Bis­(tri­phenyl­telluronium) hexa­chloro­tellurate

The title compound, (Ph₃Te)₂[TeCl₆] or 2C₁₈H₁₅Te⁺·TeCl₆²⁻, was obtained as yellow hexagonal crystals from the reaction of Ph₃TeCl with [(Ph₃PO)₂H]₂[Te₂Cl₁₀]. The structure consists of discrete octahedral [TeCl₆]²⁻ anions, with site symmetry , and trigonal pyramidal (Ph₃Te)⁺ cations, with site symmetry 3. The weak Te...Cl secondary bonds of 3.527 (1) Å between the cation and anion expand the TePh₃E coordination of the telluronium tellurium into a distorted TePh₃Cl₃E trigonal prism (E = electron lone pair).

Key indicators

• Single-crystal X-ray study
• T = 150 K
• Mean [sigma](C-C) = 0.007 Å
• R factor = 0.032
• wR factor = 0.083
• Data-to-parameter ratio = 17.3

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT432_ALERT_2_C Short Inter X...Y Contact  Te1    ..  Cl1     ..       3.53 Ang.
PLAT432_ALERT_2_C Short Inter X...Y Contact  Te1    ..  Cl1     ..       3.53 Ang.
PLAT432_ALERT_2_C Short Inter X...Y Contact  Te1    ..  Cl1     ..       3.53 Ang.

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   4 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   3 ALERT type 2 Indicator that the structure model may be wrong or deficient
   0 ALERT type 3 Indicator that the structure quality may be low
   0 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: COLLECT (Nonius, 1998); cell refinement: DENZO–SMN (Otwinowski & Minor, 1997); data reduction: DENZO–SMN; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Branderburg & Berndt, 1999); software used to prepare material for publication: WinGX (Farrugia, 1999).

Bis(triphenyltelluronium) hexachlorotellurate

Crystal data

2C18H15Te^+·Cl6Te^2^−	Dx = 1.900 Mg m^−3
Mr = 1058.10	Mo Kα radiation, λ = 0.71073 Å
Hexagonal, R3	Cell parameters from 1137 reflections
Hall symbol: -R 3	θ = 3.1–26.0°
a = 14.217 (2) Å	µ = 2.81 mm^−1
c = 15.852 (3) Å	T = 150 K
V = 2774.8 (8) Å^3	Block, yellow
Z = 3	0.25 × 0.20 × 0.18 mm
F(000) = 1512

Data collection

Bruker-Nonius KappaCCD diffractometer	1210 independent reflections
Radiation source: fine-focus sealed tube	1137 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.068
φ scans, and ω scans with κ offsets	θmax = 26.0°, θmin = 3.1°
Absorption correction: ψ scan (SHELXTL; Bruker, 2001)	h = −17→17
Tmin = 0.513, Tmax = 0.600	k = −17→17
14235 measured reflections	l = −19→19

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.032	H-atom parameters constrained
wR(F^2) = 0.083	w = 1/[σ^2(Fo^2) + (0.0462P)^2 + 22.1387P] where P = (Fo^2 + 2Fc^2)/3
S = 1.10	(Δ/σ)max < 0.001
1210 reflections	Δρmax = 1.25 e Å^−3
70 parameters	Δρmin = −0.85 e Å^−3
0 restraints	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.00072 (16)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Te1	0.3333	0.6667	0.39175 (3)	0.0169 (2)
Te2	0.3333	0.6667	0.6667	0.0134 (2)
Cl1	0.24785 (9)	0.49939 (8)	0.76098 (6)	0.0237 (3)
C1	0.2171 (3)	0.5268 (3)	0.3257 (2)	0.0177 (8)
C2	0.1097 (3)	0.4807 (3)	0.3509 (3)	0.0230 (8)
H2	0.0898	0.5119	0.3956	0.028*
C3	0.0312 (3)	0.3878 (4)	0.3096 (3)	0.0262 (9)
H3	−0.0429	0.3557	0.3257	0.031*
C4	0.0612 (4)	0.3423 (3)	0.2451 (3)	0.0243 (9)
H4	0.0073	0.2792	0.2170	0.029*
C5	0.1683 (4)	0.3875 (3)	0.2215 (3)	0.0235 (8)
H5	0.1881	0.3546	0.1782	0.028*
C6	0.2479 (3)	0.4817 (3)	0.2609 (3)	0.0218 (8)
H6	0.3217	0.5144	0.2439	0.026*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Te1	0.0182 (2)	0.0182 (2)	0.0143 (3)	0.00909 (11)	0.000	0.000
Te2	0.0145 (2)	0.0145 (2)	0.0114 (3)	0.00724 (12)	0.000	0.000
Cl1	0.0299 (5)	0.0170 (5)	0.0191 (5)	0.0078 (4)	0.0012 (4)	0.0016 (3)
C1	0.0187 (18)	0.0160 (18)	0.0165 (18)	0.0072 (15)	−0.0007 (14)	0.0013 (14)
C2	0.022 (2)	0.024 (2)	0.025 (2)	0.0128 (17)	0.0033 (16)	−0.0031 (16)
C3	0.020 (2)	0.024 (2)	0.033 (2)	0.0091 (17)	0.0029 (17)	0.0017 (17)
C4	0.029 (2)	0.0190 (19)	0.024 (2)	0.0111 (17)	−0.0032 (17)	−0.0008 (16)
C5	0.030 (2)	0.022 (2)	0.0193 (19)	0.0142 (18)	0.0004 (16)	−0.0014 (16)
C6	0.0191 (19)	0.021 (2)	0.024 (2)	0.0094 (16)	0.0034 (15)	−0.0005 (16)

Geometric parameters (Å, º)

Te1—C1^i	2.120 (4)	C1—C6	1.392 (6)
Te1—C1	2.120 (4)	C2—C3	1.394 (6)
Te1—C1^ii	2.120 (4)	C2—H2	0.9500
Te2—Cl1^i	2.5451 (10)	C3—C4	1.387 (6)
Te2—Cl1^iii	2.5451 (10)	C3—H3	0.9500
Te2—Cl1^iv	2.5451 (10)	C4—C5	1.375 (6)
Te2—Cl1^ii	2.5451 (10)	C4—H4	0.9500
Te2—Cl1	2.5451 (10)	C5—C6	1.396 (6)
Te2—Cl1^v	2.5451 (10)	C5—H5	0.9500
C1—C2	1.386 (6)	C6—H6	0.9500
C1^i—Te1—C1	97.72 (13)	C2—C1—C6	121.4 (4)
C1^i—Te1—C1^ii	97.72 (13)	C2—C1—Te1	117.3 (3)
C1—Te1—C1^ii	97.72 (13)	C6—C1—Te1	121.3 (3)
Cl1^i—Te2—Cl1^iii	91.01 (3)	C1—C2—C3	118.9 (4)
Cl1^i—Te2—Cl1^iv	91.01 (3)	C1—C2—H2	120.5
Cl1^iii—Te2—Cl1^iv	88.99 (3)	C3—C2—H2	120.5
Cl1^i—Te2—Cl1^ii	88.99 (3)	C4—C3—C2	120.1 (4)
Cl1^iii—Te2—Cl1^ii	180.0	C4—C3—H3	120.0
Cl1^iv—Te2—Cl1^ii	91.01 (3)	C2—C3—H3	120.0
Cl1^i—Te2—Cl1	88.99 (3)	C5—C4—C3	120.6 (4)
Cl1^iii—Te2—Cl1	91.01 (3)	C5—C4—H4	119.7
Cl1^iv—Te2—Cl1	180.0	C3—C4—H4	119.7
Cl1^ii—Te2—Cl1	88.99 (3)	C4—C5—C6	120.3 (4)
Cl1^i—Te2—Cl1^v	180.00 (3)	C4—C5—H5	119.9
Cl1^iii—Te2—Cl1^v	88.99 (3)	C6—C5—H5	119.9
Cl1^iv—Te2—Cl1^v	88.99 (3)	C1—C6—C5	118.7 (4)
Cl1^ii—Te2—Cl1^v	91.01 (3)	C1—C6—H6	120.6
Cl1—Te2—Cl1^v	91.01 (3)	C5—C6—H6	120.6
C1^i—Te1—C1—C2	−82.3 (4)	C1—C2—C3—C4	0.7 (6)
C1^ii—Te1—C1—C2	178.7 (3)	C2—C3—C4—C5	0.4 (6)
C1^i—Te1—C1—C6	99.1 (2)	C3—C4—C5—C6	−1.6 (6)
C1^ii—Te1—C1—C6	0.2 (4)	C2—C1—C6—C5	−0.6 (6)
C6—C1—C2—C3	−0.6 (6)	Te1—C1—C6—C5	177.9 (3)
Te1—C1—C2—C3	−179.2 (3)	C4—C5—C6—C1	1.7 (6)

Symmetry codes: (i) −x+y, −x+1, z; (ii) −y+1, x−y+1, z; (iii) y−1/3, −x+y+1/3, −z+4/3; (iv) −x+2/3, −y+4/3, −z+4/3; (v) x−y+2/3, x+1/3, −z+4/3.