Tl2Mo9Se11

Gougeon, P.; Gall, P.; Potel, M.

doi:10.1107/S1600536810026541

inorganic compounds

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Volume 66| Part 8| August 2010| Page i56

https://doi.org/10.1107/S1600536810026541

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Tl₂Mo₉Se₁₁

Patrick Gougeon,^a ^* Philippe Gall ^a and Michel Potel ^a

^aSciences Chimiques de Rennes, CSM-INSA, UMR CNRS No. 6226, Université de Rennes I, Avenue du Général Leclerc, 35042 Rennes CEDEX, France
^*Correspondence e-mail: Patrick.Gougeon@univ-rennes1.fr

(Received 24 June 2010; accepted 5 July 2010; online 10 July 2010)

The structure of Tl₂Mo₉Se₁₁, dithallium nonamolybdenum undecaselenide, is isotypic with Tl₂Mo₉S₁₁ [Potel et al. (1980 ). Acta Cryst. B36, 1319–1322]. The structural set-up is characterized by a mixture of Mo₆Seⁱ₈Se^a₆ and Mo₁₂Seⁱ₁₄Se^a₆ cluster units in a 1:1 ratio. Both components are interconnected through interunit Mo—Se bonds. The cluster units are centered at Wyckoff positions 3a and 3b (point-group symmetry $[\overline{3}]$ .). The two Tl^I atoms are situated in the voids of the three-dimensional arrangement. Two of the five independent Se atoms and the Tl atoms lie on sites with 3. symmetry (Wyckoff site 6c).

Related literature

For the crystal structure of Tl₂Mo₉S₁₁, see: Potel et al. (1980). For details of the i- and a-type ligand notation, see: Schäfer & von Schnering (1964 ). Ionic radii were compiled by Shannon (1976 ). For background to the extinction correction, see: Becker & Coppens (1974 ).

Experimental

Crystal data

Tl₂Mo₉Se₁₁
M_r = 2140.8
Trigonal, $[R \overline 3]$
a = 9.6212 (1) Å
c = 36.3316 (7) Å
V = 2912.55 (7) Å³
Z = 6
Mo Kα radiation
μ = 42.73 mm⁻¹
T = 293 K
0.13 × 0.12 × 0.11 mm

Data collection

Nonius KappaCCD diffractometer
Absorption correction: multi-scan (PLATON; Spek, 2009 ) T_min = 0.033, T_max = 0.108
21097 measured reflections
4097 independent reflections
3156 reflections with I > 2σ(I)
R_int = 0.087

Refinement

R[F² > 2σ(F²)] = 0.043
wR(F²) = 0.092
S = 1.37
4097 reflections
69 parameters
Δρ_max = 3.92 e Å⁻³
Δρ_min = −2.89 e Å⁻³

Table 1
Selected bond lengths (Å)

Tl1—Tl2ⁱ	3.5164 (7)
Tl1—Se2	4.3543 (6)
Tl1—Se2ⁱⁱ	4.3543 (7)
Tl1—Se2ⁱⁱⁱ	4.3543 (7)
Tl1—Se3	3.5840 (6)
Tl1—Se3ⁱⁱ	3.5840 (5)
Tl1—Se3ⁱⁱⁱ	3.5840 (8)
Tl1—Se3^iv	3.4547 (6)
Tl1—Se3^v	3.4547 (8)
Tl1—Se3^vi	3.4547 (5)
Tl1—Se4^vii	3.0737 (10)
Tl2—Se1	3.4032 (7)
Tl2—Se1^viii	3.4032 (6)
Tl2—Se1^ix	3.4032 (8)
Tl2—Se2ⁱ	3.1441 (4)
Tl2—Se2^x	3.1441 (7)
Tl2—Se2^xi	3.1441 (7)
Tl2—Se3ⁱ	4.2446 (7)
Tl2—Se3^x	4.2446 (6)
Tl2—Se3^xi	4.2446 (8)
Tl2—Se5	3.0483 (9)
Mo1—Mo1^xii	2.6897 (7)
Mo1—Mo1^x	2.7609 (6)
Mo1—Mo2^viii	3.4239 (8)
Mo1—Se1	2.5540 (8)
Mo1—Se1^x	2.6143 (8)
Mo1—Se1^xiii	2.5757 (6)
Mo1—Se2	2.6247 (8)
Mo1—Se4	2.5269 (8)
Mo2—Mo2^ix	2.6382 (5)
Mo2—Mo3	2.7397 (7)
Mo2—Mo3^viii	2.7901 (7)
Mo2—Se1ⁱ	2.6597 (6)
Mo2—Se2	2.6034 (9)
Mo2—Se2^ix	2.6124 (10)
Mo2—Se3	2.6721 (6)
Mo2—Se5	2.5129 (8)
Mo3—Mo3^ix	2.6780 (7)
Mo3—Mo3^xiv	2.6796 (6)
Mo3—Se2^ix	2.5634 (8)
Mo3—Se3	2.6090 (6)
Mo3—Se3^ix	2.6112 (6)
Mo3—Se3^xiv	2.7025 (8)
Symmetry codes: (i) $[-x+{\script{1\over 3}}, -y+{\script{2\over 3}}, -z+{\script{2\over 3}}]$ ; (ii) -y+1, x-y+1, z; (iii) -x+y, -x+1, z; (iv) -x+1, -y+1, -z+1; (v) y, -x+y+1, -z+1; (vi) x-y, x, -z+1; (vii) -x, -y+1, -z+1; (viii) -y, x-y, z; (ix) -x+y, -x, z; (x) $[y-{\script{2\over 3}}, -x+y-{\script{1\over 3}}, -z+{\script{2\over 3}}]$ ; (xi) $[x-y+{\script{1\over 3}}, x-{\script{1\over 3}}, -z+{\script{2\over 3}}]$ ; (xii) -x+y-1, -x, z; (xiii) $[x-y+{\script{1\over 3}}, x+{\script{2\over 3}}, -z+{\script{2\over 3}}]$ ; (xiv) y, -x+y, -z+1.

Data collection: COLLECT (Nonius, 1998 ); cell refinement: COLLECT; data reduction: EVALCCD (Duisenberg et al., 2003 ); program(s) used to solve structure: SIR97 (Altomare et al., 1999 ); program(s) used to refine structure: JANA2006 (Petříček et al., 2006 ); molecular graphics: DIAMOND (Brandenburg, 2001 ); software used to prepare material for publication: JANA2006.

Supporting information

Crystal structure: contains datablocks global, I. DOI: https://doi.org/10.1107/S1600536810026541/wm2368sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536810026541/wm2368Isup2.hkl

checkCIF report

Comment top

Potel et al. (1980) reported the crystal structure of Tl₂Mo₉S₁₁ that was the first compound containing a transition metal cluster with a nuclearity higher than 9, namely the trioctahedral Mo₁₂ cluster. The latter cluster, which results from the uniaxial face-sharing of three Mo₆ octahedra, coexists with the octahedral Mo₆ cluster in equal proportion. We present here the crystal structure of the isotypic selenide, Tl₂Mo₉Se₁₁.

The Mo—Se framework of Tl₂Mo₉Se₁₁ consists of an equal mixture of Mo₆Seⁱ₈Se^a₆ and Mo₁₂Seⁱ₁₄Se^a₆ cluster units interconnected through Mo—Se bonds (Fig.1 and 2). Details of the i- and a-type ligand notation were reported by Schäfer & von Schnering (1964). The first unit can be described as an Mo₆ octahedron surrounded by 8 face-capping inner Seⁱ and 6 apical Se^a ligands. The Mo₁₂ core of the second unit results from the face sharing of 3 octahedral Mo₆ clusters. The Mo₁₂ cluster is surrounded by 14 Seⁱ atoms capping the faces of the bioctahedron and 6 apical Se^a ligands above the ending Mo atoms. The Mo₆Seⁱ₈Se^a₆ and Mo₁₂Seⁱ₁₄Se^a₆ units are centered at 3a and 3b positions and have point-group symmetry 3. The Mo—Mo distances within the Mo₆ clusters are 2.6897 (7) Å for the intra-triangle distances (distances within the Mo₃ triangles formed by the Mo1 atoms related through the threefold axis) and 2.7609 (6) Å for the inter-triangle distances. In the sulfide, the two later values are slightly larger, viz. 2.693 (1) and 2.780 (5) Å. The Mo—Mo distances within the Mo₁₂ clusters are 2.6382 (5) and 2.6780 (7) Å for the distances in the triangles formed by the Mo2 and Mo3 atoms, respectively. In Tl₂Mo₉S₁₁, the corresponding distances are equal to 2.658 (1) and 2.688 (1) Å, respectively. The distances between the triangles formed by the Mo2 and Mo3 atoms are 2.7397 (7) and 2.7901 (7) Å and those between the Mo3₃ triangles, 2.6796 (6) Å. The average Mo—Mo distance within the Mo₁₂ cluster is similar in Tl₂Mo₉S₁₁ and Tl₂Mo₉Se₁₁ and amounts to 2.705 Å. The Se atoms bridge either one (Se1, Se2, Se4 and Se5) or two (Se3) Mo triangular faces of the clusters. Moreover, the Se1 and Se2 atoms are linked to a Mo atom of a neighboring cluster. The Mo—Se bond distances range from 2.5269 (8) to 2.6247 (8) Å within the Mo₆Seⁱ₈Se^a₆ unit and from 2.5129 (8) to 2.7025 (8) Å within the Mo₁₂Seⁱ₁₄Se^a₆ ubit. Each Mo₁₂Seⁱ₁₄Se^a₆ unit is interconnected to 6 Mo₆Seⁱ₈Se^a₆ units (and vice versa) via Mo2—Se1 bonds (respectively Mo1—Se2) to form the three-dimensional Mo—Se framework, the overall connectivity formula of which is Mo₁₂Seⁱ₈Se^i-a_6/2Se^a-i_6/2, Mo₆Seⁱ₂Se^i-a_6/2Se^a-i_6/2. It results from this arrangement that the shortest intercluster Mo1—Mo2 distance between the Mo₆ and Mo₁₂ clusters is 3.4239 (8) Å compared to 3.217 (1) in Tl₂Mo₉S₁₁, indicating only weak metal-metal interaction. The Tl atoms occupy large voids delimited by four Mo₆Seⁱ₈Se^a₆ units and four Mo₁₂Seⁱ₁₄Se^a₆ units. The Tl1 and Tl2 cations have a very similar environment which consists of seven Se atoms as nearest neighbors with Tl—Se distances in the ranges 3.0737 (10) - 3.5840 (6) Å and 3.0483 (9) - 3.4032 (6) Å for the Tl1 and Tl2 sites, respectively. These seven Se atoms form a monocapped octahedron compressed along the threefold axis. Three additional Se atoms at 4.3543 (6) and 4.2446 (6) Å from Tl1 and Tl2, respectively, are also observed (Figure 3). The average Tl—Se values are 3.72 and 3.54 Å for the Tl1 and Tl2 sites, respectively. Values of 3.57 and 3.68 Å are expected from the sum of the ionic radii for Se^2- and Tl⁺ for coordination numbers 8 and 12 (Shannon, 1976).

Related literature top

For the crystal structure of Tl₂Mo₉S₁₁, see: Potel et al. (1980). For details of the i- and a-type ligand notation, see: Schäfer & von Schnering (1964). Ionic radii were compiled by Shannon (1976). For background to the extinction correction, see: Becker & Coppens (1974).

Experimental top

Single crystals of Tl₂Mo₉Se₁₁ were prepared from a mixture of MoSe₂, TlSe and Mo with the nominal composition Tl₂Mo₁₂Se₁₄. Before use, Mo powder was reduced under H₂ flowing gas at 1273 K during ten hours in order to eliminate any trace of oxygen. The binaries MoSe₂ and TlSe were obtained by heating stoichiometric mixtures of the elements in sealed evacuated silica tubes during about 2 days at 1073 and 573 K, respectively. All handlings of materials were done in an argon-filled glove box. The initial mixture (ca 5 g) was cold pressed and loaded into a molybdenum crucible, which was sealed under a low argon pressure using an arc welding system. The charge was heated at the rate of 300 K/h up to 1773 K, the temperature which was held for 48 h, then cooled at 100 K/h down to 1373 K and finally furnace cooled.

Structure description top

For the crystal structure of Tl₂Mo₉S₁₁, see: Potel et al. (1980). For details of the i- and a-type ligand notation, see: Schäfer & von Schnering (1964). Ionic radii were compiled by Shannon (1976). For background to the extinction correction, see: Becker & Coppens (1974).

Computing details top

Data collection: COLLECT (Nonius, 1998); cell refinement: COLLECT (Nonius, 1998); data reduction: EVALCCD (Duisenberg et al., 2003); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: JANA2006 (Petříček et al., 2006); molecular graphics: DIAMOND (Brandenburg, 2001); software used to prepare material for publication: JANA2006 (Petříček et al., 2006).

Figures top

	Fig. 1. : View of Tl₂Mo₉Se₁₁ along [110].
	Fig. 2. : Plot showing the atom-numbering scheme and the linkage of the Mo₁₂Se₁₄Se₆ and Mo₆Se₈Se₆ cluster units. Displacement ellipsoids are drawn at the 97% probability level. Symmetry codes are as in Table 1.
	Fig. 3. : Environment of the Tl atoms. Symmetry codes are as in Table 1.

dithallium nonamolybdenum undecaselenide top

Crystal data top

Tl₂Mo₉Se₁₁	D_x = 7.321 Mg m⁻³
M_r = 2140.8	Mo Kα radiation, λ = 0.71069 Å
Trigonal, R3	Cell parameters from 10017 reflections
Hall symbol: -R 3	θ = 1–40.3°
a = 9.6212 (1) Å	µ = 42.73 mm⁻¹
c = 36.3316 (7) Å	T = 293 K
V = 2912.55 (7) Å³	Irregular block, black
Z = 6	0.13 × 0.12 × 0.11 mm
F(000) = 5484

Data collection top

Nonius KappaCCD diffractometer	4097 independent reflections
Radiation source: fine-focus sealed tube	3156 reflections with I > 2σ(I)
Horizontally mounted graphite crystal monochromator	R_int = 0.087
Detector resolution: 9 pixels mm^-1	θ_max = 40.2°, θ_min = 1.7°
φ– and ω–scans	h = −16→17
Absorption correction: multi-scan (PLATON; Spek, 2009)	k = −16→17
T_min = 0.033, T_max = 0.108	l = −58→66
21097 measured reflections

Refinement top

Refinement on F²	0 constraints
R[F > 3σ(F)] = 0.043	Weighting scheme based on measured s.u.'s w = 1/[σ²(I) + 0.0004I²]
wR(F) = 0.092	(Δ/σ)_max = 0.033
S = 1.37	Δρ_max = 3.92 e Å⁻³
4097 reflections	Δρ_min = −2.89 e Å⁻³
69 parameters	Extinction correction: B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)
0 restraints	Extinction coefficient: 2320 (40)

Crystal data top

Tl₂Mo₉Se₁₁	Z = 6
M_r = 2140.8	Mo Kα radiation
Trigonal, R3	µ = 42.73 mm⁻¹
a = 9.6212 (1) Å	T = 293 K
c = 36.3316 (7) Å	0.13 × 0.12 × 0.11 mm
V = 2912.55 (7) Å³

Data collection top

Nonius KappaCCD diffractometer	4097 independent reflections
Absorption correction: multi-scan (PLATON; Spek, 2009)	3156 reflections with I > 2σ(I)
T_min = 0.033, T_max = 0.108	R_int = 0.087
21097 measured reflections

Refinement top

R[F > 3σ(F)] = 0.043	69 parameters
wR(F) = 0.092	0 restraints
S = 1.37	Δρ_max = 3.92 e Å⁻³
4097 reflections	Δρ_min = −2.89 e Å⁻³

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

	x	y	z	U_iso*/U_eq
Tl1	0.333333	0.666667	0.495781 (14)	0.04933 (17)
Tl2	0	0	0.267672 (12)	0.02611 (11)
Mo1	−0.18022 (5)	0.31787 (5)	0.364749 (12)	0.01129 (13)
Mo2	0.16529 (5)	0.15027 (5)	0.406587 (12)	0.01120 (13)
Mo3	0.15606 (5)	−0.00891 (5)	0.469882 (12)	0.01087 (13)
Se1	−0.04118 (6)	0.29911 (6)	0.306626 (15)	0.01295 (17)
Se2	0.03067 (6)	0.32633 (6)	0.411871 (15)	0.01342 (17)
Se3	0.32150 (6)	0.30388 (6)	0.467628 (15)	0.01463 (17)
Se4	−0.333333	0.333333	0.41962 (2)	0.01559 (19)
Se5	0	0	0.35157 (2)	0.01474 (19)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Tl1	0.0620 (2)	0.0620 (2)	0.0239 (2)	0.03102 (12)	0	0
Tl2	0.02704 (13)	0.02704 (13)	0.0242 (2)	0.01352 (7)	0	0
Mo1	0.01119 (17)	0.01064 (17)	0.01168 (17)	0.00518 (13)	0.00061 (13)	−0.00028 (13)
Mo2	0.01129 (17)	0.01096 (17)	0.01107 (17)	0.00535 (14)	0.00023 (13)	0.00051 (13)
Mo3	0.01081 (16)	0.01111 (16)	0.01077 (17)	0.00553 (13)	0.00040 (13)	0.00014 (13)
Se1	0.0120 (2)	0.0136 (2)	0.0140 (2)	0.00691 (17)	0.00193 (16)	0.00090 (16)
Se2	0.0145 (2)	0.0121 (2)	0.0140 (2)	0.00685 (17)	−0.00087 (17)	0.00125 (16)
Se3	0.0121 (2)	0.0135 (2)	0.0151 (2)	0.00408 (17)	0.00057 (17)	0.00032 (17)
Se4	0.0181 (2)	0.0181 (2)	0.0106 (3)	0.00905 (12)	0	0
Se5	0.0167 (2)	0.0167 (2)	0.0108 (3)	0.00835 (11)	0	0

Geometric parameters (Å, º) top

Tl1—Tl2ⁱ	3.5164 (7)	Mo1—Mo1^xiv	2.7609 (7)
Tl1—Se2	4.3543 (6)	Mo1—Mo2^viii	3.4239 (8)
Tl1—Se2ⁱⁱ	4.3543 (7)	Mo1—Se1	2.5540 (8)
Tl1—Se2ⁱⁱⁱ	4.3543 (7)	Mo1—Se1^x	2.6143 (8)
Tl1—Se3	3.5840 (6)	Mo1—Se1^xiv	2.5757 (6)
Tl1—Se3ⁱⁱ	3.5840 (5)	Mo1—Se2	2.6247 (8)
Tl1—Se3ⁱⁱⁱ	3.5840 (8)	Mo1—Se4	2.5269 (8)
Tl1—Se3^iv	3.4547 (6)	Mo2—Mo2^viii	2.6382 (6)
Tl1—Se3^v	3.4547 (8)	Mo2—Mo2^ix	2.6382 (5)
Tl1—Se3^vi	3.4547 (5)	Mo2—Mo3	2.7397 (7)
Tl1—Se4^vii	3.0737 (10)	Mo2—Mo3^viii	2.7901 (7)
Tl2—Se1	3.4032 (7)	Mo2—Se1ⁱ	2.6597 (6)
Tl2—Se1^viii	3.4032 (6)	Mo2—Se2	2.6034 (9)
Tl2—Se1^ix	3.4032 (8)	Mo2—Se2^ix	2.6124 (10)
Tl2—Se2ⁱ	3.1441 (4)	Mo2—Se3	2.6721 (6)
Tl2—Se2^x	3.1441 (7)	Mo2—Se5	2.5129 (8)
Tl2—Se2^xi	3.1441 (7)	Mo3—Mo3^viii	2.6780 (9)
Tl2—Se3ⁱ	4.2446 (7)	Mo3—Mo3^ix	2.6780 (7)
Tl2—Se3^x	4.2446 (6)	Mo3—Mo3^xv	2.6796 (6)
Tl2—Se3^xi	4.2446 (8)	Mo3—Mo3^vi	2.6796 (7)
Tl2—Se5	3.0483 (9)	Mo3—Se2^ix	2.5634 (8)
Mo1—Mo1^xii	2.6897 (9)	Mo3—Se3	2.6090 (6)
Mo1—Mo1^xiii	2.6897 (7)	Mo3—Se3^ix	2.6112 (6)
Mo1—Mo1^x	2.7609 (6)	Mo3—Se3^xv	2.7025 (8)

Mo1^xii—Mo1—Mo1^xiii	60.000 (18)	Mo2—Mo3—Mo3^ix	90.11 (2)
Mo1^xii—Mo1—Mo1^x	90	Mo2—Mo3—Mo3^xv	147.49 (3)
Mo1^xii—Mo1—Mo1^xiv	60.85 (2)	Mo2—Mo3—Mo3^vi	111.83 (2)
Mo1^xiii—Mo1—Mo1^x	60.849 (16)	Mo2^ix—Mo3—Mo3^viii	89.04 (2)
Mo1^xiii—Mo1—Mo1^xiv	90	Mo2^ix—Mo3—Mo3^ix	60.094 (17)
Mo1^x—Mo1—Mo1^xiv	58.302 (17)	Mo2^ix—Mo3—Mo3^xv	110.275 (17)
Mo2^viii—Mo2—Mo2^ix	60.00 (2)	Mo2^ix—Mo3—Mo3^vi	145.90 (3)
Mo2^viii—Mo2—Mo3	90.953 (18)	Mo3^viii—Mo3—Mo3^ix	60.000 (18)
Mo2^viii—Mo2—Mo3^viii	60.546 (16)	Mo3^viii—Mo3—Mo3^xv	90
Mo2^ix—Mo2—Mo3	62.472 (16)	Mo3^viii—Mo3—Mo3^vi	60.02 (2)
Mo2^ix—Mo2—Mo3^viii	89.850 (19)	Mo3^ix—Mo3—Mo3^xv	60.019 (16)
Mo3—Mo2—Mo3^viii	57.92 (2)	Mo3^ix—Mo3—Mo3^vi	90
Mo2—Mo3—Mo2^ix	56.983 (15)	Mo3^xv—Mo3—Mo3^vi	59.962 (18)
Mo2—Mo3—Mo3^viii	61.982 (19)

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

Experimental details

Crystal data
Chemical formula	Tl₂Mo₉Se₁₁
M_r	2140.8
Crystal system, space group	Trigonal, R3
Temperature (K)	293
a, c (Å)	9.6212 (1), 36.3316 (7)
V (Å³)	2912.55 (7)
Z	6
Radiation type	Mo Kα
µ (mm⁻¹)	42.73
Crystal size (mm)	0.13 × 0.12 × 0.11

Data collection
Diffractometer	Nonius KappaCCD
Absorption correction	Multi-scan (PLATON; Spek, 2009)
T_min, T_max	0.033, 0.108
No. of measured, independent and observed [I > 2σ(I)] reflections	21097, 4097, 3156
R_int	0.087
(sin θ/λ)_max (Å⁻¹)	0.909

Refinement
R[F > 3σ(F)], wR(F), S	0.043, 0.092, 1.37
No. of reflections	4097
No. of parameters	69
Δρ_max, Δρ_min (e Å⁻³)	3.92, −2.89

Computer programs: COLLECT (Nonius, 1998), EVALCCD (Duisenberg et al., 2003), SIR97 (Altomare et al., 1999), JANA2006 (Petříček et al., 2006), DIAMOND (Brandenburg, 2001).

Selected bond lengths (Å) top

Tl1—Tl2ⁱ	3.5164 (7)	Mo1—Mo1^x	2.7609 (6)
Tl1—Se2	4.3543 (6)	Mo1—Mo2^viii	3.4239 (8)
Tl1—Se2ⁱⁱ	4.3543 (7)	Mo1—Se1	2.5540 (8)
Tl1—Se2ⁱⁱⁱ	4.3543 (7)	Mo1—Se1^x	2.6143 (8)
Tl1—Se3	3.5840 (6)	Mo1—Se1^xiii	2.5757 (6)
Tl1—Se3ⁱⁱ	3.5840 (5)	Mo1—Se2	2.6247 (8)
Tl1—Se3ⁱⁱⁱ	3.5840 (8)	Mo1—Se4	2.5269 (8)
Tl1—Se3^iv	3.4547 (6)	Mo2—Mo2^ix	2.6382 (5)
Tl1—Se3^v	3.4547 (8)	Mo2—Mo3	2.7397 (7)
Tl1—Se3^vi	3.4547 (5)	Mo2—Mo3^viii	2.7901 (7)
Tl1—Se4^vii	3.0737 (10)	Mo2—Se1ⁱ	2.6597 (6)
Tl2—Se1	3.4032 (7)	Mo2—Se2	2.6034 (9)
Tl2—Se1^viii	3.4032 (6)	Mo2—Se2^ix	2.6124 (10)
Tl2—Se1^ix	3.4032 (8)	Mo2—Se3	2.6721 (6)
Tl2—Se2ⁱ	3.1441 (4)	Mo2—Se5	2.5129 (8)
Tl2—Se2^x	3.1441 (7)	Mo3—Mo3^ix	2.6780 (7)
Tl2—Se2^xi	3.1441 (7)	Mo3—Mo3^xiv	2.6796 (6)
Tl2—Se3ⁱ	4.2446 (7)	Mo3—Se2^ix	2.5634 (8)
Tl2—Se3^x	4.2446 (6)	Mo3—Se3	2.6090 (6)
Tl2—Se3^xi	4.2446 (8)	Mo3—Se3^ix	2.6112 (6)
Tl2—Se5	3.0483 (9)	Mo3—Se3^xiv	2.7025 (8)
Mo1—Mo1^xii	2.6897 (7)

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

Acknowledgements

Intensity data were collected at the `Centre de diffractométrie de l'Université de Rennes I' (www.cdifx.univ-rennes1.fr).

References

Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115–119. Web of Science CrossRef CAS IUCr Journals Google Scholar
Becker, P. J. & Coppens, P. (1974). Acta Cryst. A30, 129–147. CrossRef IUCr Journals Web of Science Google Scholar
Brandenburg, K. (2001). DIAMOND. Crystal Impact GbR, Bonn, Germany. Google Scholar
Duisenberg, A. J. M., Kroon-Batenburg, L. M. J. & Schreurs, A. M. M. (2003). J. Appl. Cryst. 36, 220–229. Web of Science CrossRef CAS IUCr Journals Google Scholar
Nonius (1998). COLLECT. Nonius BV, Delft, The Netherlands. Google Scholar
Petříček, V., Dušek, M. & Palatinus, L. (2006). JANA2006. Institute of Physics, Praha, Czech Republic. Google Scholar
Potel, M., Chevrel, R. & Sergent, M. (1980). Acta Cryst. B36, 1319–1322. CrossRef CAS IUCr Journals Web of Science Google Scholar
Schäfer, H. & von Schnering, H. G. (1964). Angew. Chem. 76, 833–845. Google Scholar
Shannon, R. D. (1976). Acta Cryst. A32, 751–767. CrossRef CAS IUCr Journals Web of Science Google Scholar
Spek, A. L. (2009). Acta Cryst. D65, 148–155. Web of Science CrossRef CAS IUCr Journals Google Scholar