Ba(BF4)2(H2O)3, orthorhombic, space group C2221 at 300 K, becomes monoclinic at 280 K, space group P21. The spread of Ba—F distances is significantly larger in the LT modification, and one of the water molecules in the LT form exhibits positional disorder.
Keywords: low-temperature modification, phase transition, barium tetrafluoridoborate, crystal structure
Abstract
The crystal structure of the low-temperature modification of Ba(BF4)2(H2O)3, barium bis(tetrafluoridoborate) trihydrate, was determined at 150 K. In contrast to the room-temperature modification, which crystallizes in the space group C2221 [a = 7.1763 (6), b = 18.052 (2), c = 7.1631 (6) Å, V = 927.93 (15) Å3 at 300 K, Z = 4; Charkin et al. (2023 ▸). J. Struct. Chem. 64, 253–261], the low-temperature phase is monoclinic, space group P21 [a = 7.0550 (4), b = 7.1706 (3), c = 9.4182 (6) Å, β = 109.295 (7)
o
, V = 449.68 (5) Å3, Z = 2]. The structure of the low-temperature modification of Ba(BF4)2(H2O)3 features O—H⋯F and O—H⋯O hydrogen bonding between water molecules and BF4
− anions. One of the coordinating water molecules in the low-temperature modification is disordered over two sets of sites.
Structure description
Recently, the orthorhombic crystal structure of the compound Ba(BF4)2(H2O)3 was reported on the basis of room-temperature (RT) single-crystal data in space group C2221 (Charkin et al., 2023 ▸). The authors observed a phase transition at decreasing temperature but were unable to solve the crystal structure of the low-temperature (LT) modification. We have now succeeded in solving the crystal structure of LT-Ba(BF4)2(H2O)3.
The asymmetric unit of LT-Ba(BF4)2(H2O)3 contains one Ba2+ cation, two tetrahedral BF4 − anions and three water molecules, one of which (O3) is disordered over two sets of sites with approximately equal occupancy [ratio 0.56 (2):0.44 (2)]. The Ba2+ cation has a coordination number of 10 and is coordinated by seven F ligands from six BF4 − anions and by three water ligands (Fig. 1 ▸). In anhydrous Ba(BF4)2 (Bunič et al., 2007 ▸), the Ba2+ cation is surrounded by ten BF4 − anions. The B(1)F4 unit in LT-Ba(BF4)2(H2O)3 is bound to four Ba2+ cations, while the B(2)F4 unit is connected in a chelate mode to one Ba2+ cation and to another via a μ 2-bridging F ligand. Each [BaF7O3] coordination polyhedron shares two vertices with two other [BaF7O3] polyhedra. The shortest Ba⋯Ba distances amounts to 5.9210 (2) Å. Ba—F bond lengths range from 2.698 (7) to 3.035 (8) Å, and Ba—O bond lengths from 2.777 (9) to 2.821 (8) Å (for ordered water molecules). The spread of Ba—F distances in LT-Ba(BF4)2(H2O)3 is greater than for the RT-modification [2.729 (4) to 2.843 (17) Å; Charkin et al., 2023 ▸]. The B—F distances in LT-Ba(BF4)2(H2O)3 are in normal ranges, 1.352 (12)–1.406 (16) Å.
Figure 1.
The environment of the Ba2+ cation in the crystal structure of LT-Ba(BF4)2(H2O)3. Displacement ellipsoids are drawn at the 50% probability level. Hydrogen bonds are shown as dashed lines. [Symmetry codes: (i) −x + 1, y −
, −z; (ii) x + 1, y, z; (iii) −x + 1, y +
, −z; (iv) −x + 2, y +
, −z + 1; (v) x − 1, y, z; (vi) −x + 2, y −
, −z + 1.]
The packing of LT-Ba(BF4)2(H2O)3 is shown in Fig. 2 ▸. The two ordered water molecules form O—H⋯F hydrogen bonds, and the disordered water molecule forms both O—H⋯F and O—H⋯O hydrogen bonds (Fig. 1 ▸, Table 1 ▸).
Figure 2.
Crystal structure of LT-Ba(BF4)2(H2O)3 in a view approximately along [100]. Displacement ellipsoids are the same as in Fig. 1 ▸. Display of hydrogen-bonding interactions was omitted for clarity.
Table 1. Hydrogen-bond geometry (Å, °).
| D—H⋯A | D—H | H⋯A | D⋯A | D—H⋯A |
|---|---|---|---|---|
| O1—H1A⋯F5i | 0.829 (10) | 2.075 (8) | 2.892 (12) | 168.8 (7) |
| O1—H1B⋯F7ii | 0.842 (10) | 2.016 (7) | 2.849 (13) | 170.5 (7) |
| O2—H2A⋯F4 | 0.974 (9) | 2.331 (9) | 3.119 (13) | 137.4 (5) |
| O2—H2B⋯F8iii | 0.977 (9) | 2.053 (11) | 3.002 (15) | 163.5 (7) |
| O3A—H3AA⋯O2iii | 0.88 (2) | 2.191 (11) | 2.96 (3) | 146.5 (18) |
| O3A—H3AB⋯F7iv | 0.84 (2) | 2.386 (8) | 3.13 (2) | 147.7 (17) |
| O3B—H3BA⋯F5 | 0.86 (3) | 2.355 (9) | 3.15 (3) | 153.0 (16) |
Symmetry codes: (i)
; (ii)
; (iii)
; (iv)
.
The RT unit cell in space group C2221 with a = 7.1763 (6) Å, b = 18.052 (2) Å, c = 7.1631 (6) Å (Charkin et al., 2023 ▸) is related to the LT mP unit cell in P21 by the transformation –a, –c, 1/2a + 1/2b, suggesting a translationengleiche symmetry relationship of index 2 (Müller, 2013 ▸). Considering the significant difference in crystal density for both modifications (2.59 g cm-3 for the RT modification at 300 K, 2.63 g cm−3 for the LT modification at 280 K, and 2.59 g cm−3 at 150 K), it can be assumed that the formation of a structure with more effective packing is the driving force of the observed phase transition.
We also tried to determine the temperature of the phase transition. It is noteworthy that at 280 K the LT modification remains unchanged, with significantly enlarged unit-cell parameters (Table 2 ▸). At 300 K, an orthorhombic cell was indexed with 100% of all observed reflections and with similar lattice parameters as given by Charkin et al. (2023 ▸). Thus, we can conclude that the ordered oC ⇌ mP phase transition of Ba(BF4)2(H2O)3 (accompanied by twinning of the monoclinic LT phase) occurs between 280 and 300 K.
Table 2. Unit-cell parameters (Å, °, Å3) of Ba(BF4)2(H2O)3 at different temperatures (K).
| T | a | b | c | β | V |
|---|---|---|---|---|---|
| 100 | 7.0406 (5) | 7.1567 (3) | 9.3926 (9) | 109.292 (7) | 446.69 (5) |
| 150 | 7.0550 (4) | 7.1706 (3) | 9.4182 (6) | 109.295 (7) | 449.68 (5) |
| 280 | 7.1469 (5) | 7.1775 (4) | 9.5820 (7) | 110.254 (6) | 461.13 (5) |
| 300 | 7.1763 (6) | 18.052 (2) | 7.1631 (6) | 927.93 (15) |
Synthesis and crystallization
Single crystals of Ba(BF4)2(H2O)3 were grown from an aqueous solution of Ba(BF4)2. Barium carbonate was added in small portions to 40%wt HBF4. After completion of the gaseous CO2 release, the solution was decanted from residual BaCO3. Evaporation of water at room temperature yielded small crystals of Ba(BF4)2(H2O)3. Note that an excess of HBF4 led to the formation of crystals of anhydrous Ba(BF4)2 in our experiments.
Refinement
Crystal data, data collection and structure refinement details are summarized in Table 3 ▸. The obtained crystals suffer from racemic twinning and additionally show twinning by pseudo-merohedry at decreasing temperature. To avoid complicated refinement, many crystals were tested until a crystal with a Flack parameter (Flack, 1983 ▸) close to zero was found. The twin law corresponding to a 180° rotation around the [100] direction was determined, and the reflection array was indexed as a two-component twin with a negligible amount of non-indexed reflections. Because of the relatively small amount (BASF = 0.26) of the second domain, the final refinement was performed with a HKLF5-type file containing reflections from the first domain and overlapping reflections. Because of unstable refinement, EADP commands in SHELXL (Sheldrick, 2015 ▸) were applied to the pair of disordered O3 atoms and also to the pair of B atoms. Hydrogen atoms were placed on calculated positions and refined with AFIX 7 restrictions. One reflection with an error/e.s.d. ratio of 5.5 was omitted.
Table 3. Experimental details.
| Crystal data | |
| Chemical formula | Ba(BF4)2(H2O)3 |
| M r | 365.01 |
| Crystal system, space group | Monoclinic, P21 |
| Temperature (K) | 150 |
| a, b, c (Å) | 7.0550 (4), 7.1706 (3), 9.4182 (6) |
| β (°) | 109.295 (7) |
| V (Å3) | 449.68 (5) |
| Z | 2 |
| Radiation type | Mo Kα |
| μ (mm−1) | 4.53 |
| Crystal size (mm) | 0.36 × 0.27 × 0.07 |
| Data collection | |
| Diffractometer | New Gemini, Dual, Cu at home/near, Atlas |
| Absorption correction | Analytical (CrysAlis PRO; Rigaku OD, 2023) |
| T min, T max | 0.075, 0.472 |
| No. of measured, independent and observed [I > 2σ(I)] reflections | 2386, 2386, 2212 |
| (sin θ/λ)max (Å−1) | 0.674 |
| Refinement | |
| R[F 2 > 2σ(F 2)], wR(F 2), S | 0.036, 0.089, 1.07 |
| No. of reflections | 2386 |
| No. of parameters | 120 |
| No. of restraints | 1 |
| H-atom treatment | H-atom parameters constrained |
| Δρmax, Δρmin (e Å−3) | 0.93, −1.05 |
| Absolute structure | Classical Flack method preferred over Parsons because s.u. lower |
| Absolute structure parameter | −0.03 (4) |
Supplementary Material
Crystal structure: contains datablock(s) I. DOI: 10.1107/S2414314623004881/wm4190sup1.cif
Structure factors: contains datablock(s) I. DOI: 10.1107/S2414314623004881/wm4190Isup3.hkl
CCDC reference: 2267617
Additional supporting information: crystallographic information; 3D view; checkCIF report
Acknowledgments
The authors acknowledge financial support from the Slovenian Research Agency (research core funding No. P1–0045; Inorganic Chemistry and Technology).
full crystallographic data
Crystal data
| Ba(BF4)2(H2O)32(BF4)·3(H2O)·Ba | F(000) = 336 |
| Mr = 365.01 | Dx = 2.696 Mg m−3 |
| Monoclinic, P21 | Mo Kα radiation, λ = 0.71073 Å |
| a = 7.0550 (4) Å | Cell parameters from 5692 reflections |
| b = 7.1706 (3) Å | θ = 3.0–28.2° |
| c = 9.4182 (6) Å | µ = 4.53 mm−1 |
| β = 109.295 (7)° | T = 150 K |
| V = 449.68 (5) Å3 | Plate, colourless |
| Z = 2 | 0.36 × 0.27 × 0.07 mm |
Data collection
| New Gemini, Dual, Cu at home/near, Atlas diffractometer | 2386 measured reflections |
| Radiation source: fine-focus sealed X-ray tube, Enhance (Mo) X-ray Source | 2386 independent reflections |
| Graphite monochromator | 2212 reflections with I > 2σ(I) |
| Detector resolution: 10.6426 pixels mm-1 | θmax = 28.6°, θmin = 2.3° |
| ω scans | h = −9→9 |
| Absorption correction: analytical (CrysAlisPro; Rigaku OD, 2023) | k = −9→9 |
| Tmin = 0.075, Tmax = 0.472 | l = −12→12 |
Refinement
| Refinement on F2 | Hydrogen site location: difference Fourier map |
| Least-squares matrix: full | H-atom parameters constrained |
| R[F2 > 2σ(F2)] = 0.036 | w = 1/[σ2(Fo2) + (0.0656P)2] where P = (Fo2 + 2Fc2)/3 |
| wR(F2) = 0.089 | (Δ/σ)max = 0.009 |
| S = 1.07 | Δρmax = 0.93 e Å−3 |
| 2386 reflections | Δρmin = −1.05 e Å−3 |
| 120 parameters | Absolute structure: Classical Flack method preferred over Parsons because s.u. lower |
| 1 restraint | Absolute structure parameter: −0.03 (4) |
Special details
| 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. |
| Refinement. Refined as a 2-component twin.1. Twinned data refinement Scales: 0.738 (3) 0.262 (3) 2. Fixed Uiso At 1.5 times of: All O(H,H,H,H,H,H,H,H) groups 3. Uiso/Uaniso restraints and constraints Uanis(O3B) = Uanis(O3A) Uanis(B2) = Uanis(B1) Uanis(F4) = Uanis(F2) 4. Others Sof(O3B)=Sof(H3BA)=Sof(H3BB)=1-FVAR(1) Sof(O3A)=Sof(H3AA)=Sof(H3AB)=FVAR(1) Fixed X: H1A(1.393391) H1B(1.25841) H3AA(0.82474) H3AB(0.919749) H3BA(0.70805) H3BB(0.82046) H2A(1.436299) H2B(1.27384) Fixed Y: H1A(0.843861) H1B(0.70964) H3AA(1.34448) H3AB(1.39917) H3BA(1.19412) H3BB(1.354321) H2A(0.999499) H2B(1.11445) Fixed Z: H1A(0.62203) H1B(0.62415) H3AA(0.77378) H3AB(0.663441) H3BA(0.651361) H3BB(0.66705) H2A(1.1758) H2B(1.21389) |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)
| x | y | z | Uiso*/Ueq | Occ. (<1) | |
| Ba1 | 0.84596 (6) | 0.54566 (15) | 0.18707 (5) | 0.01069 (17) | |
| F1 | 0.1744 (12) | 0.6957 (9) | −0.0772 (9) | 0.0392 (19) | |
| F2 | 0.4423 (11) | 0.5754 (14) | 0.0977 (9) | 0.0449 (16) | |
| F3 | 0.1320 (13) | 0.4559 (13) | 0.0610 (12) | 0.050 (3) | |
| F4 | 0.2873 (13) | 0.4098 (13) | −0.1086 (11) | 0.0449 (16) | |
| F5 | 1.4219 (11) | 0.4296 (12) | 0.4972 (9) | 0.0361 (18) | |
| F6 | 1.2726 (11) | 0.2125 (11) | 0.5958 (8) | 0.0299 (16) | |
| F7 | 1.1150 (11) | 0.4849 (9) | 0.5097 (9) | 0.0311 (18) | |
| F8 | 1.1510 (13) | 0.2707 (18) | 0.3442 (11) | 0.035 (3) | |
| O1 | 0.6644 (13) | 0.2926 (16) | 0.3248 (12) | 0.031 (2) | |
| O2 | 0.6901 (12) | 0.565 (2) | −0.1296 (9) | 0.033 (2) | |
| B1 | 0.2610 (14) | 0.537 (4) | −0.0048 (10) | 0.0136 (15) | |
| B2 | 1.2421 (17) | 0.3491 (17) | 0.4874 (13) | 0.0136 (15) | |
| O3A | 1.128 (3) | 0.813 (4) | 0.298 (2) | 0.025 (4) | 0.56 (2) |
| O3B | 1.197 (4) | 0.756 (4) | 0.284 (3) | 0.025 (4) | 0.44 (2) |
| H1A | 0.606609 | 0.343861 | 0.377970 | 0.038* | |
| H1B | 0.741590 | 0.209640 | 0.375850 | 0.038* | |
| H3AA | 1.175261 | 0.844480 | 0.226220 | 0.038* | 0.56 (2) |
| H3AB | 1.080250 | 0.899170 | 0.336559 | 0.038* | 0.56 (2) |
| H3BA | 1.291950 | 0.694120 | 0.348640 | 0.038* | 0.44 (2) |
| H3BB | 1.179539 | 0.854321 | 0.332950 | 0.038* | 0.44 (2) |
| H2A | 0.563701 | 0.499499 | −0.175799 | 0.038* | |
| H2B | 0.726160 | 0.614450 | −0.213891 | 0.038* |
Atomic displacement parameters (Å2)
| U11 | U22 | U33 | U12 | U13 | U23 | |
| Ba1 | 0.0098 (2) | 0.0107 (2) | 0.0114 (3) | −0.0003 (4) | 0.00317 (18) | −0.0011 (4) |
| F1 | 0.044 (5) | 0.021 (3) | 0.049 (5) | 0.011 (3) | 0.010 (4) | 0.022 (3) |
| F2 | 0.029 (3) | 0.052 (4) | 0.052 (4) | 0.000 (3) | 0.011 (3) | −0.013 (3) |
| F3 | 0.043 (5) | 0.048 (5) | 0.082 (7) | 0.010 (4) | 0.051 (5) | 0.030 (5) |
| F4 | 0.029 (3) | 0.052 (4) | 0.052 (4) | 0.000 (3) | 0.011 (3) | −0.013 (3) |
| F5 | 0.014 (4) | 0.056 (5) | 0.038 (5) | −0.005 (3) | 0.008 (3) | 0.003 (4) |
| F6 | 0.037 (4) | 0.031 (4) | 0.022 (4) | 0.005 (3) | 0.010 (3) | 0.016 (3) |
| F7 | 0.028 (4) | 0.024 (4) | 0.040 (5) | 0.008 (3) | 0.009 (3) | 0.001 (3) |
| F8 | 0.040 (6) | 0.048 (6) | 0.011 (4) | 0.006 (4) | 0.000 (3) | −0.002 (5) |
| O1 | 0.029 (5) | 0.022 (5) | 0.045 (7) | 0.002 (3) | 0.017 (5) | 0.008 (4) |
| O2 | 0.026 (4) | 0.055 (7) | 0.013 (3) | 0.006 (6) | 0.000 (3) | −0.001 (6) |
| B1 | 0.010 (3) | 0.021 (4) | 0.010 (3) | −0.003 (4) | 0.003 (3) | 0.002 (4) |
| B2 | 0.010 (3) | 0.021 (4) | 0.010 (3) | −0.003 (4) | 0.003 (3) | 0.002 (4) |
| O3A | 0.020 (10) | 0.028 (11) | 0.034 (8) | −0.007 (6) | 0.017 (7) | −0.017 (7) |
| O3B | 0.020 (10) | 0.028 (11) | 0.034 (8) | −0.007 (6) | 0.017 (7) | −0.017 (7) |
Geometric parameters (Å, º)
| Ba1—F1i | 2.700 (6) | F4—B1 | 1.39 (2) |
| Ba1—F2 | 2.698 (7) | F5—B2 | 1.369 (13) |
| Ba1—F3ii | 2.735 (7) | F6—B2 | 1.379 (14) |
| Ba1—F4iii | 2.791 (9) | F7—B2 | 1.385 (14) |
| Ba1—F6iv | 2.728 (7) | F8—B2 | 1.406 (16) |
| Ba1—F7 | 3.035 (8) | O1—H1A | 0.83 |
| Ba1—F8 | 2.933 (10) | O1—H1B | 0.84 |
| Ba1—O1 | 2.777 (9) | O2—H2A | 0.97 |
| Ba1—O2 | 2.821 (8) | O2—H2B | 0.98 |
| Ba1—O3A | 2.71 (2) | O3A—H3AA | 0.88 |
| Ba1—O3B | 2.78 (2) | O3A—H3AB | 0.84 |
| F1—B1 | 1.36 (2) | O3B—H3BA | 0.86 |
| F2—B1 | 1.352 (12) | O3B—H3BB | 0.88 |
| F3—B1 | 1.387 (15) | ||
| F1i—Ba1—F3ii | 64.4 (3) | O2—Ba1—F7 | 164.1 (2) |
| F1i—Ba1—F4iii | 142.9 (3) | O2—Ba1—F8 | 122.1 (3) |
| F1i—Ba1—F6iv | 134.8 (2) | O3A—Ba1—F3ii | 77.3 (5) |
| F1i—Ba1—F7 | 100.8 (2) | O3A—Ba1—F4iii | 65.1 (6) |
| F1i—Ba1—F8 | 60.4 (3) | O3A—Ba1—F6iv | 76.6 (4) |
| F1i—Ba1—O1 | 66.3 (3) | O3A—Ba1—F7 | 65.2 (6) |
| F1i—Ba1—O2 | 71.8 (3) | O3A—Ba1—F8 | 87.7 (5) |
| F1i—Ba1—O3A | 138.1 (5) | O3A—Ba1—O1 | 132.5 (5) |
| F1i—Ba1—O3B | 123.8 (6) | O3A—Ba1—O2 | 110.6 (6) |
| F2—Ba1—F1i | 92.1 (3) | O3B—Ba1—F7 | 63.6 (6) |
| F2—Ba1—F3ii | 137.5 (3) | O3B—Ba1—F8 | 76.9 (6) |
| F2—Ba1—F4iii | 67.4 (3) | O3B—Ba1—O2 | 108.2 (6) |
| F2—Ba1—F6iv | 69.2 (2) | B1—F1—Ba1iii | 157.8 (7) |
| F2—Ba1—F7 | 124.8 (2) | B1—F2—Ba1 | 149.2 (8) |
| F2—Ba1—F8 | 137.2 (3) | B1—F3—Ba1v | 141.5 (12) |
| F2—Ba1—O1 | 66.1 (3) | B1—F4—Ba1i | 133.4 (10) |
| F2—Ba1—O2 | 70.4 (2) | B2—F6—Ba1vi | 148.7 (7) |
| F2—Ba1—O3A | 128.9 (6) | B2—F7—Ba1 | 99.9 (6) |
| F2—Ba1—O3B | 142.5 (6) | B2—F8—Ba1 | 104.0 (8) |
| F3ii—Ba1—F4iii | 109.7 (3) | Ba1—O1—H1A | 113.0 |
| F3ii—Ba1—F7 | 95.4 (3) | Ba1—O1—H1B | 115.0 |
| F3ii—Ba1—F8 | 62.4 (3) | H1A—O1—H1B | 109.0 |
| F3ii—Ba1—O1 | 124.7 (3) | Ba1—O2—H2A | 115.0 |
| F3ii—Ba1—O2 | 68.8 (3) | F1—B1—F3 | 108.8 (10) |
| F3ii—Ba1—O3B | 64.1 (6) | F1—B1—F4 | 109.7 (8) |
| F4iii—Ba1—F7 | 116.4 (2) | F2—B1—F1 | 110.5 (17) |
| F4iii—Ba1—F8 | 152.8 (3) | F2—B1—F3 | 111.8 (9) |
| F4iii—Ba1—O2 | 72.2 (4) | F2—B1—F4 | 108.7 (10) |
| F6iv—Ba1—F3ii | 151.8 (3) | F3—B1—F4 | 107.3 (17) |
| F6iv—Ba1—F4iii | 68.2 (3) | F5—B2—F6 | 109.6 (9) |
| F6iv—Ba1—F7 | 63.8 (2) | F5—B2—F7 | 109.0 (10) |
| F6iv—Ba1—F8 | 105.8 (3) | F5—B2—F8 | 110.6 (10) |
| F6iv—Ba1—O1 | 68.5 (3) | F6—B2—F7 | 109.8 (9) |
| F6iv—Ba1—O2 | 131.5 (3) | F6—B2—F8 | 109.7 (10) |
| F6iv—Ba1—O3B | 88.8 (5) | F7—B2—F8 | 108.2 (10) |
| F8—Ba1—F7 | 44.5 (2) | Ba1—O3A—H3AA | 108.0 |
| O1—Ba1—F4iii | 124.6 (3) | Ba1—O3A—H3AB | 110.0 |
| O1—Ba1—F7 | 70.8 (3) | H3AA—O3A—H3AB | 117.0 |
| O1—Ba1—F8 | 72.5 (3) | Ba1—O3B—H3BA | 111.0 |
| O1—Ba1—O2 | 116.6 (3) | Ba1—O3B—H3BB | 110.0 |
| O1—Ba1—O3B | 134.4 (6) | H3BA—O3B—H3BB | 104.0 |
| Ba1iii—F1—B1—F2 | 25 (2) | Ba1i—F4—B1—F3 | −3.8 (15) |
| Ba1iii—F1—B1—F3 | 148.0 (14) | Ba1vi—F6—B2—F5 | 136.5 (11) |
| Ba1iii—F1—B1—F4 | −95 (2) | Ba1vi—F6—B2—F7 | 16.9 (19) |
| Ba1—F2—B1—F1 | −111 (2) | Ba1vi—F6—B2—F8 | −101.9 (14) |
| Ba1—F2—B1—F3 | 127.5 (12) | Ba1—F7—B2—F5 | 103.0 (8) |
| Ba1—F2—B1—F4 | 9 (3) | Ba1—F7—B2—F6 | −137.0 (8) |
| Ba1v—F3—B1—F1 | −31.2 (17) | Ba1—F7—B2—F8 | −17.3 (9) |
| Ba1v—F3—B1—F2 | 91.1 (18) | Ba1—F8—B2—F5 | −101.1 (9) |
| Ba1v—F3—B1—F4 | −149.9 (11) | Ba1—F8—B2—F6 | 138.0 (7) |
| Ba1i—F4—B1—F1 | −121.8 (12) | Ba1—F8—B2—F7 | 18.2 (10) |
| Ba1i—F4—B1—F2 | 117.3 (11) |
Symmetry codes: (i) −x+1, y−1/2, −z; (ii) x+1, y, z; (iii) −x+1, y+1/2, −z; (iv) −x+2, y+1/2, −z+1; (v) x−1, y, z; (vi) −x+2, y−1/2, −z+1.
Hydrogen-bond geometry (Å, º)
| D—H···A | D—H | H···A | D···A | D—H···A |
| O1—H1A···F5v | 0.829 (10) | 2.075 (8) | 2.892 (12) | 168.8 (7) |
| O1—H1B···F7vi | 0.842 (10) | 2.016 (7) | 2.849 (13) | 170.5 (7) |
| O2—H2A···F4 | 0.974 (9) | 2.331 (9) | 3.119 (13) | 137.4 (5) |
| O2—H2B···F8vii | 0.977 (9) | 2.053 (11) | 3.002 (15) | 163.5 (7) |
| O3A—H3AA···O2vii | 0.88 (2) | 2.191 (11) | 2.96 (3) | 146.5 (18) |
| O3A—H3AB···F7iv | 0.84 (2) | 2.386 (8) | 3.13 (2) | 147.7 (17) |
| O3B—H3BA···F5 | 0.86 (3) | 2.355 (9) | 3.15 (3) | 153.0 (16) |
Symmetry codes: (iv) −x+2, y+1/2, −z+1; (v) x−1, y, z; (vi) −x+2, y−1/2, −z+1; (vii) −x+2, y+1/2, −z.
Transformation matrix oC–mP (HT–LT phase transition of Ba(BF4)2(H3O)3
| -1 | 0 | 0 |
| 0 | 0 | -1 |
| 1/2 | -1/2 | 0 |
Funding Statement
Funding for this research was provided by: Javna Agencija za Raziskovalno Dejavnost RS (grant No. P1-0045).
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Associated Data
This section collects any data citations, data availability statements, or supplementary materials included in this article.
Supplementary Materials
Crystal structure: contains datablock(s) I. DOI: 10.1107/S2414314623004881/wm4190sup1.cif
Structure factors: contains datablock(s) I. DOI: 10.1107/S2414314623004881/wm4190Isup3.hkl
CCDC reference: 2267617
Additional supporting information: crystallographic information; 3D view; checkCIF report