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The title compound, 2C5H6N+·TeF5·0.5Te2F6O22−, contains two anions, [TeF5] and [Te2O2F6]2−. The [Te2O2F6]2− anions are involved in H...F/O bonding with the pyridinium cations. Crystallographically imposed inversion leads to mol­ecular Cs symmetry for the [Te2O2F6]2− anions. Extended chains of inversion-related pyridinium cations are built up by π–π inter­actions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805025304/hk6029sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805025304/hk6029Isup2.hkl
Contains datablock I

CCDC reference: 215494

Key indicators

  • Single-crystal X-ray study
  • T = 200 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.029
  • wR factor = 0.064
  • Data-to-parameter ratio = 17.2

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT432_ALERT_2_B Short Inter X...Y Contact Te2 .. F8 .. 3.15 Ang.
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Te2 PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.43 Ratio PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 40.18 Deg. O -TE1 -TE1 1.555 1.555 3.666 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 35.33 Deg. O -TE1 -TE1 3.666 1.555 3.666 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 40.58 Deg. O -TE1 -N1 1.555 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 44.80 Deg. O -TE1 -F3 1.555 1.555 3.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 43.96 Deg. F3 -TE1 -F3 1.555 1.555 3.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 27.15 Deg. O -TE1 -F1 1.555 1.555 3.556 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 42.03 Deg. N1 -TE1 -F1 1.555 1.555 3.556 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 17.65 Deg. F3 -TE1 -F1 3.555 1.555 3.556 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 31.68 Deg. O -TE1 -F2 1.555 1.555 3.556 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 16.62 Deg. F3 -TE1 -F2 3.555 1.555 3.556 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 9.37 Deg. F1 -TE1 -F2 3.556 1.555 3.556 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 44.09 Deg. F4 -TE2 -F8 1.555 1.555 4.566 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 40.91 Deg. F4 -TE2 -F7 1.555 1.555 4.566 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 5.07 Deg. F8 -TE2 -F7 4.566 1.555 4.566 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 44.23 Deg. F5 -TE2 -F6 1.555 1.555 4.566 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 4.88 Deg. F8 -TE2 -F6 4.566 1.555 4.566 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 7.76 Deg. F7 -TE2 -F6 4.566 1.555 4.566 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 27.45 Deg. F5 -TE2 -N1 1.555 1.555 3.556 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 24.02 Deg. F8 -TE2 -N1 4.566 1.555 3.556 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 27.20 Deg. F7 -TE2 -N1 4.566 1.555 3.556 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 19.58 Deg. F6 -TE2 -N1 4.566 1.555 3.556 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 27.30 Deg. TE1 -N1 -H1 1.555 1.555 1.555
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 25 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 24 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 (Nonius, 2000); cell refinement: SCALEPACK (Otwinowski & Minor, 1997); data reduction: SCALEPACK and DENZO (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1996); software used to prepare material for publication: SHELXL97.

Tetrapyridinium di-µ-oxo-bis[trifluorotellurate(IV)] bis[pentafluorotellurate(IV)] top
Crystal data top
2C5H6N+·TeF5·0.5Te2O2F62F(000) = 1080
Mr = 583.42Dx = 2.473 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 35743 reflections
a = 10.1509 (2) Åθ = 3.1–27.5°
b = 20.0739 (3) ŵ = 3.81 mm1
c = 7.9950 (1) ÅT = 200 K
β = 105.8894 (8)°Block, colorless
V = 1566.88 (4) Å30.30 × 0.20 × 0.07 mm
Z = 4
Data collection top
Nonius KappaCCD
diffractometer
3586 independent reflections
Radiation source: fine-focus sealed tube2948 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.073
Detector resolution: 9 pixels mm-1θmax = 27.5°, θmin = 3.3°
area detection scansh = 1313
Absorption correction: numerical
(XRED32 and XSHAPE; Stoe & Cie, 1997)
k = 2626
Tmin = 0.350, Tmax = 0.690l = 1010
36947 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.029Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.064H-atom parameters constrained
S = 1.08 w = 1/[σ2(Fo2) + (0.0306P)2 + 0.4788P]
where P = (Fo2 + 2Fc2)/3
3586 reflections(Δ/σ)max = 0.001
208 parametersΔρmax = 1.00 e Å3
0 restraintsΔρmin = 1.10 e Å3
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.

Refinement of hydrogen atoms: H atoms calculated in geometrically idealized position with U(H) = 1.2 U(C/N)

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Te10.52043 (2)0.509365 (11)0.31119 (3)0.02514 (8)
Te20.89376 (2)0.702005 (11)0.47140 (3)0.02895 (8)
F10.6577 (2)0.43510 (10)0.3707 (3)0.0354 (5)
F20.3562 (2)0.56873 (10)0.2558 (3)0.0355 (5)
F30.4220 (2)0.45665 (10)0.1086 (3)0.0375 (5)
O0.4192 (2)0.45604 (11)0.4285 (3)0.0270 (5)
F41.0332 (2)0.63253 (11)0.5249 (3)0.0469 (6)
F50.7513 (2)0.63330 (12)0.3969 (3)0.0507 (6)
F60.7666 (2)0.76924 (11)0.3420 (3)0.0482 (6)
F71.0394 (2)0.76409 (12)0.4696 (4)0.0528 (6)
F80.9087 (3)0.68431 (12)0.2477 (3)0.0504 (6)
N10.1423 (3)0.45709 (15)0.2678 (4)0.0310 (7)
H10.23120.45430.31550.037*
C10.0730 (4)0.50523 (18)0.3203 (5)0.0317 (8)
H1A0.11910.53550.40820.038*
C20.0666 (4)0.51103 (19)0.2461 (5)0.0337 (8)
H2A0.11730.54560.28090.040*
C30.1308 (4)0.46554 (19)0.1205 (5)0.0342 (8)
H30.22690.46830.06960.041*
C40.0567 (4)0.41668 (19)0.0694 (5)0.0353 (9)
H40.10040.38570.01790.042*
C50.0832 (4)0.41281 (17)0.1462 (5)0.0327 (8)
H50.13620.37900.11260.039*
N20.3838 (3)0.68576 (17)0.4616 (5)0.0440 (9)
H20.37320.64250.47010.053*
C60.5002 (4)0.7138 (2)0.5550 (6)0.0411 (10)
H60.56980.68710.62840.049*
C70.5182 (4)0.7803 (2)0.5446 (6)0.0416 (9)
H70.60070.80080.60990.050*
C80.4152 (4)0.8180 (2)0.4377 (6)0.0420 (10)
H80.42610.86480.42990.050*
C90.2967 (4)0.7876 (2)0.3424 (6)0.0428 (10)
H90.22540.81310.26830.051*
C100.2831 (4)0.7208 (2)0.3556 (6)0.0442 (10)
H100.20240.69910.28990.053*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Te10.02339 (13)0.02542 (13)0.02513 (13)0.00086 (8)0.00415 (9)0.00096 (9)
Te20.02926 (14)0.02737 (14)0.02997 (14)0.00188 (9)0.00767 (10)0.00142 (9)
F10.0294 (11)0.0372 (12)0.0388 (13)0.0067 (9)0.0082 (9)0.0009 (10)
F20.0368 (12)0.0297 (11)0.0351 (12)0.0059 (9)0.0014 (9)0.0017 (9)
F30.0418 (12)0.0361 (12)0.0308 (12)0.0007 (10)0.0036 (9)0.0064 (9)
O0.0259 (12)0.0262 (12)0.0279 (13)0.0032 (10)0.0056 (10)0.0007 (10)
F40.0458 (14)0.0352 (12)0.0555 (15)0.0097 (10)0.0068 (11)0.0047 (11)
F50.0437 (14)0.0376 (12)0.0650 (17)0.0138 (11)0.0052 (12)0.0022 (12)
F60.0364 (13)0.0383 (13)0.0604 (16)0.0031 (10)0.0030 (11)0.0044 (11)
F70.0387 (13)0.0386 (13)0.0849 (19)0.0085 (10)0.0233 (13)0.0009 (13)
F80.0794 (18)0.0438 (13)0.0316 (13)0.0053 (13)0.0210 (12)0.0041 (10)
N10.0231 (14)0.0366 (17)0.0321 (17)0.0032 (13)0.0055 (12)0.0084 (14)
C10.0293 (19)0.037 (2)0.027 (2)0.0079 (16)0.0044 (15)0.0003 (15)
C20.034 (2)0.035 (2)0.033 (2)0.0030 (16)0.0106 (16)0.0023 (16)
C30.0245 (18)0.044 (2)0.031 (2)0.0009 (16)0.0010 (15)0.0086 (17)
C40.035 (2)0.033 (2)0.033 (2)0.0092 (16)0.0007 (16)0.0011 (16)
C50.042 (2)0.0245 (18)0.031 (2)0.0013 (16)0.0091 (16)0.0024 (15)
N20.048 (2)0.0273 (17)0.058 (2)0.0023 (15)0.0153 (18)0.0059 (16)
C60.040 (2)0.042 (2)0.041 (2)0.0083 (18)0.0087 (18)0.0070 (19)
C70.034 (2)0.046 (2)0.043 (2)0.0090 (18)0.0084 (17)0.0036 (19)
C80.047 (2)0.033 (2)0.048 (3)0.0020 (18)0.015 (2)0.0068 (18)
C90.036 (2)0.050 (3)0.041 (2)0.0114 (19)0.0066 (18)0.0054 (19)
C100.031 (2)0.050 (3)0.050 (3)0.0057 (19)0.0080 (18)0.015 (2)
Geometric parameters (Å, º) top
Te1—O1.900 (2)N1—H10.8800
Te1—F31.964 (2)C1—C21.383 (5)
Te1—F21.998 (2)C1—H1A0.9500
Te1—F12.007 (2)C2—C31.382 (5)
Te1—Oi2.119 (2)C2—H2A0.9500
Te1—Te1i3.1803 (4)C3—C41.366 (6)
Te1—N13.902 (3)C3—H30.9500
Te1—F3ii21.476 (2)C4—C51.386 (5)
Te1—F1iii22.926 (2)C4—H40.9500
Te1—F2iii24.008 (2)C5—H50.9500
Te2—F81.870 (2)N2—C101.336 (5)
Te2—F71.937 (2)N2—C61.337 (5)
Te2—F41.949 (2)N2—H20.8800
Te2—F61.956 (2)C6—C71.354 (6)
Te2—F51.969 (2)C6—H60.9500
Te2—F8iv17.924 (2)C7—C81.381 (6)
Te2—F7iv19.772 (2)C7—H70.9500
Te2—F6iv19.816 (2)C8—C91.378 (6)
Te2—N1iii25.852 (3)C8—H80.9500
O—Te1i2.119 (2)C9—C101.354 (6)
N1—C11.329 (5)C9—H90.9500
N1—C51.333 (5)C10—H100.9500
N1—Te2iii25.852 (3)
O—Te1—F383.21 (10)F6—Te2—F7iv141.76 (7)
O—Te1—F285.08 (9)F5—Te2—F7iv51.83 (7)
F3—Te1—F286.18 (8)F8iv—Te2—F7iv5.067 (11)
O—Te1—F184.17 (9)F8—Te2—F6iv88.96 (7)
F3—Te1—F187.64 (9)F7—Te2—F6iv135.67 (7)
F2—Te1—F1168.16 (8)F4—Te2—F6iv48.42 (7)
O—Te1—Oi75.51 (10)F6—Te2—F6iv134.22 (7)
F3—Te1—Oi158.70 (9)F5—Te2—F6iv44.23 (7)
F2—Te1—Oi91.22 (9)F8iv—Te2—F6iv4.877 (11)
F1—Te1—Oi90.88 (9)F7iv—Te2—F6iv7.757 (10)
O—Te1—Te1i40.18 (7)F8—Te2—N1iii92.72 (8)
F3—Te1—Te1i123.38 (7)F7—Te2—N1iii155.23 (7)
F2—Te1—Te1i87.88 (6)F4—Te2—N1iii68.00 (7)
F1—Te1—Te1i87.11 (6)F6—Te2—N1iii116.08 (7)
Oi—Te1—Te1i35.33 (6)F5—Te2—N1iii27.45 (7)
O—Te1—N140.58 (8)F8iv—Te2—N1iii24.016 (11)
F3—Te1—N161.03 (8)F7iv—Te2—N1iii27.202 (10)
F2—Te1—N153.12 (8)F6iv—Te2—N1iii19.579 (9)
F1—Te1—N1115.05 (7)Te1—O—Te1i104.49 (10)
Oi—Te1—N1100.85 (8)C1—N1—C5122.9 (3)
Te1i—Te1—N170.84 (5)C1—N1—Te1111.7 (2)
O—Te1—F3ii44.80 (7)C5—N1—Te1118.7 (2)
F3—Te1—F3ii43.96 (7)C1—N1—Te2iii111.5 (2)
F2—Te1—F3ii101.25 (6)C5—N1—Te2iii49.2 (2)
F1—Te1—F3ii67.47 (6)Te1—N1—Te2iii130.31 (5)
Oi—Te1—F3ii116.49 (6)C1—N1—H1118.5
Te1i—Te1—F3ii82.724 (10)C5—N1—H1118.5
N1—Te1—F3ii50.06 (5)Te1—N1—H127.3
O—Te1—F1iii27.15 (7)Te2iii—N1—H1107.5
F3—Te1—F1iii58.85 (7)N1—C1—C2119.7 (3)
F2—Te1—F1iii95.10 (6)N1—C1—H1A120.2
F1—Te1—F1iii73.06 (6)C2—C1—H1A120.2
Oi—Te1—F1iii100.45 (6)C3—C2—C1118.7 (4)
Te1i—Te1—F1iii65.755 (9)C3—C2—H2A120.7
N1—Te1—F1iii42.03 (4)C1—C2—H2A120.7
F3ii—Te1—F1iii17.648 (8)C4—C3—C2120.2 (3)
O—Te1—F2iii31.68 (7)C4—C3—H3119.9
F3—Te1—F2iii60.53 (6)C2—C3—H3119.9
F2—Te1—F2iii104.47 (6)C3—C4—C5119.3 (3)
F1—Te1—F2iii63.69 (6)C3—C4—H4120.3
Oi—Te1—F2iii99.94 (6)C5—C4—H4120.3
Te1i—Te1—F2iii66.844 (9)N1—C5—C4119.2 (3)
N1—Te1—F2iii51.39 (4)N1—C5—H5120.4
F3ii—Te1—F2iii16.621 (8)C4—C5—H5120.4
F1iii—Te1—F2iii9.372 (7)C10—N2—C6122.6 (4)
F8—Te2—F781.57 (11)C10—N2—H2118.7
F8—Te2—F480.22 (11)C6—N2—H2118.7
F7—Te2—F487.25 (10)N2—C6—C7119.6 (4)
F8—Te2—F680.77 (11)N2—C6—H6120.2
F7—Te2—F686.94 (10)C7—C6—H6120.2
F4—Te2—F6160.75 (11)C6—C7—C8119.1 (4)
F8—Te2—F579.79 (11)C6—C7—H7120.4
F7—Te2—F5161.35 (12)C8—C7—H7120.4
F4—Te2—F589.67 (10)C9—C8—C7119.8 (4)
F6—Te2—F589.99 (10)C9—C8—H8120.1
F8—Te2—F8iv85.94 (7)C7—C8—H8120.1
F7—Te2—F8iv131.22 (7)C10—C9—C8119.2 (4)
F4—Te2—F8iv44.09 (7)C10—C9—H9120.4
F6—Te2—F8iv137.07 (7)C8—C9—H9120.4
F5—Te2—F8iv47.36 (7)N2—C10—C9119.6 (4)
F8—Te2—F7iv89.16 (7)N2—C10—H10120.2
F7—Te2—F7iv128.14 (8)C9—C10—H10120.2
F4—Te2—F7iv40.91 (7)
F3—Te1—O—Te1i179.27 (11)O—Te1—N1—Te2iii46.32 (12)
F2—Te1—O—Te1i92.54 (10)F3—Te1—N1—Te2iii69.69 (9)
F1—Te1—O—Te1i92.43 (10)F2—Te1—N1—Te2iii178.36 (11)
Oi—Te1—O—Te1i0.0F1—Te1—N1—Te2iii2.20 (10)
N1—Te1—O—Te1i126.92 (16)Oi—Te1—N1—Te2iii98.33 (8)
F3ii—Te1—O—Te1i156.08 (14)Te1i—Te1—N1—Te2iii79.42 (5)
F1iii—Te1—O—Te1i156.1 (2)F3ii—Te1—N1—Te2iii17.246 (18)
F2iii—Te1—O—Te1i139.34 (17)F1iii—Te1—N1—Te2iii4.713 (10)
O—Te1—N1—C1102.4 (3)F2iii—Te1—N1—Te2iii4.208 (13)
F3—Te1—N1—C1141.6 (3)C5—N1—C1—C20.6 (6)
F2—Te1—N1—C132.9 (2)Te1—N1—C1—C2150.1 (3)
F1—Te1—N1—C1146.5 (2)Te2iii—N1—C1—C255.1 (4)
Oi—Te1—N1—C150.4 (2)N1—C1—C2—C31.0 (6)
Te1i—Te1—N1—C169.3 (2)C1—C2—C3—C41.1 (6)
F3ii—Te1—N1—C1166.0 (3)C2—C3—C4—C50.7 (6)
F1iii—Te1—N1—C1144.0 (3)C1—N1—C5—C40.3 (5)
F2iii—Te1—N1—C1144.5 (3)Te1—N1—C5—C4148.6 (3)
O—Te1—N1—C5105.5 (3)Te2iii—N1—C5—C491.3 (4)
F3—Te1—N1—C510.5 (2)C3—C4—C5—N10.3 (5)
F2—Te1—N1—C5119.2 (3)C10—N2—C6—C70.5 (7)
F1—Te1—N1—C561.4 (3)N2—C6—C7—C80.3 (7)
Oi—Te1—N1—C5157.5 (2)C6—C7—C8—C90.6 (7)
Te1i—Te1—N1—C5138.6 (2)C7—C8—C9—C100.1 (7)
F3ii—Te1—N1—C541.9 (2)C6—N2—C10—C90.9 (7)
F1iii—Te1—N1—C563.9 (2)C8—C9—C10—N20.6 (7)
F2iii—Te1—N1—C563.4 (2)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y, z; (iii) x, y, z+1; (iv) x, y+1/2, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1···O0.881.882.752 (3)175
N2—H2···F20.882.242.837 (4)125
N2—H2···F1i0.882.092.859 (4)146
Symmetry code: (i) x+1, y+1, z+1.
 

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