were synthesized from (NH4)2TeO4 in a KOH hydroflux at 200 °C. In the triclinic crystal structure, [TeO2(OH)4]2− octahedra are connected via hydrogen bonds to form layers, which are separated from each other by potassium cations. Yellow‐colored platelets of the ferrate(III) tellurate(VI) K2[Fe2TeO6(OH)2] ⋅ 2H2O were obtained by oxidation of TeO2 with H2O2 followed by reaction with Fe(NO3)3 ⋅ 9H2O in a KOH hydroflux. In the monoclinic crystal structure, strongly corrugated anionic layers Fe2TeO6(OH)2]2− are covered with water molecules and separated from each other by potassium cations. The octahedrally coordinated iron(III) atoms form a distorted honeycomb network, in which they are antiferromagnetically coupled at room temperature and in external fields up to at least 7 T.

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Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Oxohydroxo‐Tellurates(VI) K₂[TeO₂(OH)₄] and K₂[Fe₂TeO₆(OH)₂] ⋅ 2H₂O from Alkaline Hydroflux

He,

Li,

Albrecht

et al. 2023

Zeitschrift anorg allge chemie

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Hydroflux Synthesis and Structural Phase Transition of Rare‐Earth Borate Hydroxides Na₂[RE(BO₃)(OH)₂] (RE=Y, Gd−Er)

Li,

Carrillo‐Aravena,

et al. 2024

Chemistry A European J

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Reacting RE2O3 and H3BO3 in an ultra‐alkaline NaOH hydroflux at about 250 °C yielded pure, crystalline samples of Na2[RE(BO3)(OH)2] (RE = Y, Gd–Er). The compounds dehydrate to Na3RE(BO3)2 upon heating in air to about 500 °C. Na2[RE(BO3)(OH)2] (RE = Tb–Er) are photoluminescent under UV radiation. Their UV‐Vis spectra show the typical absorptions associated with 4f‐4f transitions and absorption edges in the UV (band gaps ≥ 5.7 eV). The RE3+ cation is coordinated by seven oxygen atoms, which define a distorted pentagonal bipyramid. The bipyramids share trans‐edges of their base forming infinite chains. Triangular (BO3)3– groups connect the chains into layers. The crystal structure of Na2[Ho(BO3)(OH)2] was investigated at various temperatures in the range 100 K ≤ T ≤ 320 K. Above 310(2) K, the compound crystallizes in the orthorhombic space group Cmcm (β‐phase), below, it undergoes a displacive phase transition of second order resulting in a monoclinic structure in space group C2/c (α‐phase). The critical exponents derived from different structural parameters indicate a cooperative distortion of the borate layers, but a rather uncorrelated adaptation of the sodium cations to their local environment. The other compounds of the series also adopt the structure of the α‐phase at 296 K.

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Rare‐Earth Hydroxometalates Ba[RE(OH)₅] with RE=Tb, Dy, Ho

Albrecht

Ruck

2022

Zeitschrift anorg allge chemie

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Dedicated to the late Professor Rudolf Hoppe on the occasion of his 100 th birthdayColorless crystals of the new hydroxometalates Ba[RE(OH) 5 ] with the rare-earth elements RE = Tb, Dy, Ho were synthesized under ultra-alkaline conditions in a KOH hydroflux at 200 °C. Singlecrystal X-ray diffraction revealed that the three compounds crystallize isostructural in the monoclinic space group P2 1 /n (no. 14). In the crystal structure, the rare-earth cations are coordinated by the oxygen atoms of seven hydroxide anions, which define a distorted pentagonal bipyramid. These polyhedra share edges of their basal ring forming infinite chains that run parallel to the [010] direction. Hydrogen bonds connect the chains into layers parallel to the (101) plane. The Ba 2 + cations are located between these layers and surrounded by nine oxygen atoms. Ba[Dy(OH) 5 ] is paramagnetic and shows no luminescence under UV light. When heated in synthetic air or argon, water is released in well-defined steps. Ba[Dy(OH) 5 ] decomposes via DyOOH to Dy 2 O 3 , which then reacts with the remaining Ba(OH) 2 to form BaDy 2 O 4 . Thus, the hydroxometalates can be used as carbon-free precursors for oxides.

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Ba(BO₂OH) – A Monoprotonated Monoborate from Hydroflux Showing Intense Second Harmonic Generation

Cited by 3 publications

References 64 publications

Oxohydroxo‐Tellurates(VI) K₂[TeO₂(OH)₄] and K₂[Fe₂TeO₆(OH)₂] ⋅ 2H₂O from Alkaline Hydroflux

Oxohydroxo‐Tellurates(VI) K₂[TeO₂(OH)₄] and K₂[Fe₂TeO₆(OH)₂] ⋅ 2H₂O from Alkaline Hydroflux

Hydroflux Synthesis and Structural Phase Transition of Rare‐Earth Borate Hydroxides Na₂[RE(BO₃)(OH)₂] (RE=Y, Gd−Er)

Rare‐Earth Hydroxometalates Ba[RE(OH)₅] with RE=Tb, Dy, Ho

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Ba(BO2OH) – A Monoprotonated Monoborate from Hydroflux Showing Intense Second Harmonic Generation

Cited by 3 publications

References 64 publications

Oxohydroxo‐Tellurates(VI) K2[TeO2(OH)4] and K2[Fe2TeO6(OH)2] ⋅ 2H2O from Alkaline Hydroflux

Oxohydroxo‐Tellurates(VI) K2[TeO2(OH)4] and K2[Fe2TeO6(OH)2] ⋅ 2H2O from Alkaline Hydroflux

Hydroflux Synthesis and Structural Phase Transition of Rare‐Earth Borate Hydroxides Na2[RE(BO3)(OH)2] (RE=Y, Gd−Er)

Rare‐Earth Hydroxometalates Ba[RE(OH)5] with RE=Tb, Dy, Ho

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Ba(BO₂OH) – A Monoprotonated Monoborate from Hydroflux Showing Intense Second Harmonic Generation

Oxohydroxo‐Tellurates(VI) K₂[TeO₂(OH)₄] and K₂[Fe₂TeO₆(OH)₂] ⋅ 2H₂O from Alkaline Hydroflux

Oxohydroxo‐Tellurates(VI) K₂[TeO₂(OH)₄] and K₂[Fe₂TeO₆(OH)₂] ⋅ 2H₂O from Alkaline Hydroflux

Hydroflux Synthesis and Structural Phase Transition of Rare‐Earth Borate Hydroxides Na₂[RE(BO₃)(OH)₂] (RE=Y, Gd−Er)

Rare‐Earth Hydroxometalates Ba[RE(OH)₅] with RE=Tb, Dy, Ho