Single crystals of rubidium tetrafluoridobromate(III), RbBrF4, were grown by melting and recrystallizing RbBrF4 from its melt. This is the first determination of the crystal structure of RbBrF4 using single-crystal X-ray diffraction data. We confirmed that the structure contains square-planar [BrF4]− anions and rubidium cations that are coordinated by F atoms in a square-antiprismatic manner. The compound crystallizes in the KBrF4 structure type. Atomic coordinates and bond lengths and angles were determined with higher precision than in a previous report based on powder X-ray diffraction data [Ivlev et al. (2015). Z. Anorg. Allg. Chem. 641, 2593–2598].
Supporting information
CCDC reference: 1968250
Key indicators
- Single-crystal X-ray study
- T = 100 K
- Mean
(Br-F) = 0.001 Å
- R factor = 0.020
- wR factor = 0.038
- Data-to-parameter ratio = 24.8
checkCIF/PLATON results
No syntax errors found
Alert level C
DENSX01_ALERT_1_C The ratio of the calculated to measured crystal density
lies outside the range 0.95 <> 1.05
Calculated density = 3.524
Measured density = 3.330
PLAT906_ALERT_3_C Large K Value in the Analysis of Variance ...... 17.413 Check
| Author Response: The reported large K value belongs to the weakest reflections, which
are likely to be high in number in RbBrF4 due to very similar scattering
factors of rubidium and bromine.
|
PLAT906_ALERT_3_C Large K Value in the Analysis of Variance ...... 3.678 Check
| Author Response: The reported large K value belongs to the weakest reflections, which
are likely to be high in number in RbBrF4 due to very similar scattering
factors of rubidium and bromine.
|
PLAT906_ALERT_3_C Large K Value in the Analysis of Variance ...... 2.436 Check
| Author Response: The reported large K value belongs to the weakest reflections, which
are likely to be high in number in RbBrF4 due to very similar scattering
factors of rubidium and bromine.
|
Alert level G
PLAT042_ALERT_1_G Calc. and Reported MoietyFormula Strings Differ Please Check
PLAT045_ALERT_1_G Calculated and Reported Z Differ by a Factor ... 0.50 Check
PLAT304_ALERT_4_G Non-Integer Number of Atoms in ...... Resd 1 4.38 Check
PLAT304_ALERT_4_G Non-Integer Number of Atoms in ...... Resd 2 0.12 Check
PLAT955_ALERT_1_G Reported (CIF) and Actual (FCF) Lmax Differ by . 1 Units
0 ALERT level A = Most likely a serious problem - resolve or explain
0 ALERT level B = A potentially serious problem, consider carefully
4 ALERT level C = Check. Ensure it is not caused by an omission or oversight
5 ALERT level G = General information/check it is not something unexpected
4 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
3 ALERT type 3 Indicator that the structure quality may be low
2 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: APEX3 (Bruker, 2018); cell refinement: APEX3 (Bruker, 2018); data reduction: APEX3 (Bruker, 2018); program(s) used to solve structure: SHELXT (Sheldrick, 2015a); program(s) used to refine structure: SHELXL (Sheldrick, 2015b); molecular graphics: DIAMOND (Brandenburg, 2018); software used to prepare material for publication: publCIF (Westrip, 2010).
Rubidium tetrafluoridobromate(III)
top
Crystal data top
RbBrF4 | Dx = 3.524 Mg m−3 Dm = 3.33 Mg m−3 Dm measured by helium pycnometry |
Mr = 241.38 | Mo Kα radiation, λ = 0.71073 Å |
Tetragonal, I4/mcm | Cell parameters from 285 reflections |
a = 6.2991 (5) Å | θ = 4.5–31.3° |
c = 11.4659 (10) Å | µ = 19.61 mm−1 |
V = 454.95 (8) Å3 | T = 100 K |
Z = 4 | Plate, colorless |
F(000) = 432 | 0.19 × 0.14 × 0.03 mm |
Data collection top
Bruker D8 QUEST area detector diffractometer | 322 independent reflections |
Radiation source: microfocus sealed X-ray tube, Incoatec Iµs | 189 reflections with I > 2σ(I) |
Detector resolution: 7.9 pixels mm-1 | Rint = 0.070 |
ω and φ scans | θmax = 36.3°, θmin = 3.6° |
Absorption correction: multi-scan (SADABS; Krause et al., 2015) | h = −9→10 |
Tmin = 0.151, Tmax = 0.480 | k = −9→10 |
5872 measured reflections | l = −19→19 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.004P)2 + 1.2951P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.020 | (Δ/σ)max < 0.001 |
wR(F2) = 0.038 | Δρmax = 0.66 e Å−3 |
S = 1.06 | Δρmin = −0.73 e Å−3 |
322 reflections | Extinction correction: SHELXL (Sheldrick, 2015b), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
13 parameters | Extinction coefficient: 0.0016 (3) |
0 restraints | |
Special details top
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Br1 | 0.500000 | 0.000000 | 0.500000 | 0.00663 (14) | |
Rb1 | 0.500000 | 0.500000 | 0.750000 | 0.00956 (15) | |
F1 | 0.6501 (2) | 0.1501 (2) | 0.61660 (13) | 0.0138 (3) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Br1 | 0.00693 (19) | 0.00693 (19) | 0.0060 (2) | 0.0008 (2) | 0.000 | 0.000 |
Rb1 | 0.0099 (2) | 0.0099 (2) | 0.0088 (2) | 0.000 | 0.000 | 0.000 |
F1 | 0.0147 (5) | 0.0147 (5) | 0.0120 (7) | −0.0003 (8) | −0.0047 (5) | −0.0047 (5) |
Geometric parameters (Å, º) top
Br1—F1 | 1.8905 (16) | Rb1—F1viii | 2.8447 (10) |
Br1—F1i | 1.8906 (16) | Rb1—F1ix | 2.8447 (9) |
Br1—F1ii | 1.8906 (16) | Rb1—F1x | 2.8447 (9) |
Br1—F1iii | 1.8906 (16) | Rb1—F1 | 2.8447 (9) |
Rb1—F1iv | 2.8447 (10) | Rb1—Rb1xi | 4.4541 (4) |
Rb1—F1v | 2.8447 (10) | Rb1—Rb1xii | 4.4541 (4) |
Rb1—F1vi | 2.8447 (10) | Rb1—Rb1xiii | 4.4541 (4) |
Rb1—F1vii | 2.8447 (10) | Rb1—Rb1vi | 4.4541 (4) |
| | | |
F1—Br1—F1i | 180.0 | F1viii—Rb1—Rb1xi | 141.53 (2) |
F1—Br1—F1ii | 90.01 (10) | F1ix—Rb1—Rb1xi | 71.76 (3) |
F1i—Br1—F1ii | 89.99 (10) | F1x—Rb1—Rb1xi | 108.24 (3) |
F1—Br1—F1iii | 89.99 (10) | F1—Rb1—Rb1xi | 71.76 (3) |
F1i—Br1—F1iii | 90.01 (10) | F1iv—Rb1—Rb1xii | 38.47 (2) |
F1ii—Br1—F1iii | 180.0 | F1v—Rb1—Rb1xii | 141.53 (2) |
F1iv—Rb1—F1v | 143.52 (7) | F1vi—Rb1—Rb1xii | 71.76 (3) |
F1iv—Rb1—F1vi | 73.20 (3) | F1vii—Rb1—Rb1xii | 141.53 (2) |
F1v—Rb1—F1vi | 141.19 (6) | F1viii—Rb1—Rb1xii | 38.47 (2) |
F1iv—Rb1—F1vii | 114.95 (5) | F1ix—Rb1—Rb1xii | 108.24 (3) |
F1v—Rb1—F1vii | 76.95 (5) | F1x—Rb1—Rb1xii | 71.76 (3) |
F1vi—Rb1—F1vii | 73.20 (3) | F1—Rb1—Rb1xii | 108.24 (3) |
F1iv—Rb1—F1viii | 76.95 (5) | Rb1xi—Rb1—Rb1xii | 180.0 |
F1v—Rb1—F1viii | 114.95 (5) | F1iv—Rb1—Rb1xiii | 71.76 (3) |
F1vi—Rb1—F1viii | 78.41 (7) | F1v—Rb1—Rb1xiii | 71.76 (3) |
F1vii—Rb1—F1viii | 143.52 (7) | F1vi—Rb1—Rb1xiii | 141.53 (2) |
F1iv—Rb1—F1ix | 73.20 (3) | F1vii—Rb1—Rb1xiii | 108.24 (3) |
F1v—Rb1—F1ix | 78.41 (7) | F1viii—Rb1—Rb1xiii | 108.24 (3) |
F1vi—Rb1—F1ix | 114.95 (5) | F1ix—Rb1—Rb1xiii | 38.47 (2) |
F1vii—Rb1—F1ix | 73.20 (3) | F1x—Rb1—Rb1xiii | 38.47 (2) |
F1viii—Rb1—F1ix | 141.19 (6) | F1—Rb1—Rb1xiii | 141.53 (2) |
F1iv—Rb1—F1x | 78.41 (7) | Rb1xi—Rb1—Rb1xiii | 90.0 |
F1v—Rb1—F1x | 73.20 (3) | Rb1xii—Rb1—Rb1xiii | 90.0 |
F1vi—Rb1—F1x | 143.52 (7) | F1iv—Rb1—Rb1vi | 108.24 (3) |
F1vii—Rb1—F1x | 141.19 (6) | F1v—Rb1—Rb1vi | 108.24 (3) |
F1viii—Rb1—F1x | 73.20 (3) | F1vi—Rb1—Rb1vi | 38.47 (2) |
F1ix—Rb1—F1x | 76.95 (5) | F1vii—Rb1—Rb1vi | 71.76 (3) |
F1iv—Rb1—F1 | 141.19 (6) | F1viii—Rb1—Rb1vi | 71.76 (3) |
F1v—Rb1—F1 | 73.19 (3) | F1ix—Rb1—Rb1vi | 141.53 (2) |
F1vi—Rb1—F1 | 76.95 (5) | F1x—Rb1—Rb1vi | 141.53 (2) |
F1vii—Rb1—F1 | 78.41 (7) | F1—Rb1—Rb1vi | 38.47 (2) |
F1viii—Rb1—F1 | 73.20 (3) | Rb1xi—Rb1—Rb1vi | 90.0 |
F1ix—Rb1—F1 | 143.52 (7) | Rb1xii—Rb1—Rb1vi | 90.0 |
F1x—Rb1—F1 | 114.95 (5) | Rb1xiii—Rb1—Rb1vi | 180.0 |
F1iv—Rb1—Rb1xi | 141.53 (2) | Br1—F1—Rb1vi | 126.98 (3) |
F1v—Rb1—Rb1xi | 38.47 (2) | Br1—F1—Rb1 | 126.98 (3) |
F1vi—Rb1—Rb1xi | 108.24 (3) | Rb1vi—F1—Rb1 | 103.05 (5) |
F1vii—Rb1—Rb1xi | 38.47 (2) | | |
Symmetry codes: (i) −x+1, −y, −z+1; (ii) x, y, −z+1; (iii) −x+1, −y, z; (iv) y+1/2, −x+3/2, −z+3/2; (v) y, −x+1, z; (vi) −x+3/2, −y+1/2, −z+3/2; (vii) −y+1/2, x−1/2, −z+3/2; (viii) −y+1, x, z; (ix) x−1/2, y+1/2, −z+3/2; (x) −x+1, −y+1, z; (xi) −x+1/2, −y+1/2, −z+3/2; (xii) −x+3/2, −y+3/2, −z+3/2; (xiii) −x+1/2, −y+3/2, −z+3/2. |