Crystal structure of dilead(II) oxochromate(VI) oxotellurate(IV)

Matthias Weil

doi:10.1107/S2056989017006995

. 2017 May 16;73(Pt 6):853–855. doi: 10.1107/S2056989017006995

Crystal structure of dilead(II) oxochromate(VI) oxotellurate(IV)

Matthias Weil ^a,^*

PMCID: PMC5458308 PMID: 28638643

The crystal structure of Pb₂(CrO₄)(TeO₃) is isotypic with its sulfate analogue Pb₂(SO₄)(TeO₃). Comparison between the structures is made with the COMPSTRU program.

Keywords: crystal structure, lead, oxochromate(VI), oxotellurate(IV), isotypism

Abstract

Reaction of chromium(III) precursors with TeO₂ in PbF₂/PbO melts in air led to oxidation of chromium(III) to chromium(VI), whereas tellurium remained its oxidation state of IV. In the resulting title compound, Pb₂(CrO₄)(TeO₃), the two types of anions are isolated from each other, hence a double salt is formed. The two independent Pb²⁺ cations exhibit coordination number nine under formation of very distorted coordination polyhedra [bond-length range = 2.363 (6)–3.276 (7) Å]. The oxochromate(VI) and oxotellurate(IV) anions have tetrahedral and trigonal–pyramidal configurations, respectively. In the crystal structure, (001) layers of metal cations alternate with layers of TeO₃ ²⁻ and CrO₄ ²⁻ anions along [001], forming a three-dimensional framework structure. Pb₂(CrO₄)(TeO₃) is isotypic with its sulfate analogue Pb₂(SO₄)(TeO₃) and is comparatively discussed.

Chemical context

Pb₃Fe₂Te₂O₁₂ is an oxotellurate(VI) with interesting structural features. It crystallizes in the non-centrosymmetric space group Cc and has Te^VI and Fe^III atoms occupationally disordered at the same sites (Müller-Buschbaum & Wedel, 1997 ▸). This compound has been prepared by solid-state reactions from a PbO, Fe₂O₃ and TeO₂ mixture in air, which led to oxidation of Te^IV to Te^VI. During an attempt to replace iron(III) by chromium(III) to prepare a possible phase with composition ‘Pb₃Cr₂Te₂O₁₂’, the title compound, Pb₂(CrO₄)(TeO₃), was obtained instead while working under similar conditions. Interestingly, chromium was then oxidized (Cr^III → Cr^VI) while tellurium remained its oxidation state of IV. Pb₂(CrO₄)(TeO₃) is isotypic with its sulfate analogue Pb₂(SO₄)(TeO₃) (Weil & Shirkhanlou, 2017 ▸).

Structural commentary

All atoms in the asymmetric unit, viz. two Pb, one Cr, one Te and seven O sites, are located on general positions.

The coordination environments of the two Pb²⁺ cations are markedly different. If only Pb—O bond lengths < 2.8 Å are considered, atom Pb1 is surrounded by six O atoms in the range 2.4–2.8 Å whereas atom Pb2 has four oxygen atoms as coordination partners, three at ∼2.38 Å and one at 2.75 Å. Taking into account the more remote oxygen atoms as well, the coordination numbers are increased to nine for both Pb²⁺ cations (Fig. 1 ▸, Table 1 ▸).

Coordination environments around the two Pb²⁺ cations in Pb₂(CrO₄)(TeO₃). Pb—O bonds < 2.8 Å are given in full and longer Pb–O bonds are open. Symmetry operators refer to Table 1 ▸.

Table 1. Comparison of bond lengths between isotypic Pb₂(CrO₄)(TeO₃) and Pb₂(SO₄)(TeO₃).

Bond	Pb₂(CrO₄)(TeO₃)	Pb₂(SO₄)(TeO₃)
Pb1—O2ⁱ	2.429 (6)	2.397 (3)
Pb1—O3ⁱⁱ	2.573 (6)	2.594 (3)
Pb1—O2ⁱⁱⁱ	2.594 (6)	2.536 (3)
Pb1—O7^iv	2.617 (7)	2.632 (3)
Pb1—O5^v	2.750 (7)	2.789 (3)
Pb1—O4ⁱ	2.777 (7)	2.677 (3)
Pb1—O6ⁱⁱⁱ	2.850 (7)	3.107 (4)
Pb1—O1ⁱⁱ	2.968 (6)	2.993 (3)
Pb1—O3ⁱⁱⁱ	3.170 (6)	3.206 (3)
Pb2—O3ⁱⁱⁱ	2.363 (6)	2.335 (3)
Pb2—O1ⁱⁱ	2.390 (6)	2.375 (3)
Pb2—O1	2.410 (6)	2.384 (3)
Pb2—O2	2.746 (6)	2.753 (3)
Pb2—O5^vi	2.956 (7)	2.981 (4)
Pb2—O4^vii	3.128 (7)	3.029 (3)
Pb2—O6ⁱⁱⁱ	3.176 (7)	3.164 (3)
Pb2—O5^vii	3.225 (7)	3.200 (4)
Pb2—O4^vi	3.276 (7)	3.455 (3)
Te1—O2	1.891 (6)	1.890 (2)
Te1—O3	1.901 (6)	1.878 (2)
Te1—O1	1.902 (6)	1.895 (3)
Cr1—O7	1.634 (7)	1.462 (3)
Cr1—O5	1.640 (7)	1.476 (3)
Cr1—O4	1.653 (7)	1.488 (3)
Cr1—O6	1.667 (7)	1.484 (3)

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Symmetry codes: (i) x − Inline graphic , −y + , z − ; (ii) −x + 2, −y + 1, −z + 1; (iii) −x + , y − , −z + ; (iv) −x + , y − , −z + ; (v) −x + 2, −y + 1, −z + 2; (vi) x, y, z − 1; (vii) −x + 3, −y + 1, −z + 2.

The chromium atom shows a tetrahedral and the tellurium a trigonal–pyramidal coordination by oxygen atoms. These two coordination polyhedra and the corresponding bond lengths ranges are typical for oxochromates(VI) (Pressprich et al., 1988 ▸) and oxotellurates(IV) (Christy et al., 2016 ▸), respectively.

In the crystal structure, the Pb²⁺ cations are arranged in layers parallel to (001) at z ∼ 0, ½ and in turn are stacked into columns extending along [010]. The two types of anion polyhedra are isolated and are likewise arranged into columnar arrangements along [010], forming anion layers situated at z ∼ ¼ and ¾. The metal cation and anion layers alternate along [001] and build up the three-dimensional framework of the crystal structure. The 5s ² and 6s ² electron lone pairs of the Te^IV atoms of the oxotellurate anions and of the Pb²⁺ cations, respectively, are stereochemically active and point into channels running parallel to the two types of columns along [010] (Fig. 2 ▸).

The crystal structure of Pb₂(CrO₄)(TeO₃) in a projection along [010]. Te atoms and TeO₃ ^2– trigonal pyramids are given in red, CrO₄ ²⁻ tetrahedra in green, Pb²⁺ cations in blue, O atoms are colourless. For clarity, only Pb—O bonds < 2.8 Å are displayed. Displacement ellipsoids are given at the 50% probability level.

Relevant bond lengths of isotypic Pb₂(CrO₄)(TeO₃) and Pb₂(SO₄)(TeO₃) are compared in Table 1 ▸. Whereas the TeO₃ ²⁻ anions in the two structures show only marginal differences, the expected differences in the X—O bond lengths (X = Cr, S) of the chromate and sulfate tetrahedra (average values 1.65 and 1.48 Å, respectively) also have consequences for those Pb—O bonds where the corresponding atoms O4–O7 are involved. These Pb—O bonds differ by up to 0.20 Å. A more quantitative comparison of the two isotypic structures was made with the program COMPSTRU (de la Flor et al., 2016 ▸). The degree of lattice distortion, S, is the spontaneous strain (sum of the squared eigenvalues of the strain tensor divided by 3) and amounts to 0.007. The maximum distance shows the maximal displacement between atomic positions of paired atoms and is 0.31 Å for atom pair O4. The next largest distances are 0.23 Å for pair O6, 0.17 Å for O5 and 0.13 Å for O7. The pairs of heavy atoms and the Cr/S pair show comparatively small distances of 0.095 Å (Pb1), 0.061 Å (Pb2), 0.087 Å (Te1) and 0.095 Å (Cr1/S1). The arithmetic mean of the distances is 0.12 Å. The measure of similarity (Δ) (Bergerhoff et al., 1999 ▸) is 0.034, revealing a close relation between the two structures. Δ takes into consideration the differences in atomic positions and the ratios of the corresponding lattice parameters of the structures.

Synthesis and crystallization

Cr(NO₃)₃·9H₂O, PbF₂, PbO and TeO₂ were mixed thoroughly in a stoichiometric ratio of 1:1:2:1 and heated in an open alumina crucible to 1033 K within six h, held at this temperature for 30 h and cooled within eight h to room temperature. Most of the material had evaporated, and only a few orange plates of the title compound were left.

Alternatively, replacement of Cr(NO₃)₃·9H₂O with Cr₂O₃ under the same reaction conditions likewise led to the formation of Pb₂(CrO₄)(TeO₃).

Refinement

Crystal data, data collection and structure refinement details are summarized in Table 2 ▸. Starting coordinates were taken from isotypic Pb₂(SO₄)(TeO₃) (Weil & Shirkhanlou, 2017 ▸). The maximum and minimum electron densities are located 1.26 and 0.81 Å, respectively, from atom Pb2.

Table 2. Experimental details.

Crystal data
Chemical formula	Pb₂(CrO₄)(TeO₃)
M _r	705.98
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	296
a, b, c (Å)	7.4736 (12), 10.8091 (16), 9.4065 (14)
β (°)	111.098 (12)
V (Å³)	708.95 (19)
Z	4
Radiation type	Mo Kα
μ (mm⁻¹)	52.91
Crystal size (mm)	0.09 × 0.06 × 0.01

Data collection
Diffractometer	Bruker APEXII CCD
Absorption correction	Multi-scan (SADABS; Bruker, 2015 ▸)
T _min, T _max	0.264, 0.494
No. of measured, independent and observed [I > 2σ(I)] reflections	23485, 2183, 1760
R _int	0.094
(sin θ/λ)_max (Å⁻¹)	0.717

Refinement
R[F ² > 2σ(F ²)], wR(F ²), S	0.031, 0.070, 1.06
No. of reflections	2183
No. of parameters	100
Δρ_max, Δρ_min (e Å⁻³)	2.47, −2.33

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Computer programs: APEX3 and SAINT (Bruker, 2015 ▸), SHELXL2014 (Sheldrick, 2015 ▸), ATOMS (Dowty, 2006 ▸) and publCIF (Westrip, 2010 ▸).

Supplementary Material

Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S2056989017006995/hb7677sup1.cif

e-73-00853-sup1.cif^{(711.5KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S2056989017006995/hb7677Isup2.hkl

e-73-00853-Isup2.hkl^{(175.2KB, hkl)}

CCDC reference: 1548953

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

Acknowledgments

The X-ray centre of the Vienna University of Technology is acknowledged for financial support and for providing access to the single-crystal diffractometer.

supplementary crystallographic information

Crystal data

Pb₂(CrO₄)(TeO₃)	F(000) = 1184
M_r = 705.98	D_x = 6.614 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
a = 7.4736 (12) Å	Cell parameters from 3031 reflections
b = 10.8091 (16) Å	θ = 3.1–28.3°
c = 9.4065 (14) Å	µ = 52.91 mm⁻¹
β = 111.098 (12)°	T = 296 K
V = 708.95 (19) Å³	Plate, orange
Z = 4	0.09 × 0.06 × 0.01 mm

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Data collection

Bruker APEXII CCD diffractometer	1760 reflections with I > 2σ(I)
ω– and φ–scans	R_int = 0.094
Absorption correction: multi-scan (SADABS; Bruker, 2015)	θ_max = 30.7°, θ_min = 3.0°
T_min = 0.264, T_max = 0.494	h = −10→10
23485 measured reflections	k = −15→15
2183 independent reflections	l = −13→13

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Refinement

Refinement on F²	100 parameters
Least-squares matrix: full	0 restraints
R[F² > 2σ(F²)] = 0.031	w = 1/[σ²(F_o²) + (0.0264P)²] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.070	(Δ/σ)_max = 0.001
S = 1.06	Δρ_max = 2.47 e Å⁻³
2183 reflections	Δρ_min = −2.33 e Å⁻³

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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
Pb1	0.86662 (5)	0.16252 (3)	0.49204 (4)	0.01746 (9)
Pb2	1.27667 (5)	0.45615 (3)	0.56450 (4)	0.01735 (9)
Te1	1.11378 (8)	0.63302 (5)	0.81301 (6)	0.01180 (12)
Cr1	1.2298 (2)	0.61161 (13)	1.21196 (16)	0.0152 (3)
O1	1.0417 (9)	0.5911 (6)	0.6035 (7)	0.0187 (13)
O2	1.3339 (8)	0.5323 (5)	0.8562 (7)	0.0159 (12)
O3	1.2413 (9)	0.7803 (5)	0.7920 (6)	0.0153 (12)
O4	1.3081 (10)	0.4675 (6)	1.2262 (8)	0.0295 (17)
O5	1.3146 (11)	0.6714 (6)	1.3836 (8)	0.0292 (16)
O6	1.3082 (11)	0.6927 (7)	1.0953 (8)	0.0331 (18)
O7	0.9957 (10)	0.6054 (7)	1.1419 (9)	0.0337 (18)

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Atomic displacement parameters (Å²)

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pb1	0.01755 (19)	0.01525 (15)	0.01860 (18)	0.00102 (12)	0.00530 (14)	−0.00226 (12)
Pb2	0.01405 (18)	0.01770 (16)	0.01959 (18)	0.00177 (12)	0.00520 (14)	0.00440 (12)
Te1	0.0107 (3)	0.0117 (2)	0.0124 (3)	0.00001 (19)	0.0036 (2)	−0.00064 (19)
Cr1	0.0131 (7)	0.0191 (7)	0.0138 (7)	−0.0005 (5)	0.0053 (6)	−0.0002 (5)
O1	0.013 (3)	0.025 (3)	0.015 (3)	0.003 (3)	0.002 (3)	−0.004 (3)
O2	0.014 (3)	0.009 (3)	0.024 (3)	0.003 (2)	0.005 (3)	0.002 (2)
O3	0.018 (3)	0.013 (3)	0.014 (3)	−0.003 (2)	0.005 (3)	0.000 (2)
O4	0.032 (4)	0.024 (3)	0.031 (4)	0.003 (3)	0.010 (3)	−0.006 (3)
O5	0.041 (4)	0.028 (4)	0.018 (3)	0.007 (3)	0.010 (3)	−0.008 (3)
O6	0.040 (5)	0.036 (4)	0.029 (4)	−0.018 (3)	0.019 (4)	0.004 (3)
O7	0.017 (4)	0.039 (4)	0.043 (5)	0.005 (3)	0.010 (3)	0.015 (4)

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Geometric parameters (Å, º)

Pb1—O2ⁱ	2.429 (6)	Cr1—Te1^x	3.8465 (15)
Pb1—O3ⁱⁱ	2.573 (6)	Cr1—Pb1^xi	3.9532 (15)
Pb1—O2ⁱⁱⁱ	2.594 (6)	Cr1—Pb1^v	3.9593 (14)
Pb1—O7^iv	2.617 (7)	Cr1—Pb1^xii	4.1534 (15)
Pb1—O5^v	2.750 (7)	O1—Pb2ⁱⁱ	2.390 (6)
Pb1—O4ⁱ	2.777 (7)	O1—Pb1ⁱⁱ	2.968 (6)
Pb1—O6ⁱⁱⁱ	2.850 (7)	O1—Pb1^xi	4.515 (6)
Pb1—O1ⁱⁱ	2.968 (6)	O2—Pb1^xi	2.429 (6)
Pb1—O3ⁱⁱⁱ	3.170 (6)	O2—Pb1^xii	2.594 (6)
Pb1—Te1ⁱⁱⁱ	3.6630 (9)	O2—Pb1ⁱⁱ	4.508 (6)
Pb2—O3ⁱⁱⁱ	2.363 (6)	O3—Pb2^xii	2.363 (6)
Pb2—O1ⁱⁱ	2.390 (6)	O3—Pb1ⁱⁱ	2.573 (6)
Pb2—O1	2.410 (6)	O3—Pb1^xii	3.170 (6)
Pb2—O2	2.746 (6)	O4—Pb1^xi	2.777 (7)
Pb2—O5^vi	2.956 (7)	O4—Pb2^vii	3.128 (7)
Pb2—O4^vii	3.128 (7)	O4—Te1^v	3.228 (7)
Pb2—O6ⁱⁱⁱ	3.176 (7)	O4—Pb2^ix	3.276 (7)
Pb2—O5^vii	3.225 (7)	O4—Pb1^xii	4.262 (7)
Pb2—O4^vi	3.276 (7)	O5—Pb1^v	2.750 (7)
Pb2—Te1	3.5567 (7)	O5—Pb2^ix	2.956 (7)
Te1—O2	1.891 (6)	O5—Pb2^vii	3.225 (7)
Te1—O3	1.901 (6)	O5—Te1^x	3.314 (8)
Te1—O1	1.902 (6)	O6—Pb1^xii	2.850 (7)
Te1—O6	2.608 (7)	O6—Te1^x	3.097 (7)
Te1—O7^v	2.782 (7)	O6—Pb2^xii	3.176 (7)
Te1—O6^viii	3.097 (7)	O6—Pb2^vii	3.912 (8)
Cr1—O7	1.634 (7)	O6—Pb1^xi	4.023 (8)
Cr1—O5	1.640 (7)	O7—Pb1^xiii	2.617 (7)
Cr1—O4	1.653 (7)	O7—Te1^v	2.782 (7)
Cr1—O6	1.667 (7)	O7—Pb2^v	4.032 (8)
Cr1—Pb2^vii	3.6027 (16)	O7—Pb1^v	4.081 (8)
Cr1—Pb2^ix	3.6204 (15)	O7—Pb2^ix	4.099 (7)
Cr1—Te1^v	3.6339 (16)	O7—Pb1^xi	4.568 (8)

O2ⁱ—Pb1—O3ⁱⁱ	74.19 (19)	O7—Cr1—Pb1^xi	101.5 (3)
O2ⁱ—Pb1—O2ⁱⁱⁱ	73.9 (2)	O5—Cr1—Pb1^xi	136.8 (3)
O3ⁱⁱ—Pb1—O2ⁱⁱⁱ	126.0 (2)	O4—Cr1—Pb1^xi	35.4 (3)
O2ⁱ—Pb1—O7^iv	69.6 (2)	O6—Cr1—Pb1^xi	80.3 (3)
O3ⁱⁱ—Pb1—O7^iv	70.9 (2)	Te1—Cr1—Pb1^xi	60.35 (2)
O2ⁱⁱⁱ—Pb1—O7^iv	132.5 (2)	Pb2^vii—Cr1—Pb1^xi	75.50 (3)
O2ⁱ—Pb1—O5^v	144.9 (2)	Pb2^ix—Cr1—Pb1^xi	99.99 (3)
O3ⁱⁱ—Pb1—O5^v	105.45 (19)	Te1^v—Cr1—Pb1^xi	74.38 (3)
O2ⁱⁱⁱ—Pb1—O5^v	125.4 (2)	Te1^x—Cr1—Pb1^xi	110.89 (4)
O7^iv—Pb1—O5^v	77.1 (2)	O7—Cr1—Pb1^v	82.5 (3)
O2ⁱ—Pb1—O4ⁱ	87.9 (2)	O5—Cr1—Pb1^v	33.7 (3)
O3ⁱⁱ—Pb1—O4ⁱ	149.93 (19)	O4—Cr1—Pb1^v	132.3 (3)
O2ⁱⁱⁱ—Pb1—O4ⁱ	68.9 (2)	O6—Cr1—Pb1^v	109.6 (3)
O7^iv—Pb1—O4ⁱ	80.3 (2)	Te1—Cr1—Pb1^v	131.89 (4)
O5^v—Pb1—O4ⁱ	75.6 (2)	Pb2^vii—Cr1—Pb1^v	97.02 (3)
O2ⁱ—Pb1—O6ⁱⁱⁱ	83.2 (2)	Pb2^ix—Cr1—Pb1^v	67.93 (3)
O3ⁱⁱ—Pb1—O6ⁱⁱⁱ	69.8 (2)	Te1^v—Cr1—Pb1^v	101.01 (4)
O2ⁱⁱⁱ—Pb1—O6ⁱⁱⁱ	64.2 (2)	Te1^x—Cr1—Pb1^v	72.07 (3)
O7^iv—Pb1—O6ⁱⁱⁱ	136.9 (2)	Pb1^xi—Cr1—Pb1^v	167.69 (4)
O5^v—Pb1—O6ⁱⁱⁱ	130.5 (2)	O7—Cr1—Pb1^xii	132.0 (3)
O4ⁱ—Pb1—O6ⁱⁱⁱ	132.9 (2)	O5—Cr1—Pb1^xii	108.4 (3)
O2ⁱ—Pb1—O1ⁱⁱ	127.50 (19)	O4—Cr1—Pb1^xii	82.4 (3)
O3ⁱⁱ—Pb1—O1ⁱⁱ	59.35 (17)	O6—Cr1—Pb1^xii	30.7 (3)
O2ⁱⁱⁱ—Pb1—O1ⁱⁱ	113.96 (17)	Te1—Cr1—Pb1^xii	56.17 (2)
O7^iv—Pb1—O1ⁱⁱ	112.2 (2)	Pb2^vii—Cr1—Pb1^xii	62.31 (3)
O5^v—Pb1—O1ⁱⁱ	75.3 (2)	Pb2^ix—Cr1—Pb1^xii	129.63 (4)
O4ⁱ—Pb1—O1ⁱⁱ	144.43 (19)	Te1^v—Cr1—Pb1^xii	132.87 (4)
O6ⁱⁱⁱ—Pb1—O1ⁱⁱ	59.76 (19)	Te1^x—Cr1—Pb1^xii	54.39 (2)
O2ⁱ—Pb1—O3ⁱⁱⁱ	125.43 (18)	Pb1^xi—Cr1—Pb1^xii	59.33 (2)
O3ⁱⁱ—Pb1—O3ⁱⁱⁱ	116.15 (16)	Pb1^v—Cr1—Pb1^xii	126.12 (4)
O2ⁱⁱⁱ—Pb1—O3ⁱⁱⁱ	56.62 (16)	Te1—O1—Pb2ⁱⁱ	125.4 (3)
O7^iv—Pb1—O3ⁱⁱⁱ	164.00 (19)	Te1—O1—Pb2	110.6 (3)
O5^v—Pb1—O3ⁱⁱⁱ	87.05 (19)	Pb2ⁱⁱ—O1—Pb2	112.1 (2)
O4ⁱ—Pb1—O3ⁱⁱⁱ	93.90 (18)	Te1—O1—Pb1ⁱⁱ	95.2 (2)
O6ⁱⁱⁱ—Pb1—O3ⁱⁱⁱ	56.72 (18)	Pb2ⁱⁱ—O1—Pb1ⁱⁱ	106.0 (2)
O1ⁱⁱ—Pb1—O3ⁱⁱⁱ	64.71 (16)	Pb2—O1—Pb1ⁱⁱ	103.7 (2)
O2ⁱ—Pb1—Te1ⁱⁱⁱ	94.34 (14)	Te1—O1—Pb1^xi	55.69 (15)
O3ⁱⁱ—Pb1—Te1ⁱⁱⁱ	114.85 (13)	Pb2ⁱⁱ—O1—Pb1^xi	121.5 (2)
O2ⁱⁱⁱ—Pb1—Te1ⁱⁱⁱ	29.32 (12)	Pb2—O1—Pb1^xi	63.04 (13)
O7^iv—Pb1—Te1ⁱⁱⁱ	161.34 (16)	Pb1ⁱⁱ—O1—Pb1^xi	132.40 (18)
O5^v—Pb1—Te1ⁱⁱⁱ	116.07 (15)	Te1—O2—Pb1^xi	121.8 (3)
O4ⁱ—Pb1—Te1ⁱⁱⁱ	90.00 (15)	Te1—O2—Pb1^xii	108.5 (2)
O6ⁱⁱⁱ—Pb1—Te1ⁱⁱⁱ	45.10 (15)	Pb1^xi—O2—Pb1^xii	106.1 (2)
O1ⁱⁱ—Pb1—Te1ⁱⁱⁱ	84.89 (12)	Te1—O2—Pb2	98.5 (2)
O3ⁱⁱⁱ—Pb1—Te1ⁱⁱⁱ	31.26 (10)	Pb1^xi—O2—Pb2	102.47 (19)
O3ⁱⁱⁱ—Pb2—O1ⁱⁱ	87.6 (2)	Pb1^xii—O2—Pb2	120.4 (2)
O3ⁱⁱⁱ—Pb2—O1	101.9 (2)	Te1—O2—Pb1ⁱⁱ	52.16 (15)
O1ⁱⁱ—Pb2—O1	67.9 (2)	Pb1^xi—O2—Pb1ⁱⁱ	163.9 (2)
O3ⁱⁱⁱ—Pb2—O2	72.00 (18)	Pb1^xii—O2—Pb1ⁱⁱ	89.88 (14)
O1ⁱⁱ—Pb2—O2	119.0 (2)	Pb2—O2—Pb1ⁱⁱ	66.54 (12)
O1—Pb2—O2	61.76 (19)	Te1—O3—Pb2^xii	118.7 (3)
O3ⁱⁱⁱ—Pb2—O5^vi	177.4 (2)	Te1—O3—Pb1ⁱⁱ	109.1 (2)
O1ⁱⁱ—Pb2—O5^vi	93.8 (2)	Pb2^xii—O3—Pb1ⁱⁱ	109.8 (2)
O1—Pb2—O5^vi	80.6 (2)	Te1—O3—Pb1^xii	88.8 (2)
O2—Pb2—O5^vi	109.06 (17)	Pb2^xii—O3—Pb1^xii	100.75 (19)
O3ⁱⁱⁱ—Pb2—O4^vii	95.8 (2)	Pb1ⁱⁱ—O3—Pb1^xii	129.3 (2)
O1ⁱⁱ—Pb2—O4^vii	176.63 (19)	Te1—O3—Pb2	58.39 (14)
O1—Pb2—O4^vii	110.89 (19)	Pb2^xii—O3—Pb2	176.2 (2)
O2—Pb2—O4^vii	61.95 (18)	Pb1ⁱⁱ—O3—Pb2	73.89 (13)
O5^vi—Pb2—O4^vii	82.9 (2)	Pb1^xii—O3—Pb2	77.08 (11)
O3ⁱⁱⁱ—Pb2—O6ⁱⁱⁱ	60.41 (19)	Cr1—O4—Pb1^xi	124.4 (4)
O1ⁱⁱ—Pb2—O6ⁱⁱⁱ	60.90 (19)	Cr1—O4—Pb2^vii	92.6 (3)
O1—Pb2—O6ⁱⁱⁱ	125.6 (2)	Pb1^xi—O4—Pb2^vii	103.2 (2)
O2—Pb2—O6ⁱⁱⁱ	132.40 (18)	Cr1—O4—Te1^v	90.3 (3)
O5^vi—Pb2—O6ⁱⁱⁱ	118.53 (18)	Pb1^xi—O4—Te1^v	99.5 (2)
O4^vii—Pb2—O6ⁱⁱⁱ	121.22 (17)	Pb2^vii—O4—Te1^v	150.2 (3)
O3ⁱⁱⁱ—Pb2—O5^vii	79.3 (2)	Cr1—O4—Pb2^ix	88.1 (3)
O1ⁱⁱ—Pb2—O5^vii	132.23 (19)	Pb1^xi—O4—Pb2^ix	147.0 (2)
O1—Pb2—O5^vii	159.74 (19)	Pb2^vii—O4—Pb2^ix	78.49 (16)
O2—Pb2—O5^vii	100.28 (16)	Te1^v—O4—Pb2^ix	71.93 (15)
O5^vi—Pb2—O5^vii	98.15 (17)	Cr1—O4—Te1	60.7 (2)
O4^vii—Pb2—O5^vii	49.20 (17)	Pb1^xi—O4—Te1	64.28 (14)
O6ⁱⁱⁱ—Pb2—O5^vii	72.86 (18)	Pb2^vii—O4—Te1	114.8 (2)
O3ⁱⁱⁱ—Pb2—O4^vi	128.57 (18)	Te1^v—O4—Te1	92.34 (16)
O1ⁱⁱ—Pb2—O4^vi	76.61 (19)	Pb2^ix—O4—Te1	145.4 (2)
O1—Pb2—O4^vi	115.84 (19)	Cr1—O4—Pb1^xii	75.0 (3)
O2—Pb2—O4^vi	156.81 (17)	Pb1^xi—O4—Pb1^xii	65.68 (15)
O5^vi—Pb2—O4^vi	49.92 (17)	Pb2^vii—O4—Pb1^xii	64.16 (13)
O4^vii—Pb2—O4^vi	101.51 (16)	Te1^v—O4—Pb1^xii	144.5 (2)
O6ⁱⁱⁱ—Pb2—O4^vi	69.25 (17)	Pb2^ix—O4—Pb1^xii	137.7 (2)
O5^vii—Pb2—O4^vi	76.56 (18)	Te1—O4—Pb1^xii	52.26 (9)
O3ⁱⁱⁱ—Pb2—Te1	87.36 (14)	Cr1—O5—Pb1^v	126.9 (4)
O1ⁱⁱ—Pb2—Te1	93.13 (15)	Cr1—O5—Pb2^ix	100.0 (3)
O1—Pb2—Te1	30.03 (14)	Pb1^v—O5—Pb2^ix	96.0 (2)
O2—Pb2—Te1	31.73 (12)	Cr1—O5—Pb2^vii	89.4 (3)
O5^vi—Pb2—Te1	94.68 (13)	Pb1^v—O5—Pb2^vii	143.1 (2)
O4^vii—Pb2—Te1	86.63 (13)	Pb2^ix—O5—Pb2^vii	81.85 (17)
O6ⁱⁱⁱ—Pb2—Te1	137.38 (13)	Cr1—O5—Te1^x	95.9 (3)
O5^vii—Pb2—Te1	131.31 (12)	Pb1^v—O5—Te1^x	98.0 (2)
O4^vi—Pb2—Te1	141.21 (12)	Pb2^ix—O5—Te1^x	146.0 (3)
O2—Te1—O3	94.3 (3)	Pb2^vii—O5—Te1^x	68.42 (15)
O2—Te1—O1	89.2 (3)	Cr1—O6—Te1	109.9 (3)
O3—Te1—O1	93.3 (3)	Cr1—O6—Pb1^xii	131.9 (4)
O2—Te1—O6	78.5 (3)	Te1—O6—Pb1^xii	84.2 (2)
O3—Te1—O6	77.4 (2)	Cr1—O6—Te1^x	103.6 (3)
O1—Te1—O6	163.8 (2)	Te1—O6—Te1^x	146.3 (3)
O2—Te1—O7^v	73.4 (2)	Pb1^xii—O6—Te1^x	75.99 (17)
O3—Te1—O7^v	167.7 (2)	Cr1—O6—Pb2^xii	136.5 (4)
O1—Te1—O7^v	87.0 (2)	Te1—O6—Pb2^xii	78.27 (18)
O6—Te1—O7^v	99.2 (2)	Pb1^xii—O6—Pb2^xii	90.68 (17)
O2—Te1—O6^viii	150.4 (2)	Te1^x—O6—Pb2^xii	75.03 (16)
O3—Te1—O6^viii	72.5 (2)	Cr1—O6—Pb2^vii	67.0 (2)
O1—Te1—O6^viii	66.0 (2)	Te1—O6—Pb2^vii	135.9 (3)
O6—Te1—O6^viii	122.06 (13)	Pb1^xii—O6—Pb2^vii	71.42 (16)
O7^v—Te1—O6^viii	118.5 (2)	Te1^x—O6—Pb2^vii	61.99 (13)
O7—Cr1—O5	113.0 (4)	Pb2^xii—O6—Pb2^vii	136.1 (2)
O7—Cr1—O4	106.9 (4)	Cr1—O6—Pb1^xi	75.6 (3)
O5—Cr1—O4	106.9 (3)	Te1—O6—Pb1^xi	65.61 (16)
O7—Cr1—O6	109.6 (4)	Pb1^xii—O6—Pb1^xi	69.10 (16)
O5—Cr1—O6	109.8 (4)	Te1^x—O6—Pb1^xi	128.5 (2)
O4—Cr1—O6	110.5 (4)	Pb2^xii—O6—Pb1^xi	139.7 (2)
O7—Cr1—Te1	76.0 (3)	Pb2^vii—O6—Pb1^xi	71.46 (13)
O5—Cr1—Te1	151.4 (3)	Cr1—O7—Pb1^xiii	163.1 (4)
O4—Cr1—Te1	95.3 (3)	Cr1—O7—Te1^v	107.9 (3)
O6—Cr1—Te1	43.8 (3)	Pb1^xiii—O7—Te1^v	89.0 (2)
O7—Cr1—Pb2^vii	161.7 (3)	Cr1—O7—Te1	77.3 (3)
O5—Cr1—Pb2^vii	63.5 (3)	Pb1^xiii—O7—Te1	95.7 (2)
O4—Cr1—Pb2^vii	60.2 (3)	Te1^v—O7—Te1	113.1 (2)
O6—Cr1—Pb2^vii	87.8 (3)	Cr1—O7—Pb2^v	117.5 (3)
Te1—Cr1—Pb2^vii	116.13 (4)	Pb1^xiii—O7—Pb2^v	71.26 (16)
O7—Cr1—Pb2^ix	95.0 (3)	Te1^v—O7—Pb2^v	59.62 (13)
O5—Cr1—Pb2^ix	53.5 (3)	Te1—O7—Pb2^v	164.5 (2)
O4—Cr1—Pb2^ix	64.8 (3)	Cr1—O7—Pb1^v	74.1 (3)
O6—Cr1—Pb2^ix	154.9 (3)	Pb1^xiii—O7—Pb1^v	99.4 (2)
Te1—Cr1—Pb2^ix	155.08 (4)	Te1^v—O7—Pb1^v	116.1 (2)
Pb2^vii—Cr1—Pb2^ix	68.28 (3)	Te1—O7—Pb1^v	128.5 (2)
O7—Cr1—Te1^v	46.7 (3)	Pb2^v—O7—Pb1^v	63.88 (12)
O5—Cr1—Te1^v	111.3 (3)	Cr1—O7—Pb2^ix	61.6 (2)
O4—Cr1—Te1^v	62.7 (3)	Pb1^xiii—O7—Pb2^ix	129.8 (2)
O6—Cr1—Te1^v	138.4 (3)	Te1^v—O7—Pb2^ix	64.15 (14)
Te1—Cr1—Te1^v	94.66 (4)	Te1—O7—Pb2^ix	133.03 (19)
Pb2^vii—Cr1—Te1^v	116.17 (4)	Pb2^v—O7—Pb2^ix	58.65 (10)
Pb2^ix—Cr1—Te1^v	63.55 (3)	Pb1^v—O7—Pb2^ix	62.50 (11)
O7—Cr1—Te1^x	136.4 (3)	Cr1—O7—Pb1^xi	58.0 (2)
O5—Cr1—Te1^x	59.0 (3)	Pb1^xiii—O7—Pb1^xi	129.7 (2)
O4—Cr1—Te1^x	116.4 (3)	Te1^v—O7—Pb1^xi	72.81 (16)
O6—Cr1—Te1^x	51.5 (3)	Te1—O7—Pb1^xi	53.91 (10)
Te1—Cr1—Te1^x	95.23 (3)	Pb2^v—O7—Pb1^xi	128.24 (17)
Pb2^vii—Cr1—Te1^x	59.04 (2)	Pb1^v—O7—Pb1^xi	130.79 (17)
Pb2^ix—Cr1—Te1^x	106.81 (4)	Pb2^ix—O7—Pb1^xi	83.91 (12)
Te1^v—Cr1—Te1^x	170.10 (4)

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Symmetry codes: (i) x−1/2, −y+1/2, z−1/2; (ii) −x+2, −y+1, −z+1; (iii) −x+5/2, y−1/2, −z+3/2; (iv) −x+3/2, y−1/2, −z+3/2; (v) −x+2, −y+1, −z+2; (vi) x, y, z−1; (vii) −x+3, −y+1, −z+2; (viii) x−1/2, −y+3/2, z−1/2; (ix) x, y, z+1; (x) x+1/2, −y+3/2, z+1/2; (xi) x+1/2, −y+1/2, z+1/2; (xii) −x+5/2, y+1/2, −z+3/2; (xiii) −x+3/2, y+1/2, −z+3/2.

References

Bergerhoff, G., Berndt, M., Brandenburg, K. & Degen, T. (1999). Acta Cryst. B55, 147–156. [DOI] [PubMed]
Bruker (2015). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
Christy, A. G., Mills, S. J. & Kampf, A. R. (2016). Mineral. Mag. 80, 415–545.
Dowty, E. (2006). ATOMS. Shape Software, Kingsport, Tennessee, USA.
Flor, G. de la, Orobengoa, D., Tasci, E., Perez-Mato, J. M. & Aroyo, M. I. (2016). J. Appl. Cryst. 49, 653–664.
Müller-Buschbaum, H.-K. & Wedel, B. (1997). Z. Naturforsch. Teil B, 52, 35–39.
Pressprich, M. R., Willett, R. D., Poshusta, R. D., Saunders, S. C., Davis, H. B. & Gard, H. B. (1988). Inorg. Chem. 27, 260–264.
Sheldrick, G. M. (2015). Acta Cryst. C71, 3–8.
Weil, M. & Shirkhanlou, M. (2017). Z. Anorg. Allg. Chem. Accepted. doi:10.1002/zaac.201700016.
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920–925.

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, global. DOI: 10.1107/S2056989017006995/hb7677sup1.cif

e-73-00853-sup1.cif^{(711.5KB, cif)}

Structure factors: contains datablock(s) I. DOI: 10.1107/S2056989017006995/hb7677Isup2.hkl

e-73-00853-Isup2.hkl^{(175.2KB, hkl)}

CCDC reference: 1548953

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

[bb1] Bergerhoff, G., Berndt, M., Brandenburg, K. & Degen, T. (1999). Acta Cryst. B55, 147–156. [DOI] [PubMed]

[bb2] Bruker (2015). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.

[bb3] Christy, A. G., Mills, S. J. & Kampf, A. R. (2016). Mineral. Mag. 80, 415–545.

[bb4] Dowty, E. (2006). ATOMS. Shape Software, Kingsport, Tennessee, USA.

[bb5] Flor, G. de la, Orobengoa, D., Tasci, E., Perez-Mato, J. M. & Aroyo, M. I. (2016). J. Appl. Cryst. 49, 653–664.

[bb6] Müller-Buschbaum, H.-K. & Wedel, B. (1997). Z. Naturforsch. Teil B, 52, 35–39.

[bb7] Pressprich, M. R., Willett, R. D., Poshusta, R. D., Saunders, S. C., Davis, H. B. & Gard, H. B. (1988). Inorg. Chem. 27, 260–264.

[bb8] Sheldrick, G. M. (2015). Acta Cryst. C71, 3–8.

[bb9] Weil, M. & Shirkhanlou, M. (2017). Z. Anorg. Allg. Chem. Accepted. doi:10.1002/zaac.201700016.

[bb10] Westrip, S. P. (2010). J. Appl. Cryst. 43, 920–925.

PERMALINK

Crystal structure of dilead(II) oxochromate(VI) oxotellurate(IV)

Matthias Weil

Abstract

Chemical context

Structural commentary

Figure 1.

Table 1. Comparison of bond lengths between isotypic Pb₂(CrO₄)(TeO₃) and Pb₂(SO₄)(TeO₃).

Figure 2.

Synthesis and crystallization

Refinement

Table 2. Experimental details.

Supplementary Material

Acknowledgments

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)

References

Associated Data

Supplementary Materials

ACTIONS

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PERMALINK

Crystal structure of dilead(II) oxochromate(VI) oxotellurate(IV)

Matthias Weil

Abstract

Chemical context

Structural commentary

Figure 1.

Table 1. Comparison of bond lengths between isotypic Pb2(CrO4)(TeO3) and Pb2(SO4)(TeO3).

Figure 2.

Synthesis and crystallization

Refinement

Table 2. Experimental details.

Supplementary Material

Acknowledgments

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)

References

Associated Data

Supplementary Materials

ACTIONS

PERMALINK

RESOURCES

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Table 1. Comparison of bond lengths between isotypic Pb₂(CrO₄)(TeO₃) and Pb₂(SO₄)(TeO₃).

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

Atomic displacement parameters (Å²)