Hydro­flux synthesis and crystal structure of Tl3IO

Ralf Albrecht; Heinrich Menning; Thomas Doert; Michael Ruck

doi:10.1107/S2056989020012359

. 2020 Sep 11;76(Pt 10):1638–1640. doi: 10.1107/S2056989020012359

Hydroflux synthesis and crystal structure of Tl₃IO

Ralf Albrecht ^a, Heinrich Menning ^a, Thomas Doert ^a, Michael Ruck ^a,^b,^*

PMCID: PMC7534229 PMID: 33117579

Single-crystals of thallium(I) iodide oxide Tl₃IO were obtained as by-product in a hydroflux synthesis at 473 K for 10 h. The oxygen atoms center thallium octahedra. The [OTl₆] octahedra share trans faces, forming a linear chain along [001]. Twelve thallium atoms surround each iodine atom in an [ITl₁₂] anti-cuboctahedron. Thallium and iodine atoms together form a hexagonal close-sphere packing, in which every fourth octahedral void is occupied by oxygen.

Keywords: crystal structure, hydroflux synthesis, thallium, oxide iodide, single-crystal XRD

Abstract

Single-crystals of thallium(I) iodide oxide Tl₃IO were obtained as by-product in a hydroflux synthesis at 473 K for 10 h. A potassium hydroxide hydroflux with a water-base molar ratio of 1.6 and the starting materials TlNO₃, RhI₃ and Ba(NO₃)₂ was used, resulting in a few black needle-shaped crystals. X-ray diffraction on a single-crystal revealed the hexagonal space group P6₃/mmc (No. 194) with lattice parameters a = 7.1512 (3) Å and c = 6.3639 (3) Å. Tl₃IO crystallizes as hexagonal anti-perovskite (anti-BaNiO₃ type) and is thus structurally related to the alkali-metal halide/auride oxides M ₃ XO (M = K, Rb, Cs; X = Cl, Br, I, Au). The oxygen atoms center thallium octahedra. The [OTl₆] octahedra share trans faces, forming a linear chain along [001]. Twelve thallium atoms surround each iodine atom in an [ITl₁₂] anti-cuboctahedron. Thallium and iodine atoms together form a hexagonal close-sphere packing, in which every fourth octahedral void is occupied by oxygen.

Chemical context

The class of alkali-metal halide/auride oxides comprises several compounds with the general formula M ₃ XO (M = K, Rb, Cs; X = Cl, Br, I, Au) (Sitta et al., 1991a ▸,b ▸; Feldmann & Jansen, 1995a ▸,b ▸,c ▸; Sabrowsky et al., 1996 ▸), Li₃BrO (Wortmann et al., 1989 ▸), Na₃ X′O (X′ = Cl, Br) (Sabrowsky et al., 1988 ▸; Hippler et al., 1990 ▸). These ternary oxides crystallize typically as anti-perovskites, i.e. in the cubic anti-CaTiO₃ type. The cesium derivatives Cs₃BrO, Cs₃IO and Cs₃AuO adopt hexagonal anti-perovskite structures (anti-BaNiO₃ type), whereas the Cs₃ClO crystallizes as anti-NH₄CdCl₃ type and thus does not form a perovskite structure. The crystal structure of Rb₃IO has both face and corner-sharing [ORb₆] octahedra (anti-BaFeO_3–x type). The adopted structure type depends on the size of the alkali-metal and halide/auride ions and their ratio. The stability range of the different perovskite phases can be estimated by using Goldschmidt’s tolerance factor, where larger M and X ions tend to destabilize the cubic anti-perovskite structure resulting in the hexagonal polymorph (Babel, 1969 ▸; Feldmann & Jansen, 1995b ▸).

For the synthesis of the title compound, the hydroflux method was used, which can be classified as intermediate between hydrothermal and flux synthesis (Chance et al., 2013 ▸). An approximately equimolar mixture of alkali-metal hydroxide (typically NaOH or KOH) and water is used as reaction medium (Albrecht et al., 2020a ▸). Good solubility of oxides and hydroxides, highly crystalline reaction products suitable for single-crystal X-ray diffraction analysis, comparably low reaction temperatures and a pressureless setup are essential advantages of the hydroflux method. In this communication, we report on the synthesis and crystal structure analysis of the thallium(I) iodide oxide Tl₃IO.

Structural commentary

Single-crystal X-ray diffraction on a black needle revealed the composition Tl₃IO and a hexagonal structure in the space group P6₃/mmc (no. 194) with lattice parameters a = 7.1512 (3) Å and c = 6.3639 (3) Å at 100 (1) K. Tl₃IO crystallizes as hexagonal anti-perovskite (anti-BaNiO₃ type; Fig. 1 ▸, Tables 1 ▸ and 2 ▸). The asymmetric unit consists of three atoms, thallium (site symmetry mm2, Wyckoff position 6h), iodine ( Inline graphic m2, 2d) and oxygen ( m., 2a). The oxygen atoms center thallium octahedra. The [OTl₆] octahedra share trans faces, forming a linear chain along [001]. Twelve thallium atoms surround each iodine atom in a [ITl₁₂] anti-cuboctahedron (triangular orthobicupola). Thallium and iodine atoms together form a hexagonal close-sphere packing, in which every fourth octahedral void is occupied by oxygen. Thus, also the thallium atom centers an anti-cuboctahedron, which has the composition [Tl(I₄Tl₈)].

Crystal structure of Tl₃IO in P6₃/*mmc*, highlighting the one-dimensional chains consisting of [OTl₆] octahedra. Ellipsoids enclose 99% of the probability density of the atoms.

Table 1. Atomic coordinates and equivalent isotropic displacement parameters (in 10 ⁴ Å²) in Tl₃IO at 100 (1) K.

Atom	Wyckoff symbol	x	y	z	U _iso/U _eq
Tl	6h	0.1608 (1)	0.3216 (1)	1/4	47 (1)
I	2d	2/3	1/3	1/4	53 (1)
O	2a	0	0	0	68 (7)

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Table 2. Anisotropic displacement parameters (in 10 ⁴ Å²) in Tl₃IO at 100 (1) K.

Atom	U ₁₁	U ₂₂	U ₃₃	U ₁₃
Tl	38 (1)	24 (1)	73 (1)	12 (1)
I	42 (1)	42 (1)	77 (2)	21 (1)
O	68 (10)	68 (10)	68 (19)	34 (5)

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The [OTl₆] octahedron is slightly elongated along the chain direction. The O—Tl bond length of 2.549 (1) Å is about 1% longer than in Tl₂O, at 2.517 (1) Å (Sabrowsky, 1971 ▸). The Tl—O—Tl angles along the chain parallel to c are 94.8 (1)°. The shortest Tl⋯Tl distances in Tl₃IO are with 3.449 (1) Å, very similar to those in thallium metal, which has Tl⋯Tl distances of 3.405 (1) and 3.455 (1) Å in its hexagonal sphere packing (Barrett, 1958 ▸). Accordingly, the [ITl₁₂] anticuboctahedra are also stretched along [001], with Tl—I distances of 3.576 (1) Å and 3.833 (1) Å. Although thallium(I) has a larger ionic radius (1.70 Å for c.n. = 12; Shannon, 1976 ▸) than potassium (1.64 Å for c.n. = 12), the M—O, M⋯M and the average M—I distances in Tl₃IO are smaller than in K₃IO by 3.5%, 7.5% and 1%, respectively (Feldmann & Jansen, 1995b ▸).

Synthesis and crystallization

Thallium(I) iodide oxide, Tl₃IO, was synthesized in a potassium hydroxide hydroflux. The reaction was carried out in a PTFE-lined 50 mL Berghof type DAB-2 stainless steel autoclave starting from TlNO₃ (0.38 mmol; abcr, 99.5%), RhI₃ (0.06 mmol; abcr, 99%), and Ba(NO₃)₂ (0.19 mmol; VEB Laborchemie Apolda, 99%). Water and potassium hydroxide (86%, Fisher Scientific) in the molar ratio of 1.6:1.0 were added to these compounds. The sealed autoclave was heated at a heating rate of 2 K min⁻¹ to 473 K and after 10 h cooled to room temperature at a rate of 0.1 K min⁻¹. The reaction product after washing with water mainly consisted of thallium(I) iodide, thallium(III) oxide, barium carbonate and a brown powder of an unidentified rhodium-containing compound. A few black single crystals of Tl₃IO with a needle-like morphology were found, which are sensitive to water and other protic solvents. In contact with water, the Tl₃IO crystals immediately turn yellow, probably due to the formation of thallium(I) hydroxide and thallium(I) iodide, which are both yellow. Energy-dispersive X-ray spectroscopy on Tl₃IO single-crystals revealed a disproportionately high oxygen content, indicating surface decomposition.

Several experiments failed to exchange rhodium(III) iodide with other iodine sources like potassium iodide, copper(I) iodide or silver(I) iodide. Likewise, experiments without barium nitrate were not successful. However, when both starting materials were used, Tl₃IO was obtained reproducibly, also at reaction temperatures of 423 K or 523 K. Similarly, the hydrothermal synthesis of Na₃[Tl(OH)₆] starting from thallium(I) sulfate required heavy metal salts like bismuth nitrate (Giesselbach, 2002 ▸). The oxidation of thallium(I) to thallium(III) in this reaction was achieved by oxygen in alkaline solutions (Rich, 2007 ▸).

The alkali-metal oxide halides M ₃ XO are reported to be very sensitive to traces of moisture or carbon dioxide due to their highly basic nature (Feldmann & Jansen, 1995b ▸). Remarkably, Tl₃IO crystallizes in the presence of water from the hydroflux. In other experiments, we synthesized a water sensitive oxohydroxoferrate (Albrecht et al., 2019 ▸) or an oxidation sensitive manganate(V) from hydroflux (Albrecht et al., 2020b ▸). Obviously, the activity of water is dramatically reduced in these aqueous salt melts.

Refinement

Crystal data, data collection and structure refinement details are summarized in Table 3 ▸.

Table 3. Experimental details.

Crystal data
Chemical formula	Tl₃IO
M _r	756.01
Crystal system, space group	Hexagonal, P6₃/m m c
Temperature (K)	100
a, c (Å)	7.1512 (3), 6.3639 (3)
V (Å³)	281.85 (3)
Z	2
Radiation type	Mo Kα
μ (mm⁻¹)	90.87
Crystal size (mm)	0.09 × 0.05 × 0.03

Data collection
Diffractometer	Bruker APEXII CCD
Absorption correction	Multi-scan (SADABS; Bruker, 2016 ▸)
T _min, T _max	0.113, 0.749
No. of measured, independent and observed [I > 2σ(I)] reflections	15853, 480, 442
R _int	0.049
(sin θ/λ)_max (Å⁻¹)	0.995

Refinement
R[F ² > 2σ(F ²)], wR(F ²), S	0.018, 0.041, 1.29
No. of reflections	480
No. of parameters	10
Δρ_max, Δρ_min (e Å⁻³)	2.80, −2.01

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Computer programs: APEX3 and SAINT (Bruker, 2016 ▸), SHELXT (Sheldrick, 2015a ▸), SHELXL (Sheldrick, 2015b ▸) and OLEX2 (Dolomanov et al., 2009 ▸).

Supplementary Material

Crystal structure: contains datablock(s) I. DOI: 10.1107/S2056989020012359/pk2648sup1.cif

e-76-01638-sup1.cif^{(498.8KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S2056989020012359/pk2648Isup2.hkl

e-76-01638-Isup2.hkl^{(42.1KB, hkl)}

CCDC reference: 2030857

Additional supporting information: crystallographic information; 3D view; checkCIF report

supplementary crystallographic information

Crystal data

Tl₃IO	D_x = 8.908 Mg m⁻³
M_r = 756.01	Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P6₃/mmc	Cell parameters from 8223 reflections
a = 7.1512 (3) Å	θ = 3.2–46.5°
c = 6.3639 (3) Å	µ = 90.87 mm⁻¹
V = 281.85 (3) Å³	T = 100 K
Z = 2	Needle, black
F(000) = 608	0.09 × 0.05 × 0.03 mm

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Data collection

Bruker APEXII CCD diffractometer	442 reflections with I > 2σ(I)
φ and ω scans	R_int = 0.049
Absorption correction: multi-scan (SADABS; Bruker, 2016)	θ_max = 45.0°, θ_min = 3.3°
T_min = 0.113, T_max = 0.749	h = −14→14
15853 measured reflections	k = −11→14
480 independent reflections	l = −11→12

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Refinement

Refinement on F²	0 restraints
Least-squares matrix: full	w = 1/[σ²(F_o²) + (0.0193P)²] where P = (F_o² + 2F_c²)/3
R[F² > 2σ(F²)] = 0.018	(Δ/σ)_max < 0.001
wR(F²) = 0.041	Δρ_max = 2.80 e Å⁻³
S = 1.29	Δρ_min = −2.01 e Å⁻³
480 reflections	Extinction correction: SHELXL-2016/6 (Sheldrick 2015b), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
10 parameters	Extinction coefficient: 0.0035 (2)

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Special details

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

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Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²)

	x	y	z	U_iso*/U_eq
Tl	0.16078 (2)	0.32156 (2)	0.250000	0.00465 (5)
I	0.666667	0.333333	0.250000	0.00534 (7)
O	0.000000	0.000000	0.000000	0.0068 (7)

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Atomic displacement parameters (Å²)

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Tl	0.00378 (6)	0.00238 (6)	0.00733 (9)	0.00119 (3)	0.000	0.000
I	0.00418 (9)	0.00418 (9)	0.00765 (18)	0.00209 (5)	0.000	0.000
O	0.0068 (10)	0.0068 (10)	0.0068 (19)	0.0034 (5)	0.000	0.000

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Geometric parameters (Å, º)

Tl—Tlⁱ	3.4494 (3)	Tl—Tl^vi	3.7538 (1)
Tl—Tlⁱⁱ	3.7538 (1)	Tl—Tl^vii	3.7018 (3)
Tl—Tlⁱⁱⁱ	3.7538 (1)	Tl—Tl^viii	3.7018 (3)
Tl—Tl^iv	3.4494 (3)	Tl—O	2.5490 (1)
Tl—Tl^v	3.7538 (1)	Tl—O^ix	2.5490 (1)

Tlⁱ—Tl—Tl^iv	60.0	O—Tl—Tl^viii	132.580 (2)
Tl^iv—Tl—Tlⁱⁱⁱ	62.648 (2)	O^ix—Tl—Tl^viii	132.580 (2)
Tl^vii—Tl—Tl^vi	90.0	O^ix—Tl—Tl^iv	47.420 (2)
Tlⁱ—Tl—Tl^viii	180.0	O^ix—Tl—Tlⁱ	47.420 (2)
Tl^v—Tl—Tlⁱⁱⁱ	115.917 (5)	O—Tl—Tlⁱⁱⁱ	42.580 (2)
Tl^iv—Tl—Tl^viii	120.0	O—Tl—Tl^iv	47.420 (2)
Tlⁱⁱ—Tl—Tl^v	149.235 (3)	O^ix—Tl—Tl^vii	132.580 (2)
Tlⁱ—Tl—Tl^vii	120.0	O—Tl—Tl^vii	132.580 (2)
Tlⁱⁱⁱ—Tl—Tl^vi	149.235 (3)	O—Tl—Tlⁱ	47.420 (2)
Tl^iv—Tl—Tl^vii	180.0	O—Tl—Tl^v	108.774 (4)
Tl^iv—Tl—Tl^vi	90.0	O—Tl—Tlⁱⁱ	42.580 (2)
Tl^viii—Tl—Tl^vii	60.0	O—Tl—Tl^vi	108.774 (4)
Tl^v—Tl—Tl^vi	54.704 (4)	O^ix—Tl—Tl^vi	42.580 (2)
Tlⁱ—Tl—Tlⁱⁱ	62.648 (2)	O^ix—Tl—Tlⁱⁱⁱ	108.774 (4)
Tlⁱ—Tl—Tlⁱⁱⁱ	90.0	O—Tl—O^ix	77.242 (5)
Tl^iv—Tl—Tlⁱⁱ	90.0	Tl^x—O—Tlⁱ	94.839 (4)
Tl^viii—Tl—Tlⁱⁱⁱ	90.0	Tl^x—O—Tlⁱⁱⁱ	85.161 (4)
Tl^viii—Tl—Tlⁱⁱ	117.352 (2)	Tl—O—Tl^x	180.0
Tlⁱⁱ—Tl—Tlⁱⁱⁱ	54.704 (4)	Tl^iv—O—Tlⁱ	85.161 (4)
Tl^vii—Tl—Tlⁱⁱ	90.0	Tl—O—Tlⁱⁱ	94.840 (4)
Tlⁱ—Tl—Tl^vi	62.648 (2)	Tl^iv—O—Tlⁱⁱⁱ	94.839 (4)
Tlⁱ—Tl—Tl^v	90.0	Tl^x—O—Tlⁱⁱ	85.160 (4)
Tl^viii—Tl—Tl^vi	117.352 (2)	Tlⁱⁱ—O—Tlⁱ	94.839 (4)
Tl^iv—Tl—Tl^v	62.648 (2)	Tl—O—Tl^iv	85.160 (4)
Tlⁱⁱ—Tl—Tl^vi	115.917 (5)	Tl—O—Tlⁱⁱⁱ	94.840 (4)
Tl^viii—Tl—Tl^v	90.0	Tl^x—O—Tl^iv	94.840 (4)
Tl^vii—Tl—Tl^v	117.352 (2)	Tlⁱⁱ—O—Tlⁱⁱⁱ	85.161 (4)
Tl^vii—Tl—Tlⁱⁱⁱ	117.352 (2)	Tlⁱⁱ—O—Tl^iv	180.0
O^ix—Tl—Tlⁱⁱ	108.774 (4)	Tlⁱ—O—Tlⁱⁱⁱ	180.0
O^ix—Tl—Tl^v	42.580 (2)	Tl—O—Tlⁱ	85.160 (4)

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Symmetry codes: (i) −y, x−y, z; (ii) x−y, x, −z; (iii) y, −x+y, −z; (iv) −x+y, −x, z; (v) y, −x+y, −z+1; (vi) x−y, x, −z+1; (vii) −x+y, −x+1, z; (viii) −y+1, x−y+1, z; (ix) −x, −y, z+1/2; (x) −x, −y, −z.

Funding Statement

This work was funded by Deutsche Forschungsgemeinschaft grant 438795198 to Michael Ruck.

References

Albrecht, R., Doert, T. & Ruck, M. (2019). ChemistryOpen 8, 1399–1406. [DOI] [PMC free article] [PubMed]
Albrecht, R., Doert, T. & Ruck, M. (2020a). Z. Anorg. Allg. Chem. In the press. https://doi.org/10.1002/zaac.202000031
Albrecht, R., Doert, T. & Ruck, M. (2020b). Z. Anorg. Allg. Chem. In the press. https://doi.org/10.1002/zaac.202000065.
Babel, D. (1969). Z. Anorg. Allg. Chem. 369, 117–130.
Barrett, C. S. (1958). Phys. Rev. 110, 1071–1072.
Bruker (2016). APEX3 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.
Chance, W. M., Bugaris, D. E., Sefat, A. S. & zur Loye, H.-K. (2013). Inorg. Chem. 52, 11723–11733. [DOI] [PubMed]
Dolomanov, O. V., Bourhis, L. J., Gildea, R. J., Howard, J. A. K. & Puschmann, H. (2009). J. Appl. Cryst. 42, 339–341.
Feldmann, C. & Jansen, M. (1995a). Z. Anorg. Allg. Chem. 621, 201–206.
Feldmann, C. & Jansen, M. (1995b). Z. Anorg. Allg. Chem. 621, 1907–1912.
Feldmann, C. & Jansen, M. (1995c). Z. Naturforsch. Teil B, 50, 1415–1416.
Giesselbach, M. (2002). Neue komplexe Hydroxide, Oxidhydroxide und Oxide von schweren Hauptgruppenmetallen. PhD Thesis, Universität Köln, Germany.
Hippler, K., Sitta, S., Vogt, P. & Sabrowsky, H. (1990). Acta Cryst. C46, 736–738.
Rich, R. (2007). Inorganic Reactions in Water, p. 321. Berlin Heidelberg: Springer-Verlag.
Sabrowsky, H. (1971). Z. Anorg. Allg. Chem. 381, 266–279.
Sabrowsky, H., Feldbaum-Möller, E., Fischer, K., Sitta, S., Vogt, P. & Winter, V. (1996). Z. Anorg. Allg. Chem. 622, 153–156.
Sabrowsky, H., Paszkowski, K., Reddig, D. & Vogt, P. (1988). Z. Naturforsch. Teil B, 43, 238–239.
Shannon, R. D. (1976). Acta Cryst. A32, 751–767.
Sheldrick, G. M. (2015a). Acta Cryst. A71, 3–8.
Sheldrick, G. M. (2015b). Acta Cryst. C71, 3–8.
Sitta, S., Hippler, K., Vogt, P. & Sabrowsky, H. (1991a). Z. Anorg. Allg. Chem. 597, 197–200.
Sitta, S., Hippler, K., Vogt, P. & Sabrowsky, H. (1991b). Z. Kristallogr. 196, 193–196.
Wortmann, R., Sitta, S. & Sabrowsky, H. (1989). Z. Naturforsch. Teil B, 44, 1348–1350.

Associated Data

This section collects any data citations, data availability statements, or supplementary materials included in this article.

Supplementary Materials

Crystal structure: contains datablock(s) I. DOI: 10.1107/S2056989020012359/pk2648sup1.cif

e-76-01638-sup1.cif^{(498.8KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S2056989020012359/pk2648Isup2.hkl

e-76-01638-Isup2.hkl^{(42.1KB, hkl)}

CCDC reference: 2030857

Additional supporting information: crystallographic information; 3D view; checkCIF report

[bb1] Albrecht, R., Doert, T. & Ruck, M. (2019). ChemistryOpen 8, 1399–1406. [DOI] [PMC free article] [PubMed]

[bb2] Albrecht, R., Doert, T. & Ruck, M. (2020a). Z. Anorg. Allg. Chem. In the press. https://doi.org/10.1002/zaac.202000031

[bb3] Albrecht, R., Doert, T. & Ruck, M. (2020b). Z. Anorg. Allg. Chem. In the press. https://doi.org/10.1002/zaac.202000065.

[bb4] Babel, D. (1969). Z. Anorg. Allg. Chem. 369, 117–130.

[bb5] Barrett, C. S. (1958). Phys. Rev. 110, 1071–1072.

[bb6] Bruker (2016). APEX3 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.

[bb7] Chance, W. M., Bugaris, D. E., Sefat, A. S. & zur Loye, H.-K. (2013). Inorg. Chem. 52, 11723–11733. [DOI] [PubMed]

[bb8] Dolomanov, O. V., Bourhis, L. J., Gildea, R. J., Howard, J. A. K. & Puschmann, H. (2009). J. Appl. Cryst. 42, 339–341.

[bb9] Feldmann, C. & Jansen, M. (1995a). Z. Anorg. Allg. Chem. 621, 201–206.

[bb10] Feldmann, C. & Jansen, M. (1995b). Z. Anorg. Allg. Chem. 621, 1907–1912.

[bb11] Feldmann, C. & Jansen, M. (1995c). Z. Naturforsch. Teil B, 50, 1415–1416.

[bb12] Giesselbach, M. (2002). Neue komplexe Hydroxide, Oxidhydroxide und Oxide von schweren Hauptgruppenmetallen. PhD Thesis, Universität Köln, Germany.

[bb13] Hippler, K., Sitta, S., Vogt, P. & Sabrowsky, H. (1990). Acta Cryst. C46, 736–738.

[bb14] Rich, R. (2007). Inorganic Reactions in Water, p. 321. Berlin Heidelberg: Springer-Verlag.

[bb15] Sabrowsky, H. (1971). Z. Anorg. Allg. Chem. 381, 266–279.

[bb16] Sabrowsky, H., Feldbaum-Möller, E., Fischer, K., Sitta, S., Vogt, P. & Winter, V. (1996). Z. Anorg. Allg. Chem. 622, 153–156.

[bb17] Sabrowsky, H., Paszkowski, K., Reddig, D. & Vogt, P. (1988). Z. Naturforsch. Teil B, 43, 238–239.

[bb18] Shannon, R. D. (1976). Acta Cryst. A32, 751–767.

[bb19] Sheldrick, G. M. (2015a). Acta Cryst. A71, 3–8.

[bb20] Sheldrick, G. M. (2015b). Acta Cryst. C71, 3–8.

[bb21] Sitta, S., Hippler, K., Vogt, P. & Sabrowsky, H. (1991a). Z. Anorg. Allg. Chem. 597, 197–200.

[bb22] Sitta, S., Hippler, K., Vogt, P. & Sabrowsky, H. (1991b). Z. Kristallogr. 196, 193–196.

[bb23] Wortmann, R., Sitta, S. & Sabrowsky, H. (1989). Z. Naturforsch. Teil B, 44, 1348–1350.

PERMALINK

Hydroflux synthesis and crystal structure of Tl₃IO

Ralf Albrecht

Heinrich Menning

Thomas Doert

Michael Ruck

Abstract

Chemical context

Structural commentary

Figure 1.

Table 1. Atomic coordinates and equivalent isotropic displacement parameters (in 10 ⁴ Å²) in Tl₃IO at 100 (1) K.

Table 2. Anisotropic displacement parameters (in 10 ⁴ Å²) in Tl₃IO at 100 (1) K.

Synthesis and crystallization

Refinement

Table 3. Experimental details.

Supplementary Material

supplementary crystallographic information

Crystal data

Data collection

Refinement

Special details

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²)

Atomic displacement parameters (Å²)

Geometric parameters (Å, º)

Funding Statement

References

Associated Data

Supplementary Materials

ACTIONS

PERMALINK

RESOURCES

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PERMALINK

Hydro­flux synthesis and crystal structure of Tl3IO

Ralf Albrecht

Heinrich Menning

Thomas Doert

Michael Ruck

Abstract

Chemical context

Structural commentary

Figure 1.

Table 1. Atomic coordinates and equivalent isotropic displacement parameters (in 10 4 Å2) in Tl3IO at 100 (1) K.

Table 2. Anisotropic displacement parameters (in 10 4 Å2) in Tl3IO at 100 (1) K.

Synthesis and crystallization

Refinement

Table 3. Experimental details.

Supplementary Material

supplementary crystallographic information

Crystal data

Data collection

Refinement

Special details

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

Atomic displacement parameters (Å2)

Geometric parameters (Å, º)

Funding Statement

References

Associated Data

Supplementary Materials

ACTIONS

PERMALINK

RESOURCES

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Links to NCBI Databases

Hydroflux synthesis and crystal structure of Tl₃IO

Table 1. Atomic coordinates and equivalent isotropic displacement parameters (in 10 ⁴ Å²) in Tl₃IO at 100 (1) K.

Table 2. Anisotropic displacement parameters (in 10 ⁴ Å²) in Tl₃IO at 100 (1) K.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²)

Atomic displacement parameters (Å²)