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Cs2[IrF6] possesses a framework structure constructed from Cs+ cations and [IrF6]2- complex anions. The cation is 12-coordinated by F atoms, forming a slightly distorted anti­cubocta­hedron; the anion has the shape of an almost ideal octa­hedron. Cs, Ir and F atoms are located on special positions of 3m, \overline{3}m and m symmetry, respectively.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680706000X/mg2040sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680706000X/mg2040Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 296 K
  • Mean [sigma](Ir-F) = 0.002 Å
  • R factor = 0.013
  • wR factor = 0.028
  • Data-to-parameter ratio = 16.2

checkCIF/PLATON results

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Alert level B PLAT731_ALERT_1_B Bond Calc 3.156(3), Rep 3.1564(4) ...... 7.50 su-Ra CS1 -F1 1.555 2.655 PLAT731_ALERT_1_B Bond Calc 3.1561(17), Rep 3.1564(4) ...... 4.25 su-Ra CS1 -F1 1.555 3.665 PLAT731_ALERT_1_B Bond Calc 3.1567(18), Rep 3.1564(4) ...... 4.50 su-Ra CS1 -F1 1.555 1.655 PLAT731_ALERT_1_B Bond Calc 3.1561(18), Rep 3.1564(4) ...... 4.50 su-Ra CS1 -F1 1.555 1.555 PLAT731_ALERT_1_B Bond Calc 3.1567(19), Rep 3.1564(4) ...... 4.75 su-Ra CS1 -F1 1.555 3.555 PLAT731_ALERT_1_B Bond Calc 3.157(3), Rep 3.1564(4) ...... 7.50 su-Ra CS1 -F1 1.555 2.665 PLAT731_ALERT_1_B Bond Calc 3.1567(18), Rep 3.1564(4) ...... 4.50 su-Ra F1 -CS1 1.555 1.455 PLAT732_ALERT_1_B Angle Calc 53.31(5), Rep 53.32(1) ...... 7.14 su-Ra F1 -IR1 -CS1 1.555 1.555 1.555
Alert level C PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.12
0 ALERT level A = In general: serious problem 8 ALERT level B = Potentially serious problem 1 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 8 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 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 0 ALERT type 5 Informative message, check

Comment top

For general discussion and comments on the figures, see Smolentsev, Gubanov, Naumov & Danilenko (2007).

Related literature top

The title compound was first characterized by X-ray powder diffraction (Babel, 1967). It is isomorphous with the potassium analogue, K2[IrF6] (Fitz et al., 2002). The stucture of Rb2[IrF6] has also been reported (Smolentsev, Gubanov, Naumov & Danilenko, 2007). The precursor, H2[IrF6], was prepared as described by Smolentsev, Gubanov & Danilenko (2007).

Experimental top

Cs2CO3 was reacted with an aqueous solution of H2[IrF6] acid. Subsequent slow evaporation at room temperature yielded light-pink crystals in the form of needles or hexagonal plates of the title compound. The precursor, H2[IrF6], was prepared as described in Smolentsev, Gubanov & Danilenko (2007).

Refinement top

The maximum peak and deepest hole are located 0.82 Å and 0.70 Å, both from Ir1.

Computing details top

Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT (Bruker, 2004); program(s) used to solve structure: SHELXTL (Bruker, 2004); program(s) used to refine structure: SHELXTL (Bruker, 2004); molecular graphics: BS (Ozawa & Kang, 2004) and POV-RAY (Cason, 2002); software used to prepare material for publication: SHELXTL (Bruker, 2004).

Figures top
[Figure 1] Fig. 1. A fragment of the Cs2[IrF6] structure showing the complex anion surrounded by the cations. Displacement ellipsoids are drawn at the 50% probability level.
[Figure 2] Fig. 2. Packing diagram for Cs2[IrF6], viewed in perspective, with Cs-centered anticuboctahedra (orange) and Ir-centered octahedra (purple).
Caesium hexafluoridoiridate(IV) top
Crystal data top
Cs2[IrF6]Dx = 5.620 Mg m3
Mr = 572.02Mo Kα radiation, λ = 0.71073 Å
Trigonal, P3m1Cell parameters from 982 reflections
Hall symbol: -P 3 2"θ = 3.8–30.0°
a = 6.2421 (3) ŵ = 30.40 mm1
c = 5.0084 (5) ÅT = 296 K
V = 169.00 (2) Å3Needle, light-pink
Z = 10.08 × 0.06 × 0.04 mm
F(000) = 241
Data collection top
Bruker–Nonius X8 APEX CCD area-detector
diffractometer
211 independent reflections
Radiation source: fine-focus sealed tube207 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.019
Detector resolution: 25 pixels mm-1θmax = 30.0°, θmin = 3.8°
ϕ scansh = 88
Absorption correction: multi-scan
(SADABS; Bruker, 2004)
k = 85
Tmin = 0.134, Tmax = 0.288l = 77
1513 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)] = 0.013 w = 1/[σ2(Fo2) + (0.0133P)2 + 0.3436P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.028(Δ/σ)max < 0.001
S = 1.06Δρmax = 1.04 e Å3
211 reflectionsΔρmin = 0.49 e Å3
13 parametersExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.0058 (8)
Crystal data top
Cs2[IrF6]Z = 1
Mr = 572.02Mo Kα radiation
Trigonal, P3m1µ = 30.40 mm1
a = 6.2421 (3) ÅT = 296 K
c = 5.0084 (5) Å0.08 × 0.06 × 0.04 mm
V = 169.00 (2) Å3
Data collection top
Bruker–Nonius X8 APEX CCD area-detector
diffractometer
211 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2004)
207 reflections with I > 2σ(I)
Tmin = 0.134, Tmax = 0.288Rint = 0.019
1513 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.01313 parameters
wR(F2) = 0.0280 restraints
S = 1.06Δρmax = 1.04 e Å3
211 reflectionsΔρmin = 0.49 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ir10.00000.00000.50000.01382 (13)
Cs10.66670.33330.19957 (9)0.02036 (14)
F10.1497 (2)0.2995 (4)0.2862 (5)0.0233 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ir10.01221 (14)0.01221 (14)0.0171 (2)0.00610 (7)0.0000.000
Cs10.01903 (16)0.01903 (16)0.0230 (3)0.00951 (8)0.0000.000
F10.0245 (10)0.0171 (12)0.0258 (13)0.0085 (6)0.0037 (5)0.0075 (10)
Geometric parameters (Å, º) top
Ir1—F1i1.941 (2)Cs1—F1xii3.140 (2)
Ir1—F1ii1.941 (2)Cs1—F1xiii3.1564 (4)
Ir1—F1iii1.941 (2)Cs1—F1xiv3.1564 (4)
Ir1—F1iv1.941 (2)Cs1—F1xv3.1564 (4)
Ir1—F11.941 (2)Cs1—F13.1564 (4)
Ir1—F1v1.941 (2)Cs1—F1v3.1564 (4)
Ir1—Cs1vi3.9054 (2)Cs1—F1xvi3.1564 (4)
Ir1—Cs1vii3.9054 (2)Cs1—F1xvii3.252 (3)
Ir1—Cs1viii3.9054 (2)Cs1—F1viii3.252 (3)
Ir1—Cs1ix3.9054 (2)Cs1—F1i3.252 (3)
Ir1—Cs13.9054 (2)F1—Cs1xii3.140 (2)
Ir1—Cs1iv3.9054 (2)F1—Cs1vii3.1564 (4)
Cs1—F1x3.140 (2)F1—Cs1viii3.252 (3)
Cs1—F1xi3.140 (2)
F1i—Ir1—F1ii180.00 (11)F1xii—Cs1—F1xiii129.02 (2)
F1i—Ir1—F1iii92.50 (10)F1x—Cs1—F1xiv98.23 (4)
F1ii—Ir1—F1iii87.50 (10)F1xi—Cs1—F1xiv129.02 (2)
F1i—Ir1—F1iv92.50 (10)F1xii—Cs1—F1xiv63.06 (8)
F1ii—Ir1—F1iv87.50 (10)F1xiii—Cs1—F1xiv118.14 (2)
F1iii—Ir1—F1iv92.50 (10)F1x—Cs1—F1xv63.06 (8)
F1i—Ir1—F187.50 (10)F1xi—Cs1—F1xv129.02 (2)
F1ii—Ir1—F192.50 (10)F1xii—Cs1—F1xv98.23 (4)
F1iii—Ir1—F187.50 (10)F1xiii—Cs1—F1xv52.74 (9)
F1iv—Ir1—F1180.00 (11)F1xiv—Cs1—F1xv66.00 (9)
F1i—Ir1—F1v87.50 (10)F1x—Cs1—F1129.02 (2)
F1ii—Ir1—F1v92.50 (10)F1xi—Cs1—F163.06 (8)
F1iii—Ir1—F1v180.0F1xii—Cs1—F198.23 (4)
F1iv—Ir1—F1v87.50 (10)F1xiii—Cs1—F1118.14 (2)
F1—Ir1—F1v92.50 (10)F1xiv—Cs1—F1118.14 (2)
F1i—Ir1—Cs1vi53.317 (7)F1xv—Cs1—F1162.83 (9)
F1ii—Ir1—Cs1vi126.683 (7)F1x—Cs1—F1v98.23 (4)
F1iii—Ir1—Cs1vi123.86 (8)F1xi—Cs1—F1v63.06 (8)
F1iv—Ir1—Cs1vi53.317 (7)F1xii—Cs1—F1v129.02 (2)
F1—Ir1—Cs1vi126.683 (7)F1xiii—Cs1—F1v66.00 (9)
F1v—Ir1—Cs1vi56.14 (8)F1xiv—Cs1—F1v162.83 (9)
F1i—Ir1—Cs1vii126.683 (7)F1xv—Cs1—F1v118.14 (2)
F1ii—Ir1—Cs1vii53.317 (7)F1—Cs1—F1v52.74 (9)
F1iii—Ir1—Cs1vii56.14 (8)F1x—Cs1—F1xvi129.02 (2)
F1iv—Ir1—Cs1vii126.683 (7)F1xi—Cs1—F1xvi98.23 (4)
F1—Ir1—Cs1vii53.317 (7)F1xii—Cs1—F1xvi63.06 (8)
F1v—Ir1—Cs1vii123.86 (8)F1xiii—Cs1—F1xvi162.83 (9)
Cs1vi—Ir1—Cs1vii180.0F1xiv—Cs1—F1xvi52.74 (9)
F1i—Ir1—Cs1viii53.317 (7)F1xv—Cs1—F1xvi118.14 (2)
F1ii—Ir1—Cs1viii126.683 (7)F1—Cs1—F1xvi66.00 (9)
F1iii—Ir1—Cs1viii53.317 (7)F1v—Cs1—F1xvi118.14 (2)
F1iv—Ir1—Cs1viii123.86 (8)F1x—Cs1—F1xvii103.17 (7)
F1—Ir1—Cs1viii56.14 (8)F1xi—Cs1—F1xvii143.77 (3)
F1v—Ir1—Cs1viii126.683 (7)F1xii—Cs1—F1xvii143.77 (3)
Cs1vi—Ir1—Cs1viii106.101 (7)F1xiii—Cs1—F1xvii49.50 (7)
Cs1vii—Ir1—Cs1viii73.899 (7)F1xiv—Cs1—F1xvii85.78 (5)
F1i—Ir1—Cs1ix126.683 (7)F1xv—Cs1—F1xvii49.50 (7)
F1ii—Ir1—Cs1ix53.317 (7)F1—Cs1—F1xvii113.34 (3)
F1iii—Ir1—Cs1ix126.683 (7)F1v—Cs1—F1xvii85.78 (5)
F1iv—Ir1—Cs1ix56.14 (8)F1xvi—Cs1—F1xvii113.34 (3)
F1—Ir1—Cs1ix123.86 (8)F1x—Cs1—F1viii143.77 (3)
F1v—Ir1—Cs1ix53.317 (7)F1xi—Cs1—F1viii143.77 (3)
Cs1vi—Ir1—Cs1ix73.899 (7)F1xii—Cs1—F1viii103.17 (7)
Cs1vii—Ir1—Cs1ix106.101 (7)F1xiii—Cs1—F1viii113.34 (3)
Cs1viii—Ir1—Cs1ix180.0F1xiv—Cs1—F1viii49.50 (7)
F1i—Ir1—Cs156.14 (8)F1xv—Cs1—F1viii85.78 (5)
F1ii—Ir1—Cs1123.86 (8)F1—Cs1—F1viii85.78 (5)
F1iii—Ir1—Cs1126.683 (7)F1v—Cs1—F1viii113.34 (3)
F1iv—Ir1—Cs1126.683 (7)F1xvi—Cs1—F1viii49.50 (7)
F1—Ir1—Cs153.317 (7)F1xvii—Cs1—F1viii63.83 (7)
F1v—Ir1—Cs153.317 (7)F1x—Cs1—F1i143.77 (3)
Cs1vi—Ir1—Cs173.899 (7)F1xi—Cs1—F1i103.17 (7)
Cs1vii—Ir1—Cs1106.101 (7)F1xii—Cs1—F1i143.77 (3)
Cs1viii—Ir1—Cs173.899 (7)F1xiii—Cs1—F1i85.78 (5)
Cs1ix—Ir1—Cs1106.101 (7)F1xiv—Cs1—F1i113.34 (3)
F1i—Ir1—Cs1iv123.86 (8)F1xv—Cs1—F1i113.34 (3)
F1ii—Ir1—Cs1iv56.14 (8)F1—Cs1—F1i49.50 (7)
F1iii—Ir1—Cs1iv53.317 (7)F1v—Cs1—F1i49.50 (7)
F1iv—Ir1—Cs1iv53.317 (7)F1xvi—Cs1—F1i85.78 (5)
F1—Ir1—Cs1iv126.683 (7)F1xvii—Cs1—F1i63.83 (7)
F1v—Ir1—Cs1iv126.683 (7)F1viii—Cs1—F1i63.83 (7)
Cs1vi—Ir1—Cs1iv106.101 (7)Ir1—F1—Cs1xii162.69 (12)
Cs1vii—Ir1—Cs1iv73.899 (7)Ir1—F1—Cs1vii97.14 (4)
Cs1viii—Ir1—Cs1iv106.101 (7)Cs1xii—F1—Cs1vii81.77 (4)
Cs1ix—Ir1—Cs1iv73.899 (7)Ir1—F1—Cs197.14 (4)
Cs1—Ir1—Cs1iv180.0Cs1xii—F1—Cs181.77 (4)
F1x—Cs1—F1xi66.39 (7)Cs1vii—F1—Cs1162.83 (9)
F1x—Cs1—F1xii66.39 (7)Ir1—F1—Cs1viii94.15 (9)
F1xi—Cs1—F1xii66.39 (7)Cs1xii—F1—Cs1viii103.17 (7)
F1x—Cs1—F1xiii63.06 (8)Cs1vii—F1—Cs1viii94.22 (5)
F1xi—Cs1—F1xiii98.23 (4)Cs1—F1—Cs1viii94.22 (5)
Symmetry codes: (i) y, x+y, z+1; (ii) y, xy, z; (iii) xy, x, z+1; (iv) x, y, z+1; (v) x+y, x, z; (vi) x+1, y, z+1; (vii) x1, y, z; (viii) x+1, y+1, z+1; (ix) x1, y1, z; (x) xy+1, x, z; (xi) y, x+y, z; (xii) x+1, y+1, z; (xiii) y+1, xy, z; (xiv) x+y+1, x+1, z; (xv) x+1, y, z; (xvi) y+1, xy+1, z; (xvii) xy+1, x, z+1.

Experimental details

Crystal data
Chemical formulaCs2[IrF6]
Mr572.02
Crystal system, space groupTrigonal, P3m1
Temperature (K)296
a, c (Å)6.2421 (3), 5.0084 (5)
V3)169.00 (2)
Z1
Radiation typeMo Kα
µ (mm1)30.40
Crystal size (mm)0.08 × 0.06 × 0.04
Data collection
DiffractometerBruker–Nonius X8 APEX CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2004)
Tmin, Tmax0.134, 0.288
No. of measured, independent and
observed [I > 2σ(I)] reflections
1513, 211, 207
Rint0.019
(sin θ/λ)max1)0.704
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.013, 0.028, 1.06
No. of reflections211
No. of parameters13
Δρmax, Δρmin (e Å3)1.04, 0.49

Computer programs: APEX2 (Bruker, 2004), SAINT (Bruker, 2004), SHELXTL (Bruker, 2004), BS (Ozawa & Kang, 2004) and POV-RAY (Cason, 2002).

Selected bond lengths (Å) top
Ir1—F11.941 (2)Cs1—F13.1564 (4)
Cs1—F1i3.140 (2)Cs1—F1ii3.252 (3)
Symmetry codes: (i) y, x+y, z; (ii) y, x+y, z+1.
 

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