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Rb2[IrF6] possesses a framework structure constructed from Rb+ 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. Rb, 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/S1600536807059995/mg2039sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807059995/mg2039Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 296 K
  • Mean [sigma](Ir-F) = 0.002 Å
  • R factor = 0.009
  • wR factor = 0.024
  • Data-to-parameter ratio = 13.9

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT731_ALERT_1_B Bond Calc 3.0101(16), Rep 3.0101(3) ...... 5.33 su-Ra RB1 -F1 1.555 1.655 PLAT731_ALERT_1_B Bond Calc 3.010(2), Rep 3.0101(3) ...... 6.67 su-Ra RB1 -F1 1.555 2.655 PLAT731_ALERT_1_B Bond Calc 3.0101(15), Rep 3.0101(3) ...... 5.00 su-Ra RB1 -F1 1.555 3.665 PLAT731_ALERT_1_B Bond Calc 3.0101(16), Rep 3.0101(3) ...... 5.33 su-Ra RB1 -F1 1.555 3.555 PLAT731_ALERT_1_B Bond Calc 3.010(2), Rep 3.0101(3) ...... 6.67 su-Ra RB1 -F1 1.555 2.665 PLAT731_ALERT_1_B Bond Calc 3.0101(16), Rep 3.0101(3) ...... 5.33 su-Ra RB1 -F1 1.555 1.555 PLAT731_ALERT_1_B Bond Calc 3.0101(16), Rep 3.0101(3) ...... 5.33 su-Ra F1 -RB1 1.555 1.455
Alert level G ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 1.069 Tmax scaled 0.097 Tmin scaled 0.079
0 ALERT level A = In general: serious problem 7 ALERT level B = Potentially serious problem 0 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 7 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 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Comment top

In Rb2[IrF6], the Rb+ cation is coordinated to twelve F atoms belonging to six anions, forming a slightly distorted anticuboctahedron. Each anion, in the form of a nearly ideal octahedron, interconnects twelve cations (Fig. 1). The Rb–F distances have slightly different values. Anticuboctahedra share all their rectangular faces and two triangular faces with each other, and share three other triangular faces with octahedra, giving rise to the framework structure (Fig. 2).

Related literature top

The title compound was first characterized by X-ray powder diffraction (Babel, 1967). It is isomorphous with the potassium (K2[IrF6]; Fitz et al., 2002) and caesium analogues (Cs2[IrF6]; Smolentsev, Gubanov, Naumov & Danilenko, 2007). The alkaline earth metal hexafluoridoiridates Ca[IrF6]·2H2O, Sr[IrF6]·2H2O and Ba[IrF6] were recently reported (Smolentsev, Gubanov & Danilenko, 2007).

Experimental top

Rb2CO3 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 0.84 Å and 0.81 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 Rb2[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 Rb2[IrF6], viewed in perspective, with Rb-centered anticuboctahedra (orange) and Ir-centered octahedra (purple).
Rubidium hexafluoridoiridate(IV) top
Crystal data top
Rb2[IrF6]Dx = 5.351 Mg m3
Mr = 477.14Mo Kα radiation, λ = 0.71073 Å
Trigonal, P3m1Cell parameters from 1219 reflections
Hall symbol: -P 3 2"θ = 3.9–29.7°
a = 5.9718 (2) ŵ = 38.91 mm1
c = 4.7939 (2) ÅT = 296 K
V = 148.06 (1) Å3Needle, light-pink
Z = 10.14 × 0.06 × 0.06 mm
F(000) = 205
Data collection top
Bruker–Nonius X8 APEX CCD area-detector
diffractometer
181 independent reflections
Radiation source: fine-focus sealed tube180 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.018
Detector resolution: 25 pixels mm-1θmax = 29.9°, θmin = 3.9°
ϕ scansh = 88
Absorption correction: multi-scan
(SADABS; Bruker, 2004)
k = 88
Tmin = 0.074, Tmax = 0.091l = 63
1328 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)] = 0.009 w = 1/[σ2(Fo2) + (0.0105P)2 + 0.2201P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.024(Δ/σ)max < 0.001
S = 1.21Δρmax = 0.60 e Å3
181 reflectionsΔρmin = 1.16 e Å3
13 parametersExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.029 (2)
Crystal data top
Rb2[IrF6]Z = 1
Mr = 477.14Mo Kα radiation
Trigonal, P3m1µ = 38.91 mm1
a = 5.9718 (2) ÅT = 296 K
c = 4.7939 (2) Å0.14 × 0.06 × 0.06 mm
V = 148.06 (1) Å3
Data collection top
Bruker–Nonius X8 APEX CCD area-detector
diffractometer
181 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2004)
180 reflections with I > 2σ(I)
Tmin = 0.074, Tmax = 0.091Rint = 0.018
1328 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.00913 parameters
wR(F2) = 0.0240 restraints
S = 1.21Δρmax = 0.60 e Å3
181 reflectionsΔρmin = 1.16 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
Ir10.00000.00000.50000.01235 (12)
Rb10.66670.33330.20338 (12)0.01942 (13)
F10.15652 (18)0.3130 (4)0.2798 (4)0.0224 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ir10.01143 (13)0.01143 (13)0.01420 (16)0.00571 (7)0.0000.000
Rb10.01815 (17)0.01815 (17)0.0219 (2)0.00908 (8)0.0000.000
F10.0230 (7)0.0175 (9)0.0249 (8)0.0088 (4)0.0032 (4)0.0065 (7)
Geometric parameters (Å, º) top
Ir1—F1i1.9328 (19)Rb1—F1xi3.0101 (3)
Ir1—F1ii1.9328 (19)Rb1—F1iii3.0101 (3)
Ir1—F1iii1.9328 (19)Rb1—F1xii3.0101 (3)
Ir1—F1iv1.9328 (19)Rb1—F13.0101 (3)
Ir1—F11.9328 (19)Rb1—F1xiii3.080 (2)
Ir1—F1v1.9328 (19)Rb1—F1xiv3.080 (2)
Rb1—F1vi2.9511 (19)Rb1—F1ii3.080 (2)
Rb1—F1vii2.9511 (19)F1—Rb1xv2.9511 (19)
Rb1—F1viii2.9511 (19)F1—Rb1xvi3.0101 (3)
Rb1—F1ix3.0101 (3)F1—Rb1xvii3.080 (2)
Rb1—F1x3.0101 (3)
F1i—Ir1—F1ii180.00 (10)F1ix—Rb1—F1165.46 (7)
F1i—Ir1—F1iii93.01 (8)F1x—Rb1—F1118.542 (16)
F1ii—Ir1—F1iii86.99 (8)F1xi—Rb1—F1118.542 (16)
F1i—Ir1—F1iv86.99 (8)F1iii—Rb1—F155.52 (7)
F1ii—Ir1—F1iv93.01 (8)F1xii—Rb1—F163.49 (7)
F1iii—Ir1—F1iv180.0F1vi—Rb1—F1xiii105.27 (6)
F1i—Ir1—F193.01 (8)F1vii—Rb1—F1xiii144.63 (2)
F1ii—Ir1—F186.99 (8)F1viii—Rb1—F1xiii144.63 (2)
F1iii—Ir1—F193.01 (8)F1ix—Rb1—F1xiii51.80 (6)
F1iv—Ir1—F186.99 (8)F1x—Rb1—F1xiii51.80 (6)
F1i—Ir1—F1v86.99 (8)F1xi—Rb1—F1xiii85.57 (4)
F1ii—Ir1—F1v93.01 (8)F1iii—Rb1—F1xiii85.57 (4)
F1iii—Ir1—F1v86.99 (8)F1xii—Rb1—F1xiii113.70 (3)
F1iv—Ir1—F1v93.01 (8)F1—Rb1—F1xiii113.70 (3)
F1—Ir1—F1v180.00 (9)F1vi—Rb1—F1xiv144.63 (2)
F1vi—Rb1—F1vii64.92 (6)F1vii—Rb1—F1xiv144.63 (2)
F1vi—Rb1—F1viii64.92 (6)F1viii—Rb1—F1xiv105.27 (6)
F1vii—Rb1—F1viii64.92 (6)F1ix—Rb1—F1xiv85.57 (4)
F1vi—Rb1—F1ix63.40 (7)F1x—Rb1—F1xiv113.70 (3)
F1vii—Rb1—F1ix128.10 (2)F1xi—Rb1—F1xiv51.80 (6)
F1viii—Rb1—F1ix96.72 (4)F1iii—Rb1—F1xiv113.70 (3)
F1vi—Rb1—F1x63.40 (7)F1xii—Rb1—F1xiv51.80 (6)
F1vii—Rb1—F1x96.72 (4)F1—Rb1—F1xiv85.57 (4)
F1viii—Rb1—F1x128.10 (2)F1xiii—Rb1—F1xiv61.90 (6)
F1ix—Rb1—F1x55.52 (7)F1vi—Rb1—F1ii144.63 (2)
F1vi—Rb1—F1xi96.72 (4)F1vii—Rb1—F1ii105.27 (6)
F1vii—Rb1—F1xi128.10 (2)F1viii—Rb1—F1ii144.63 (2)
F1viii—Rb1—F1xi63.40 (7)F1ix—Rb1—F1ii113.70 (3)
F1ix—Rb1—F1xi63.49 (7)F1x—Rb1—F1ii85.57 (4)
F1x—Rb1—F1xi118.542 (16)F1xi—Rb1—F1ii113.70 (3)
F1vi—Rb1—F1iii96.72 (4)F1iii—Rb1—F1ii51.80 (6)
F1vii—Rb1—F1iii63.40 (7)F1xii—Rb1—F1ii85.57 (4)
F1viii—Rb1—F1iii128.10 (2)F1—Rb1—F1ii51.80 (6)
F1ix—Rb1—F1iii118.542 (16)F1xiii—Rb1—F1ii61.90 (6)
F1x—Rb1—F1iii63.49 (7)F1xiv—Rb1—F1ii61.90 (6)
F1xi—Rb1—F1iii165.46 (7)Ir1—F1—Rb1xv161.40 (10)
F1vi—Rb1—F1xii128.10 (2)Ir1—F1—Rb1xvi95.49 (4)
F1vii—Rb1—F1xii96.72 (4)Rb1xv—F1—Rb1xvi83.28 (4)
F1viii—Rb1—F1xii63.40 (7)Ir1—F1—Rb195.49 (4)
F1ix—Rb1—F1xii118.542 (16)Rb1xv—F1—Rb183.28 (4)
F1x—Rb1—F1xii165.46 (7)Rb1xvi—F1—Rb1165.46 (7)
F1xi—Rb1—F1xii55.52 (7)Ir1—F1—Rb1xvii93.32 (7)
F1iii—Rb1—F1xii118.542 (16)Rb1xv—F1—Rb1xvii105.27 (6)
F1vi—Rb1—F1128.10 (2)Rb1xvi—F1—Rb1xvii94.43 (4)
F1vii—Rb1—F163.40 (7)Rb1—F1—Rb1xvii94.43 (4)
F1viii—Rb1—F196.72 (4)
Symmetry codes: (i) y, xy, z; (ii) y, x+y, z+1; (iii) x+y, x, z; (iv) xy, x, z+1; (v) x, y, z+1; (vi) xy+1, x, z; (vii) y, x+y, z; (viii) x+1, y+1, z; (ix) x+1, y, z; (x) y+1, xy, z; (xi) x+y+1, x+1, z; (xii) y+1, xy+1, z; (xiii) xy+1, x, z+1; (xiv) x+1, y+1, z+1; (xv) xy, y+1, z; (xvi) x1, y, z; (xvii) xy, y+1, z+1.

Experimental details

Crystal data
Chemical formulaRb2[IrF6]
Mr477.14
Crystal system, space groupTrigonal, P3m1
Temperature (K)296
a, c (Å)5.9718 (2), 4.7939 (2)
V3)148.06 (1)
Z1
Radiation typeMo Kα
µ (mm1)38.91
Crystal size (mm)0.14 × 0.06 × 0.06
Data collection
DiffractometerBruker–Nonius X8 APEX CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2004)
Tmin, Tmax0.074, 0.091
No. of measured, independent and
observed [I > 2σ(I)] reflections
1328, 181, 180
Rint0.018
(sin θ/λ)max1)0.702
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.009, 0.024, 1.21
No. of reflections181
No. of parameters13
Δρmax, Δρmin (e Å3)0.60, 1.16

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

Selected bond lengths (Å) top
Ir1—F11.9328 (19)Rb1—F13.0101 (3)
Rb1—F1i2.9511 (19)Rb1—F1ii3.080 (2)
Symmetry codes: (i) y, x+y, z; (ii) y, x+y, z+1.
 

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