Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807059995/mg2039sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807059995/mg2039Isup2.hkl |
Key indicators
- Single-crystal X-ray study
- T = 296 K
- Mean (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
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).
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).
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).
Rb2[IrF6] | Dx = 5.351 Mg m−3 |
Mr = 477.14 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, P3m1 | Cell parameters from 1219 reflections |
Hall symbol: -P 3 2" | θ = 3.9–29.7° |
a = 5.9718 (2) Å | µ = 38.91 mm−1 |
c = 4.7939 (2) Å | T = 296 K |
V = 148.06 (1) Å3 | Needle, light-pink |
Z = 1 | 0.14 × 0.06 × 0.06 mm |
F(000) = 205 |
Bruker–Nonius X8 APEX CCD area-detector diffractometer | 181 independent reflections |
Radiation source: fine-focus sealed tube | 180 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.018 |
Detector resolution: 25 pixels mm-1 | θmax = 29.9°, θmin = 3.9° |
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 on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary 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 = 1.21 | Δρmax = 0.60 e Å−3 |
181 reflections | Δρmin = −1.16 e Å−3 |
13 parameters | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
0 restraints | Extinction coefficient: 0.029 (2) |
Rb2[IrF6] | Z = 1 |
Mr = 477.14 | Mo Kα radiation |
Trigonal, P3m1 | µ = 38.91 mm−1 |
a = 5.9718 (2) Å | T = 296 K |
c = 4.7939 (2) Å | 0.14 × 0.06 × 0.06 mm |
V = 148.06 (1) Å3 |
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 |
R[F2 > 2σ(F2)] = 0.009 | 13 parameters |
wR(F2) = 0.024 | 0 restraints |
S = 1.21 | Δρmax = 0.60 e Å−3 |
181 reflections | Δρmin = −1.16 e Å−3 |
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. |
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) |
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) |
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. |
Experimental details
Crystal data | |
Chemical formula | Rb2[IrF6] |
Mr | 477.14 |
Crystal system, space group | Trigonal, P3m1 |
Temperature (K) | 296 |
a, c (Å) | 5.9718 (2), 4.7939 (2) |
V (Å3) | 148.06 (1) |
Z | 1 |
Radiation type | Mo Kα |
µ (mm−1) | 38.91 |
Crystal size (mm) | 0.14 × 0.06 × 0.06 |
Data collection | |
Diffractometer | Bruker–Nonius X8 APEX CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Bruker, 2004) |
Tmin, Tmax | 0.074, 0.091 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 1328, 181, 180 |
Rint | 0.018 |
(sin θ/λ)max (Å−1) | 0.702 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.009, 0.024, 1.21 |
No. of reflections | 181 |
No. of parameters | 13 |
Δρmax, Δρmin (e Å−3) | 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).
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. |
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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).