The crystal structure of quaternary (Sn,Pb,Bi)Pt

Rössner, L.; Prots, Y.; Grin, Y.; Armbrüster, M.

doi:10.1107/S2056989023000956

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Volume 79| Part 3| March 2023| Pages 129-131

https://doi.org/10.1107/S2056989023000956

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The crystal structure of quaternary (Sn,Pb,Bi)Pt

Leonard Rössner,^a Yurii Prots,^b Yuri Grin ^b and Marc Armbrüster ^a ^*

^aFaculty of Natural Sciences, Institute of Chemistry, Materials for Innovative Energy Concepts, Chemnitz University of Technology, 09107 Chemnitz, Germany, and ^bMax-Planck-Institut für Chemische Physik fester Stoffe, Nöthnitzer Strasse 40, 01187 Dresden, Germany
^*Correspondence e-mail: marc.armbruester@chemie.tu-chemnitz.de

Edited by M. Weil, Vienna University of Technology, Austria (Received 2 November 2022; accepted 2 February 2023; online 7 February 2023)

Quaternary (Sn,Pb,Bi)Pt was synthesized by melting of the elements in an evacuated silica glass ampoule. The crystal structure was established by single-crystal X-ray diffraction and adopts an atomic arrangement of the NiAs type with additional occupation of the voids. Decisive for the refinement was the composition of the crystals as determined by energy dispersive X-ray spectroscopy (EDXS), resulting in a formula of (Sn_0.15Pb_0.54Bi_0.31)Pt.

Keywords: crystal structure; NiAs structure type; single-crystal X-ray diffraction; (Sn,Pb,Bi)Pt.

CCDC reference: 2239531

1. Chemical context

Platinum-based intermetallic compounds possess promising properties as electrocatalysts and provide necessary stability for the harsh application conditions in acidic electrolytes (Rössner & Armbrüster, 2019 ). SnPt, PbPt and BiPt are interesting electrocatalysts for the oxidation of small organic molecules and have the NiAs type of crystal structure (Oftedal, 1928 ; Nowotny et al., 1946 ; Zhuravlev et al., 1962 ). So far, the existence of a substitutional solid solution between PtPb and PtBi was confirmed by powder X-ray diffraction, with the site occupancy deduced from the nominal composition (Zhuravlev et al., 1962), which also holds for all three binary end members. To obtain material for electrocatalytic investigations, the synthesis of single-phase (Sn,Pb,Bi)Pt was attempted. Large hexagonal crystals were found on the top of an otherwise microgranular ingot. Preliminary EDXS analysis indicated the presence of all four elements in the crystal. Further structural investigations besides the original structure reports for PtSn (Harris et al., 1968 ; Shelton et al., 1981 ; Durussel et al., 1994 ), PtPb (Zhuravlev et al. 1962; Sidorov et al., 2021 ) and PtBi (Zhuravlev & Stepanova, 1962a ,b ) provide no full structural characterization by means of single-crystal X-ray diffraction. Thus, structural data for binary, ternary or quaternary samples in the (Sn,Pb,Bi)Pt system are incomplete. To provide such data, one of the obtained crystals was studied by means of single-crystal X-ray diffraction.

2. Structural commentary

As a result of the very similar scattering power of three of the four atoms (Bi, Pb and Pt), the direct assignment of the atomic positions to the respective elements was not possible. Atoms were distributed based on crystal-chemical considerations as well as by achieving an agreement between the refined composition and the result of the EDXS analysis (Fig. 1). The 2a site was assigned to Pt in agreement with structural studies of binary endmembers. A mixed occupancy of Sn, Pb and Bi was assumed for the 2c position. The statistical distribution of these elements at the same atomic site is based on the full miscibility of the elements in the molten state and on the missing site preference in the only known binary phase Pb_0.7Bi_0.3 (Mg type of crystal structure; Kurnakov & Ageeva, 1937 ). Additional electron density was detected on the 2c ( $[\overline{6}]$ m2) and 4f (3m.) sites, for which two possible scenarios can be considered. Either those positions are occupied by the smaller Sn atoms as a result of the enlarged unit-cell volume of 84.84 Å³, which is 7.2% higher compared to 79.14 Å³ for SnPt (Oftedal, 1928), or the presence of stacking faults. Neither can be proven here.

Figure 1
Representation of the unit cell of quaternary (Sn,Pb,Bi)Pt. Color code: Grey – Pt1; red – Sn1, Pb1, Bi1; blue – Sn2; green – Sn3. Displacement ellipsoids are drawn at the 95% probability level..

As a result of the potential partial occupation of 2c ( $[\overline{6}]$ m2) and 4f (3m.) in the hexagonal lattice of the quaternary sample, we assign the crystal structure to the NiAs type. The refined composition of 7.5%_at Sn, 27.0%_at Pb, 15.5%_at Bi and 50%_at Pt is in broad agreement with the results of EDXS measurements (12.35%_at Sn, 25.87%_at Pb, 9.49%_at Bi and 52.29%_at Pt) considering the error of this method, which to our experience is up to 5%_at for standardless quantifications of non-ideal samples, i.e. mirror-finished surfaces.

3. Synthesis and crystallization

Elements were weighed in an Ar-filled glove-box (O₂ and H₂O content < 0.1 ppm) according to the nominal composition of 20.83%_at Sn (99.999%, granules, ChemPUR), 20.83%_at Pb (99.999%, granules, AlutervFKI), 8.33%_at Bi (99.997%, granules, AlfaAesar) and 50.00%_at Pt (99.95%, foil, Goodfellow), then sealed in an evacuated silica glass ampoule. The ampoule was placed into a furnace at 1473 K for 24 h, then cooled down from 1473 K to 873 K at a rate of 0.2 K min⁻¹. The temperature of 873 K was held for seven days and subsequently the ampoule was quenched in cold water. Single crystals with a hexagonal shape were selected from the top of an otherwise microgranular sample, which was composed of phases with the Cu₃Au and NiAs type of crystal structure, based on powder X-ray diffraction data. As a result of the high X-ray absorption of the investigated material, hexagonal-shaped specimens were too large for single crystal X-ray data collection. For this experiment, a relatively small piece was mechanically separated from a hexagonally shaped block. The composition of the investigated single crystal was determined by EDXS (Quantax, Bruker).

4. Refinement

Crystallographic data, data collection and structure refinement details are summarized in Table 1.

Table 1
Experimental details

Crystal data
Chemical formula	(Sn·Pb·Bi)Pt
M_r	389.32
Crystal system, space group	Hexagonal, P6₃/mmc
Temperature (K)	293
a, c (Å)	4.228 (1), 5.481 (2)
V (Å³)	84.84 (5)
Z	2
Radiation type	Mo Kα
μ (mm⁻¹)	169.4
Crystal size (mm)	0.04 × 0.03 × 0.02

Data collection
Diffractometer	Rigaku AFC7 four-circle
Absorption correction	Multi-scan (Blessing, 1995 )
T_min, T_max	0.037, 0.081
No. of measured, independent and observed [I > 2σ(I)] reflections	1549, 123, 120
R_int	0.043
(sin θ/λ)_max (Å⁻¹)	0.900

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.025, 0.041, 1.51
No. of reflections	123
No. of parameters	13
No. of restraints	1
Δρ_max, Δρ_min (e Å⁻³)	2.08, −1.43
Computer programs: CrystalClear (Rigaku, 2008 ), SIR-2014 (Burla et al., 2015 ), SHELXL (Sheldrick, 2015 ) and DIAMOND (Brandenburg & Putz, 2018 ).

To decrease the number of parameters, the Pt site was constrained to full occupation at the 2a ( $[\overline{3}]$ m.) site. Even though the standardless quantification by means of EDXS data is 52.3%_at Pt, recent results of bulk samples from the quasi-ternary cut of the quaternary Sn–Pb–Bi–Pt system indicate a strict upper compositional limit of 50%_at Pt (Rössner et al., 2023 ). An initial refinement was done for Pb and Bi, using EDXS values as a starting point, then the additional electron density was considered by adding Sn. After multiple cycles, it was decided that a compromise had to be made between excellent refinement results and compositions close to the ones from EDXS results. The final model is presented here.

Furthermore, it has to be noted that Sn3 was refined with isotropic displacement parameters, as the minor site occupancy (2.7%), does not justify to add additional parameters to enable a refinement with anisotropic displacement parameters. It has to be stressed that the ratio of 13 parameters for 123 independent reflections is already at the recommended upper limit (ratio parameters:reflections < 1:10).

Supporting information

CCDC reference: 2239531

Crystal structure: contains datablocks I, quarternary. DOI: https://doi.org/10.1107/S2056989023000956/wm5665sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S2056989023000956/wm5665Isup2.hkl

checkCIF report

Computing details top

Data collection: CrystalClear (Rigaku, 2008); cell refinement: CrystalClear (Rigaku, 2008); data reduction: CrystalClear (Rigaku, 2008); program(s) used to solve structure: SIR-2014 (Burla et al., 2015); program(s) used to refine structure: SHELXL (Sheldrick, 2015); molecular graphics: DIAMOND (Brandenburg & Putz, 2018); software used to prepare material for publication: SHELXL (Sheldrick, 2015).

(Tin, lead, bismuth) platinum top

Crystal data top

(Sn·Pb·Bi)Pt	D_x = 15.23 Mg m⁻³
M_r = 389.32	Mo Kα radiation, λ = 0.710730 Å
Hexagonal, P6₃/mmc	Cell parameters from 924 reflections
a = 4.228 (1) Å	θ = 9.3–43.0°
c = 5.481 (2) Å	µ = 169.4 mm⁻¹
V = 84.84 (5) Å³	T = 293 K
Z = 2	Irregular shaped, grey
F(000) = 311	0.04 × 0.03 × 0.02 mm

Data collection top

Rigaku AFC7 four-circle diffractometer	123 independent reflections
Radiation source: Sealed Tube	120 reflections with I > 2σ(I)
Graphite Monochromator monochromator	R_int = 0.043
Detector resolution: 28.5714 pixels mm^-1	θ_max = 39.8°, θ_min = 5.6°
profile data from φ–scans	h = −7→5
Absorption correction: multi-scan (Blessing, 1995)	k = −6→7
T_min = 0.037, T_max = 0.081	l = −5→9
1549 measured reflections

Refinement top

Refinement on F²	13 parameters
Least-squares matrix: full	1 restraint
R[F² > 2σ(F²)] = 0.025	w = 1/[σ²(F_o²) + (0.012P)² + 0.2655P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.041	(Δ/σ)_max = 0.013
S = 1.51	Δρ_max = 2.08 e Å⁻³
123 reflections	Δρ_min = −1.43 e Å⁻³

Special details top

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.

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Pt1	0	0	0	0.0110 (2)
Bi1	0.3333	0.6667	0.2500	0.0077 (3)	0.31 (5)
Pb1	0.3333	0.6667	0.2500	0.0077	0.54 (5)
Sn1	0.3333	0.6667	0.2500	0.0077	0.03 (4)
Sn2	0.3333	0.6667	0.7500	0.0077	0.064 (6)
Sn3	0.3333	0.6667	0.501 (5)	0.012 (7)*	0.027 (4)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pt1	0.0133 (3)	0.0133	0.0063 (3)	0.00667 (13)	0	0
Bi1	0.0061 (3)	0.0061	0.0108 (4)	0.00307 (14)	0	0
Pb1	0.0061	0.0061	0.0108	0.00307	0	0
Sn1	0.0061	0.0061	0.0108	0.00307	0	0
Sn2	0.0061	0.0061	0.0108	0.00307	0	0

Geometric parameters (Å, º) top

Pt1—Sn3ⁱ	2.4410 (6)	Pb1—Sn3^x	2.797 (13)
Pt1—Sn3ⁱⁱ	2.4410 (6)	Pb1—Sn3^xiii	2.797 (13)
Pt1—Sn3ⁱⁱⁱ	2.4410 (6)	Sn1—Sn3	1.37 (3)
Pt1—Sn3^iv	2.4410 (6)	Sn1—Sn3ⁱ	1.37 (3)
Pt1—Sn3^v	2.4411 (6)	Sn1—Sn2^ix	2.4410 (6)
Pt1—Sn3^vi	2.4411 (6)	Sn1—Sn2^x	2.4410 (6)
Pt1—Pt1^vii	2.7402 (9)	Sn1—Sn2^xi	2.4410 (6)
Pt1—Pt1ⁱⁱ	2.7402 (9)	Sn1—Sn2	2.7403 (8)
Pt1—Bi1^viii	2.7993 (5)	Sn1—Sn2^xii	2.7402 (9)
Pt1—Sn1^viii	2.7993 (5)	Sn1—Sn3^iv	2.797 (13)
Pt1—Pb1^viii	2.7993 (5)	Sn1—Sn3^ix	2.797 (13)
Pt1—Sn2^ix	2.7993 (5)	Sn1—Sn3^vi	2.797 (13)
Bi1—Sn3	1.37 (3)	Sn1—Sn3^x	2.797 (13)
Bi1—Sn3ⁱ	1.37 (3)	Sn1—Sn3^xiii	2.797 (13)
Bi1—Sn2^ix	2.4410 (6)	Sn2—Sn3^xiv	1.37 (3)
Bi1—Sn2^x	2.4410 (6)	Sn2—Sn3	1.37 (3)
Bi1—Sn2^xi	2.4410 (6)	Sn2—Sn1^ix	2.4410 (6)
Bi1—Sn2	2.7403 (8)	Sn2—Pb1^ix	2.4410 (6)
Bi1—Sn2^xii	2.7402 (9)	Sn2—Bi1^ix	2.4410 (6)
Bi1—Sn3^iv	2.797 (13)	Sn2—Sn1^x	2.4410 (6)
Bi1—Sn3^ix	2.797 (13)	Sn2—Sn1^xi	2.4410 (6)
Bi1—Sn3^vi	2.797 (13)	Sn2—Pb1^x	2.4410 (6)
Bi1—Sn3^x	2.797 (13)	Sn2—Pb1^xi	2.4410 (6)
Bi1—Sn3^xiii	2.797 (13)	Sn2—Bi1^x	2.4410 (6)
Pb1—Sn3	1.37 (3)	Sn2—Bi1^xi	2.4410 (6)
Pb1—Sn3ⁱ	1.37 (3)	Sn3—Sn3^ix	2.4410 (6)
Pb1—Sn2^ix	2.4410 (6)	Sn3—Pt1^xv	2.4410 (6)
Pb1—Sn2^x	2.4410 (6)	Sn3—Pt1^xvi	2.4410 (6)
Pb1—Sn2^xi	2.4410 (6)	Sn3—Pt1^vii	2.4410 (6)
Pb1—Sn2	2.7403 (8)	Sn3—Sn3^x	2.4411 (6)
Pb1—Sn2^xii	2.7402 (9)	Sn3—Sn3^xi	2.4411 (7)
Pb1—Sn3^iv	2.797 (13)	Sn3—Sn3^xiv	2.73 (5)
Pb1—Sn3^ix	2.797 (13)	Sn3—Sn3ⁱ	2.75 (5)
Pb1—Sn3^vi	2.797 (13)

Sn3ⁱ—Pt1—Sn3ⁱⁱ	180.0	Sn3ⁱ—Sn1—Sn2^x	90.000 (4)
Sn3ⁱⁱⁱ—Pt1—Sn3^iv	180.0	Sn2^ix—Sn1—Sn2^x	120.0
Sn3ⁱ—Pt1—Sn3^v	119.999 (5)	Sn3—Sn1—Sn2^xi	90.000 (5)
Sn3ⁱⁱⁱ—Pt1—Sn3^v	119.999 (4)	Sn3ⁱ—Sn1—Sn2^xi	90.000 (4)
Sn3ⁱⁱ—Pt1—Sn3^vi	119.999 (5)	Sn2^ix—Sn1—Sn2^xi	120.0
Sn3^iv—Pt1—Sn3^vi	119.999 (4)	Sn2^x—Sn1—Sn2^xi	120.0
Sn3^v—Pt1—Sn3^vi	180.0	Sn3—Sn1—Sn2	0.000 (6)
Sn3ⁱ—Pt1—Pt1^vii	90.1 (6)	Sn3ⁱ—Sn1—Sn2	180.0
Sn3ⁱⁱ—Pt1—Pt1^vii	89.9 (6)	Sn2^ix—Sn1—Sn2	90.0
Sn3ⁱⁱⁱ—Pt1—Pt1^vii	90.1 (6)	Sn2^x—Sn1—Sn2	90.0
Sn3^iv—Pt1—Pt1^vii	89.9 (6)	Sn2^xi—Sn1—Sn2	90.0
Sn3^v—Pt1—Pt1^vii	90.1 (6)	Sn3—Sn1—Sn2^xii	180.0
Sn3^vi—Pt1—Pt1^vii	89.9 (6)	Sn3ⁱ—Sn1—Sn2^xii	0.000 (1)
Sn3ⁱ—Pt1—Pt1ⁱⁱ	89.9 (6)	Sn2^ix—Sn1—Sn2^xii	90.0
Sn3ⁱⁱ—Pt1—Pt1ⁱⁱ	90.1 (6)	Sn2^x—Sn1—Sn2^xii	90.0
Sn3ⁱⁱⁱ—Pt1—Pt1ⁱⁱ	89.9 (6)	Sn2^xi—Sn1—Sn2^xii	90.0
Sn3^iv—Pt1—Pt1ⁱⁱ	90.1 (6)	Sn2—Sn1—Sn2^xii	180.0
Sn3^v—Pt1—Pt1ⁱⁱ	89.9 (6)	Sn3—Sn1—Sn3^iv	119.2 (5)
Sn3^vi—Pt1—Pt1ⁱⁱ	90.1 (6)	Sn3ⁱ—Sn1—Sn3^iv	60.8 (5)
Pt1^vii—Pt1—Pt1ⁱⁱ	180.0	Sn2^ix—Sn1—Sn3^iv	29.2 (5)
Sn3ⁱ—Pt1—Bi1^viii	150.6 (6)	Sn2^x—Sn1—Sn3^iv	115.87 (13)
Sn3ⁱⁱ—Pt1—Bi1^viii	29.4 (6)	Sn2^xi—Sn1—Sn3^iv	115.87 (13)
Sn3ⁱⁱⁱ—Pt1—Bi1^viii	64.1 (3)	Sn2—Sn1—Sn3^iv	119.2 (5)
Sn3^iv—Pt1—Bi1^viii	115.9 (3)	Sn2^xii—Sn1—Sn3^iv	60.8 (5)
Sn3^v—Pt1—Bi1^viii	64.1 (3)	Sn3—Sn1—Sn3^ix	60.8 (5)
Sn3^vi—Pt1—Bi1^viii	115.9 (3)	Sn3ⁱ—Sn1—Sn3^ix	119.2 (5)
Pt1^vii—Pt1—Bi1^viii	119.305 (9)	Sn2^ix—Sn1—Sn3^ix	29.2 (5)
Pt1ⁱⁱ—Pt1—Bi1^viii	60.695 (9)	Sn2^x—Sn1—Sn3^ix	115.87 (13)
Sn3ⁱ—Pt1—Sn1^viii	150.6 (6)	Sn2^xi—Sn1—Sn3^ix	115.87 (13)
Sn3ⁱⁱ—Pt1—Sn1^viii	29.4 (6)	Sn2—Sn1—Sn3^ix	60.8 (5)
Sn3ⁱⁱⁱ—Pt1—Sn1^viii	64.1 (3)	Sn2^xii—Sn1—Sn3^ix	119.2 (5)
Sn3^iv—Pt1—Sn1^viii	115.9 (3)	Sn3^iv—Sn1—Sn3^ix	58.5 (10)
Sn3^v—Pt1—Sn1^viii	64.1 (3)	Sn3—Sn1—Sn3^vi	119.2 (5)
Sn3^vi—Pt1—Sn1^viii	115.9 (3)	Sn3ⁱ—Sn1—Sn3^vi	60.8 (5)
Pt1^vii—Pt1—Sn1^viii	119.305 (9)	Sn2^ix—Sn1—Sn3^vi	115.87 (13)
Pt1ⁱⁱ—Pt1—Sn1^viii	60.695 (9)	Sn2^x—Sn1—Sn3^vi	115.87 (13)
Bi1^viii—Pt1—Sn1^viii	0.0	Sn2^xi—Sn1—Sn3^vi	29.2 (5)
Sn3ⁱ—Pt1—Pb1^viii	150.6 (6)	Sn2—Sn1—Sn3^vi	119.2 (5)
Sn3ⁱⁱ—Pt1—Pb1^viii	29.4 (6)	Sn2^xii—Sn1—Sn3^vi	60.8 (5)
Sn3ⁱⁱⁱ—Pt1—Pb1^viii	64.1 (3)	Sn3^iv—Sn1—Sn3^vi	98.2 (6)
Sn3^iv—Pt1—Pb1^viii	115.9 (3)	Sn3^ix—Sn1—Sn3^vi	128.3 (3)
Sn3^v—Pt1—Pb1^viii	64.1 (3)	Sn3—Sn1—Sn3^x	60.8 (5)
Sn3^vi—Pt1—Pb1^viii	115.9 (3)	Sn3ⁱ—Sn1—Sn3^x	119.2 (5)
Pt1^vii—Pt1—Pb1^viii	119.305 (9)	Sn2^ix—Sn1—Sn3^x	115.87 (13)
Pt1ⁱⁱ—Pt1—Pb1^viii	60.695 (9)	Sn2^x—Sn1—Sn3^x	29.2 (5)
Bi1^viii—Pt1—Pb1^viii	0.0	Sn2^xi—Sn1—Sn3^x	115.87 (13)
Sn1^viii—Pt1—Pb1^viii	0.0	Sn2—Sn1—Sn3^x	60.8 (5)
Sn3ⁱ—Pt1—Sn2^ix	64.2 (3)	Sn2^xii—Sn1—Sn3^x	119.2 (5)
Sn3ⁱⁱ—Pt1—Sn2^ix	115.8 (3)	Sn3^iv—Sn1—Sn3^x	128.3 (3)
Sn3ⁱⁱⁱ—Pt1—Sn2^ix	150.8 (6)	Sn3^ix—Sn1—Sn3^x	98.2 (6)
Sn3^iv—Pt1—Sn2^ix	29.2 (6)	Sn3^vi—Sn1—Sn3^x	128.3 (3)
Sn3^v—Pt1—Sn2^ix	64.2 (3)	Sn3—Sn1—Sn3^xiii	119.2 (5)
Sn3^vi—Pt1—Sn2^ix	115.8 (3)	Sn3ⁱ—Sn1—Sn3^xiii	60.8 (5)
Pt1^vii—Pt1—Sn2^ix	60.695 (9)	Sn2^ix—Sn1—Sn3^xiii	115.87 (13)
Pt1ⁱⁱ—Pt1—Sn2^ix	119.305 (10)	Sn2^x—Sn1—Sn3^xiii	29.2 (5)
Sn3—Bi1—Sn3ⁱ	180.0	Sn2^xi—Sn1—Sn3^xiii	115.87 (13)
Sn3—Bi1—Sn2^ix	90.000 (1)	Sn2—Sn1—Sn3^xiii	119.2 (5)
Sn3ⁱ—Bi1—Sn2^ix	89.999 (1)	Sn2^xii—Sn1—Sn3^xiii	60.8 (5)
Sn3—Bi1—Sn2^x	90.000 (4)	Sn3^iv—Sn1—Sn3^xiii	98.2 (6)
Sn3ⁱ—Bi1—Sn2^x	90.000 (4)	Sn3^ix—Sn1—Sn3^xiii	128.3 (3)
Sn2^ix—Bi1—Sn2^x	120.0	Sn3^vi—Sn1—Sn3^xiii	98.2 (6)
Sn3—Bi1—Sn2^xi	90.000 (5)	Sn3^x—Sn1—Sn3^xiii	58.5 (10)
Sn3ⁱ—Bi1—Sn2^xi	90.000 (4)	Sn3^xiv—Sn2—Sn3	180.0
Sn2^ix—Bi1—Sn2^xi	120.0	Sn3^xiv—Sn2—Sn1^ix	89.999 (1)
Sn2^x—Bi1—Sn2^xi	120.0	Sn3—Sn2—Sn1^ix	90.000 (1)
Sn3—Bi1—Sn2	0.000 (6)	Sn3^xiv—Sn2—Pb1^ix	89.999 (1)
Sn3ⁱ—Bi1—Sn2	180.0	Sn3—Sn2—Pb1^ix	90.000 (1)
Sn2^ix—Bi1—Sn2	90.0	Sn1^ix—Sn2—Pb1^ix	0.0
Sn2^x—Bi1—Sn2	90.0	Sn3^xiv—Sn2—Bi1^ix	89.999 (1)
Sn2^xi—Bi1—Sn2	90.0	Sn3—Sn2—Bi1^ix	90.000 (1)
Sn3—Bi1—Sn2^xii	180.0	Sn1^ix—Sn2—Bi1^ix	0.0
Sn3ⁱ—Bi1—Sn2^xii	0.000 (1)	Pb1^ix—Sn2—Bi1^ix	0.0
Sn2^ix—Bi1—Sn2^xii	90.0	Sn3^xiv—Sn2—Sn1^x	90.000 (6)
Sn2^x—Bi1—Sn2^xii	90.0	Sn3—Sn2—Sn1^x	90.000 (6)
Sn2^xi—Bi1—Sn2^xii	90.0	Sn1^ix—Sn2—Sn1^x	120.0
Sn2—Bi1—Sn2^xii	180.0	Pb1^ix—Sn2—Sn1^x	120.0
Sn3—Bi1—Sn3^iv	119.2 (5)	Bi1^ix—Sn2—Sn1^x	120.0
Sn3ⁱ—Bi1—Sn3^iv	60.8 (5)	Sn3^xiv—Sn2—Sn1^xi	90.000 (7)
Sn2^ix—Bi1—Sn3^iv	29.2 (5)	Sn3—Sn2—Sn1^xi	90.000 (7)
Sn2^x—Bi1—Sn3^iv	115.87 (13)	Sn1^ix—Sn2—Sn1^xi	120.0
Sn2^xi—Bi1—Sn3^iv	115.87 (13)	Pb1^ix—Sn2—Sn1^xi	120.0
Sn2—Bi1—Sn3^iv	119.2 (5)	Bi1^ix—Sn2—Sn1^xi	120.0
Sn2^xii—Bi1—Sn3^iv	60.8 (5)	Sn1^x—Sn2—Sn1^xi	120.0
Sn3—Bi1—Sn3^ix	60.8 (5)	Sn3^xiv—Sn2—Pb1^x	90.000 (6)
Sn3ⁱ—Bi1—Sn3^ix	119.2 (5)	Sn3—Sn2—Pb1^x	90.000 (6)
Sn2^ix—Bi1—Sn3^ix	29.2 (5)	Sn1^ix—Sn2—Pb1^x	120.0
Sn2^x—Bi1—Sn3^ix	115.87 (13)	Pb1^ix—Sn2—Pb1^x	120.0
Sn2^xi—Bi1—Sn3^ix	115.87 (13)	Bi1^ix—Sn2—Pb1^x	120.0
Sn2—Bi1—Sn3^ix	60.8 (5)	Sn1^x—Sn2—Pb1^x	0.0
Sn2^xii—Bi1—Sn3^ix	119.2 (5)	Sn1^xi—Sn2—Pb1^x	120.0
Sn3^iv—Bi1—Sn3^ix	58.5 (10)	Sn3^xiv—Sn2—Pb1^xi	90.000 (7)
Sn3—Bi1—Sn3^vi	119.2 (5)	Sn3—Sn2—Pb1^xi	90.000 (7)
Sn3ⁱ—Bi1—Sn3^vi	60.8 (5)	Sn1^ix—Sn2—Pb1^xi	120.0
Sn2^ix—Bi1—Sn3^vi	115.87 (13)	Pb1^ix—Sn2—Pb1^xi	120.0
Sn2^x—Bi1—Sn3^vi	115.87 (13)	Bi1^ix—Sn2—Pb1^xi	120.0
Sn2^xi—Bi1—Sn3^vi	29.2 (5)	Sn1^x—Sn2—Pb1^xi	120.0
Sn2—Bi1—Sn3^vi	119.2 (5)	Sn1^xi—Sn2—Pb1^xi	0.0
Sn2^xii—Bi1—Sn3^vi	60.8 (5)	Pb1^x—Sn2—Pb1^xi	120.0
Sn3^iv—Bi1—Sn3^vi	98.2 (6)	Sn3^xiv—Sn2—Bi1^x	90.000 (6)
Sn3^ix—Bi1—Sn3^vi	128.3 (3)	Sn3—Sn2—Bi1^x	90.000 (6)
Sn3—Bi1—Sn3^x	60.8 (5)	Sn1^ix—Sn2—Bi1^x	120.0
Sn3ⁱ—Bi1—Sn3^x	119.2 (5)	Pb1^ix—Sn2—Bi1^x	120.0
Sn2^ix—Bi1—Sn3^x	115.87 (13)	Bi1^ix—Sn2—Bi1^x	120.0
Sn2^x—Bi1—Sn3^x	29.2 (5)	Sn1^x—Sn2—Bi1^x	0.0
Sn2^xi—Bi1—Sn3^x	115.87 (13)	Sn1^xi—Sn2—Bi1^x	120.0
Sn2—Bi1—Sn3^x	60.8 (5)	Pb1^x—Sn2—Bi1^x	0.0
Sn2^xii—Bi1—Sn3^x	119.2 (5)	Pb1^xi—Sn2—Bi1^x	120.0
Sn3^iv—Bi1—Sn3^x	128.3 (3)	Sn3^xiv—Sn2—Bi1^xi	90.000 (7)
Sn3^ix—Bi1—Sn3^x	98.2 (6)	Sn3—Sn2—Bi1^xi	90.000 (7)
Sn3^vi—Bi1—Sn3^x	128.3 (3)	Sn1^ix—Sn2—Bi1^xi	120.0
Sn3—Bi1—Sn3^xiii	119.2 (5)	Pb1^ix—Sn2—Bi1^xi	120.0
Sn3ⁱ—Bi1—Sn3^xiii	60.8 (5)	Bi1^ix—Sn2—Bi1^xi	120.0
Sn2^ix—Bi1—Sn3^xiii	115.87 (13)	Sn1^x—Sn2—Bi1^xi	120.0
Sn2^x—Bi1—Sn3^xiii	29.2 (5)	Sn1^xi—Sn2—Bi1^xi	0.0
Sn2^xi—Bi1—Sn3^xiii	115.87 (13)	Pb1^x—Sn2—Bi1^xi	120.0
Sn2—Bi1—Sn3^xiii	119.2 (5)	Pb1^xi—Sn2—Bi1^xi	0.0
Sn2^xii—Bi1—Sn3^xiii	60.8 (5)	Bi1^x—Sn2—Bi1^xi	120.0
Sn3^iv—Bi1—Sn3^xiii	98.2 (6)	Sn3^xiv—Sn2—Bi1	180.0
Sn3^ix—Bi1—Sn3^xiii	128.3 (3)	Sn3—Sn2—Bi1	0.000 (6)
Sn3^vi—Bi1—Sn3^xiii	98.2 (6)	Sn1^ix—Sn2—Bi1	90.0
Sn3^x—Bi1—Sn3^xiii	58.5 (10)	Pb1^ix—Sn2—Bi1	90.0
Sn3—Pb1—Sn3ⁱ	180.0	Bi1^ix—Sn2—Bi1	90.0
Sn3—Pb1—Sn2^ix	90.000 (1)	Sn1^x—Sn2—Bi1	90.0
Sn3ⁱ—Pb1—Sn2^ix	89.999 (1)	Sn1^xi—Sn2—Bi1	90.0
Sn3—Pb1—Sn2^x	90.000 (4)	Pb1^x—Sn2—Bi1	90.0
Sn3ⁱ—Pb1—Sn2^x	90.000 (4)	Pb1^xi—Sn2—Bi1	90.0
Sn2^ix—Pb1—Sn2^x	120.0	Bi1^x—Sn2—Bi1	90.0
Sn3—Pb1—Sn2^xi	90.000 (5)	Bi1^xi—Sn2—Bi1	90.0
Sn3ⁱ—Pb1—Sn2^xi	90.000 (4)	Sn2—Sn3—Bi1	180.0
Sn2^ix—Pb1—Sn2^xi	120.0	Sn2—Sn3—Pb1	180.0
Sn2^x—Pb1—Sn2^xi	120.0	Bi1—Sn3—Pb1	0.0
Sn3—Pb1—Sn2	0.000 (6)	Sn2—Sn3—Sn1	180.0
Sn3ⁱ—Pb1—Sn2	180.0	Bi1—Sn3—Sn1	0.0
Sn2^ix—Pb1—Sn2	90.0	Pb1—Sn3—Sn1	0.0
Sn2^x—Pb1—Sn2	90.0	Sn2—Sn3—Sn3^ix	90.2 (13)
Sn2^xi—Pb1—Sn2	90.0	Bi1—Sn3—Sn3^ix	89.8 (13)
Sn3—Pb1—Sn2^xii	180.0	Pb1—Sn3—Sn3^ix	89.8 (13)
Sn3ⁱ—Pb1—Sn2^xii	0.000 (1)	Sn1—Sn3—Sn3^ix	89.8 (13)
Sn2^ix—Pb1—Sn2^xii	90.0	Sn2—Sn3—Pt1^xv	90.1 (6)
Sn2^x—Pb1—Sn2^xii	90.0	Bi1—Sn3—Pt1^xv	89.9 (6)
Sn2^xi—Pb1—Sn2^xii	90.0	Pb1—Sn3—Pt1^xv	89.9 (6)
Sn2—Pb1—Sn2^xii	180.0	Sn1—Sn3—Pt1^xv	89.9 (6)
Sn3—Pb1—Sn3^iv	119.2 (5)	Sn3^ix—Sn3—Pt1^xv	179.7 (19)
Sn3ⁱ—Pb1—Sn3^iv	60.8 (5)	Sn2—Sn3—Pt1^xvi	90.1 (6)
Sn2^ix—Pb1—Sn3^iv	29.2 (5)	Bi1—Sn3—Pt1^xvi	89.9 (6)
Sn2^x—Pb1—Sn3^iv	115.87 (13)	Pb1—Sn3—Pt1^xvi	89.9 (6)
Sn2^xi—Pb1—Sn3^iv	115.87 (13)	Sn1—Sn3—Pt1^xvi	89.9 (6)
Sn2—Pb1—Sn3^iv	119.2 (5)	Sn3^ix—Sn3—Pt1^xvi	60.000 (1)
Sn2^xii—Pb1—Sn3^iv	60.8 (5)	Pt1^xv—Sn3—Pt1^xvi	120.000 (4)
Sn3—Pb1—Sn3^ix	60.8 (5)	Sn2—Sn3—Pt1^vii	90.1 (6)
Sn3ⁱ—Pb1—Sn3^ix	119.2 (5)	Bi1—Sn3—Pt1^vii	89.9 (6)
Sn2^ix—Pb1—Sn3^ix	29.2 (5)	Pb1—Sn3—Pt1^vii	89.9 (6)
Sn2^x—Pb1—Sn3^ix	115.87 (13)	Sn1—Sn3—Pt1^vii	89.9 (6)
Sn2^xi—Pb1—Sn3^ix	115.87 (13)	Sn3^ix—Sn3—Pt1^vii	60.000 (5)
Sn2—Pb1—Sn3^ix	60.8 (5)	Pt1^xv—Sn3—Pt1^vii	120.000 (4)
Sn2^xii—Pb1—Sn3^ix	119.2 (5)	Pt1^xvi—Sn3—Pt1^vii	120.000 (4)
Sn3^iv—Pb1—Sn3^ix	58.5 (10)	Sn2—Sn3—Sn3^x	90.2 (13)
Sn3—Pb1—Sn3^vi	119.2 (5)	Bi1—Sn3—Sn3^x	89.8 (13)
Sn3ⁱ—Pb1—Sn3^vi	60.8 (5)	Pb1—Sn3—Sn3^x	89.8 (13)
Sn2^ix—Pb1—Sn3^vi	115.87 (13)	Sn1—Sn3—Sn3^x	89.8 (13)
Sn2^x—Pb1—Sn3^vi	115.87 (13)	Pt1^xv—Sn3—Sn3^x	60.0
Sn2^xi—Pb1—Sn3^vi	29.2 (5)	Pt1^xvi—Sn3—Sn3^x	60.000 (1)
Sn2—Pb1—Sn3^vi	119.2 (5)	Pt1^vii—Sn3—Sn3^x	179.7 (19)
Sn2^xii—Pb1—Sn3^vi	60.8 (5)	Sn2—Sn3—Sn3^xi	90.2 (13)
Sn3^iv—Pb1—Sn3^vi	98.2 (6)	Bi1—Sn3—Sn3^xi	89.8 (13)
Sn3^ix—Pb1—Sn3^vi	128.3 (3)	Pb1—Sn3—Sn3^xi	89.8 (13)
Sn3—Pb1—Sn3^x	60.8 (5)	Sn1—Sn3—Sn3^xi	89.8 (13)
Sn3ⁱ—Pb1—Sn3^x	119.2 (5)	Pt1^xv—Sn3—Sn3^xi	59.999 (4)
Sn2^ix—Pb1—Sn3^x	115.87 (13)	Pt1^xvi—Sn3—Sn3^xi	179.7 (19)
Sn2^x—Pb1—Sn3^x	29.2 (5)	Pt1^vii—Sn3—Sn3^xi	60.000 (6)
Sn2^xi—Pb1—Sn3^x	115.87 (13)	Sn2—Sn3—Sn3^xiv	0.0
Sn2—Pb1—Sn3^x	60.8 (5)	Bi1—Sn3—Sn3^xiv	180.0
Sn2^xii—Pb1—Sn3^x	119.2 (5)	Pb1—Sn3—Sn3^xiv	180.0
Sn3^iv—Pb1—Sn3^x	128.3 (3)	Sn1—Sn3—Sn3^xiv	180.0
Sn3^ix—Pb1—Sn3^x	98.2 (6)	Sn3^ix—Sn3—Sn3^xiv	90.2 (13)
Sn3^vi—Pb1—Sn3^x	128.3 (3)	Pt1^xv—Sn3—Sn3^xiv	90.1 (6)
Sn3—Pb1—Sn3^xiii	119.2 (5)	Pt1^xvi—Sn3—Sn3^xiv	90.1 (6)
Sn3ⁱ—Pb1—Sn3^xiii	60.8 (5)	Pt1^vii—Sn3—Sn3^xiv	90.1 (6)
Sn2^ix—Pb1—Sn3^xiii	115.87 (13)	Sn3^x—Sn3—Sn3^xiv	90.2 (13)
Sn2^x—Pb1—Sn3^xiii	29.2 (5)	Sn3^xi—Sn3—Sn3^xiv	90.2 (13)
Sn2^xi—Pb1—Sn3^xiii	115.87 (13)	Sn2—Sn3—Sn3ⁱ	180.0
Sn2—Pb1—Sn3^xiii	119.2 (5)	Bi1—Sn3—Sn3ⁱ	0.0
Sn2^xii—Pb1—Sn3^xiii	60.8 (5)	Pb1—Sn3—Sn3ⁱ	0.0
Sn3^iv—Pb1—Sn3^xiii	98.2 (6)	Sn1—Sn3—Sn3ⁱ	0.0
Sn3^ix—Pb1—Sn3^xiii	128.3 (3)	Sn3^ix—Sn3—Sn3ⁱ	89.8 (13)
Sn3^vi—Pb1—Sn3^xiii	98.2 (6)	Pt1^xv—Sn3—Sn3ⁱ	89.9 (6)
Sn3^x—Pb1—Sn3^xiii	58.5 (10)	Pt1^xvi—Sn3—Sn3ⁱ	89.9 (6)
Sn3—Sn1—Sn3ⁱ	180.0	Pt1^vii—Sn3—Sn3ⁱ	89.9 (6)
Sn3—Sn1—Sn2^ix	90.000 (1)	Sn3^x—Sn3—Sn3ⁱ	89.8 (13)
Sn3ⁱ—Sn1—Sn2^ix	89.999 (1)	Sn3^xi—Sn3—Sn3ⁱ	89.8 (13)
Sn3—Sn1—Sn2^x	90.000 (4)	Sn3^xiv—Sn3—Sn3ⁱ	180.0

Symmetry codes: (i) x, y, −z+1/2; (ii) −x, −y, z−1/2; (iii) x−1, y−1, −z+1/2; (iv) −x+1, −y+1, z−1/2; (v) x, y−1, −z+1/2; (vi) −x, −y+1, z−1/2; (vii) −x, −y, z+1/2; (viii) −x, −y, −z; (ix) −x+1, −y+1, −z+1; (x) −x+1, −y+2, −z+1; (xi) −x, −y+1, −z+1; (xii) x, y, z−1; (xiii) −x+1, −y+2, z−1/2; (xiv) x, y, −z+3/2; (xv) −x, −y+1, z+1/2; (xvi) −x+1, −y+1, z+1/2.

Funding information

LR and MA gratefully acknowledge the financial support of the European Social Fund and the State of Saxony provided for the NeMaCell project (project No. 100382169). YG acknowledges the support of the Deutsche Forschungsgemeinschaft (grant: GR1793/19–1).

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Volume 79| Part 3| March 2023| Pages 129-131

https://doi.org/10.1107/S2056989023000956

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research communications\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

The crystal structure of quaternary (Sn,Pb,Bi)Pt

1. Chemical context

2. Structural commentary

3. Synthesis and crystallization

4. Refinement

Supporting information

Funding information

References

research communications