Buy article online - an online subscription or single-article purchase is required to access this article.
The crystal structure of thallium perfluorotetraphenylborate, Tl
+·B(C
6F
5)
4−, consists of discrete partial occupancy Tl cations lying on threefold rotation axes, surrounded by perfluorotetraphenylborate anions, with Tl
F interactions in the range 2.942 (4)–3.663 (4) Å.
Supporting information
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
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. |
Subscribe to Acta Crystallographica Section E: Crystallographic Communications
The full text of this article is available to subscribers to the journal.
If you have already registered and are using a computer listed in your registration details, please email
support@iucr.org for assistance.