Bis(tetra­phenyl­phospho­nium) di-μ-iodido-bis[di­iodido­tellurate(II)]

Närhi, S.M.; Oilunkaniemi, R.; Laitinen, R.S.

doi:10.1107/S1600536808035927

metal-organic compounds

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ISSN: 2056-9890

Volume 64| Part 12| December 2008| Page m1561

doi:10.1107/S1600536808035927

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Bis(tetraphenylphosphonium) di-μ-iodido-bis[diiodidotellurate(II)]

Sari M. Närhi,^a Raija Oilunkaniemi ^a ^* and Risto S. Laitinen ^a

^aDepartment of Chemistry, P.O. Box 3000, FI-90014 University of Oulu, Finland
^*Correspondence e-mail: raija.oilunkaniemi@oulu.fi

(Received 31 October 2008; accepted 1 November 2008; online 20 November 2008)

The structure of the title compound, (C₂₄H₂₀P)₂[Te₂I₆], is composed of discrete PPh₄⁺ cations and centrosymmetric [Te₂I₆]²⁻ anions. The tellurium(II) atom shows a sligthly distorted square-planar TeI₄ geometry and is coordinated to two bridging and two terminal iodine atoms. The planar [Te₂I₆]²⁻ ions are isolated by the cations and no intermolecular tellurium–halogen or halogen–halogen interactions are present.

Related literature

For a review of halidotellurate anions, see Krebs & Ahlers (1990 ). For the structure of the [Te₂I₆]²⁻ anion, see: Konu & Chivers (2006 ); Fujiwara et al. (2002 ). For related materials, see: Janickis et al. (2002 , 2003 ).

Experimental

Crystal data

(C₂₄H₂₀P)₂[Te₂I₆]
M_r = 1695.34
Monoclinic, P 2₁ /n
a = 13.252 (3) Å
b = 14.494 (3) Å
c = 14.109 (3) Å
β = 107.48 (3)°
V = 2584.8 (9) Å³
Z = 2
Mo Kα radiation
μ = 4.80 mm⁻¹
T = 100 (2) K
0.15 × 0.15 × 0.10 mm

Data collection

Bruker–Nonius KappaCCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ) T_min = 0.511, T_max = 0.619
23569 measured reflections
5009 independent reflections
4225 reflections with I > 2σ(I)
R_int = 0.103

Refinement

R[F² > 2σ(F²)] = 0.041
wR(F²) = 0.107
S = 1.02
5009 reflections
263 parameters
H-atom parameters constrained
Δρ_max = 1.08 e Å⁻³
Δρ_min = −1.03 e Å⁻³

Table 1
Selected bond lengths (Å)

Te1—I2	2.8103 (8)
Te1—I1	2.8590 (8)
Te1—I3	3.0676 (8)
Te1—I3ⁱ	3.2244 (8)
Symmetry code: (i) -x+1, -y+1, -z+1.

Data collection: COLLECT (Nonius, 1998 ); cell refinement: DENZO-SMN (Otwinowski & Minor, 1997 ); data reduction: DENZO-SMN; program(s) used to solve structure: SIR92 (Altomare et al., 1993 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ); molecular graphics: DIAMOND (Brandenburg & Berndt, 2008 ); software used to prepare material for publication: WinGX (Farrugia, 1999 ).

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808035927/hb2834sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808035927/hb2834Isup2.hkl

checkCIF report

Comment top

The asymmetric unit of the title compound, (I), [PPh₄]₂[Te₂I₆], consists of one tetraphenylphosphonium cation and half of the anion (Fig. 1). The tellurium atoms show a distorted square planar coordination geometry and are coordinated to two bridging and two terminal iodine atoms (Table 1). The terminal Te—I bond lengths of 2.8103 (8) Å and 2.8590 (8) Å as well as the bridging Te—I bond lengths of 3.0676 (8) Å and 3.2244 (8) Å can be compared to the corresponding Te—I bonds in [(Et₃PO)₂H]₂[Te₂I₆] (Konu & Chivers, 2006) and (C₁₀H₈S₈)₂[Te₂I₆].3(C₁₀H₈S₈) (Fujiwara et al. 2002). In [(Et₃PO)₂H]₂[Te₂I₆] and (C₁₀H₈S₈)₂[Te₂I₆].3(C₁₀H₈S₈) the anions are involved in interionic I···I interactions shorter than the van der Waals radii of two iodine atoms, whereas in the present compound intermolecular iodine-iodine contacts are absent. The planar [Te₂I₆]^2- ions are isolated by the cations as shown in Fig. 2.

The present salt was obtained from the reaction mixture of PPh₄Cl, KI, Te, TeI₄, and I₂ in acetonitrile. Corresponding reactions with selenium, tellurium and bromine containing starting materials have yielded interesting mixed-valence bromidotellurate(IV)-selenate(II) and -selenate(I) anions [for illustrative examples, see Janickis et al. (2002, 2003)].

Related literature top

For a review of halidotellurate anions, see Krebs & Ahlers (1990). For the structure of the [Te₂I₆]^2- anion, see: Konu & Chivers (2006); Fujiwara et al. (2002). For related materials, see: Janickis et al. (2002, 2003).

Experimental top

The mixture of PPh₄Cl (0.3750 g, 1.00 mmol), KI (0.2 g, 1 mmol), Te (0.1452 g, 1.14 mmol), TeI₄ (0.3172 g, 0.50 mmol), and I₂ (0.1274 g, 0.50 mmol) in 15 ml acetonitrile gave a grey precipitate and a dark red solution after refluxing 2 h. A mixture of crystals of (I) and PPh₄I₃ was isolated from the filtrate after subsequent concentration of the solution.

Computing details top

Data collection: COLLECT (Nonius, 1998); cell refinement: DENZO-SMN (Otwinowski & Minor, 1997); data reduction: DENZO-SMN (Otwinowski & Minor, 1997); program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg & Berndt, 2008); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figures top

	Fig. 1. The molecular structure of (I) showing displacement ellipsoids drawn at 50% probability (arbitrary spheres for the H atoms). The unlabelled atoms are generated by the symmetry operation (1–x, 1–y, 1–z).
	Fig. 2. Space filling representations of the packing of the molecules.

Bis(tetraphenylphosphonium) di-µ-iodido-bis[diiodidotellurate(II)] top

Crystal data top

(C₂₄H₂₀P)₂[Te₂I₆]	F(000) = 1560
M_r = 1695.34	D_x = 2.178 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 4225 reflections
a = 13.252 (3) Å	θ = 3.0–26.0°
b = 14.494 (3) Å	µ = 4.81 mm⁻¹
c = 14.109 (3) Å	T = 100 K
β = 107.48 (3)°	Plate, brown
V = 2584.8 (9) Å³	0.15 × 0.15 × 0.10 mm
Z = 2

Data collection top

Bruker Nonius KappaCCD diffractometer	5009 independent reflections
Radiation source: fine-focus sealed tube	4225 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.103
ϕ scans, and ω scans with κ offsets	θ_max = 26.0°, θ_min = 3.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −16→16
T_min = 0.511, T_max = 0.619	k = −17→17
23569 measured reflections	l = −17→16

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.041	H-atom parameters constrained
wR(F²) = 0.107	w = 1/[σ²(F_o²) + (0.0555P)² + 5.4856P] where P = (F_o² + 2F_c²)/3
S = 1.03	(Δ/σ)_max = 0.001
5009 reflections	Δρ_max = 1.09 e Å⁻³
263 parameters	Δρ_min = −1.03 e Å⁻³
0 restraints	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.00320 (19)

Crystal data top

(C₂₄H₂₀P)₂[Te₂I₆]	V = 2584.8 (9) Å³
M_r = 1695.34	Z = 2
Monoclinic, P2₁/n	Mo Kα radiation
a = 13.252 (3) Å	µ = 4.81 mm⁻¹
b = 14.494 (3) Å	T = 100 K
c = 14.109 (3) Å	0.15 × 0.15 × 0.10 mm
β = 107.48 (3)°

Data collection top

Bruker Nonius KappaCCD diffractometer	5009 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	4225 reflections with I > 2σ(I)
T_min = 0.511, T_max = 0.619	R_int = 0.103
23569 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.041	0 restraints
wR(F²) = 0.107	H-atom parameters constrained
S = 1.03	Δρ_max = 1.09 e Å⁻³
5009 reflections	Δρ_min = −1.03 e Å⁻³
263 parameters

Special details top

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

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

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

	x	y	z	U_iso*/U_eq
Te1	0.39145 (3)	0.49167 (2)	0.59757 (3)	0.02321 (13)
I1	0.18308 (3)	0.56474 (3)	0.56278 (3)	0.02848 (14)
I2	0.39684 (3)	0.41640 (3)	0.78259 (3)	0.03878 (15)
I3	0.61278 (3)	0.41817 (3)	0.61252 (3)	0.02757 (13)
P1	0.32106 (11)	0.11106 (9)	0.54406 (10)	0.0195 (3)
C11	0.2712 (4)	−0.0042 (4)	0.5160 (4)	0.0229 (12)
C12	0.3382 (5)	−0.0802 (4)	0.5366 (5)	0.0270 (13)
H12	0.4121	−0.0718	0.5661	0.032*
C13	0.2973 (5)	−0.1679 (4)	0.5144 (4)	0.0316 (13)
H13	0.3432	−0.2198	0.5295	0.038*
C14	0.1894 (5)	−0.1807 (4)	0.4700 (4)	0.0330 (14)
H14	0.1613	−0.2411	0.4555	0.040*
C15	0.1229 (5)	−0.1046 (4)	0.4470 (5)	0.0304 (13)
H15	0.0496	−0.1133	0.4146	0.036*
C16	0.1620 (5)	−0.0163 (4)	0.4706 (4)	0.0268 (12)
H16	0.1157	0.0353	0.4564	0.032*
C21	0.4391 (4)	0.1058 (4)	0.6475 (4)	0.0216 (11)
C22	0.5306 (4)	0.1552 (4)	0.6471 (4)	0.0268 (12)
H22	0.5306	0.1916	0.5911	0.032*
C23	0.6208 (5)	0.1507 (4)	0.7286 (5)	0.0323 (14)
H23	0.6825	0.1841	0.7285	0.039*
C24	0.6208 (5)	0.0973 (4)	0.8100 (4)	0.0305 (13)
H24	0.6829	0.0934	0.8652	0.037*
C25	0.5306 (5)	0.0497 (4)	0.8112 (4)	0.0263 (12)
H25	0.5307	0.0144	0.8680	0.032*
C26	0.4407 (4)	0.0530 (4)	0.7304 (4)	0.0223 (11)
H26	0.3796	0.0191	0.7314	0.027*
C31	0.3505 (4)	0.1619 (4)	0.4396 (4)	0.0208 (11)
C32	0.3740 (4)	0.2572 (4)	0.4442 (4)	0.0233 (11)
H32	0.3701	0.2926	0.4996	0.028*
C33	0.4029 (4)	0.2990 (4)	0.3680 (4)	0.0268 (12)
H33	0.4193	0.3630	0.3711	0.032*
C34	0.4077 (4)	0.2469 (4)	0.2870 (4)	0.0266 (12)
H34	0.4288	0.2752	0.2353	0.032*
C35	0.3818 (4)	0.1534 (4)	0.2808 (4)	0.0267 (12)
H35	0.3834	0.1190	0.2240	0.032*
C36	0.3537 (4)	0.1101 (4)	0.3574 (4)	0.0247 (12)
H36	0.3370	0.0462	0.3536	0.030*
C41	0.2233 (4)	0.1829 (4)	0.5724 (4)	0.0221 (11)
C42	0.2246 (5)	0.1973 (4)	0.6707 (4)	0.0301 (13)
H42	0.2766	0.1680	0.7235	0.036*
C43	0.1496 (5)	0.2545 (4)	0.6908 (5)	0.0357 (15)
H43	0.1511	0.2652	0.7577	0.043*
C44	0.0728 (5)	0.2959 (4)	0.6140 (5)	0.0314 (14)
H44	0.0219	0.3353	0.6281	0.038*
C45	0.0702 (5)	0.2800 (4)	0.5171 (5)	0.0342 (14)
H45	0.0164	0.3078	0.4645	0.041*
C46	0.1445 (5)	0.2242 (4)	0.4954 (5)	0.0296 (13)
H46	0.1421	0.2139	0.4282	0.036*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Te1	0.0210 (2)	0.0221 (2)	0.0260 (2)	−0.00164 (14)	0.00639 (16)	−0.00285 (14)
I1	0.0232 (2)	0.0348 (2)	0.0277 (2)	0.00469 (15)	0.00807 (16)	−0.00166 (15)
I2	0.0337 (3)	0.0505 (3)	0.0295 (3)	−0.00871 (18)	0.00551 (19)	0.00788 (18)
I3	0.0228 (2)	0.0278 (2)	0.0317 (2)	0.00296 (14)	0.00762 (17)	0.00327 (15)
P1	0.0181 (7)	0.0196 (7)	0.0205 (7)	0.0006 (5)	0.0053 (5)	−0.0005 (5)
C11	0.026 (3)	0.027 (3)	0.018 (3)	−0.002 (2)	0.010 (2)	0.002 (2)
C12	0.020 (3)	0.029 (3)	0.032 (3)	0.002 (2)	0.008 (3)	−0.003 (2)
C13	0.033 (3)	0.033 (3)	0.028 (3)	0.007 (3)	0.008 (3)	0.004 (3)
C14	0.044 (4)	0.025 (3)	0.029 (3)	−0.009 (3)	0.010 (3)	0.000 (3)
C15	0.026 (3)	0.031 (3)	0.030 (3)	−0.004 (2)	0.003 (2)	−0.004 (3)
C16	0.026 (3)	0.022 (3)	0.029 (3)	−0.002 (2)	0.004 (2)	−0.002 (2)
C21	0.018 (3)	0.020 (3)	0.026 (3)	0.001 (2)	0.004 (2)	−0.003 (2)
C22	0.027 (3)	0.024 (3)	0.031 (3)	0.006 (2)	0.011 (2)	0.003 (2)
C23	0.024 (3)	0.035 (3)	0.036 (3)	−0.006 (2)	0.005 (3)	0.001 (3)
C24	0.026 (3)	0.035 (3)	0.024 (3)	0.007 (2)	−0.003 (2)	−0.003 (2)
C25	0.026 (3)	0.027 (3)	0.024 (3)	0.006 (2)	0.005 (2)	−0.002 (2)
C26	0.022 (3)	0.024 (3)	0.021 (3)	0.004 (2)	0.007 (2)	−0.003 (2)
C31	0.018 (3)	0.023 (3)	0.019 (3)	0.001 (2)	0.002 (2)	0.002 (2)
C32	0.024 (3)	0.022 (3)	0.023 (3)	−0.001 (2)	0.007 (2)	−0.004 (2)
C33	0.024 (3)	0.024 (3)	0.032 (3)	0.002 (2)	0.008 (2)	0.005 (2)
C34	0.021 (3)	0.035 (3)	0.026 (3)	0.004 (2)	0.009 (2)	0.011 (2)
C35	0.029 (3)	0.027 (3)	0.025 (3)	0.005 (2)	0.008 (2)	−0.002 (2)
C36	0.023 (3)	0.020 (3)	0.029 (3)	0.000 (2)	0.005 (2)	−0.002 (2)
C41	0.015 (3)	0.023 (3)	0.028 (3)	−0.001 (2)	0.007 (2)	0.001 (2)
C42	0.023 (3)	0.046 (4)	0.021 (3)	0.006 (3)	0.006 (2)	−0.002 (3)
C43	0.030 (3)	0.037 (4)	0.043 (4)	0.000 (3)	0.016 (3)	−0.009 (3)
C44	0.026 (3)	0.028 (3)	0.046 (4)	0.001 (2)	0.020 (3)	−0.003 (3)
C45	0.036 (3)	0.030 (3)	0.046 (4)	0.013 (3)	0.024 (3)	0.016 (3)
C46	0.026 (3)	0.037 (3)	0.029 (3)	0.000 (2)	0.013 (3)	0.004 (3)

Geometric parameters (Å, º) top

Te1—I2	2.8103 (8)	C24—H24	0.9500
Te1—I1	2.8590 (8)	C25—C26	1.380 (8)
Te1—I3	3.0676 (8)	C25—H25	0.9500
Te1—I3ⁱ	3.2244 (8)	C26—H26	0.9500
I3—Te1ⁱ	3.2244 (8)	C31—C36	1.393 (8)
P1—C31	1.792 (6)	C31—C32	1.414 (7)
P1—C21	1.793 (6)	C32—C33	1.385 (8)
P1—C11	1.796 (6)	C32—H32	0.9500
P1—C41	1.799 (5)	C33—C34	1.386 (8)
C11—C12	1.389 (8)	C33—H33	0.9500
C11—C16	1.407 (8)	C34—C35	1.395 (8)
C12—C13	1.381 (8)	C34—H34	0.9500
C12—H12	0.9500	C35—C36	1.394 (8)
C13—C14	1.391 (9)	C35—H35	0.9500
C13—H13	0.9500	C36—H36	0.9500
C14—C15	1.387 (9)	C41—C46	1.396 (8)
C14—H14	0.9500	C41—C42	1.397 (8)
C15—C16	1.383 (8)	C42—C43	1.387 (8)
C15—H15	0.9500	C42—H42	0.9500
C16—H16	0.9500	C43—C44	1.381 (9)
C21—C26	1.393 (8)	C43—H43	0.9500
C21—C22	1.410 (8)	C44—C45	1.377 (9)
C22—C23	1.390 (8)	C44—H44	0.9500
C22—H22	0.9500	C45—C46	1.378 (8)
C23—C24	1.383 (9)	C45—H45	0.9500
C23—H23	0.9500	C46—H46	0.9500
C24—C25	1.385 (9)

I2—Te1—I1	93.27 (3)	C26—C25—C24	120.5 (6)
I2—Te1—I3	92.54 (3)	C26—C25—H25	119.8
I1—Te1—I3	174.091 (17)	C24—C25—H25	119.8
I2—Te1—I3ⁱ	178.851 (17)	C25—C26—C21	120.2 (5)
I1—Te1—I3ⁱ	86.73 (3)	C25—C26—H26	119.9
I3—Te1—I3ⁱ	87.49 (3)	C21—C26—H26	119.9
Te1—I3—Te1ⁱ	92.51 (3)	C36—C31—C32	120.2 (5)
C31—P1—C21	109.5 (3)	C36—C31—P1	122.1 (4)
C31—P1—C11	110.9 (2)	C32—C31—P1	117.6 (4)
C21—P1—C11	108.2 (3)	C33—C32—C31	120.0 (5)
C31—P1—C41	107.1 (3)	C33—C32—H32	120.0
C21—P1—C41	110.8 (3)	C31—C32—H32	120.0
C11—P1—C41	110.2 (3)	C32—C33—C34	119.6 (5)
C12—C11—C16	120.1 (5)	C32—C33—H33	120.2
C12—C11—P1	121.5 (4)	C34—C33—H33	120.2
C16—C11—P1	118.5 (4)	C33—C34—C35	120.6 (5)
C13—C12—C11	120.1 (6)	C33—C34—H34	119.7
C13—C12—H12	120.0	C35—C34—H34	119.7
C11—C12—H12	120.0	C36—C35—C34	120.5 (5)
C12—C13—C14	120.3 (6)	C36—C35—H35	119.8
C12—C13—H13	119.9	C34—C35—H35	119.8
C14—C13—H13	119.9	C31—C36—C35	119.0 (5)
C15—C14—C13	119.7 (6)	C31—C36—H36	120.5
C15—C14—H14	120.2	C35—C36—H36	120.5
C13—C14—H14	120.2	C46—C41—C42	119.5 (5)
C16—C15—C14	120.9 (6)	C46—C41—P1	119.7 (4)
C16—C15—H15	119.6	C42—C41—P1	120.8 (4)
C14—C15—H15	119.6	C43—C42—C41	119.7 (6)
C15—C16—C11	119.0 (5)	C43—C42—H42	120.1
C15—C16—H16	120.5	C41—C42—H42	120.1
C11—C16—H16	120.5	C44—C43—C42	120.2 (6)
C26—C21—C22	119.2 (5)	C44—C43—H43	119.9
C26—C21—P1	119.7 (4)	C42—C43—H43	119.9
C22—C21—P1	121.1 (4)	C45—C44—C43	120.0 (6)
C23—C22—C21	119.9 (5)	C45—C44—H44	120.0
C23—C22—H22	120.0	C43—C44—H44	120.0
C21—C22—H22	120.0	C44—C45—C46	120.8 (6)
C24—C23—C22	119.9 (6)	C44—C45—H45	119.6
C24—C23—H23	120.1	C46—C45—H45	119.6
C22—C23—H23	120.1	C45—C46—C41	119.7 (6)
C23—C24—C25	120.3 (5)	C45—C46—H46	120.1
C23—C24—H24	119.9	C41—C46—H46	120.1
C25—C24—H24	119.9

I2—Te1—I3—Te1ⁱ	−178.850 (17)	P1—C21—C26—C25	−178.9 (4)
I3ⁱ—Te1—I3—Te1ⁱ	0.0	C21—P1—C31—C36	107.5 (5)
C31—P1—C11—C12	92.1 (5)	C11—P1—C31—C36	−12.0 (5)
C21—P1—C11—C12	−28.1 (6)	C41—P1—C31—C36	−132.3 (4)
C41—P1—C11—C12	−149.4 (5)	C21—P1—C31—C32	−70.6 (5)
C31—P1—C11—C16	−86.9 (5)	C11—P1—C31—C32	169.9 (4)
C21—P1—C11—C16	152.9 (4)	C41—P1—C31—C32	49.6 (5)
C41—P1—C11—C16	31.6 (5)	C36—C31—C32—C33	−1.6 (8)
C16—C11—C12—C13	−1.2 (9)	P1—C31—C32—C33	176.6 (4)
P1—C11—C12—C13	179.8 (5)	C31—C32—C33—C34	0.5 (8)
C11—C12—C13—C14	0.9 (9)	C32—C33—C34—C35	1.2 (8)
C12—C13—C14—C15	0.7 (9)	C33—C34—C35—C36	−1.9 (8)
C13—C14—C15—C16	−2.1 (9)	C32—C31—C36—C35	0.9 (8)
C14—C15—C16—C11	1.8 (9)	P1—C31—C36—C35	−177.1 (4)
C12—C11—C16—C15	−0.2 (9)	C34—C35—C36—C31	0.8 (8)
P1—C11—C16—C15	178.9 (5)	C31—P1—C41—C46	36.7 (5)
C31—P1—C21—C26	−167.4 (4)	C21—P1—C41—C46	156.1 (4)
C11—P1—C21—C26	−46.3 (5)	C11—P1—C41—C46	−84.1 (5)
C41—P1—C21—C26	74.7 (5)	C31—P1—C41—C42	−143.9 (5)
C31—P1—C21—C22	13.4 (5)	C21—P1—C41—C42	−24.5 (5)
C11—P1—C21—C22	134.5 (4)	C11—P1—C41—C42	95.3 (5)
C41—P1—C21—C22	−104.6 (5)	C46—C41—C42—C43	−1.9 (9)
C26—C21—C22—C23	0.2 (8)	P1—C41—C42—C43	178.7 (5)
P1—C21—C22—C23	179.4 (5)	C41—C42—C43—C44	1.1 (9)
C21—C22—C23—C24	0.2 (9)	C42—C43—C44—C45	0.4 (9)
C22—C23—C24—C25	−1.1 (9)	C43—C44—C45—C46	−1.1 (9)
C23—C24—C25—C26	1.6 (9)	C44—C45—C46—C41	0.3 (9)
C24—C25—C26—C21	−1.2 (8)	C42—C41—C46—C45	1.2 (9)
C22—C21—C26—C25	0.3 (8)	P1—C41—C46—C45	−179.4 (5)

Symmetry code: (i) −x+1, −y+1, −z+1.

Experimental details

Crystal data
Chemical formula	(C₂₄H₂₀P)₂[Te₂I₆]
M_r	1695.34
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	100
a, b, c (Å)	13.252 (3), 14.494 (3), 14.109 (3)
β (°)	107.48 (3)
V (Å³)	2584.8 (9)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	4.81
Crystal size (mm)	0.15 × 0.15 × 0.10

Data collection
Diffractometer	Bruker Nonius KappaCCD diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.511, 0.619
No. of measured, independent and observed [I > 2σ(I)] reflections	23569, 5009, 4225
R_int	0.103
(sin θ/λ)_max (Å⁻¹)	0.617

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.041, 0.107, 1.03
No. of reflections	5009
No. of parameters	263
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	1.09, −1.03

Computer programs: COLLECT (Nonius, 1998), DENZO-SMN (Otwinowski & Minor, 1997), SIR92 (Altomare et al., 1993), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg & Berndt, 2008), WinGX (Farrugia, 1999).

Selected bond lengths (Å) top

Te1—I2	2.8103 (8)	Te1—I3	3.0676 (8)
Te1—I1	2.8590 (8)	Te1—I3ⁱ	3.2244 (8)

Symmetry code: (i) −x+1, −y+1, −z+1.

Acknowledgements

Financial support from the Academy of Finland is gratefully acknowledged.

References

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