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The title compound, (Ph
3Te)
2[TeCl
6] or 2C
18H
15Te
+·TeCl
62−, was obtained as yellow hexagonal crystals from the reaction of Ph
3TeCl with [(Ph
3PO)
2H]
2[Te
2Cl
10]. The structure consists of discrete octahedral [TeCl
6]
2− anions, with site symmetry
, and trigonal pyramidal (Ph
3Te)
+ cations, with site symmetry 3. The weak Te
Cl secondary bonds of 3.527 (1) Å between the cation and anion expand the TePh
3E coordination of the telluronium tellurium into a distorted TePh
3Cl
3E trigonal prism (
E = electron lone pair).
Supporting information
CCDC reference: 239255
Key indicators
- Single-crystal X-ray study
- T = 150 K
- Mean (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
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
top
Crystal data top
2C18H15Te+·Cl6Te2− | 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) Å3 | Block, yellow |
Z = 3 | 0.25 × 0.20 × 0.18 mm |
F(000) = 1512 | |
Data collection top
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 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)] = 0.032 | H-atom parameters constrained |
wR(F2) = 0.083 | w = 1/[σ2(Fo2) + (0.0462P)2 + 22.1387P] where P = (Fo2 + 2Fc2)/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+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.00072 (16) |
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 | 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 (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
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) top
Te1—C1i | 2.120 (4) | C1—C6 | 1.392 (6) |
Te1—C1 | 2.120 (4) | C2—C3 | 1.394 (6) |
Te1—C1ii | 2.120 (4) | C2—H2 | 0.9500 |
Te2—Cl1i | 2.5451 (10) | C3—C4 | 1.387 (6) |
Te2—Cl1iii | 2.5451 (10) | C3—H3 | 0.9500 |
Te2—Cl1iv | 2.5451 (10) | C4—C5 | 1.375 (6) |
Te2—Cl1ii | 2.5451 (10) | C4—H4 | 0.9500 |
Te2—Cl1 | 2.5451 (10) | C5—C6 | 1.396 (6) |
Te2—Cl1v | 2.5451 (10) | C5—H5 | 0.9500 |
C1—C2 | 1.386 (6) | C6—H6 | 0.9500 |
| | | |
C1i—Te1—C1 | 97.72 (13) | C2—C1—C6 | 121.4 (4) |
C1i—Te1—C1ii | 97.72 (13) | C2—C1—Te1 | 117.3 (3) |
C1—Te1—C1ii | 97.72 (13) | C6—C1—Te1 | 121.3 (3) |
Cl1i—Te2—Cl1iii | 91.01 (3) | C1—C2—C3 | 118.9 (4) |
Cl1i—Te2—Cl1iv | 91.01 (3) | C1—C2—H2 | 120.5 |
Cl1iii—Te2—Cl1iv | 88.99 (3) | C3—C2—H2 | 120.5 |
Cl1i—Te2—Cl1ii | 88.99 (3) | C4—C3—C2 | 120.1 (4) |
Cl1iii—Te2—Cl1ii | 180.0 | C4—C3—H3 | 120.0 |
Cl1iv—Te2—Cl1ii | 91.01 (3) | C2—C3—H3 | 120.0 |
Cl1i—Te2—Cl1 | 88.99 (3) | C5—C4—C3 | 120.6 (4) |
Cl1iii—Te2—Cl1 | 91.01 (3) | C5—C4—H4 | 119.7 |
Cl1iv—Te2—Cl1 | 180.0 | C3—C4—H4 | 119.7 |
Cl1ii—Te2—Cl1 | 88.99 (3) | C4—C5—C6 | 120.3 (4) |
Cl1i—Te2—Cl1v | 180.00 (3) | C4—C5—H5 | 119.9 |
Cl1iii—Te2—Cl1v | 88.99 (3) | C6—C5—H5 | 119.9 |
Cl1iv—Te2—Cl1v | 88.99 (3) | C1—C6—C5 | 118.7 (4) |
Cl1ii—Te2—Cl1v | 91.01 (3) | C1—C6—H6 | 120.6 |
Cl1—Te2—Cl1v | 91.01 (3) | C5—C6—H6 | 120.6 |
| | | |
C1i—Te1—C1—C2 | −82.3 (4) | C1—C2—C3—C4 | 0.7 (6) |
C1ii—Te1—C1—C2 | 178.7 (3) | C2—C3—C4—C5 | 0.4 (6) |
C1i—Te1—C1—C6 | 99.1 (2) | C3—C4—C5—C6 | −1.6 (6) |
C1ii—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. |
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