metal-organic compounds
The crystal structure of thallium perfluorotetraphenylborate, Tl+·B(C6F5)4−, consists of discrete partial occupancy Tl cations lying on threefold rotation axes, surrounded by perfluorotetraphenylborate anions, with TlF interactions in the range 2.942 (4)–3.663 (4) Å.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805025808/lh6488sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805025808/lh6488Isup2.hkl |
CCDC reference: 283957
Key indicators
- Single-crystal X-ray study
- T = 123 K
- Mean (C-C) = 0.009 Å
- Disorder in solvent or counterion
- R factor = 0.040
- wR factor = 0.087
- Data-to-parameter ratio = 11.7
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT040_ALERT_1_C No H-atoms in this Carbon Containing Compound .. ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 75.00 Perc. PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 9
Alert level G REFLT03_ALERT_1_G ALERT: Expected hkl max differ from CIF values From the CIF: _diffrn_reflns_theta_max 27.50 From the CIF: _reflns_number_total 1236 From the CIF: _diffrn_reflns_limit_ max hkl 24. 17. 17. From the CIF: _diffrn_reflns_limit_ min hkl -24. -17. -17. TEST1: Expected hkl limits for theta max Calculated maximum hkl 24. 24. 24. Calculated minimum hkl -24. -24. -24. REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 27.50 From the CIF: _reflns_number_total 1236 Count of symmetry unique reflns 732 Completeness (_total/calc) 168.85% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 504 Fraction of Friedel pairs measured 0.689 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion
Computing details top
Data collection: Please supply; cell refinement: Please supply; data reduction: Please supply; program(s) used to solve structure: Please supply; program(s) used to refine structure: Please supply; molecular graphics: Please supply; software used to prepare material for publication: Please supply.
Thallium perfluorotetraphenylborate top
Crystal data top
Tl+·C24BF20− | Dx = 2.528 Mg m−3 |
Mr = 883.42 | Mo Kα radiation, λ = 0.71073 Å |
Cubic, I43d | Cell parameters from 2240 reflections |
Hall symbol: I -4bd 2c 3 | θ = 4.0–27.5° |
a = 19.095 (12) Å | µ = 7.14 mm−1 |
V = 6962 (8) Å3 | T = 123 K |
Z = 12 | Plate, colorless |
F(000) = 4920 | 0.10 × 0.08 × 0.05 mm |
Data collection top
Nonius KappaCCD diffractometer | 1236 independent reflections |
Radiation source: fine-focus sealed tube | 949 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.051 |
ω and φ scans | θmax = 27.5°, θmin = 4.0° |
Absorption correction: multi-scan (SORTAV; Blessing, 1997) | h = −24→24 |
Tmin = 0.523, Tmax = 0.703 | k = −17→17 |
2240 measured reflections | l = −17→17 |
Refinement top
Refinement on F2 | w = 1/[σ2(Fo2) + (0.0365P)2 + 3.02P] where P = (Fo2 + 2Fc2)/3 |
Least-squares matrix: full | (Δ/σ)max = 0.001 |
R[F2 > 2σ(F2)] = 0.040 | Δρmax = 0.65 e Å−3 |
wR(F2) = 0.087 | Δρmin = −0.69 e Å−3 |
S = 1.03 | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
1236 reflections | Extinction coefficient: 0.00038 (5) |
106 parameters | Absolute structure: Flack (1983), 504 Friedel pairs |
0 restraints | Absolute structure parameter: 0.007 (13) |
Primary atom site location: structure-invariant direct methods |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Tl1 | 0.24315 (2) | 0.24315 (2) | 0.24315 (2) | 0.0396 (2) | 0.75 |
F1 | 0.10699 (18) | 0.08402 (18) | 0.43741 (18) | 0.0278 (8) | |
F2 | 0.08684 (18) | −0.0109 (2) | 0.3404 (2) | 0.0418 (10) | |
F3 | 0.1950 (2) | −0.0853 (2) | 0.28459 (19) | 0.0389 (10) | |
F4 | 0.3274 (2) | −0.0575 (2) | 0.3284 (2) | 0.0390 (10) | |
F5 | 0.35129 (18) | 0.03994 (17) | 0.42775 (19) | 0.0267 (9) | |
C1 | 0.2318 (3) | 0.0702 (3) | 0.4353 (3) | 0.0198 (13) | |
C2 | 0.1656 (3) | 0.0527 (3) | 0.4113 (3) | 0.0267 (15) | |
C3 | 0.1528 (3) | 0.0022 (4) | 0.3601 (3) | 0.0298 (14) | |
C4 | 0.2073 (4) | −0.0349 (3) | 0.3329 (3) | 0.0286 (16) | |
C5 | 0.2745 (3) | −0.0207 (3) | 0.3552 (3) | 0.0230 (14) | |
C6 | 0.2839 (3) | 0.0303 (3) | 0.4056 (3) | 0.0234 (14) | |
B1 | 0.2500 | 0.1250 | 0.5000 | 0.018 (2) |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
Tl1 | 0.0396 (2) | 0.0396 (2) | 0.0396 (2) | −0.0020 (2) | −0.0020 (2) | −0.0020 (2) |
F1 | 0.020 (2) | 0.029 (2) | 0.034 (2) | −0.001 (2) | −0.001 (2) | −0.003 (2) |
F2 | 0.032 (2) | 0.043 (2) | 0.050 (2) | −0.006 (2) | −0.014 (2) | −0.013 (2) |
F3 | 0.053 (3) | 0.030 (2) | 0.033 (2) | 0.004 (2) | −0.006 (2) | −0.009 (2) |
F4 | 0.045 (2) | 0.038 (2) | 0.034 (2) | 0.010 (2) | 0.006 (2) | −0.012 (2) |
F5 | 0.023 (2) | 0.027 (2) | 0.030 (2) | 0.002 (2) | 0.001 (2) | −0.005 (2) |
C1 | 0.026 (3) | 0.016 (3) | 0.017 (3) | −0.005 (2) | −0.002 (3) | 0.006 (2) |
C2 | 0.025 (3) | 0.023 (3) | 0.032 (4) | 0.009 (3) | 0.003 (3) | 0.002 (3) |
C3 | 0.035 (3) | 0.026 (3) | 0.028 (3) | −0.004 (4) | −0.009 (3) | 0.002 (3) |
C4 | 0.052 (5) | 0.013 (3) | 0.021 (3) | −0.002 (3) | −0.005 (3) | −0.003 (3) |
C5 | 0.031 (3) | 0.016 (3) | 0.022 (3) | 0.009 (2) | 0.004 (3) | 0.000 (3) |
C6 | 0.015 (3) | 0.022 (3) | 0.032 (4) | −0.003 (2) | −0.001 (3) | 0.007 (3) |
B1 | 0.018 (4) | 0.017 (6) | 0.018 (4) | 0.000 | 0.000 | 0.000 |
Geometric parameters (Å, º) top
F1—C2 | 1.364 (7) | C2—C3 | 1.394 (9) |
F2—C3 | 1.338 (7) | C3—C4 | 1.363 (9) |
F3—C4 | 1.353 (7) | C4—C5 | 1.378 (9) |
F4—C5 | 1.333 (6) | C5—C6 | 1.381 (9) |
F5—C6 | 1.368 (7) | B1—C1i | 1.655 (6) |
C1—C6 | 1.375 (8) | B1—C1ii | 1.655 (6) |
C1—C2 | 1.386 (8) | B1—C1iii | 1.656 (6) |
C1—B1 | 1.656 (6) | ||
C6—C1—C2 | 112.9 (5) | F4—C5—C4 | 118.8 (6) |
C6—C1—B1 | 120.4 (5) | F4—C5—C6 | 122.7 (6) |
C2—C1—B1 | 126.2 (5) | C4—C5—C6 | 118.4 (5) |
F1—C2—C1 | 121.4 (6) | F5—C6—C1 | 118.6 (5) |
F1—C2—C3 | 114.6 (5) | F5—C6—C5 | 115.7 (5) |
C1—C2—C3 | 124.0 (6) | C1—C6—C5 | 125.8 (6) |
F2—C3—C4 | 121.0 (6) | C1i—B1—C1ii | 101.6 (4) |
F2—C3—C2 | 119.4 (6) | C1i—B1—C1 | 113.6 (2) |
C4—C3—C2 | 119.5 (5) | C1ii—B1—C1 | 113.6 (2) |
F3—C4—C3 | 119.7 (6) | C1i—B1—C1iii | 113.6 (2) |
F3—C4—C5 | 120.9 (6) | C1ii—B1—C1iii | 113.6 (2) |
C3—C4—C5 | 119.3 (5) | C1—B1—C1iii | 101.6 (4) |
C6—C1—C2—F1 | 176.5 (5) | C3—C4—C5—C6 | 1.1 (10) |
B1—C1—C2—F1 | 4.3 (9) | C2—C1—C6—F5 | −176.6 (5) |
C6—C1—C2—C3 | −2.7 (9) | B1—C1—C6—F5 | −3.9 (8) |
B1—C1—C2—C3 | −175.0 (5) | C2—C1—C6—C5 | 2.3 (9) |
F1—C2—C3—F2 | 0.8 (9) | B1—C1—C6—C5 | 175.0 (5) |
C1—C2—C3—F2 | −179.9 (6) | F4—C5—C6—F5 | −1.3 (8) |
F1—C2—C3—C4 | −176.7 (6) | C4—C5—C6—F5 | 177.3 (5) |
C1—C2—C3—C4 | 2.5 (11) | F4—C5—C6—C1 | 179.8 (5) |
F2—C3—C4—F3 | 0.7 (9) | C4—C5—C6—C1 | −1.6 (10) |
C2—C3—C4—F3 | 178.2 (6) | C6—C1—B1—C1i | 168.2 (5) |
F2—C3—C4—C5 | −179.1 (6) | C2—C1—B1—C1i | −20.1 (5) |
C2—C3—C4—C5 | −1.6 (10) | C6—C1—B1—C1ii | 52.8 (4) |
F3—C4—C5—F4 | 0.0 (9) | C2—C1—B1—C1ii | −135.5 (7) |
C3—C4—C5—F4 | 179.8 (5) | C6—C1—B1—C1iii | −69.5 (5) |
F3—C4—C5—C6 | −178.7 (5) | C2—C1—B1—C1iii | 102.2 (6) |
Symmetry codes: (i) z−1/4, −y+1/4, −x+3/4; (ii) −z+3/4, −y+1/4, x+1/4; (iii) −x+1/2, y, −z+1. |