Redetermination of Te6[AsF6]4·2SO2 at 125 K

Beck, J.; Steden, F.

doi:10.1107/S1600536803024887

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Redetermination of Te₆[AsF₆]₄·2SO₂ at 125 K

J. Beck and F. Steden

The crystal structure of the title compound, hexatellurium tetrakis(hexafluoroarsenate) sulfur dioxide disolvate, Te₆[AsF₆]₄·2SO₂, was first determined by Burns, Gillespie, Luk & Slim [Inorg. Chem. (1979), 18, 3086-3094]. We present here a redetermination at low temperature and of improved precision, in which all atoms were refined with anisotropic displacement parameters.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803024887/hb6000sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536803024887/hb6000Isup2.hkl Contains datablock I

checkCIF report

Key indicators

Single-crystal X-ray study
T = 125 K
Mean (S-O) = 0.005 Å
R factor = 0.029
wR factor = 0.077
Data-to-parameter ratio = 17.5

checkCIF/PLATON results

No syntax errors found



Alert level A
PLAT432_ALERT_2_A Short Inter X...Y Contact  Te1    ..  F41      =       2.99 Ang.
PLAT432_ALERT_2_A Short Inter X...Y Contact  Te1    ..  F33      =       3.00 Ang.
PLAT432_ALERT_2_A Short Inter X...Y Contact  Te1    ..  F22      =       3.01 Ang.
PLAT432_ALERT_2_A Short Inter X...Y Contact  Te3    ..  O22      =       2.94 Ang.
PLAT432_ALERT_2_A Short Inter X...Y Contact  Te4    ..  O21      =       3.06 Ang.
PLAT432_ALERT_2_A Short Inter X...Y Contact  Te5    ..  O11      =       2.94 Ang.
PLAT432_ALERT_2_A Short Inter X...Y Contact  Te5    ..  F44      =       2.95 Ang.

Alert level B
PLAT242_ALERT_2_B Check Low    U(eq) as Compared to Neighbors ....        As2
PLAT432_ALERT_2_B Short Inter X...Y Contact  Te2    ..  F15      =       3.10 Ang.
PLAT432_ALERT_2_B Short Inter X...Y Contact  Te2    ..  F23      =       3.13 Ang.
PLAT432_ALERT_2_B Short Inter X...Y Contact  Te2    ..  F12      =       3.22 Ang.
PLAT432_ALERT_2_B Short Inter X...Y Contact  Te3    ..  F16      =       3.10 Ang.
PLAT432_ALERT_2_B Short Inter X...Y Contact  Te3    ..  F14      =       3.15 Ang.
PLAT432_ALERT_2_B Short Inter X...Y Contact  Te3    ..  F25      =       3.20 Ang.
PLAT432_ALERT_2_B Short Inter X...Y Contact  Te4    ..  F11      =       3.05 Ang.
PLAT432_ALERT_2_B Short Inter X...Y Contact  Te4    ..  F13      =       3.11 Ang.
PLAT432_ALERT_2_B Short Inter X...Y Contact  Te4    ..  F42      =       3.11 Ang.
PLAT432_ALERT_2_B Short Inter X...Y Contact  Te5    ..  F36      =       3.07 Ang.
PLAT432_ALERT_2_B Short Inter X...Y Contact  Te5    ..  F14      =       3.13 Ang.
PLAT432_ALERT_2_B Short Inter X...Y Contact  Te5    ..  F46      =       3.20 Ang.

Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT155_ALERT_4_C The Triclinic Unitcell is NOT Reduced ..........          ?
PLAT213_ALERT_2_C Atom F46     has ADP max/min Ratio .............       3.70 prolat
PLAT242_ALERT_2_C Check Low    U(eq) as Compared to Neighbors ....        As3
PLAT242_ALERT_2_C Check Low    U(eq) as Compared to Neighbors ....        As4
PLAT250_ALERT_2_C Large U3/U1 ratio for average U(i,j) tensor ....       3.04
PLAT250_ALERT_2_C Large U3/U1 ratio for average U(i,j) tensor ....       2.81
PLAT250_ALERT_2_C Large U3/U1 ratio for average U(i,j) tensor ....       2.83
PLAT432_ALERT_2_C Short Inter X...Y Contact  Te1    ..  O12      =       3.30 Ang.
PLAT432_ALERT_2_C Short Inter X...Y Contact  Te4    ..  F25      =       3.25 Ang.
PLAT432_ALERT_2_C Short Inter X...Y Contact  Te4    ..  F23      =       3.28 Ang.
PLAT432_ALERT_2_C Short Inter X...Y Contact  Te6    ..  F43      =       3.26 Ang.
PLAT432_ALERT_2_C Short Inter X...Y Contact  Te6    ..  F45      =       3.30 Ang.
PLAT432_ALERT_2_C Short Inter X...Y Contact  Te6    ..  F36      =       3.30 Ang.
PLAT432_ALERT_2_C Short Inter X...Y Contact  Te6    ..  F32      =       3.32 Ang.

Alert level G
FORMU01_ALERT_1_G  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and _chemical_formula_moiety. This is
            usually due to the moiety formula being in the wrong format.
            Atom count from _chemical_formula_sum:   As4 F24 O4 S2 Te6
            Atom count from _chemical_formula_moiety:Te12

   7 ALERT level A = In general: serious problem
  13 ALERT level B = Potentially serious problem
  15 ALERT level C = Check and explain
   1 ALERT level G = General alerts; check

   2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
  33 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
   1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: COLLECT (Enraf-Nonius, 2000); cell refinement: COLLECT; data reduction: COLLECT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Berndt et al., 2001); software used to prepare material for publication: PARST (Narelli, 1983).

(I) top

Crystal data top

Te₆[AsF₆]₄·2SO₂	Z = 2
M_r = 1649.4	F(000) = 1448
Triclinic, P1	D_x = 3.962 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 9.9163 (1) Å	Cell parameters from 12374 reflections
b = 10.593 (1) Å	θ = 2.0–27.5°
c = 16.375 (1) Å	µ = 11.32 mm⁻¹
α = 106.92 (1)°	T = 125 K
β = 93.83 (1)°	Prismatic block, light brown
γ = 119.716 (2)°	0.30 × 0.20 × 0.20 mm
V = 1382.4 (2) Å³

Data collection top

Nonius KappaCCD diffractometer	6036 reflections with I > 2σ(I)
Horizonally mounted graphite crystal monochromator	R_int = 0.070
CCD scans	θ_max = 27.5°, θ_min = 4.4°
Absorption correction: numerical (HABITUS; Herrendorf & Bärnighausen, 1993)	h = −12→12
T_min = 0.083, T_max = 0.104	k = −13→13
12374 measured reflections	l = −21→21
6359 independent reflections

Refinement top

Refinement on F²	361 parameters
Least-squares matrix: full	0 restraints
R[F² > 2σ(F²)] = 0.029	w = 1/[σ²(F_o²) + (0.0389P)² + 6.4919P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.077	(Δ/σ)_max = 0.012
S = 1.14	Δρ_max = 1.25 e Å⁻³
6331 reflections	Δρ_min = −1.62 e Å⁻³

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.

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

	x	y	z	U_iso*/U_eq
Te1	0.95493 (4)	0.67415 (3)	0.21556 (2)	0.01444 (8)
Te2	0.88493 (4)	0.65252 (3)	0.39741 (2)	0.01259 (8)
Te3	0.71952 (4)	0.33649 (3)	0.32226 (2)	0.01230 (8)
Te4	0.56594 (4)	0.48652 (4)	0.32340 (2)	0.01277 (8)
Te5	0.78668 (4)	0.35883 (3)	0.14104 (2)	0.01317 (8)
Te6	0.63573 (4)	0.51193 (4)	0.14501 (2)	0.01553 (8)
As1	0.80916 (5)	0.51414 (6)	0.61586 (3)	0.01197 (10)
F11	0.6412 (3)	0.3782 (4)	0.6353 (2)	0.0199 (6)
F12	0.6925 (4)	0.5065 (5)	0.5304 (2)	0.0315 (8)
F13	0.7977 (4)	0.6607 (4)	0.6876 (2)	0.0265 (7)
F14	0.9286 (4)	0.5213 (4)	0.7012 (2)	0.0254 (7)
F15	0.8261 (4)	0.3704 (4)	0.5448 (2)	0.0286 (7)
F16	0.9810 (4)	0.6520 (4)	0.5975 (2)	0.0308 (8)
As2	0.27896 (6)	0.05439 (5)	0.41649 (3)	0.01496 (11)
F21	0.2587 (4)	−0.1111 (4)	0.3417 (2)	0.0340 (9)
F22	0.0930 (4)	−0.0081 (4)	0.3571 (3)	0.0387 (9)
F23	0.2905 (5)	0.2132 (4)	0.4901 (3)	0.0365 (9)
F24	0.1858 (7)	−0.0536 (5)	0.4787 (3)	0.0598 (15)
F25	0.3686 (5)	0.1581 (4)	0.3533 (3)	0.0477 (11)
F26	0.4594 (5)	0.1072 (5)	0.4729 (3)	0.0584 (14)
As3	0.30334 (6)	0.02678 (6)	0.10126 (3)	0.01519 (11)
F31	0.4709 (4)	0.0693 (4)	0.1718 (3)	0.0394 (10)
F32	0.3344 (4)	0.2024 (4)	0.1694 (2)	0.0298 (8)
F33	0.1827 (5)	−0.0665 (4)	0.1605 (2)	0.0397 (9)
F34	0.2791 (5)	−0.1435 (4)	0.0347 (3)	0.0414 (10)
F35	0.1432 (4)	−0.0062 (4)	0.0328 (2)	0.0344 (8)
F36	0.4297 (5)	0.1271 (5)	0.0446 (3)	0.0536 (13)
As4	0.75457 (6)	0.50135 (6)	0.90506 (3)	0.01649 (11)
F41	0.7791 (5)	0.3631 (4)	0.8348 (3)	0.0388 (9)
F42	0.6445 (4)	0.4941 (5)	0.8161 (2)	0.0354 (9)
F43	0.7234 (5)	0.6365 (5)	0.9727 (3)	0.0420 (10)
F44	0.9264 (4)	0.6455 (4)	0.8925 (2)	0.0322 (8)
F45	0.5798 (5)	0.3584 (5)	0.9159 (4)	0.0548 (13)
F46	0.8622 (6)	0.5084 (8)	0.9932 (3)	0.0659 (16)
S1	0.08721 (16)	−0.04307 (16)	0.84230 (9)	0.0215 (3)
O11	0.1755 (5)	−0.1170 (5)	0.8285 (3)	0.0263 (8)
O12	0.1561 (6)	0.1039 (5)	0.8322 (3)	0.0351 (10)
S2	0.41090 (18)	0.10930 (16)	0.67394 (11)	0.0274 (3)
O21	0.3352 (5)	0.1954 (4)	0.6851 (3)	0.0256 (8)
O22	0.3235 (6)	−0.0432 (5)	0.6736 (4)	0.0403 (11)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Te1	0.01256 (15)	0.01040 (14)	0.01324 (15)	0.00098 (12)	0.00400 (11)	0.00491 (12)
Te2	0.01256 (14)	0.01002 (14)	0.00765 (14)	0.00266 (12)	0.00080 (11)	0.00049 (11)
Te3	0.01441 (15)	0.00966 (14)	0.01539 (15)	0.00705 (12)	0.00443 (11)	0.00678 (11)
Te4	0.01157 (14)	0.01766 (15)	0.01386 (15)	0.01010 (12)	0.00621 (11)	0.00723 (12)
Te5	0.01700 (15)	0.01166 (15)	0.01099 (15)	0.00914 (12)	0.00477 (11)	0.00153 (11)
Te6	0.01463 (15)	0.02629 (17)	0.01367 (15)	0.01449 (14)	0.00460 (12)	0.01105 (13)
As1	0.0103 (2)	0.0176 (2)	0.0101 (2)	0.00812 (18)	0.00394 (16)	0.00631 (18)
F11	0.0143 (14)	0.0212 (15)	0.0240 (16)	0.0068 (12)	0.0098 (12)	0.0120 (13)
F12	0.0294 (18)	0.056 (2)	0.0230 (17)	0.0269 (18)	0.0088 (14)	0.0246 (17)
F13	0.0237 (16)	0.0218 (16)	0.0312 (18)	0.0142 (14)	0.0083 (14)	0.0024 (14)
F14	0.0228 (16)	0.046 (2)	0.0155 (15)	0.0230 (15)	0.0037 (12)	0.0133 (14)
F15	0.0263 (17)	0.0334 (18)	0.0249 (17)	0.0201 (15)	0.0096 (14)	0.0012 (14)
F16	0.0204 (16)	0.0344 (19)	0.040 (2)	0.0110 (15)	0.0160 (15)	0.0221 (16)
As2	0.0140 (2)	0.0078 (2)	0.0141 (2)	0.00218 (18)	0.00211 (18)	−0.00029 (18)
F21	0.0260 (17)	0.0216 (17)	0.038 (2)	0.0149 (15)	−0.0048 (15)	−0.0107 (15)
F22	0.0231 (17)	0.0276 (18)	0.051 (2)	0.0156 (15)	−0.0072 (16)	−0.0044 (17)
F23	0.044 (2)	0.0201 (17)	0.034 (2)	0.0167 (16)	0.0106 (17)	−0.0042 (15)
F24	0.084 (3)	0.0211 (19)	0.027 (2)	−0.004 (2)	0.012 (2)	0.0106 (16)
F25	0.057 (3)	0.0244 (19)	0.031 (2)	0.0007 (18)	0.0223 (19)	0.0096 (16)
F26	0.037 (2)	0.032 (2)	0.069 (3)	0.0167 (19)	−0.030 (2)	−0.015 (2)
As3	0.0114 (2)	0.0100 (2)	0.0128 (2)	0.00114 (18)	0.00228 (17)	−0.00137 (18)
F31	0.0280 (18)	0.0310 (19)	0.039 (2)	0.0191 (16)	−0.0144 (16)	−0.0134 (16)
F32	0.0350 (19)	0.0197 (16)	0.0237 (17)	0.0160 (15)	−0.0037 (14)	−0.0056 (13)
F33	0.038 (2)	0.0286 (19)	0.0294 (19)	0.0000 (16)	0.0127 (16)	0.0146 (16)
F34	0.038 (2)	0.0269 (19)	0.036 (2)	0.0183 (17)	−0.0045 (17)	−0.0160 (16)
F35	0.0307 (19)	0.0327 (19)	0.0257 (18)	0.0148 (16)	−0.0082 (15)	0.0003 (15)
F36	0.041 (2)	0.045 (2)	0.029 (2)	−0.0061 (19)	0.0183 (18)	0.0073 (18)
As4	0.0148 (2)	0.0291 (3)	0.0144 (2)	0.0150 (2)	0.00791 (18)	0.0126 (2)
F41	0.038 (2)	0.034 (2)	0.059 (3)	0.0271 (18)	0.0279 (19)	0.0198 (19)
F42	0.0329 (19)	0.071 (3)	0.0210 (17)	0.039 (2)	0.0078 (14)	0.0209 (18)
F43	0.042 (2)	0.049 (2)	0.031 (2)	0.029 (2)	0.0188 (17)	0.0000 (18)
F44	0.0214 (16)	0.0302 (18)	0.037 (2)	0.0086 (14)	0.0146 (15)	0.0106 (15)
F45	0.043 (2)	0.054 (3)	0.097 (4)	0.029 (2)	0.052 (3)	0.052 (3)
F46	0.065 (3)	0.149 (5)	0.040 (2)	0.080 (4)	0.027 (2)	0.063 (3)
S1	0.0250 (6)	0.0213 (6)	0.0250 (7)	0.0156 (5)	0.0104 (5)	0.0106 (5)
O11	0.028 (2)	0.025 (2)	0.036 (2)	0.0186 (18)	0.0124 (17)	0.0142 (18)
O12	0.051 (3)	0.026 (2)	0.045 (3)	0.026 (2)	0.020 (2)	0.023 (2)
S2	0.0267 (7)	0.0177 (6)	0.0462 (9)	0.0139 (6)	0.0156 (6)	0.0176 (6)
O21	0.030 (2)	0.0189 (18)	0.035 (2)	0.0159 (17)	0.0131 (17)	0.0132 (17)
O22	0.050 (3)	0.020 (2)	0.058 (3)	0.019 (2)	0.020 (2)	0.021 (2)

Geometric parameters (Å, º) top

Te1—Te5	2.6946 (4)	As2—F22	1.720 (3)
Te1—Te6	2.6963 (4)	As2—F21	1.726 (3)
Te1—Te2	3.1493 (4)	As3—F35	1.698 (3)
Te2—Te4	2.7019 (4)	As3—F33	1.700 (3)
Te2—Te3	2.7021 (4)	As3—F34	1.700 (3)
Te3—Te4	2.6892 (4)	As3—F36	1.723 (4)
Te3—Te5	3.1340 (4)	As3—F32	1.726 (3)
Te4—Te6	3.1027 (4)	As3—F31	1.731 (4)
Te5—Te6	2.6895 (4)	As4—F46	1.697 (4)
As1—F11	1.705 (3)	As4—F45	1.710 (4)
As1—F12	1.711 (3)	As4—F44	1.711 (3)
As1—F13	1.713 (3)	As4—F43	1.713 (4)
As1—F15	1.717 (3)	As4—F41	1.714 (4)
As1—F16	1.727 (3)	As4—F42	1.721 (3)
As1—F14	1.729 (3)	S1—O12	1.425 (4)
As2—F26	1.689 (4)	S1—O11	1.426 (4)
As2—F25	1.698 (4)	S2—O22	1.402 (4)
As2—F23	1.705 (3)	S2—O21	1.424 (4)
As2—F24	1.719 (4)

Te5—Te1—Te6	59.853 (11)	F25—As2—F22	90.4 (2)
Te5—Te1—Te2	89.735 (11)	F23—As2—F22	91.12 (18)
Te6—Te1—Te2	88.730 (12)	F24—As2—F22	88.9 (2)
Te4—Te2—Te3	59.687 (11)	F26—As2—F21	90.62 (19)
Te4—Te2—Te1	90.276 (11)	F25—As2—F21	90.7 (2)
Te3—Te2—Te1	89.938 (11)	F23—As2—F21	177.59 (18)
Te4—Te3—Te2	60.152 (11)	F24—As2—F21	88.5 (2)
Te4—Te3—Te5	89.804 (11)	F22—As2—F21	86.97 (17)
Te2—Te3—Te5	89.921 (11)	F35—As3—F33	90.8 (2)
Te3—Te4—Te2	60.161 (11)	F35—As3—F34	91.22 (18)
Te3—Te4—Te6	90.196 (11)	F33—As3—F34	91.0 (2)
Te2—Te4—Te6	89.605 (11)	F35—As3—F36	90.4 (2)
Te6—Te5—Te1	60.105 (11)	F33—As3—F36	177.96 (19)
Te6—Te5—Te3	89.527 (11)	F34—As3—F36	90.6 (2)
Te1—Te5—Te3	90.400 (11)	F35—As3—F32	90.19 (17)
Te5—Te6—Te1	60.042 (11)	F33—As3—F32	90.11 (19)
Te5—Te6—Te4	90.466 (12)	F34—As3—F32	178.18 (18)
Te1—Te6—Te4	91.380 (12)	F36—As3—F32	88.2 (2)
F11—As1—F12	90.07 (16)	F35—As3—F31	177.42 (19)
F11—As1—F13	89.83 (15)	F33—As3—F31	90.8 (2)
F12—As1—F13	90.26 (18)	F34—As3—F31	90.81 (18)
F11—As1—F15	91.42 (16)	F36—As3—F31	88.0 (2)
F12—As1—F15	90.61 (18)	F32—As3—F31	87.75 (16)
F13—As1—F15	178.48 (17)	F46—As4—F45	91.1 (3)
F11—As1—F16	179.15 (17)	F46—As4—F44	90.4 (2)
F12—As1—F16	90.78 (18)	F45—As4—F44	178.4 (2)
F13—As1—F16	90.16 (17)	F46—As4—F43	90.9 (2)
F15—As1—F16	88.58 (18)	F45—As4—F43	87.9 (2)
F11—As1—F14	90.40 (16)	F44—As4—F43	91.56 (19)
F12—As1—F14	179.19 (16)	F46—As4—F41	90.9 (2)
F13—As1—F14	90.40 (17)	F45—As4—F41	91.0 (2)
F15—As1—F14	88.72 (17)	F44—As4—F41	89.51 (18)
F16—As1—F14	88.74 (17)	F43—As4—F41	177.9 (2)
F26—As2—F25	90.6 (3)	F46—As4—F42	179.65 (19)
F26—As2—F23	91.3 (2)	F45—As4—F42	88.6 (2)
F25—As2—F23	90.8 (2)	F44—As4—F42	89.85 (19)
F26—As2—F24	90.1 (3)	F43—As4—F42	88.9 (2)
F25—As2—F24	178.9 (2)	F41—As4—F42	89.4 (2)
F23—As2—F24	90.0 (2)	O12—S1—O11	116.6 (3)
F26—As2—F22	177.39 (19)	O22—S2—O21	117.9 (3)

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