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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoIUCrDATA
ISSN: 2414-3146
Volume 8| Part 9| September 2023| x230716
https://doi.org/10.1107/S2414314623007162

Bis­(di­meth­­oxy­ethane-1κ2O,O′)penta­kis­(1,1,1,3,3,3-hexa­fluoro­propan-2-olato)-2κ3O,3κ2O-μ-hy­droxido-1:3κ2O-μ3-oxido-1:2:3κ3O-magnesiumdialuminium

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Matic Lozinšek,a* Tjaša Pavčnikb,c and Jan Bitencb,c

aJožef Stefan Institute, Jamova cesta 39, 1000 Ljubljana, Slovenia, bNational Institute of Chemistry, Hajdrihova 19, 1000 Ljubljana, Slovenia, and cFaculty of Chemistry and Chemical Technology, University of Ljubljana, Večna pot 113, 1000 Ljubljana, Slovenia
*Correspondence e-mail: matic.lozinsek@ijs.si

Edited by W. T. A. Harrison, University of Aberdeen, United Kingdom (Received 10 August 2023; accepted 15 August 2023; online 8 September 2023)

Partial hydrolysis of a sample of [Mg(dme)3][Al(hfip)4]2 crystals led to the formation of the title complex, [Mg(dme)2{HOAl(hfip)2OAl(hfip)3}] (dme = di­meth­oxy­ethane and hfipH = hexa­fluoro­iso­propanol) or [Mg(C4H10O2)2O(OH)Al2(C3HF6O)5]. The magnesium cation exhibits a distorted octa­hedral coordination with two bidentate di­meth­oxy­ethane mol­ecules and a dinuclear aluminate anion, coordinated to Mg2+ via oxido and hydroxido units. The anion is an oxido-bridged species, [HOAl(hfip)2(μ-O)Al(hfip)3]2–, with one Al3+ cation tetra­hedrally coordinated by an oxido (O2–) anion, a hydroxido anion, and two hfip groups, whereas the second Al3+ cation is coordinated by the oxido anion and three hfip groups.

CCDC reference: 2156683

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[Scheme 3D1]
Chemical scheme
[Scheme 1]

Structure description

Salts of weakly coordinating anions (Barthélemy et al., 2023[Barthélemy, A., Dabringhaus, P., Jacob, E., Koger, H., Röhner, D., Schmitt, M., Sellin, M. & Krossing, I. (2023). Chemistry with weakly coordinating aluminates [Al(ORF)4]- and borates [B(ORF)4]-: From fundamentals to application. In Comprehensive Inorganic Chemistry III, 3rd ed., edited by J. Reedijk & K. R. Poeppelmeier. Oxford: Elsevier.]), such as [Al(hfip)4]− [tetra­kis­(1,1,1,3,3,3-hexa­fluoro­propan-2-olato)aluminate; hfipH = hexa­fluoro­iso­pro­pan­ol], have recently emerged as state-of-the-art electrolytes for rechargeable multivalent metal batteries (Herb et al., 2016[Herb, J. T., Nist-Lund, C. A. & Arnold, C. B. (2016). ACS Energy Lett. 1, 1227-1232.]; Mandai et al., 2021[Mandai, T., Youn, Y. & Tateyama, Y. (2021). Mater. Adv. 2, 6283-6296.]; Pavčnik et al., 2023[Pavčnik, T., Forero-Saboya, J. D., Ponrouch, A., Robba, A., Dominko, R. & Bitenc, J. (2023). J. Mater. Chem. A, 11, 14738-14747.]). The title compound formed upon partial hydrolysis of the complex [Mg(dme)3][Al(hfip)4]2 (dme = di­meth­oxy­ethane), which is a promising electrolyte salt for magnesium batteries (Pavčnik et al., 2022[Pavčnik, T., Lozinšek, M., Pirnat, K., Vizintin, A., Mandai, T., Aurbach, D., Dominko, R. & Bitenc, J. (2022). Appl. Mater. Interfaces, 14, 26766-26774.]).

The title compound crystallizes in the monoclinic space group P21/n with four mol­ecules in the unit cell. The magnesium cation is coordinated by two bidentate dme mol­ecules with Mg—O distances of 2.0813 (6)–2.1185 (6) Å and by the oxido and hydroxido groups of the anion with slightly shorter Mg—O bond lengths of 2.0383 (6) and 2.0470 (6) Å, respectively (Fig. 1[link]). In the dinuclear [HOAl(hfip)2OAl(hfip)3]2– anion, the first central aluminium cation, Al1, is coordinated by two hfip ((CF3)2CHO–) [1.7374 (6), 1.7425 (6) Å], hydroxido [1.7644 (6) Å] and a bridging oxido ligand [1.7456 (6) Å], whereas the second Al3+ cation, Al2, is coordinated by three hfip moieties [1.7307 (6)–1.7645 (6) Å] and by the oxido bridge [1.7384 (6) Å] (Fig. 1[link]). The tetra­hedral shape of the [AlO4] unit is more distorted in the case of the Al1 atom than in the case of the Al2 atom, with the corresponding O—Al—O angles being 92.84 (3)–117.93 (3)° and 102.33 (3)–115.11 (3)°, respectively. The nearly right angle involves the oxido and hydroxido groups (O—Al1—OH). The anion coordinates to the magnesium cation via hydroxido and oxido units, thus making these ligands μ- and μ3-bridges, respectively, resulting in an Mg1⋯Al1 distance of 2.8074 (3) Å. The angles at the hydroxido and oxido bridges between Al1 and Mg1 are similar [Al1—O5—Mg1 = 94.59 (3)°, Al1—O6—Mg1 = 95.48 (3)°], whereas the angles involving μ3-oxido and Al2 are more obtuse [Al1—O6—Al2 = 128.72 (3)°, Al2—O6—Mg1 = 135.07 (3)°]. The Mg2+ cation has a distorted octa­hedral coordination with cis-O—Mg—O angles ranging from 76.40° (2) to 101.00 (2)° and trans-O—Mg—O angles in the range 164.77 (3)–168.38 (3)°. The O—Mg—O bite angles of the dme ligands [76.40 (3) and 77.08 (3)°] and the anion [76.99 (2)°] are nearly identical.

[Figure 1]
Figure 1
The asymmetric unit and selected atom labels of the [Mg(dme)2{HOAl(hfip)2OAl(hfip)3}] crystal structure (dme: di­meth­oxy­ethane, hfip: 1,1,1,3,3,3-hexa­fluoro­iso­propano­lato). Displacement ellipsoids are plot­ted at the 50% probability level and hydrogen atoms are depicted as small spheres of arbitrary radius.

Similar Mg—O distances and bite angles have been observed in other magnesium complexes with coordinating dme, for example: 2.0688 (11), 2.1146 (12) Å, 77.49 (5)° in [Mg(dme)2(CF3SO3)2] (Cambridge Structural Database refcode EJUYEQ; Nguyen et al., 2020[Nguyen, D.-T., Eng, A. Y. S., Ng, M.-F., Kumar, V., Sofer, Z., Handoko, A. D., Subramanian, G. S. & Seh, Z. W. (2020). Cell. Rep. Phys. Sci. 1, 100265.]) and 2.0645 (12)–2.0854 (13) Å, 77.39 (5)–78.25 (5)° in [Mg(dme)3](CB9H10)2 (LATRUW; McArthur et al., 2017[McArthur, S. G., Jay, R., Geng, L., Guo, J. & Lavallo, V. (2017). Chem. Commun. 53, 4453-4456.]). The Al—O(hfip) distances of the title compound are in agreement with bond lengths observed in compounds of the [Al(hfip)4]− anion: 1.7367 (10)–1.7444 (10) Å in NMe4[Al(hfip)4] (FOZRIW; Raabe et al., 2009[Raabe, I., Wagner, K., Guttsche, K., Wang, M., Grätzel, M., Santiso-Quiñones, G. & Krossing, I. (2009). Chem. Eur. J. 15, 1966-1976.]) and 1.7140 (13)–1.7624 (14) Å in [Ag(CO)2Al(hfip)4] (XARFED; Schaefer et al., 2013[Schaefer, J., Kraft, A., Reininger, S., Santiso-Quinones, G., Himmel, D., Trapp, N., Gellrich, U., Breit, B. & Krossing, I. (2013). Chem. Eur. J. 19, 12468-12485.]). The geometric parameters of the CF3 groups are consistent with those reported in crystal structures of other tri­fluoro­methyl­ated organic compounds (Motaln et al., 2023[Motaln, K., Cotman, A. E. & Lozinšek, M. (2023). IUCrData, 8, x221209.]; Radan et al., 2023[Radan, K., Cotman, A. E. & Lozinšek, M. (2023). IUCrData, 8, x230217.]).

In the extended structure, the hydroxido unit forms an inter­molecular O—H⋯F hydrogen bond (Table 1[link]) to the hfip moiety of the OAl(hfip)3 group.

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A D⋯A D—H⋯A
O5—H5⋯F18i 0.750 (18) 2.315 (18) 2.9816 (8) 148.7 (17)
Symmetry code: (i) [-x+{\script{1\over 2}}, y-{\script{1\over 2}}, -z+{\script{1\over 2}}].

Bond-valence calculations (Brown, 2009[Brown, I. D. (2009). Chem. Rev. 109, 6858-6919.], 2016[Brown, I. D. (2016). The Chemical Bond in Inorganic Chemistry. The Bond Valence Model, 2nd ed., IUCr Monographs on Crystallography 27. Oxford University Press.]) for the magnesium, aluminium, and oxygen atoms of the μ-hydroxido and μ3-oxido ligands agree well with the expected values (in valence units) and confirm the atom assignments: Mg1 2.09, Al1 3.08, Al2 3.10, O5 1.95, O6 1.96. Calculations were performed using the following parameters: b = 0.37 Å, R0 = 1.693 Å (Mg—O), 1.651 Å (Al—O); and b = 0.94 Å, R0 = 0.569 Å (H—O) (Brown & Altermatt, 1985[Brown, I. D. & Altermatt, D. (1985). Acta Cryst. B41, 244-247.]; Brown, 2020[Brown, I. D. (2020). bvparm2020.cif, Accumulated Table of Bond Valence Parameters, (IUCr) Bond valence parameters. https://www.iucr.org/resources/data/datasets/bond-valence-parameters. Brockhouse Institute for Materials Research, McMaster University, Hamilton, ON, Canada.], 2016[Brown, I. D. (2016). The Chemical Bond in Inorganic Chemistry. The Bond Valence Model, 2nd ed., IUCr Monographs on Crystallography 27. Oxford University Press.]).

Synthesis and crystallization

Single crystals of the title compound formed in a partial hydrolysis of the [Mg(dme)3][Al(hfip)4] sample (Pavčnik et al., 2022[Pavčnik, T., Lozinšek, M., Pirnat, K., Vizintin, A., Mandai, T., Aurbach, D., Dominko, R. & Bitenc, J. (2022). Appl. Mater. Interfaces, 14, 26766-26774.]) that was kept on a watch glass under the layer of perfluoro­deca­line, upon storage in refrigerator at about 8 °C for a day. The formation of this hydrolysis product could be tentatively described with the following equation:

[Mg(dme)3][Al(hfip)4]2 + 2H2O → [Mg(dme)2{HOAl(hfip)2OAl(hfip)3}] + dme + 3hfipH.

Refinement

The crystal data, data collection, and structure refinement details are summarized in Table 2[link]. Hydrogen atoms were refined freely including their isotropic thermal parameters (Cooper et al., 2010[Cooper, R. I., Thompson, A. L. & Watkin, D. J. (2010). J. Appl. Cryst. 43, 1100-1107.]).

Table 2
Experimental details

Crystal data
Chemical formula [Mg(C4H10O2)2O(OH)Al2(C3HF6O)5]
Mr 1126.71
Crystal system, space group Monoclinic, P21/n
Temperature (K) 100
a, b, c (Å) 10.68706 (9), 19.53919 (16), 19.31983 (17)
β (°) 91.7888 (7)
V (Å3) 4032.33 (6)
Z 4
Radiation type Ag Kα, λ = 0.56087 Å
μ (mm−1) 0.15
Crystal size (mm) 0.74 × 0.58 × 0.36
 
Data collection
Diffractometer XtaLAB Synergy-S, Dualflex, Eiger2 R CdTe 1M
Absorption correction Gaussian (CrysAlis PRO; Rigaku OD, 2022[Rigaku OD (2022). CrysAlis PRO. Rigaku Corporation, Wrocław, Poland.])
Tmin, Tmax 0.190, 1.000
No. of measured, independent and observed [I > 2σ(I)] reflections 271135, 20244, 16165
Rint 0.030
(sin θ/λ)max (Å−1) 0.870
 
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.033, 0.091, 1.04
No. of reflections 20244
No. of parameters 708
H-atom treatment All H-atom parameters refined
Δρmax, Δρmin (e Å−3) 0.51, −0.41
Computer programs: CrysAlis PRO (Rigaku OD, 2022[Rigaku OD (2022). CrysAlis PRO. Rigaku Corporation, Wrocław, Poland.]), OLEX2.solve (Dolomanov et al., 2009[Dolomanov, O. V., Bourhis, L. J., Gildea, R. J., Howard, J. A. K. & Puschmann, H. (2009). J. Appl. Cryst. 42, 339-341.]), OLEX2 (Dolomanov et al., 2009[Dolomanov, O. V., Bourhis, L. J., Gildea, R. J., Howard, J. A. K. & Puschmann, H. (2009). J. Appl. Cryst. 42, 339-341.]), SHELXL2019/2 (Sheldrick, 2015[Sheldrick, G. M. (2015). Acta Cryst. C71, 3-8.]), DIAMOND (Brandenburg, 2005[Brandenburg, K. (2005). DIAMOND. Crystal Impact GbR, Bonn, Germany.]) and publCIF (Westrip, 2010[Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.]).

Structural data

CCDC reference: 2156683

Crystal structure: contains datablock I. DOI: https://doi.org/10.1107/S2414314623007162/hb4443sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S2414314623007162/hb4443Isup2.hkl

checkCIF report


Computing details top

Data collection: CrysAlis PRO 1.171.41.123a (Rigaku OD, 2022); cell refinement: CrysAlis PRO 1.171.41.123a (Rigaku OD, 2022); data reduction: CrysAlis PRO 1.171.41.123a (Rigaku OD, 2022); program(s) used to solve structure: olex2.solve 1.5 (Dolomanov et al., 2009); program(s) used to refine structure: SHELXL2019/2 (Sheldrick, 2015); molecular graphics: DIAMOND (Brandenburg, 2005); software used to prepare material for publication: Olex2 1.5 (Dolomanov et al., 2009), publCIF (Westrip, 2010).

Bis(dimethoxyethane-1κ2O,O')pentakis(1,1,1,3,3,3-hexafluoropropan-2-olato)-2κ3O,3κ2O-µ-hydroxido-1:3κ2O-µ3-oxido-1:2:3κ3O-magnesiumdialuminium top
Crystal data top
[Al2Mg(C3HF6O)5O(OH)(C4H10O2)2]F(000) = 2240
Mr = 1126.71Dx = 1.856 Mg m−3
Monoclinic, P21/nAg Kα radiation, λ = 0.56087 Å
a = 10.68706 (9) ÅCell parameters from 111325 reflections
b = 19.53919 (16) Åθ = 1.9–29.3°
c = 19.31983 (17) ŵ = 0.15 mm−1
β = 91.7888 (7)°T = 100 K
V = 4032.33 (6) Å3Block, colourless
Z = 40.74 × 0.58 × 0.36 mm
Data collection top
XtaLAB Synergy, Dualflex, Eiger2 R CdTe 1M
diffractometer		20244 independent reflections
Radiation source: micro-focus sealed X-ray tube, PhotonJet (Ag) X-ray Source16165 reflections with I > 2σ(I)
Mirror monochromatorRint = 0.030
Detector resolution: 13.3333 pixels mm-1θmax = 29.2°, θmin = 1.7°
ω scansh = −18→17
Absorption correction: gaussian
(CrysAlisPro; Rigaku OD, 2022)		k = −31→29
Tmin = 0.190, Tmax = 1.000l = −33→31
271135 measured reflections
Refinement top
Refinement on F2Primary atom site location: iterative
Least-squares matrix: fullHydrogen site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.033All H-atom parameters refined
wR(F2) = 0.091 w = 1/[σ2(Fo2) + (0.0393P)2 + 1.1133P]
where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max = 0.001
20244 reflectionsΔρmax = 0.51 e Å−3
708 parametersΔρmin = −0.41 e Å−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
xyzUiso*/Ueq
Al10.41472 (2)0.33992 (2)0.19998 (2)0.01624 (4)
Al20.56934 (2)0.45794 (2)0.27249 (2)0.01543 (4)
Mg10.46648 (3)0.30191 (2)0.33805 (2)0.01728 (5)
F10.06620 (6)0.46975 (3)0.17179 (3)0.03163 (12)
F20.22151 (6)0.51573 (3)0.12258 (4)0.04067 (16)
F30.07180 (7)0.47128 (4)0.06062 (4)0.04243 (16)
F40.04732 (7)0.33194 (4)0.16943 (5)0.04363 (17)
F50.19142 (6)0.27618 (3)0.11852 (4)0.03338 (12)
F60.05329 (8)0.33255 (4)0.05821 (5)0.0517 (2)
F70.73093 (7)0.27815 (4)0.09021 (5)0.04776 (18)
F80.66025 (9)0.21707 (5)0.17359 (4)0.0572 (2)
F90.67081 (8)0.17495 (4)0.07174 (4)0.04579 (17)
F100.55645 (7)0.30952 (4)−0.01500 (3)0.04094 (15)
F110.36460 (6)0.28918 (4)0.00501 (3)0.03925 (14)
F120.48778 (10)0.20632 (4)−0.01903 (4)0.0544 (2)
F130.49310 (7)0.65885 (3)0.36062 (3)0.03434 (13)
F140.60216 (6)0.63480 (3)0.27238 (4)0.03464 (13)
F150.43057 (7)0.69180 (3)0.25870 (4)0.03847 (14)
F160.27865 (6)0.58285 (4)0.37760 (3)0.03851 (14)
F170.22303 (5)0.51681 (3)0.29389 (3)0.03107 (12)
F180.21428 (6)0.62570 (3)0.27978 (5)0.04278 (17)
F190.81725 (6)0.51700 (4)0.11235 (4)0.03499 (13)
F200.77974 (6)0.41675 (3)0.15412 (4)0.03677 (13)
F210.74822 (7)0.43637 (4)0.04498 (4)0.04225 (16)
F220.61743 (6)0.60467 (3)0.11394 (3)0.03073 (12)
F230.44244 (6)0.55794 (3)0.08514 (3)0.03263 (12)
F240.59871 (6)0.54889 (3)0.01780 (3)0.03319 (12)
F250.96494 (6)0.46007 (4)0.30957 (4)0.03830 (14)
F260.86681 (6)0.53893 (4)0.25256 (3)0.03504 (13)
F270.96813 (6)0.56408 (4)0.34683 (4)0.04336 (17)
F280.86092 (7)0.42067 (3)0.43543 (3)0.03476 (13)
F290.69549 (6)0.47610 (3)0.46362 (3)0.03220 (12)
F300.87415 (6)0.52693 (4)0.46509 (3)0.03517 (13)
O10.29692 (6)0.34050 (3)0.37637 (3)0.02293 (10)
O20.52465 (6)0.34968 (3)0.43109 (3)0.02254 (10)
O30.44219 (6)0.20753 (3)0.38991 (3)0.02446 (11)
O40.63661 (6)0.25207 (3)0.32627 (3)0.02330 (11)
O50.37785 (6)0.26714 (3)0.24941 (3)0.02023 (10)
H50.3322 (16)0.2404 (9)0.2369 (9)0.049 (4)*
O60.50145 (5)0.37714 (3)0.26817 (3)0.01686 (9)
O70.28867 (6)0.39253 (3)0.17783 (3)0.02079 (10)
O80.49285 (6)0.31877 (3)0.12510 (3)0.02178 (10)
O90.47985 (5)0.52008 (3)0.31503 (3)0.01874 (9)
O100.58483 (6)0.49367 (3)0.19124 (3)0.02288 (11)
O110.70824 (5)0.45135 (3)0.32217 (3)0.01976 (10)
C10.17918 (9)0.34707 (5)0.33840 (5)0.02870 (16)
H1A0.1831 (14)0.3858 (8)0.3053 (8)0.038 (4)*
H1C0.1646 (15)0.3046 (8)0.3152 (8)0.040 (4)*
H1B0.1156 (14)0.3533 (8)0.3718 (8)0.040 (4)*
C20.32258 (10)0.39816 (5)0.42095 (5)0.02961 (17)
H2A0.3473 (14)0.4374 (8)0.3930 (8)0.037 (4)*
H2B0.2469 (14)0.4092 (8)0.4451 (8)0.039 (4)*
C30.42423 (10)0.37570 (5)0.47120 (5)0.03070 (17)
H3B0.4521 (13)0.4121 (7)0.4995 (7)0.031 (3)*
H3A0.3943 (14)0.3386 (8)0.5004 (8)0.035 (4)*
C40.62251 (11)0.32156 (5)0.47528 (5)0.03130 (18)
H4B0.6448 (14)0.3529 (8)0.5115 (8)0.037 (4)*
H4C0.6937 (16)0.3137 (8)0.4477 (9)0.045 (4)*
H4A0.5926 (15)0.2781 (9)0.4935 (9)0.045 (4)*
C50.32458 (11)0.18162 (5)0.41272 (6)0.0359 (2)
H5C0.2789 (14)0.2185 (8)0.4320 (8)0.038 (4)*
H5A0.2754 (16)0.1637 (9)0.3727 (9)0.048 (4)*
H5B0.3371 (17)0.1489 (9)0.4475 (10)0.052 (5)*
C60.51608 (9)0.15551 (4)0.35816 (5)0.02861 (16)
H6A0.4813 (12)0.1462 (7)0.3124 (7)0.027 (3)*
H6B0.5159 (13)0.1139 (8)0.3857 (8)0.034 (4)*
C70.64631 (9)0.18360 (4)0.35300 (5)0.02821 (16)
H7A0.6873 (14)0.1849 (8)0.3989 (8)0.035 (4)*
H7B0.6992 (13)0.1562 (7)0.3216 (7)0.029 (3)*
C80.75742 (9)0.28065 (5)0.31208 (6)0.03016 (17)
H8A0.8135 (15)0.2785 (8)0.3543 (8)0.043 (4)*
H8C0.7467 (14)0.3266 (8)0.2988 (8)0.038 (4)*
H8B0.7958 (14)0.2541 (8)0.2782 (8)0.039 (4)*
C90.14136 (8)0.46345 (5)0.11889 (5)0.02515 (14)
C100.21298 (7)0.39570 (4)0.11929 (4)0.02025 (12)
H100.2557 (12)0.3934 (7)0.0767 (7)0.024 (3)*
C110.12361 (9)0.33443 (5)0.11643 (5)0.02846 (16)
C120.64542 (10)0.23239 (5)0.10666 (5)0.03190 (18)
C130.51129 (8)0.25717 (4)0.09276 (4)0.02233 (13)
H130.4584 (12)0.2203 (6)0.1078 (7)0.022 (3)*
C140.48145 (9)0.26547 (5)0.01520 (4)0.02813 (16)
C150.48497 (8)0.64011 (4)0.29406 (5)0.02447 (14)
C160.41558 (7)0.57232 (4)0.28234 (4)0.01904 (12)
H160.4087 (11)0.5678 (6)0.2321 (6)0.021 (3)*
C170.28263 (8)0.57470 (4)0.30916 (5)0.02403 (14)
C180.73865 (9)0.46338 (5)0.10836 (5)0.02699 (15)
C190.60311 (8)0.48311 (4)0.12248 (4)0.02093 (12)
H190.5527 (13)0.4469 (7)0.1023 (7)0.030 (3)*
C200.56621 (8)0.54919 (4)0.08447 (4)0.02334 (14)
C210.89578 (8)0.51608 (5)0.31614 (5)0.02559 (15)
C220.77568 (7)0.50234 (4)0.35500 (4)0.01897 (12)
H220.7350 (12)0.5469 (7)0.3583 (7)0.025 (3)*
C230.80330 (8)0.48113 (4)0.43008 (4)0.02438 (14)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Al10.01831 (9)0.01458 (9)0.01574 (9)0.00019 (7)−0.00074 (7)−0.00034 (7)
Al20.01654 (9)0.01461 (9)0.01512 (9)−0.00019 (7)0.00018 (7)0.00011 (7)
Mg10.02029 (11)0.01498 (10)0.01656 (11)0.00142 (8)0.00043 (9)0.00067 (8)
F10.0274 (3)0.0332 (3)0.0347 (3)0.0076 (2)0.0061 (2)−0.0026 (2)
F20.0327 (3)0.0230 (3)0.0664 (5)−0.0001 (2)0.0036 (3)0.0121 (3)
F30.0431 (4)0.0506 (4)0.0329 (3)0.0187 (3)−0.0094 (3)0.0102 (3)
F40.0331 (3)0.0345 (3)0.0642 (5)−0.0082 (2)0.0178 (3)−0.0005 (3)
F50.0364 (3)0.0228 (2)0.0407 (3)0.0001 (2)−0.0032 (2)−0.0059 (2)
F60.0488 (4)0.0464 (4)0.0577 (5)0.0000 (3)−0.0317 (4)−0.0112 (3)
F70.0272 (3)0.0464 (4)0.0694 (5)0.0010 (3)−0.0019 (3)−0.0088 (4)
F80.0619 (5)0.0781 (6)0.0311 (3)0.0354 (5)−0.0087 (3)0.0025 (4)
F90.0512 (4)0.0343 (3)0.0523 (4)0.0177 (3)0.0092 (3)−0.0090 (3)
F100.0406 (3)0.0548 (4)0.0280 (3)0.0016 (3)0.0094 (3)0.0131 (3)
F110.0321 (3)0.0574 (4)0.0278 (3)0.0024 (3)−0.0062 (2)−0.0015 (3)
F120.0884 (6)0.0434 (4)0.0309 (3)0.0099 (4)−0.0071 (4)−0.0201 (3)
F130.0451 (3)0.0271 (3)0.0307 (3)−0.0072 (2)−0.0010 (2)−0.0088 (2)
F140.0308 (3)0.0285 (3)0.0450 (3)−0.0077 (2)0.0078 (2)−0.0005 (2)
F150.0503 (4)0.0182 (2)0.0465 (4)0.0015 (2)−0.0046 (3)0.0093 (2)
F160.0319 (3)0.0528 (4)0.0313 (3)−0.0010 (3)0.0091 (2)−0.0138 (3)
F170.0242 (2)0.0264 (2)0.0424 (3)−0.00347 (19)−0.0005 (2)−0.0038 (2)
F180.0292 (3)0.0297 (3)0.0692 (5)0.0119 (2)−0.0024 (3)0.0103 (3)
F190.0233 (2)0.0422 (3)0.0397 (3)−0.0061 (2)0.0044 (2)−0.0007 (3)
F200.0380 (3)0.0344 (3)0.0378 (3)0.0111 (2)−0.0008 (3)0.0007 (2)
F210.0451 (4)0.0529 (4)0.0293 (3)0.0044 (3)0.0098 (3)−0.0140 (3)
F220.0386 (3)0.0233 (2)0.0297 (3)−0.0088 (2)−0.0080 (2)0.00409 (19)
F230.0251 (3)0.0375 (3)0.0350 (3)−0.0014 (2)−0.0043 (2)0.0082 (2)
F240.0394 (3)0.0418 (3)0.0183 (2)−0.0107 (2)0.0001 (2)0.0072 (2)
F250.0263 (3)0.0432 (3)0.0460 (4)0.0102 (2)0.0106 (3)−0.0001 (3)
F260.0377 (3)0.0402 (3)0.0276 (3)−0.0050 (2)0.0060 (2)0.0064 (2)
F270.0316 (3)0.0530 (4)0.0457 (4)−0.0215 (3)0.0060 (3)−0.0140 (3)
F280.0428 (3)0.0315 (3)0.0295 (3)0.0118 (2)−0.0062 (2)0.0031 (2)
F290.0361 (3)0.0365 (3)0.0244 (2)−0.0020 (2)0.0077 (2)−0.0015 (2)
F300.0378 (3)0.0406 (3)0.0265 (3)−0.0049 (2)−0.0085 (2)−0.0095 (2)
O10.0240 (3)0.0205 (2)0.0244 (3)0.00244 (19)0.0033 (2)−0.00119 (19)
O20.0286 (3)0.0220 (2)0.0170 (2)0.0018 (2)0.0000 (2)−0.00050 (18)
O30.0308 (3)0.0172 (2)0.0256 (3)0.0007 (2)0.0030 (2)0.00293 (19)
O40.0218 (2)0.0196 (2)0.0284 (3)0.00416 (19)−0.0010 (2)−0.0006 (2)
O50.0246 (3)0.0155 (2)0.0205 (2)−0.00338 (18)−0.00220 (19)0.00048 (17)
O60.0194 (2)0.0147 (2)0.0165 (2)−0.00084 (16)−0.00088 (17)−0.00027 (15)
O70.0213 (2)0.0201 (2)0.0207 (2)0.00311 (18)−0.00353 (19)−0.00046 (18)
O80.0271 (3)0.0192 (2)0.0192 (2)0.00076 (19)0.0030 (2)−0.00330 (18)
O90.0221 (2)0.0158 (2)0.0182 (2)0.00351 (17)0.00021 (18)0.00063 (16)
O100.0296 (3)0.0233 (3)0.0159 (2)0.0006 (2)0.0033 (2)0.00277 (18)
O110.0188 (2)0.0186 (2)0.0217 (2)0.00000 (17)−0.00343 (18)−0.00258 (18)
C10.0224 (4)0.0315 (4)0.0323 (4)0.0038 (3)0.0033 (3)0.0013 (3)
C20.0323 (4)0.0255 (4)0.0314 (4)0.0050 (3)0.0057 (3)−0.0073 (3)
C30.0364 (5)0.0350 (4)0.0210 (3)0.0013 (3)0.0057 (3)−0.0065 (3)
C40.0396 (5)0.0304 (4)0.0233 (4)0.0023 (3)−0.0094 (3)−0.0001 (3)
C50.0415 (5)0.0237 (4)0.0431 (5)−0.0048 (3)0.0132 (4)0.0057 (4)
C60.0332 (4)0.0168 (3)0.0356 (4)0.0042 (3)−0.0025 (3)−0.0003 (3)
C70.0295 (4)0.0202 (3)0.0346 (4)0.0073 (3)−0.0050 (3)−0.0003 (3)
C80.0220 (4)0.0286 (4)0.0400 (5)0.0028 (3)0.0020 (3)−0.0042 (3)
C90.0220 (3)0.0260 (4)0.0274 (4)0.0044 (3)−0.0003 (3)0.0060 (3)
C100.0196 (3)0.0227 (3)0.0184 (3)0.0023 (2)−0.0001 (2)0.0015 (2)
C110.0253 (4)0.0268 (4)0.0329 (4)−0.0008 (3)−0.0049 (3)−0.0038 (3)
C120.0364 (5)0.0312 (4)0.0281 (4)0.0113 (3)−0.0002 (3)−0.0035 (3)
C130.0287 (4)0.0193 (3)0.0191 (3)0.0010 (2)0.0021 (3)−0.0019 (2)
C140.0338 (4)0.0307 (4)0.0199 (3)0.0019 (3)0.0010 (3)−0.0048 (3)
C150.0294 (4)0.0172 (3)0.0267 (4)−0.0003 (3)−0.0001 (3)0.0004 (2)
C160.0217 (3)0.0159 (3)0.0194 (3)0.0017 (2)−0.0008 (2)−0.0003 (2)
C170.0230 (3)0.0199 (3)0.0290 (4)0.0036 (2)−0.0011 (3)−0.0024 (3)
C180.0276 (4)0.0304 (4)0.0231 (3)0.0008 (3)0.0035 (3)−0.0034 (3)
C190.0233 (3)0.0223 (3)0.0173 (3)−0.0040 (2)0.0014 (2)0.0011 (2)
C200.0252 (3)0.0260 (3)0.0187 (3)−0.0069 (3)−0.0022 (3)0.0039 (2)
C210.0210 (3)0.0288 (4)0.0270 (4)−0.0030 (3)0.0016 (3)−0.0030 (3)
C220.0174 (3)0.0193 (3)0.0201 (3)0.0004 (2)−0.0006 (2)−0.0022 (2)
C230.0268 (4)0.0252 (3)0.0210 (3)0.0015 (3)−0.0022 (3)−0.0031 (3)
Geometric parameters (Å, º) top
Al1—Mg12.8074 (3)O2—C41.4384 (11)
Al1—O51.7644 (6)O3—C51.4370 (12)
Al1—O61.7456 (6)O3—C61.4365 (11)
Al1—O71.7374 (6)O4—C71.4367 (11)
Al1—O81.7425 (6)O4—C81.4409 (11)
Al2—O61.7384 (6)O5—H50.750 (18)
Al2—O91.7645 (6)O7—C101.3713 (9)
Al2—O101.7307 (6)O8—C131.3731 (9)
Al2—O111.7472 (6)O9—C161.3731 (9)
Mg1—O12.1175 (7)O10—C191.3644 (9)
Mg1—O22.1021 (6)O11—C221.3731 (9)
Mg1—O32.1185 (6)C1—H1A0.993 (16)
Mg1—O42.0813 (6)C1—H1C0.953 (16)
Mg1—O52.0470 (6)C1—H1B0.960 (16)
Mg1—O62.0383 (6)C2—H2A0.979 (15)
F1—C91.3252 (11)C2—H2B0.970 (16)
F2—C91.3336 (11)C2—C31.4998 (15)
F3—C91.3384 (11)C3—H3B0.940 (14)
F4—C111.3296 (12)C3—H3A0.978 (15)
F5—C111.3491 (11)C4—H4B0.954 (15)
F6—C111.3337 (11)C4—H4C0.955 (17)
F7—C121.3242 (14)C4—H4A0.977 (17)
F8—C121.3320 (12)C5—H5C0.953 (16)
F9—C121.3417 (12)C5—H5A0.985 (18)
F10—C141.3239 (12)C5—H5B0.934 (18)
F11—C141.3406 (12)C6—H6A0.965 (13)
F12—C141.3344 (11)C6—H6B0.973 (15)
F13—C151.3372 (11)C6—C71.5023 (14)
F14—C151.3369 (11)C7—H7A0.977 (15)
F15—C151.3418 (10)C7—H7B0.997 (14)
F16—C171.3337 (11)C8—H8A0.997 (16)
F17—C171.3269 (10)C8—H8C0.940 (16)
F18—C171.3502 (10)C8—H8B0.940 (16)
F19—C181.3436 (11)C9—C101.5289 (11)
F20—C181.3342 (11)C10—H100.955 (13)
F21—C181.3401 (11)C10—C111.5314 (12)
F22—C201.3341 (10)C12—C131.5288 (13)
F23—C201.3342 (10)C13—H130.966 (13)
F24—C201.3447 (10)C13—C141.5309 (12)
F25—C211.3290 (11)C15—C161.5313 (11)
F26—C211.3342 (11)C16—H160.975 (12)
F27—C211.3418 (10)C16—C171.5282 (12)
F28—C231.3347 (10)C18—C191.5317 (12)
F29—C231.3430 (11)C19—H190.964 (14)
F30—C231.3416 (10)C19—C201.5308 (12)
O1—C11.4423 (11)C21—C221.5308 (11)
O1—C21.4393 (11)C22—H220.976 (13)
O2—C31.4362 (11)C22—C231.5284 (11)
O5—Al1—Mg146.62 (2)C6—C7—H7A109.9 (9)
O6—Al1—Mg146.280 (19)C6—C7—H7B112.9 (8)
O6—Al1—O592.84 (3)H7A—C7—H7B108.6 (11)
O7—Al1—Mg1121.25 (2)O4—C8—H8A110.3 (9)
O7—Al1—O5115.19 (3)O4—C8—H8C108.7 (9)
O7—Al1—O6109.19 (3)O4—C8—H8B109.4 (9)
O7—Al1—O8108.90 (3)H8A—C8—H8C109.1 (13)
O8—Al1—Mg1129.85 (2)H8A—C8—H8B106.3 (13)
O8—Al1—O5112.28 (3)H8C—C8—H8B113.0 (13)
O8—Al1—O6117.93 (3)F1—C9—F2106.94 (8)
O6—Al2—O9114.57 (3)F1—C9—F3107.70 (7)
O6—Al2—O11107.80 (3)F1—C9—C10113.08 (7)
O10—Al2—O6111.99 (3)F2—C9—F3107.24 (8)
O10—Al2—O9102.33 (3)F2—C9—C10110.02 (7)
O10—Al2—O11115.11 (3)F3—C9—C10111.59 (8)
O11—Al2—O9104.97 (3)O7—C10—C9108.99 (7)
O1—Mg1—Al195.31 (2)O7—C10—H10115.1 (8)
O1—Mg1—O391.48 (3)O7—C10—C11110.22 (7)
O2—Mg1—Al1137.67 (2)C9—C10—H10106.8 (8)
O2—Mg1—O177.08 (3)C9—C10—C11111.41 (7)
O2—Mg1—O391.11 (3)C11—C10—H10104.2 (8)
O3—Mg1—Al1131.01 (2)F4—C11—F5106.72 (8)
O4—Mg1—Al199.60 (2)F4—C11—F6107.79 (9)
O4—Mg1—O1164.77 (3)F4—C11—C10113.43 (8)
O4—Mg1—O293.74 (3)F5—C11—C10108.94 (7)
O4—Mg1—O376.40 (3)F6—C11—F5106.86 (8)
O5—Mg1—Al138.791 (17)F6—C11—C10112.73 (8)
O5—Mg1—O191.83 (3)F7—C12—F8108.82 (10)
O5—Mg1—O2168.38 (3)F7—C12—F9106.99 (9)
O5—Mg1—O392.66 (3)F7—C12—C13113.23 (8)
O5—Mg1—O497.83 (3)F8—C12—F9106.27 (9)
O6—Mg1—Al138.241 (16)F8—C12—C13108.92 (8)
O6—Mg1—O198.71 (3)F9—C12—C13112.33 (9)
O6—Mg1—O2101.00 (2)O8—C13—C12110.17 (7)
O6—Mg1—O3165.62 (3)O8—C13—H13115.0 (7)
O6—Mg1—O494.94 (3)O8—C13—C14108.92 (7)
O6—Mg1—O576.99 (2)C12—C13—H13105.4 (8)
C1—O1—Mg1126.61 (5)C12—C13—C14111.77 (7)
C2—O1—Mg1109.81 (5)C14—C13—H13105.6 (8)
C2—O1—C1112.43 (7)F10—C14—F11106.54 (8)
C3—O2—Mg1114.36 (6)F10—C14—F12107.70 (8)
C3—O2—C4110.90 (7)F10—C14—C13112.93 (8)
C4—O2—Mg1121.88 (5)F11—C14—C13110.17 (7)
C5—O3—Mg1124.96 (6)F12—C14—F11106.74 (8)
C6—O3—Mg1109.69 (5)F12—C14—C13112.41 (8)
C6—O3—C5112.30 (7)F13—C15—F15107.31 (7)
C7—O4—Mg1116.74 (5)F13—C15—C16113.31 (7)
C7—O4—C8111.98 (7)F14—C15—F13106.81 (8)
C8—O4—Mg1129.09 (5)F14—C15—F15107.11 (7)
Al1—O5—Mg194.59 (3)F14—C15—C16109.92 (7)
Al1—O5—H5122.8 (13)F15—C15—C16112.06 (7)
Mg1—O5—H5141.3 (13)O9—C16—C15110.00 (6)
Al1—O6—Mg195.48 (3)O9—C16—H16114.3 (7)
Al2—O6—Al1128.72 (3)O9—C16—C17108.89 (6)
Al2—O6—Mg1135.07 (3)C15—C16—H16104.3 (7)
C10—O7—Al1131.50 (5)C17—C16—C15112.01 (6)
C13—O8—Al1131.68 (5)C17—C16—H16107.4 (7)
C16—O9—Al2124.61 (5)F16—C17—F18107.16 (7)
C19—O10—Al2147.43 (6)F16—C17—C16113.48 (7)
C22—O11—Al2128.68 (5)F17—C17—F16107.00 (8)
O1—C1—H1A110.0 (9)F17—C17—F18106.62 (7)
O1—C1—H1C106.8 (10)F17—C17—C16110.10 (7)
O1—C1—H1B107.1 (9)F18—C17—C16112.11 (7)
H1A—C1—H1C111.6 (13)F19—C18—C19112.73 (7)
H1A—C1—H1B112.5 (13)F20—C18—F19107.59 (8)
H1C—C1—H1B108.6 (13)F20—C18—F21107.68 (8)
O1—C2—H2A109.4 (9)F20—C18—C19110.33 (7)
O1—C2—H2B108.4 (9)F21—C18—F19107.10 (8)
O1—C2—C3106.19 (7)F21—C18—C19111.19 (8)
H2A—C2—H2B109.6 (13)O10—C19—C18112.11 (7)
C3—C2—H2A112.6 (9)O10—C19—H19114.2 (8)
C3—C2—H2B110.6 (9)O10—C19—C20107.27 (7)
O2—C3—C2107.02 (7)C18—C19—H19105.3 (8)
O2—C3—H3B110.7 (9)C20—C19—C18110.97 (7)
O2—C3—H3A108.2 (9)C20—C19—H19107.0 (8)
C2—C3—H3B111.4 (9)F22—C20—F23106.59 (8)
C2—C3—H3A110.2 (9)F22—C20—F24107.31 (7)
H3B—C3—H3A109.3 (12)F22—C20—C19112.61 (7)
O2—C4—H4B110.5 (9)F23—C20—F24107.19 (7)
O2—C4—H4C107.9 (10)F23—C20—C19110.13 (7)
O2—C4—H4A107.8 (10)F24—C20—C19112.68 (7)
H4B—C4—H4C109.1 (13)F25—C21—F26107.54 (8)
H4B—C4—H4A111.8 (13)F25—C21—F27107.66 (8)
H4C—C4—H4A109.7 (14)F25—C21—C22112.32 (7)
O3—C5—H5C108.5 (9)F26—C21—F27106.68 (8)
O3—C5—H5A109.6 (10)F26—C21—C22109.65 (7)
O3—C5—H5B110.8 (11)F27—C21—C22112.72 (7)
H5C—C5—H5A108.0 (13)O11—C22—C21109.68 (6)
H5C—C5—H5B107.4 (14)O11—C22—H22116.7 (8)
H5A—C5—H5B112.4 (15)O11—C22—C23108.94 (6)
O3—C6—H6A108.8 (8)C21—C22—H22104.9 (8)
O3—C6—H6B110.4 (9)C23—C22—C21111.90 (7)
O3—C6—C7107.01 (7)C23—C22—H22104.7 (8)
H6A—C6—H6B109.7 (12)F28—C23—F29107.37 (8)
C7—C6—H6A109.8 (8)F28—C23—F30107.43 (7)
C7—C6—H6B111.1 (9)F28—C23—C22112.86 (7)
O4—C7—C6107.91 (7)F29—C23—C22109.54 (7)
O4—C7—H7A109.1 (9)F30—C23—F29106.55 (7)
O4—C7—H7B108.5 (8)F30—C23—C22112.76 (7)
Al1—O7—C10—C9−164.38 (6)O6—Al2—O10—C19−31.10 (12)
Al1—O7—C10—C1173.05 (9)O6—Al2—O11—C22−160.88 (6)
Al1—O8—C13—C12−104.13 (8)O7—Al1—O5—Mg1−110.14 (3)
Al1—O8—C13—C14132.95 (7)O7—Al1—O6—Al2−56.01 (5)
Al2—O9—C16—C15−105.20 (7)O7—Al1—O6—Mg1115.29 (3)
Al2—O9—C16—C17131.71 (6)O7—Al1—O8—C13−116.23 (7)
Al2—O10—C19—C18−73.76 (12)O7—C10—C11—F461.25 (10)
Al2—O10—C19—C20164.18 (8)O7—C10—C11—F5−57.46 (9)
Al2—O11—C22—C21−107.26 (7)O7—C10—C11—F6−175.90 (8)
Al2—O11—C22—C23129.95 (6)O8—Al1—O5—Mg1124.45 (3)
Mg1—Al1—O6—Al2−171.30 (6)O8—Al1—O6—Al268.93 (5)
Mg1—Al1—O7—C10−148.45 (6)O8—Al1—O6—Mg1−119.77 (3)
Mg1—Al1—O8—C1363.88 (8)O8—Al1—O7—C1031.66 (8)
Mg1—O1—C2—C3−49.83 (8)O8—C13—C14—F1062.80 (10)
Mg1—O2—C3—C2−32.68 (9)O8—C13—C14—F11−56.19 (10)
Mg1—O3—C6—C750.27 (8)O8—C13—C14—F12−175.09 (8)
Mg1—O4—C7—C621.82 (9)O9—Al2—O6—Al197.72 (4)
F1—C9—C10—O7−62.37 (9)O9—Al2—O6—Mg1−69.97 (5)
F1—C9—C10—C1159.47 (10)O9—Al2—O10—C19−154.29 (10)
F2—C9—C10—O757.12 (9)O9—Al2—O11—C22−38.33 (7)
F2—C9—C10—C11178.96 (8)O9—C16—C17—F1657.58 (9)
F3—C9—C10—O7176.03 (7)O9—C16—C17—F17−62.31 (9)
F3—C9—C10—C11−62.13 (10)O9—C16—C17—F18179.17 (7)
F7—C12—C13—O8−53.87 (10)O10—Al2—O6—Al1−18.24 (5)
F7—C12—C13—C1467.37 (10)O10—Al2—O6—Mg1174.06 (4)
F8—C12—C13—O867.34 (11)O10—Al2—O9—C1614.74 (7)
F8—C12—C13—C14−171.42 (9)O10—Al2—O11—C2273.34 (7)
F9—C12—C13—O8−175.20 (8)O10—C19—C20—F2248.57 (9)
F9—C12—C13—C14−53.97 (11)O10—C19—C20—F23−70.24 (8)
F13—C15—C16—O9−63.10 (9)O10—C19—C20—F24170.13 (7)
F13—C15—C16—C1758.14 (9)O11—Al2—O6—Al1−145.85 (4)
F14—C15—C16—O956.31 (9)O11—Al2—O6—Mg146.46 (5)
F14—C15—C16—C17177.55 (7)O11—Al2—O9—C16135.28 (6)
F15—C15—C16—O9175.29 (7)O11—Al2—O10—C1992.49 (11)
F15—C15—C16—C17−63.47 (9)O11—C22—C23—F2855.14 (9)
F19—C18—C19—O10−75.70 (9)O11—C22—C23—F29−64.43 (8)
F19—C18—C19—C2044.23 (10)O11—C22—C23—F30177.10 (7)
F20—C18—C19—O1044.60 (10)C1—O1—C2—C3163.61 (8)
F20—C18—C19—C20164.53 (7)C4—O2—C3—C2−175.18 (8)
F21—C18—C19—O10164.01 (7)C5—O3—C6—C7−166.16 (8)
F21—C18—C19—C20−76.06 (9)C8—O4—C7—C6−173.46 (8)
F25—C21—C22—O11−56.24 (9)C9—C10—C11—F4−59.88 (10)
F25—C21—C22—C2364.78 (9)C9—C10—C11—F5−178.59 (7)
F26—C21—C22—O1163.25 (9)C9—C10—C11—F662.97 (10)
F26—C21—C22—C23−175.73 (7)C12—C13—C14—F10−59.15 (10)
F27—C21—C22—O11−178.07 (7)C12—C13—C14—F11−178.15 (8)
F27—C21—C22—C23−57.05 (10)C12—C13—C14—F1262.95 (11)
O1—C2—C3—O253.21 (10)C15—C16—C17—F16−64.29 (9)
O3—C6—C7—O4−46.18 (10)C15—C16—C17—F17175.82 (7)
O5—Al1—O6—Al2−173.95 (4)C15—C16—C17—F1857.30 (9)
O5—Al1—O6—Mg1−2.65 (3)C18—C19—C20—F22−74.20 (9)
O5—Al1—O7—C10−95.49 (7)C18—C19—C20—F23166.98 (7)
O5—Al1—O8—C1312.55 (8)C18—C19—C20—F2447.35 (9)
O6—Al1—O5—Mg12.63 (3)C21—C22—C23—F28−66.31 (9)
O6—Al1—O7—C10161.70 (7)C21—C22—C23—F29174.12 (7)
O6—Al1—O8—C13118.68 (7)C21—C22—C23—F3055.65 (9)
O6—Al2—O9—C16−106.68 (6)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O5—H5···F18i0.750 (18)2.315 (18)2.9816 (8)148.7 (17)
C2—H2B···F30ii0.970 (16)2.527 (16)3.4204 (11)153.1 (12)
C4—H4A···F6iii0.977 (17)2.539 (17)3.5007 (13)168.1 (13)
C7—H7B···F22iv0.997 (14)2.500 (14)3.0101 (10)111.3 (10)
C8—H8C···O110.940 (16)2.515 (16)3.3831 (11)153.7 (13)
C19—H19···O80.964 (14)2.625 (14)3.4214 (10)140.2 (11)
Symmetry codes: (i) −x+1/2, y−1/2, −z+1/2; (ii) −x+1, −y+1, −z+1; (iii) x+1/2, −y+1/2, z+1/2; (iv) −x+3/2, y−1/2, −z+1/2.
 

Acknowledgements

ML is grateful to Prof. Andrej Šmalc for helpful discussions.

Funding information

Funding for this research was provided by: European Research Council (ERC) under the European Union's Horizon 2020 research and innovation programme (grant No. 950625); Jožef Stefan Institute Director's Fund; Slovenian Research Agency (grant Nos. P2-0423 and N2-0279).

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ISSN: 2414-3146
Volume 8| Part 9| September 2023| x230716
https://doi.org/10.1107/S2414314623007162