supplementary materials
Rubidium hexafluoridoiridate(IV)
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, 
m and m symmetry, respectively.
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).
The maximum peak and deepest hole are located 0.84 Å and 0.81 Å, both from Ir1.
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).
Rubidium hexafluoridoiridate(IV)
top
Crystal data top
| Rb2[IrF6] | Z = 1 |
| Mr = 477.14 | F000 = 205 |
| Trigonal, P3m1 | Dx = 5.351 Mg m−3 |
| Hall symbol: -P 3 2" | Mo Kα radiation
λ = 0.71073 Å |
| a = 5.9718 (2) Å | Cell parameters from 1219 reflections |
| b = 5.9718 (2) Å | θ = 3.9–29.7º |
| c = 4.7939 (2) Å | µ = 38.91 mm−1 |
| α = 90º | T = 296 (2) K |
| β = 90º | Needle, light-pink |
| γ = 120º | 0.14 × 0.06 × 0.06 mm |
| V = 148.057 (9) Å3 | |
Data collection top
Bruker–Nonius X8 APEX CCD area-detector
diffractometer | 181 independent reflections |
| Radiation source: fine-focus sealed tube | 180 reflections with I > 2σ(I) |
| Monochromator: graphite | Rint = 0.018 |
| Detector resolution: 25 pixels mm-1 | θmax = 29.9º |
| T = 296(2) K | θmin = 3.9º |
| φ scans | h = −8→8 |
Absorption correction: multi-scan
(SADABS; Bruker, 2004) | k = −8→8 |
| Tmin = 0.074, Tmax = 0.091 | l = −6→3 |
| 1328 measured reflections | |
Refinement top
| Refinement on F2 | Secondary atom site location: difference Fourier map |
| Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0105P)2 + 0.2201P]
where P = (Fo2 + 2Fc2)/3 |
| R[F2 > 2σ(F2)] = 0.009 | (Δ/σ)max < 0.001 |
| wR(F2) = 0.024 | Δρmax = 0.60 e Å−3 |
| S = 1.21 | Δρmin = −1.16 e Å−3 |
| 181 reflections | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
| 13 parameters | Extinction coefficient: 0.029 (2) |
| Primary atom site location: structure-invariant direct methods | |
Crystal data top
| Rb2[IrF6] | γ = 120º |
| Mr = 477.14 | V = 148.057 (9) Å3 |
| Trigonal, P3m1 | Z = 1 |
| a = 5.9718 (2) Å | Mo Kα |
| b = 5.9718 (2) Å | µ = 38.91 mm−1 |
| c = 4.7939 (2) Å | T = 296 (2) K |
| α = 90º | 0.14 × 0.06 × 0.06 mm |
| β = 90º | |
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 = 0.091 | Rint = 0.018 |
| 1328 measured reflections | |
Refinement top
| R[F2 > 2σ(F2)] = 0.009 | 13 parameters |
| wR(F2) = 0.024 | Δρmax = 0.60 e Å−3 |
| S = 1.21 | Δρmin = −1.16 e Å−3 |
| 181 reflections | |
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 > 2sigma(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| | x | y | z | Uiso*/Ueq | |
| Ir1 | 0.0000 | 0.0000 | 0.5000 | 0.01235 (12) | |
| Rb1 | 0.6667 | 0.3333 | 0.20338 (12) | 0.01942 (13) | |
| F1 | 0.15652 (18) | 0.3130 (4) | 0.2798 (4) | 0.0224 (4) | |
Atomic displacement parameters (Å2) top| | U11 | U22 | U33 | U12 | U13 | U23 |
| Ir1 | 0.01143 (13) | 0.01143 (13) | 0.01420 (16) | 0.00571 (7) | 0.000 | 0.000 |
| Rb1 | 0.01815 (17) | 0.01815 (17) | 0.0219 (2) | 0.00908 (8) | 0.000 | 0.000 |
| F1 | 0.0230 (7) | 0.0175 (9) | 0.0249 (8) | 0.0088 (4) | 0.0032 (4) | 0.0065 (7) |
Geometric parameters (Å, °) top
| Ir1—F1i | 1.9328 (19) | Rb1—F1xi | 3.0101 (3) |
| Ir1—F1ii | 1.9328 (19) | Rb1—F1iii | 3.0101 (3) |
| Ir1—F1iii | 1.9328 (19) | Rb1—F1xii | 3.0101 (3) |
| Ir1—F1iv | 1.9328 (19) | Rb1—F1 | 3.0101 (3) |
| Ir1—F1 | 1.9328 (19) | Rb1—F1xiii | 3.080 (2) |
| Ir1—F1v | 1.9328 (19) | Rb1—F1xiv | 3.080 (2) |
| Rb1—F1vi | 2.9511 (19) | Rb1—F1ii | 3.080 (2) |
| Rb1—F1vii | 2.9511 (19) | F1—Rb1xv | 2.9511 (19) |
| Rb1—F1viii | 2.9511 (19) | F1—Rb1xvi | 3.0101 (3) |
| Rb1—F1ix | 3.0101 (3) | F1—Rb1xvii | 3.080 (2) |
| Rb1—F1x | 3.0101 (3) | | |
| | | |
| F1i—Ir1—F1ii | 180.00 (10) | F1ix—Rb1—F1 | 165.46 (7) |
| F1i—Ir1—F1iii | 93.01 (8) | F1x—Rb1—F1 | 118.542 (16) |
| F1ii—Ir1—F1iii | 86.99 (8) | F1xi—Rb1—F1 | 118.542 (16) |
| F1i—Ir1—F1iv | 86.99 (8) | F1iii—Rb1—F1 | 55.52 (7) |
| F1ii—Ir1—F1iv | 93.01 (8) | F1xii—Rb1—F1 | 63.49 (7) |
| F1iii—Ir1—F1iv | 180.0 | F1vi—Rb1—F1xiii | 105.27 (6) |
| F1i—Ir1—F1 | 93.01 (8) | F1vii—Rb1—F1xiii | 144.63 (2) |
| F1ii—Ir1—F1 | 86.99 (8) | F1viii—Rb1—F1xiii | 144.63 (2) |
| F1iii—Ir1—F1 | 93.01 (8) | F1ix—Rb1—F1xiii | 51.80 (6) |
| F1iv—Ir1—F1 | 86.99 (8) | F1x—Rb1—F1xiii | 51.80 (6) |
| F1i—Ir1—F1v | 86.99 (8) | F1xi—Rb1—F1xiii | 85.57 (4) |
| F1ii—Ir1—F1v | 93.01 (8) | F1iii—Rb1—F1xiii | 85.57 (4) |
| F1iii—Ir1—F1v | 86.99 (8) | F1xii—Rb1—F1xiii | 113.70 (3) |
| F1iv—Ir1—F1v | 93.01 (8) | F1—Rb1—F1xiii | 113.70 (3) |
| F1—Ir1—F1v | 180.00 (9) | F1vi—Rb1—F1xiv | 144.63 (2) |
| F1vi—Rb1—F1vii | 64.92 (6) | F1vii—Rb1—F1xiv | 144.63 (2) |
| F1vi—Rb1—F1viii | 64.92 (6) | F1viii—Rb1—F1xiv | 105.27 (6) |
| F1vii—Rb1—F1viii | 64.92 (6) | F1ix—Rb1—F1xiv | 85.57 (4) |
| F1vi—Rb1—F1ix | 63.40 (7) | F1x—Rb1—F1xiv | 113.70 (3) |
| F1vii—Rb1—F1ix | 128.10 (2) | F1xi—Rb1—F1xiv | 51.80 (6) |
| F1viii—Rb1—F1ix | 96.72 (4) | F1iii—Rb1—F1xiv | 113.70 (3) |
| F1vi—Rb1—F1x | 63.40 (7) | F1xii—Rb1—F1xiv | 51.80 (6) |
| F1vii—Rb1—F1x | 96.72 (4) | F1—Rb1—F1xiv | 85.57 (4) |
| F1viii—Rb1—F1x | 128.10 (2) | F1xiii—Rb1—F1xiv | 61.90 (6) |
| F1ix—Rb1—F1x | 55.52 (7) | F1vi—Rb1—F1ii | 144.63 (2) |
| F1vi—Rb1—F1xi | 96.72 (4) | F1vii—Rb1—F1ii | 105.27 (6) |
| F1vii—Rb1—F1xi | 128.10 (2) | F1viii—Rb1—F1ii | 144.63 (2) |
| F1viii—Rb1—F1xi | 63.40 (7) | F1ix—Rb1—F1ii | 113.70 (3) |
| F1ix—Rb1—F1xi | 63.49 (7) | F1x—Rb1—F1ii | 85.57 (4) |
| F1x—Rb1—F1xi | 118.542 (16) | F1xi—Rb1—F1ii | 113.70 (3) |
| F1vi—Rb1—F1iii | 96.72 (4) | F1iii—Rb1—F1ii | 51.80 (6) |
| F1vii—Rb1—F1iii | 63.40 (7) | F1xii—Rb1—F1ii | 85.57 (4) |
| F1viii—Rb1—F1iii | 128.10 (2) | F1—Rb1—F1ii | 51.80 (6) |
| F1ix—Rb1—F1iii | 118.542 (16) | F1xiii—Rb1—F1ii | 61.90 (6) |
| F1x—Rb1—F1iii | 63.49 (7) | F1xiv—Rb1—F1ii | 61.90 (6) |
| F1xi—Rb1—F1iii | 165.46 (7) | Ir1—F1—Rb1xv | 161.40 (10) |
| F1vi—Rb1—F1xii | 128.10 (2) | Ir1—F1—Rb1xvi | 95.49 (4) |
| F1vii—Rb1—F1xii | 96.72 (4) | Rb1xv—F1—Rb1xvi | 83.28 (4) |
| F1viii—Rb1—F1xii | 63.40 (7) | Ir1—F1—Rb1 | 95.49 (4) |
| F1ix—Rb1—F1xii | 118.542 (16) | Rb1xv—F1—Rb1 | 83.28 (4) |
| F1x—Rb1—F1xii | 165.46 (7) | Rb1xvi—F1—Rb1 | 165.46 (7) |
| F1xi—Rb1—F1xii | 55.52 (7) | Ir1—F1—Rb1xvii | 93.32 (7) |
| F1iii—Rb1—F1xii | 118.542 (16) | Rb1xv—F1—Rb1xvii | 105.27 (6) |
| F1vi—Rb1—F1 | 128.10 (2) | Rb1xvi—F1—Rb1xvii | 94.43 (4) |
| F1vii—Rb1—F1 | 63.40 (7) | Rb1—F1—Rb1xvii | 94.43 (4) |
| F1viii—Rb1—F1 | 96.72 (4) | | |
| Symmetry codes: (i) −y, x−y, z; (ii) y, −x+y, −z+1; (iii) −x+y, −x, z; (iv) x−y, x, −z+1; (v) −x, −y, −z+1; (vi) x−y+1, x, −z; (vii) y, −x+y, −z; (viii) −x+1, −y+1, −z; (ix) x+1, y, z; (x) −y+1, x−y, z; (xi) −x+y+1, −x+1, z; (xii) −y+1, x−y+1, z; (xiii) x−y+1, x, −z+1; (xiv) −x+1, −y+1, −z+1; (xv) x−y, −y+1, −z; (xvi) x−1, y, z; (xvii) x−y, −y+1, −z+1. |
Selected geometric parameters (Å) top| Ir1—F1 | 1.9328 (19) | Rb1—F1 | 3.0101 (3) |
| Rb1—F1i | 2.9511 (19) | Rb1—F1ii | 3.080 (2) |
| Symmetry codes: (i) y, −x+y, −z; (ii) y, −x+y, −z+1. |
(type here to add acknowledgements)
Babel, D. (1967). Structure and Bonding, Vol.3, pp. 1-87. Berlin, Heidelberg, New York: Springer-Verlag.
Bruker (2004). APEX2 (Version 1.08), SAINT (Version 7.03), SADABS (Version 2.11) and SHELXTL (Version 6.12). Bruker AXS Inc., Madison, Wisconsin, USA.
Cason, C. J. (2002). POV-RAY for Windows. Version 3.5. (URL: http://www.povray.org)
Fitz, H., Müller, B. G., Graudejus, O. & Bartlett, N. (2002). Z. Anorg. Allg. Chem. 628, 133–137.
Ozawa, T. C. & Kang, S. J. (2004). Balls & Sticks (BS). Version 1.51. (URL: http://www.softbug.com/toycrate/bs)
Smolentsev, A. I., Gubanov, A. I. & Danilenko, A. M. (2007). Acta Cryst. C63, i99–i101.
Smolentsev, A. I., Gubanov, A. I., Naumov, D. Yu. & Danilenko, A. M. (2007). Acta Cryst. E63 MG2040
![[Figure 1]](./mg2039fig1thm.gif)
![[Figure 2]](./mg2039fig2thm.gif)
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).