Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229614014302/fn3170sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S2053229614014302/fn3170AlCl3_15H2O_150Ksup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2053229614014302/fn3170AlBr3_15H2O_120Ksup3.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2053229614014302/fn3170AlI3_15H2O_100Ksup4.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2053229614014302/fn3170AlI3_17H2O_150Ksup5.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S2053229614014302/fn3170AlBr3_9H2O_100Ksup6.hkl | |
Chemical Markup Language (CML) file https://doi.org/10.1107/S2053229614014302/fn3170AlCl3_15H2O_150Ksup7.cml |
CCDC references: 1009022; 1009023; 1009024; 1009025; 1009026
In recent years a wealth of evidence for the occurrence of large quantities of salts (sulfates, chlorides) and water on Mars has been accumulated from orbiter observations (McEwen et al., 2011; Chevrier & Rivera-Valentin, 2012) and robot missions (Boynton et al., 2009; Chevrier et al., 2009; Hecht et al., 2009; Navarro-González et al., 2010; Toulmin et al., 1977). Fairly direct observations of liquid drops at the Phoenix lander (Chevrier et al., 2009; Renno et al., 2009), in combination with unexpectedly large concentrations of perchlorate, magnesium and sodium, support the view that surface processes of redistribution of water on Mars take place due to the presence of salts capable of hydration/dehydration and liquefaction caused by deliquescence (Kite et al., 2013; Davila et al., 2010), depending on seasonal and diurnal variations of temperature between 190 and 283 K. From available phase equilibrium data, Möhlmann & Thomsen (2011) listed a number of ionic compounds enabling the formation of at least temporary aqueous solutions on Mars, liquid at temperatures down to 200 K. These could serve as an environment for life, and should have a large impact on the processes of chemical weathering and chemical-element redistribution. Explanations and predictions of possible surface or sub-surface processes on Mars require a deeper insight into the behaviour of salt solutions at very low temperatures, particularly crystallization and dissolution. However, present knowledge does not allow profound predictions of crystallization and dissolution processes in low-temperature aqueous salt solutions, called cryo-brines (Möhlmann & Thomsen, 2011).
In Parts I and II of this series, the hydrates of magnesium (Hennings et al., 2013) and calcium halides (Hennings et al., 2014), respectively, crystallizing at low temperatures, were identified and structurally characterized. Crystal structures of hydrates of aluminium halides are known only for the room-temperature stable AlCl3.6H2O (Buchanan & Harris, 1968; Andress & Carpenter, 1934) and AlF3.9H2O (Kemnitz et al., 2006), not for those stable in aqueous solution at low temperature. This paper continues the series by presenting five new crystal structures of interesting hydrates with extremely high water contents, namely AlCl3.15H2O, AlBr3.15H2O, AlI3.15H2O, AlI3.17H2O and AlBr3.9H2O. The novel crystal structures AlI3.15H2O and AlI3.17H2O will be described with a complete second hydration sphere around the cations, an aspect often discussed in structure–property relations of multivalent metal salt solutions (Geiger et al., 1979; Waluyo et al., 2011; Valyashko & Ivanov, 1979; Bergström et al., 1991).
AlCl3.15H2O crystallized from an aqueous solution of 25.3 wt% AlCl3 maintained at 228 K for 2 d. Aluminium chloride hexahydrate (Riedel de Haen, pure) was used to prepare this solution. AlBr3.15H2O crystallized from an aqueous solution of 38.1 wt% AlBr3 mainained at 228 K for 10 d, and AlBr3.9H2O from an aqueous solution of 53.3 wt% AlBr3 maintained at 273 K for 3d. Aluminium bromide (VEB Feinchemikalien, pure, anhydrous) was used to prepare these solutions. AlI3.15H2O crystallized from an aqueous solution of 53.5 wt% AlI3 at 228 K after 30 d, and AlI3.17H2O crystallized from an aqueous solution of 53.5 wt% AlI3 at 228 K after 5 d. Crystals of the latter were metastable at these conditions and converted into the pentadecahydrate after some days. Aluminium iodide (Schuchardt München, pure, anhydrous) was used to prepare these solutions. The halide ion content of all the solutions was analysed by means of argentometric titration. All crystals (except AlI3.17H2O) are stable in their saturated solution over a period of at least four weeks. Crystal shape and size are given in Table 1.
The samples were stored in a freezer or cryostat at low temperatures. The crystals were separated and embedded in perflourinated ether (Galden 1438OB, Solvay Solexis) for X-ray analysis at an appropriate temperature.
Crystal data, data collection and structure refinement details are summarized in Table 1. H atoms were placed in the positions indicated by difference Fourier maps and refined with the riding-atom model; only in the case of AlCl3.15H2O could some of the H atoms be refined isotropically. For the geometries of all the water molecules, O—H and H···H distance restraints of 0.84 (1) and 1.4 (1) Å, respectively, were applied.
These three pentadecahydrates are the most water-rich hydrates known for aluminium salts, crystallizing from aqueous solutions as stable phases. Of the three halides (Cl, Br, I), only the crystal structure of aluminium chloride hexahydrate has been investigated previously (Buchanan & Harris, 1968; Andress & Carpenter, 1934). Higher hydrates are Al(ClO4)3.9H2O (Davidian et al., 2012), Al(NO3)3.9H2O (Herpin & Sudarsanan, 1965) and AlF3.9H2O (Kemnitz et al., 2006). For iodides or bromides, no structures are available in the ICSD (Inorganic Crystal Structure Database; YEAR?; https://icsd.fiz-karlsruhe.de/icsd/). For the chloride, no hints existed for the existence of a hydrate with a water content higher than six. Only the phase diagram, with a change in the slope of the hydrate curve at lower temperatures, gives clues that there should be another higher hydrated phase. For the bromide and iodide, Panfilow (1896) described the preparation of pentadecahydrates at temperatures below 261 K. He determined water content by chemical analysis, after drying the obtained crystals between sheets of filter paper.
The asymmetric units in the crystal structures of the three pentadecahydrates are illustrated in Figs. 1(a)–1(c). AlCl3.15H2O and AlBr3.15H2O crystallize in the same space group and have very similar unit-cell dimensions (Table 1). The difference in lattice parameters is only due to the larger anion in the bromide structure. The crystal structure of AlI3.15H2O is different to the others, crystallizing in a higher-symmetry space group.
As expected in all three hydrates, the Al3+ cation is octahedrally coordinated by six water molecules. For each hydrate, one can also recognize a second coordination sphere around the cations, albeit built up differently. In the chloride and bromide salts, 11 water molecules and one halide anion enter this secondary sphere. Thus, every water molecule of the primary sphere acts as a two-fold hydrogen-bond donor for the second hydration sphere, except for one water molecule which also points to one chloride or bromide ion, respectively (Fig. 2a). In this way, nearly complete secondary hydration shells are achieved around the cations. Since the given hydration spheres require 17 molecules of water per Al3+ cation, the secondary hydration spheres share four water molecules along their edges. Representing the geometry of the second coordination spheres as icosahedra, chains are formed running along the b direction (Fig. 3a). In the structure of AlI3.15H2O, this is the first time a complete developed secondary hydration shell has been observed for the cations, where the aluminium positions are split off into two different environments, atom Al1 with only ten molecules of water in the second sphere (Fig. 2b) and atom Al2 with 12 molecules of water in the second sphere (Fig. 2c). The latter provides an interesting link to the discussion about the structure of electrolyte solutions containing cations with a high charge/radius ratio, as in the case of Al3+. For such electrolytes the formation of a second hydration shell was assumed (Geiger et al., 1979; Waluyo et al., 2011; Valyashko & Ivanov, 1979; Bergström et al., 1991), but until now not directly observed. The second sphere of Al1 consists of ten water molecules and two iodide ions, as shown in Fig. 2(b). In this environment there is some disorder, dynamic or static, related to the water molecules of O14 and O8, as well as to iodide anion I3. Refinement into positional disorder yields only small variations in the coordinates of O and I. Fig. 4 illustrates the two extreme positions of the orientation of these water molecules relative to each other and in correlation with atom I3. As already shown for AlCl3.15H2O and AlBr3.15H2O (Fig 3a) and also in AlI3.15H2O, the secondary coordination spheres of both Al1 and Al2 share two edges, forming chains (Figs. 3b and 3c). The sharing water molecules are those from O13 for Al1 and O7 for Al2.
The heptadecahydrate, AlI3.17H2O, is the most water-rich hydrate ever prepared from an aluminium salt. It crystallized only as an intermediate phase and changed its habit and composition after some days into the pentadecahydrate. The asymmetric unit contains two formula units with two crystallographically distinct octahedrally coordinated Al atoms (Fig. 5a). Both Al atoms are coordinated in the first shell by six and in the second shell by an additional 12 water molecules, as shown in Fig. 5(b) for atom Al1, for example. Atom Al2 exhibits the same coordination as atom Al1.
The second coordination spheres are linked via edge sharing to form zig-zag chains. This happens for both Al atoms in the same way and is shown in Fig. 6(a) for atom Al2. An enlarged view of the crystal structure in the a direction (Fig. 6b) shows the arrangement of the I atoms around the chains. The chains are oriented into the viewing direction and the I atoms form layers between the chains. The different chains formed by different Al atoms are located at alternate positions in the unit cell. The Al1 chains are located at the corners, whereas the Al2 chains are located in the centre of the unit cell (Fig. 6b).
Aluminium bromide hexahydrate was reported (Panfilow, 1896) as the stable solid phase at room temperature. However, the composition was derived from chemical analyses after drying the salt over sulfuric acid. According to our investigations, this composition and stability are not confirmed for room temperature.
The Al3+ cation of AlBr3.9H2O is surrounded octahedrally in the first coordination shell. All water molecules of the first shell are connected via hydrogen bonds towards one Br atom and another water molecule in the second shell, except water molecule O2, which forms two hydrogen bonds towards Br atoms. The formation of the second shell around the Al atom is shown in Fig. 7. Consequently, the second coordination sphere of Al3+ consists of four molecules of water (highlighted in orange) and eight bromide ions. This is different to the coordination in the nonahydrates of magnesium bromide and iodide (Hennings et al., 2013). In those structures, each water molecule of the first shell forms hydrogen bonds towards one anion and another water molecule from the second shell, thus also comprising six water molecules and six halide ions in the second shell.
One water molecule (O6) does not participate in the hydration spheres, but connects them within the bc plane, as shown in Fig. 8(a) (Br atoms not drawn). Rotating the view onto the ab plane, the connections of the second hydration spheres along the a axis become visible (Fig. 8b). All four water molecules of the second hydration sphere are shared along the chains. Also shown in Fig. 8(b) are the solvent water molecules, highlighted in orange. The representation reveals that every water molecule in the second hydration sphere of Al3+ donates one hydrogen bond to the solvent water. The latter connects the hydration complexes of Al3+ in the bc plane, as mentioned above. A complete picture of the hydrogen-bond network, including the Br atoms, is given in Fig. 9.
For related literature, see: Andress & Carpenter (1934); Bergström et al. (1991); Boynton (2009); Buchanan & Harris (1968); Chevrier (2009); Chevrier & Rivera-Valentin (2012); Davidian (2012); Davila et al. (2010); Geiger et al. (1979); Hecht (2009); Hennings (2014); Hennings et al. (2013); Herpin & Sudarsanan (1965); Kemnitz et al. (2006); Kite et al. (2013); Möhlmann & Thomsen (2011); McEwen et al. (2011); Navarro-González (2010); Panfilow (1896); Renno (2009); Toulmin, Baird, Clark, Keil, Rose, Christian, Evans & Kelliher (1977); Valyashko & Ivanov (1979); Waluyo (2011).
For all compounds, data collection: X-AREA (Stoe & Cie, 2003); cell refinement: X-AREA (Stoe & Cie, 2003); data reduction: X-RED (Stoe & Cie, 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2012 (Sheldrick, 2008); molecular graphics: SHELXL2012 (Sheldrick, 2008); software used to prepare material for publication: SHELXL2012 (Sheldrick, 2008).
[Al(H2O)6]Cl3·9H2O | F(000) = 856 |
Mr = 403.57 | Dx = 1.473 Mg m−3 |
Monoclinic, Cc | Mo Kα radiation, λ = 0.71073 Å |
a = 18.6568 (19) Å | Cell parameters from 14771 reflections |
b = 6.5415 (4) Å | θ = 2.5–29.6° |
c = 18.0351 (18) Å | µ = 0.61 mm−1 |
β = 124.223 (7)° | T = 150 K |
V = 1820.0 (3) Å3 | , colourless |
Z = 4 | 0.59 × 0.37 × 0.16 mm |
Stoe IPDS 2T diffractometer | 4973 independent reflections |
Radiation source: sealed X-ray tube | 4480 reflections with I > 2σ(I) |
Detector resolution: 6.67 pixels mm-1 | Rint = 0.050 |
rotation method scans | θmax = 29.5°, θmin = 2.5° |
Absorption correction: integration (Coppens, 1970) | h = −24→24 |
Tmin = 0.761, Tmax = 0.908 | k = −7→9 |
17267 measured reflections | l = −23→23 |
Refinement on F2 | Hydrogen site location: difference Fourier map |
Least-squares matrix: full | All H-atom parameters refined |
R[F2 > 2σ(F2)] = 0.028 | w = 1/[σ2(Fo2) + (0.0512P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.074 | (Δ/σ)max < 0.001 |
S = 1.01 | Δρmax = 0.30 e Å−3 |
4973 reflections | Δρmin = −0.18 e Å−3 |
292 parameters | Absolute structure: Classical Flack (1983) method preferred over Parsons (2003) because s.u. is lower |
47 restraints | Absolute structure parameter: 0.67 (6) |
[Al(H2O)6]Cl3·9H2O | V = 1820.0 (3) Å3 |
Mr = 403.57 | Z = 4 |
Monoclinic, Cc | Mo Kα radiation |
a = 18.6568 (19) Å | µ = 0.61 mm−1 |
b = 6.5415 (4) Å | T = 150 K |
c = 18.0351 (18) Å | 0.59 × 0.37 × 0.16 mm |
β = 124.223 (7)° |
Stoe IPDS 2T diffractometer | 4973 independent reflections |
Absorption correction: integration (Coppens, 1970) | 4480 reflections with I > 2σ(I) |
Tmin = 0.761, Tmax = 0.908 | Rint = 0.050 |
17267 measured reflections |
R[F2 > 2σ(F2)] = 0.028 | All H-atom parameters refined |
wR(F2) = 0.074 | Δρmax = 0.30 e Å−3 |
S = 1.01 | Δρmin = −0.18 e Å−3 |
4973 reflections | Absolute structure: Classical Flack (1983) method preferred over Parsons (2003) because s.u. is lower |
292 parameters | Absolute structure parameter: 0.67 (6) |
47 restraints |
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. |
x | y | z | Uiso*/Ueq | ||
Cl1 | 0.51081 (4) | 0.73394 (10) | 0.76989 (4) | 0.02079 (14) | |
Cl2 | 0.21030 (4) | 0.75631 (10) | 0.21665 (4) | 0.02192 (15) | |
Al1 | 0.35894 (5) | 0.24057 (13) | 0.49522 (6) | 0.01217 (13) | |
Cl3 | 0.60593 (4) | 0.27390 (12) | 0.52200 (5) | 0.02719 (16) | |
O5 | 0.39882 (12) | 0.3501 (3) | 0.60825 (13) | 0.0161 (4) | |
O3 | 0.32082 (13) | 0.1296 (3) | 0.38194 (13) | 0.0160 (3) | |
O1 | 0.46835 (12) | 0.1194 (3) | 0.54401 (13) | 0.0160 (4) | |
O2 | 0.39543 (13) | 0.4802 (3) | 0.46729 (13) | 0.0166 (4) | |
O4 | 0.24957 (12) | 0.3575 (3) | 0.44710 (14) | 0.0164 (4) | |
O6 | 0.32273 (13) | −0.0002 (3) | 0.52327 (13) | 0.0163 (4) | |
O9 | 0.00889 (13) | 0.7690 (3) | 0.09744 (13) | 0.0186 (4) | |
O8 | 0.21161 (13) | 0.7462 (3) | 0.39188 (14) | 0.0184 (4) | |
O7 | 0.68137 (14) | 0.2142 (4) | 0.73193 (14) | 0.0209 (4) | |
O14 | 0.31940 (15) | 0.9728 (4) | 0.66825 (15) | 0.0232 (4) | |
O13 | 0.29682 (15) | 0.5524 (4) | 0.64031 (18) | 0.0271 (5) | |
O10 | 0.40996 (15) | 0.5307 (4) | 0.33072 (16) | 0.0222 (4) | |
O11 | 0.43670 (15) | 0.9561 (4) | 0.35889 (17) | 0.0244 (4) | |
O12 | 0.11666 (14) | 0.1882 (4) | 0.43428 (15) | 0.0271 (4) | |
O15 | 0.54114 (14) | 0.2030 (4) | 0.75315 (14) | 0.0215 (4) | |
H2A | 0.433 (3) | 0.559 (7) | 0.507 (3) | 0.056 (16)* | |
H2B | 0.400 (3) | 0.483 (7) | 0.424 (2) | 0.035 (12)* | |
H8B | 0.1590 (13) | 0.766 (7) | 0.371 (3) | 0.034 (11)* | |
H8A | 0.214 (3) | 0.762 (7) | 0.348 (2) | 0.036 (12)* | |
H4A | 0.242 (3) | 0.480 (3) | 0.432 (3) | 0.032 (11)* | |
H4B | 0.213 (3) | 0.294 (8) | 0.451 (4) | 0.049 (14)* | |
H5B | 0.445 (2) | 0.309 (9) | 0.655 (2) | 0.052 (15)* | |
H5A | 0.368 (2) | 0.420 (5) | 0.618 (3) | 0.021 (9)* | |
H1A | 0.482 (3) | −0.004 (3) | 0.558 (3) | 0.030 (11)* | |
H3A | 0.355 (3) | 0.067 (8) | 0.373 (4) | 0.056 (16)* | |
H3B | 0.2780 (19) | 0.177 (7) | 0.3349 (18) | 0.030 (10)* | |
H11B | 0.440 (3) | 0.828 (2) | 0.359 (3) | 0.029 (10)* | |
H7B | 0.689 (3) | 0.091 (3) | 0.726 (3) | 0.033 (11)* | |
H10B | 0.445 (3) | 0.452 (7) | 0.330 (4) | 0.050 (15)* | |
H15B | 0.534 (3) | 0.078 (3) | 0.757 (3) | 0.039 (12)* | |
H13B | 0.305 (3) | 0.680 (3) | 0.648 (3) | 0.040 (13)* | |
H14B | 0.3651 (19) | 0.979 (7) | 0.7198 (16) | 0.038 (12)* | |
H14A | 0.286 (3) | 1.047 (6) | 0.674 (4) | 0.042 (14)* | |
H6A | 0.289 (2) | −0.080 (6) | 0.482 (2) | 0.027 (10)* | |
H6B | 0.322 (4) | −0.005 (8) | 0.569 (2) | 0.043 (14)* | |
H13A | 0.2440 (13) | 0.520 (8) | 0.612 (3) | 0.050 (15)* | |
H9A | 0.006 (3) | 0.779 (8) | 0.142 (2) | 0.044 (14)* | |
H9B | 0.0631 (10) | 0.767 (9) | 0.124 (4) | 0.048 (15)* | |
H10A | 0.365 (3) | 0.530 (10) | 0.2787 (19) | 0.064 (17)* | |
H11A | 0.4880 (16) | 0.999 (9) | 0.392 (3) | 0.065 (18)* | |
H12A | 0.088 (3) | 0.160 (9) | 0.3796 (13) | 0.054 (15)* | |
H12B | 0.113 (3) | 0.082 (5) | 0.458 (3) | 0.039 (12)* | |
H1B | 0.506 (2) | 0.175 (6) | 0.540 (3) | 0.022 (9)* | |
H15A | 0.584 (2) | 0.213 (7) | 0.750 (3) | 0.033 (11)* | |
H7A | 0.663 (3) | 0.272 (7) | 0.6832 (19) | 0.042 (13)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cl1 | 0.0187 (3) | 0.0241 (3) | 0.0196 (3) | −0.0012 (3) | 0.0108 (2) | −0.0005 (3) |
Cl2 | 0.0206 (3) | 0.0226 (3) | 0.0238 (3) | −0.0012 (2) | 0.0133 (3) | −0.0005 (2) |
Al1 | 0.0119 (2) | 0.0123 (3) | 0.0110 (3) | −0.0005 (2) | 0.0056 (2) | −0.0004 (2) |
Cl3 | 0.0185 (3) | 0.0372 (4) | 0.0239 (3) | −0.0017 (3) | 0.0107 (2) | 0.0099 (3) |
O5 | 0.0156 (9) | 0.0191 (9) | 0.0125 (8) | 0.0012 (7) | 0.0072 (7) | −0.0020 (7) |
O3 | 0.0147 (8) | 0.0187 (8) | 0.0115 (8) | 0.0008 (7) | 0.0055 (7) | −0.0023 (7) |
O1 | 0.0132 (8) | 0.0159 (8) | 0.0182 (9) | 0.0010 (7) | 0.0085 (7) | 0.0017 (7) |
O2 | 0.0187 (8) | 0.0160 (8) | 0.0133 (8) | −0.0039 (7) | 0.0080 (7) | −0.0016 (7) |
O4 | 0.0137 (8) | 0.0150 (8) | 0.0195 (9) | −0.0001 (7) | 0.0086 (7) | 0.0017 (7) |
O6 | 0.0191 (8) | 0.0158 (8) | 0.0143 (8) | −0.0033 (7) | 0.0095 (7) | 0.0000 (7) |
O9 | 0.0167 (9) | 0.0189 (9) | 0.0172 (9) | 0.0010 (7) | 0.0076 (8) | −0.0001 (7) |
O8 | 0.0154 (8) | 0.0191 (10) | 0.0183 (9) | −0.0005 (7) | 0.0080 (7) | 0.0000 (7) |
O7 | 0.0217 (10) | 0.0212 (9) | 0.0152 (9) | 0.0002 (8) | 0.0076 (8) | 0.0013 (8) |
O14 | 0.0235 (10) | 0.0292 (11) | 0.0197 (10) | 0.0056 (9) | 0.0139 (9) | 0.0023 (8) |
O13 | 0.0221 (10) | 0.0271 (12) | 0.0363 (12) | −0.0016 (8) | 0.0190 (10) | −0.0073 (9) |
O10 | 0.0237 (10) | 0.0255 (11) | 0.0205 (10) | 0.0004 (8) | 0.0143 (9) | −0.0004 (8) |
O11 | 0.0219 (10) | 0.0232 (11) | 0.0302 (11) | 0.0003 (8) | 0.0159 (9) | −0.0019 (9) |
O12 | 0.0226 (9) | 0.0330 (11) | 0.0239 (10) | −0.0039 (9) | 0.0119 (9) | 0.0051 (9) |
O15 | 0.0200 (9) | 0.0216 (9) | 0.0192 (9) | 0.0013 (8) | 0.0088 (8) | 0.0006 (8) |
Al1—O4 | 1.874 (2) | Al1—O2 | 1.887 (2) |
Al1—O5 | 1.875 (2) | Al1—O3 | 1.890 (2) |
Al1—O1 | 1.884 (2) | Al1—O6 | 1.891 (2) |
O4—Al1—O5 | 90.60 (10) | O1—Al1—O3 | 89.63 (9) |
O4—Al1—O1 | 179.15 (11) | O2—Al1—O3 | 90.20 (9) |
O5—Al1—O1 | 89.41 (10) | O4—Al1—O6 | 90.23 (10) |
O4—Al1—O2 | 89.98 (10) | O5—Al1—O6 | 90.59 (10) |
O5—Al1—O2 | 89.46 (9) | O1—Al1—O6 | 88.91 (9) |
O1—Al1—O2 | 90.88 (10) | O2—Al1—O6 | 179.78 (12) |
O4—Al1—O3 | 90.38 (10) | O3—Al1—O6 | 89.73 (9) |
O5—Al1—O3 | 178.97 (12) |
D—H···A | D—H | H···A | D···A | D—H···A |
O7—H7A···Cl3 | 0.84 (1) | 2.47 (3) | 3.236 (2) | 153 (4) |
O15—H15A···O7 | 0.83 (1) | 2.02 (2) | 2.850 (3) | 174 (4) |
O1—H1B···Cl3 | 0.84 (1) | 2.15 (2) | 2.986 (2) | 171 (4) |
O12—H12B···Cl3i | 0.84 (1) | 2.36 (2) | 3.200 (2) | 177 (5) |
O12—H12A···O15ii | 0.84 (1) | 2.13 (4) | 2.826 (3) | 141 (5) |
O11—H11A···Cl3iii | 0.84 (2) | 2.79 (3) | 3.535 (3) | 149 (5) |
O10—H10A···O13iv | 0.83 (2) | 2.14 (3) | 2.897 (3) | 151 (6) |
O10—H10A···Cl2 | 0.83 (2) | 2.86 (5) | 3.416 (2) | 126 (5) |
O9—H9B···Cl2 | 0.84 (1) | 2.28 (2) | 3.108 (2) | 171 (6) |
O9—H9A···Cl1v | 0.84 (1) | 2.26 (2) | 3.090 (2) | 172 (5) |
O13—H13A···Cl3vi | 0.84 (1) | 2.71 (5) | 3.284 (3) | 127 (5) |
O13—H13A···Cl2vii | 0.84 (1) | 2.93 (5) | 3.329 (3) | 111 (4) |
O6—H6B···O14viii | 0.84 (1) | 1.82 (2) | 2.656 (3) | 178 (5) |
O6—H6A···O8viii | 0.84 (1) | 1.84 (2) | 2.672 (3) | 177 (4) |
O14—H14A···Cl2ix | 0.84 (1) | 2.34 (2) | 3.169 (2) | 170 (5) |
O14—H14B···O11ix | 0.84 (2) | 2.12 (3) | 2.892 (3) | 153 (4) |
O14—H14B···Cl1 | 0.84 (2) | 2.83 (4) | 3.345 (2) | 122 (4) |
O13—H13B···O14 | 0.84 (2) | 1.94 (2) | 2.785 (4) | 177 (5) |
O15—H15B···Cl1viii | 0.84 (1) | 2.33 (2) | 3.165 (2) | 178 (4) |
O10—H10B···Cl1iv | 0.84 (1) | 2.37 (2) | 3.172 (2) | 159 (5) |
O7—H7B···Cl2x | 0.84 (1) | 2.33 (2) | 3.164 (2) | 177 (4) |
O11—H11B···O10 | 0.84 (1) | 2.01 (2) | 2.822 (4) | 163 (4) |
O3—H3B···O7ii | 0.83 (1) | 1.85 (2) | 2.686 (3) | 178 (5) |
O3—H3A···O11viii | 0.84 (1) | 1.84 (2) | 2.673 (3) | 174 (6) |
O1—H1A···O9x | 0.84 (1) | 1.84 (2) | 2.671 (3) | 174 (5) |
O5—H5A···O13 | 0.84 (1) | 1.80 (2) | 2.635 (3) | 175 (4) |
O5—H5B···O15 | 0.84 (2) | 1.81 (2) | 2.646 (3) | 176 (6) |
O4—H4B···O12 | 0.84 (1) | 1.78 (2) | 2.605 (3) | 166 (6) |
O4—H4A···O8 | 0.83 (1) | 1.85 (2) | 2.676 (3) | 173 (5) |
O8—H8A···Cl2 | 0.84 (1) | 2.32 (2) | 3.147 (2) | 171 (5) |
O8—H8B···Cl1v | 0.84 (1) | 2.30 (2) | 3.102 (2) | 159 (5) |
O2—H2B···O10 | 0.84 (1) | 1.82 (2) | 2.646 (3) | 171 (5) |
O2—H2A···O9xi | 0.84 (2) | 1.83 (2) | 2.663 (3) | 175 (6) |
O7—H7A···Cl3 | 0.84 (1) | 2.47 (3) | 3.236 (2) | 153 (4) |
O15—H15A···O7 | 0.83 (1) | 2.02 (2) | 2.850 (3) | 174 (4) |
O1—H1B···Cl3 | 0.84 (1) | 2.15 (2) | 2.986 (2) | 171 (4) |
O12—H12B···Cl3i | 0.84 (1) | 2.36 (2) | 3.200 (2) | 177 (5) |
O12—H12A···O15ii | 0.84 (1) | 2.13 (4) | 2.826 (3) | 141 (5) |
O11—H11A···Cl3iii | 0.84 (2) | 2.79 (3) | 3.535 (3) | 149 (5) |
O10—H10A···O13iv | 0.83 (2) | 2.14 (3) | 2.897 (3) | 151 (6) |
O10—H10A···Cl2 | 0.83 (2) | 2.86 (5) | 3.416 (2) | 126 (5) |
O9—H9B···Cl2 | 0.84 (1) | 2.28 (2) | 3.108 (2) | 171 (6) |
O9—H9A···Cl1v | 0.84 (1) | 2.26 (2) | 3.090 (2) | 172 (5) |
O13—H13A···Cl3vi | 0.84 (1) | 2.71 (5) | 3.284 (3) | 127 (5) |
O13—H13A···Cl2vii | 0.84 (1) | 2.93 (5) | 3.329 (3) | 111 (4) |
O6—H6B···O14viii | 0.84 (1) | 1.82 (2) | 2.656 (3) | 178 (5) |
O6—H6A···O8viii | 0.84 (1) | 1.84 (2) | 2.672 (3) | 177 (4) |
O14—H14A···Cl2ix | 0.84 (1) | 2.34 (2) | 3.169 (2) | 170 (5) |
O14—H14B···O11ix | 0.84 (2) | 2.12 (3) | 2.892 (3) | 153 (4) |
O14—H14B···Cl1 | 0.84 (2) | 2.83 (4) | 3.345 (2) | 122 (4) |
O13—H13B···O14 | 0.84 (2) | 1.94 (2) | 2.785 (4) | 177 (5) |
O15—H15B···Cl1viii | 0.84 (1) | 2.33 (2) | 3.165 (2) | 178 (4) |
O10—H10B···Cl1iv | 0.84 (1) | 2.37 (2) | 3.172 (2) | 159 (5) |
O7—H7B···Cl2x | 0.84 (1) | 2.33 (2) | 3.164 (2) | 177 (4) |
O11—H11B···O10 | 0.84 (1) | 2.01 (2) | 2.822 (4) | 163 (4) |
O3—H3B···O7ii | 0.83 (1) | 1.85 (2) | 2.686 (3) | 178 (5) |
O3—H3A···O11viii | 0.84 (1) | 1.84 (2) | 2.673 (3) | 174 (6) |
O1—H1A···O9x | 0.84 (1) | 1.84 (2) | 2.671 (3) | 174 (5) |
O5—H5A···O13 | 0.84 (1) | 1.80 (2) | 2.635 (3) | 175 (4) |
O5—H5B···O15 | 0.84 (2) | 1.81 (2) | 2.646 (3) | 176 (6) |
O4—H4B···O12 | 0.84 (1) | 1.78 (2) | 2.605 (3) | 166 (6) |
O4—H4A···O8 | 0.83 (1) | 1.85 (2) | 2.676 (3) | 173 (5) |
O8—H8A···Cl2 | 0.84 (1) | 2.32 (2) | 3.147 (2) | 171 (5) |
O8—H8B···Cl1v | 0.84 (1) | 2.30 (2) | 3.102 (2) | 159 (5) |
O2—H2B···O10 | 0.84 (1) | 1.82 (2) | 2.646 (3) | 171 (5) |
O2—H2A···O9xi | 0.84 (2) | 1.83 (2) | 2.663 (3) | 175 (6) |
O7—H7A···Cl3 | 0.84 (1) | 2.47 (3) | 3.236 (2) | 153 (4) |
O15—H15A···O7 | 0.83 (1) | 2.02 (2) | 2.850 (3) | 174 (4) |
O1—H1B···Cl3 | 0.84 (1) | 2.15 (2) | 2.986 (2) | 171 (4) |
O12—H12B···Cl3i | 0.84 (1) | 2.36 (2) | 3.200 (2) | 177 (5) |
O12—H12A···O15ii | 0.84 (1) | 2.13 (4) | 2.826 (3) | 141 (5) |
O11—H11A···Cl3iii | 0.84 (2) | 2.79 (3) | 3.535 (3) | 149 (5) |
O10—H10A···O13iv | 0.83 (2) | 2.14 (3) | 2.897 (3) | 151 (6) |
O10—H10A···Cl2 | 0.83 (2) | 2.86 (5) | 3.416 (2) | 126 (5) |
O9—H9B···Cl2 | 0.84 (1) | 2.28 (2) | 3.108 (2) | 171 (6) |
O9—H9A···Cl1v | 0.84 (1) | 2.26 (2) | 3.090 (2) | 172 (5) |
O13—H13A···Cl3vi | 0.84 (1) | 2.71 (5) | 3.284 (3) | 127 (5) |
O13—H13A···Cl2vii | 0.84 (1) | 2.93 (5) | 3.329 (3) | 111 (4) |
O6—H6B···O14viii | 0.84 (1) | 1.82 (2) | 2.656 (3) | 178 (5) |
O6—H6A···O8viii | 0.84 (1) | 1.84 (2) | 2.672 (3) | 177 (4) |
O14—H14A···Cl2ix | 0.84 (1) | 2.34 (2) | 3.169 (2) | 170 (5) |
O14—H14B···O11ix | 0.84 (2) | 2.12 (3) | 2.892 (3) | 153 (4) |
O14—H14B···Cl1 | 0.84 (2) | 2.83 (4) | 3.345 (2) | 122 (4) |
O13—H13B···O14 | 0.84 (2) | 1.94 (2) | 2.785 (4) | 177 (5) |
O15—H15B···Cl1viii | 0.84 (1) | 2.33 (2) | 3.165 (2) | 178 (4) |
O10—H10B···Cl1iv | 0.84 (1) | 2.37 (2) | 3.172 (2) | 159 (5) |
O7—H7B···Cl2x | 0.84 (1) | 2.33 (2) | 3.164 (2) | 177 (4) |
O11—H11B···O10 | 0.84 (1) | 2.01 (2) | 2.822 (4) | 163 (4) |
O3—H3B···O7ii | 0.83 (1) | 1.85 (2) | 2.686 (3) | 178 (5) |
O3—H3A···O11viii | 0.84 (1) | 1.84 (2) | 2.673 (3) | 174 (6) |
O1—H1A···O9x | 0.84 (1) | 1.84 (2) | 2.671 (3) | 174 (5) |
O5—H5A···O13 | 0.84 (1) | 1.80 (2) | 2.635 (3) | 175 (4) |
O5—H5B···O15 | 0.84 (2) | 1.81 (2) | 2.646 (3) | 176 (6) |
O4—H4B···O12 | 0.84 (1) | 1.78 (2) | 2.605 (3) | 166 (6) |
O4—H4A···O8 | 0.83 (1) | 1.85 (2) | 2.676 (3) | 173 (5) |
O8—H8A···Cl2 | 0.84 (1) | 2.32 (2) | 3.147 (2) | 171 (5) |
O8—H8B···Cl1v | 0.84 (1) | 2.30 (2) | 3.102 (2) | 159 (5) |
O2—H2B···O10 | 0.84 (1) | 1.82 (2) | 2.646 (3) | 171 (5) |
O2—H2A···O9xi | 0.84 (2) | 1.83 (2) | 2.663 (3) | 175 (6) |
O7—H7A···Cl3 | 0.84 (1) | 2.47 (3) | 3.236 (2) | 153 (4) |
O15—H15A···O7 | 0.83 (1) | 2.02 (2) | 2.850 (3) | 174 (4) |
O1—H1B···Cl3 | 0.84 (1) | 2.15 (2) | 2.986 (2) | 171 (4) |
O12—H12B···Cl3i | 0.84 (1) | 2.36 (2) | 3.200 (2) | 177 (5) |
O12—H12A···O15ii | 0.84 (1) | 2.13 (4) | 2.826 (3) | 141 (5) |
O11—H11A···Cl3iii | 0.84 (2) | 2.79 (3) | 3.535 (3) | 149 (5) |
O10—H10A···O13iv | 0.83 (2) | 2.14 (3) | 2.897 (3) | 151 (6) |
O10—H10A···Cl2 | 0.83 (2) | 2.86 (5) | 3.416 (2) | 126 (5) |
O9—H9B···Cl2 | 0.84 (1) | 2.28 (2) | 3.108 (2) | 171 (6) |
O9—H9A···Cl1v | 0.84 (1) | 2.26 (2) | 3.090 (2) | 172 (5) |
O13—H13A···Cl3vi | 0.84 (1) | 2.71 (5) | 3.284 (3) | 127 (5) |
O13—H13A···Cl2vii | 0.84 (1) | 2.93 (5) | 3.329 (3) | 111 (4) |
O6—H6B···O14viii | 0.84 (1) | 1.82 (2) | 2.656 (3) | 178 (5) |
O6—H6A···O8viii | 0.84 (1) | 1.84 (2) | 2.672 (3) | 177 (4) |
O14—H14A···Cl2ix | 0.84 (1) | 2.34 (2) | 3.169 (2) | 170 (5) |
O14—H14B···O11ix | 0.84 (2) | 2.12 (3) | 2.892 (3) | 153 (4) |
O14—H14B···Cl1 | 0.84 (2) | 2.83 (4) | 3.345 (2) | 122 (4) |
O13—H13B···O14 | 0.84 (2) | 1.94 (2) | 2.785 (4) | 177 (5) |
O15—H15B···Cl1viii | 0.84 (1) | 2.33 (2) | 3.165 (2) | 178 (4) |
O10—H10B···Cl1iv | 0.84 (1) | 2.37 (2) | 3.172 (2) | 159 (5) |
O7—H7B···Cl2x | 0.84 (1) | 2.33 (2) | 3.164 (2) | 177 (4) |
O11—H11B···O10 | 0.84 (1) | 2.01 (2) | 2.822 (4) | 163 (4) |
O3—H3B···O7ii | 0.83 (1) | 1.85 (2) | 2.686 (3) | 178 (5) |
O3—H3A···O11viii | 0.84 (1) | 1.84 (2) | 2.673 (3) | 174 (6) |
O1—H1A···O9x | 0.84 (1) | 1.84 (2) | 2.671 (3) | 174 (5) |
O5—H5A···O13 | 0.84 (1) | 1.80 (2) | 2.635 (3) | 175 (4) |
O5—H5B···O15 | 0.84 (2) | 1.81 (2) | 2.646 (3) | 176 (6) |
O4—H4B···O12 | 0.84 (1) | 1.78 (2) | 2.605 (3) | 166 (6) |
O4—H4A···O8 | 0.83 (1) | 1.85 (2) | 2.676 (3) | 173 (5) |
O8—H8A···Cl2 | 0.84 (1) | 2.32 (2) | 3.147 (2) | 171 (5) |
O8—H8B···Cl1v | 0.84 (1) | 2.30 (2) | 3.102 (2) | 159 (5) |
O2—H2B···O10 | 0.84 (1) | 1.82 (2) | 2.646 (3) | 171 (5) |
O2—H2A···O9xi | 0.84 (2) | 1.83 (2) | 2.663 (3) | 175 (6) |
O7—H7A···Cl3 | 0.84 (1) | 2.47 (3) | 3.236 (2) | 153 (4) |
O15—H15A···O7 | 0.83 (1) | 2.02 (2) | 2.850 (3) | 174 (4) |
O1—H1B···Cl3 | 0.84 (1) | 2.15 (2) | 2.986 (2) | 171 (4) |
O12—H12B···Cl3i | 0.84 (1) | 2.36 (2) | 3.200 (2) | 177 (5) |
O12—H12A···O15ii | 0.84 (1) | 2.13 (4) | 2.826 (3) | 141 (5) |
O11—H11A···Cl3iii | 0.84 (2) | 2.79 (3) | 3.535 (3) | 149 (5) |
O10—H10A···O13iv | 0.83 (2) | 2.14 (3) | 2.897 (3) | 151 (6) |
O10—H10A···Cl2 | 0.83 (2) | 2.86 (5) | 3.416 (2) | 126 (5) |
O9—H9B···Cl2 | 0.84 (1) | 2.28 (2) | 3.108 (2) | 171 (6) |
O9—H9A···Cl1v | 0.84 (1) | 2.26 (2) | 3.090 (2) | 172 (5) |
O13—H13A···Cl3vi | 0.84 (1) | 2.71 (5) | 3.284 (3) | 127 (5) |
O13—H13A···Cl2vii | 0.84 (1) | 2.93 (5) | 3.329 (3) | 111 (4) |
O6—H6B···O14viii | 0.84 (1) | 1.82 (2) | 2.656 (3) | 178 (5) |
O6—H6A···O8viii | 0.84 (1) | 1.84 (2) | 2.672 (3) | 177 (4) |
O14—H14A···Cl2ix | 0.84 (1) | 2.34 (2) | 3.169 (2) | 170 (5) |
O14—H14B···O11ix | 0.84 (2) | 2.12 (3) | 2.892 (3) | 153 (4) |
O14—H14B···Cl1 | 0.84 (2) | 2.83 (4) | 3.345 (2) | 122 (4) |
O13—H13B···O14 | 0.84 (2) | 1.94 (2) | 2.785 (4) | 177 (5) |
O15—H15B···Cl1viii | 0.84 (1) | 2.33 (2) | 3.165 (2) | 178 (4) |
O10—H10B···Cl1iv | 0.84 (1) | 2.37 (2) | 3.172 (2) | 159 (5) |
O7—H7B···Cl2x | 0.84 (1) | 2.33 (2) | 3.164 (2) | 177 (4) |
O11—H11B···O10 | 0.84 (1) | 2.01 (2) | 2.822 (4) | 163 (4) |
O3—H3B···O7ii | 0.83 (1) | 1.85 (2) | 2.686 (3) | 178 (5) |
O3—H3A···O11viii | 0.84 (1) | 1.84 (2) | 2.673 (3) | 174 (6) |
O1—H1A···O9x | 0.84 (1) | 1.84 (2) | 2.671 (3) | 174 (5) |
O5—H5A···O13 | 0.84 (1) | 1.80 (2) | 2.635 (3) | 175 (4) |
O5—H5B···O15 | 0.84 (2) | 1.81 (2) | 2.646 (3) | 176 (6) |
O4—H4B···O12 | 0.84 (1) | 1.78 (2) | 2.605 (3) | 166 (6) |
O4—H4A···O8 | 0.83 (1) | 1.85 (2) | 2.676 (3) | 173 (5) |
O8—H8A···Cl2 | 0.84 (1) | 2.32 (2) | 3.147 (2) | 171 (5) |
O8—H8B···Cl1v | 0.84 (1) | 2.30 (2) | 3.102 (2) | 159 (5) |
O2—H2B···O10 | 0.84 (1) | 1.82 (2) | 2.646 (3) | 171 (5) |
O2—H2A···O9xi | 0.84 (2) | 1.83 (2) | 2.663 (3) | 175 (6) |
O2—H2A···O9xi | 0.84 (2) | 1.83 (2) | 2.663 (3) | 175 (6) |
O2—H2B···O10 | 0.84 (1) | 1.82 (2) | 2.646 (3) | 171 (5) |
O8—H8B···Cl1v | 0.84 (1) | 2.30 (2) | 3.102 (2) | 159 (5) |
O8—H8A···Cl2 | 0.84 (1) | 2.32 (2) | 3.147 (2) | 171 (5) |
O4—H4A···O8 | 0.83 (1) | 1.85 (2) | 2.676 (3) | 173 (5) |
O4—H4B···O12 | 0.84 (1) | 1.78 (2) | 2.605 (3) | 166 (6) |
O5—H5B···O15 | 0.84 (2) | 1.81 (2) | 2.646 (3) | 176 (6) |
O5—H5A···O13 | 0.84 (1) | 1.80 (2) | 2.635 (3) | 175 (4) |
O1—H1A···O9x | 0.84 (1) | 1.84 (2) | 2.671 (3) | 174 (5) |
O3—H3A···O11viii | 0.84 (1) | 1.84 (2) | 2.673 (3) | 174 (6) |
O3—H3B···O7ii | 0.83 (1) | 1.85 (2) | 2.686 (3) | 178 (5) |
O11—H11B···O10 | 0.84 (1) | 2.01 (2) | 2.822 (4) | 163 (4) |
O7—H7B···Cl2x | 0.84 (1) | 2.33 (2) | 3.164 (2) | 177 (4) |
O10—H10B···Cl1iv | 0.84 (1) | 2.37 (2) | 3.172 (2) | 159 (5) |
O15—H15B···Cl1viii | 0.84 (1) | 2.33 (2) | 3.165 (2) | 178 (4) |
O13—H13B···O14 | 0.84 (2) | 1.94 (2) | 2.785 (4) | 177 (5) |
O14—H14B···Cl1 | 0.84 (2) | 2.83 (4) | 3.345 (2) | 122 (4) |
O14—H14B···O11ix | 0.84 (2) | 2.12 (3) | 2.892 (3) | 153 (4) |
O14—H14A···Cl2ix | 0.84 (1) | 2.34 (2) | 3.169 (2) | 170 (5) |
O6—H6A···O8viii | 0.84 (1) | 1.84 (2) | 2.672 (3) | 177 (4) |
O6—H6B···O14viii | 0.84 (1) | 1.82 (2) | 2.656 (3) | 178 (5) |
O13—H13A···Cl2vii | 0.84 (1) | 2.93 (5) | 3.329 (3) | 111 (4) |
O13—H13A···Cl3vi | 0.84 (1) | 2.71 (5) | 3.284 (3) | 127 (5) |
O9—H9A···Cl1v | 0.84 (1) | 2.26 (2) | 3.090 (2) | 172 (5) |
O9—H9B···Cl2 | 0.84 (1) | 2.28 (2) | 3.108 (2) | 171 (6) |
O10—H10A···Cl2 | 0.83 (2) | 2.86 (5) | 3.416 (2) | 126 (5) |
O10—H10A···O13iv | 0.83 (2) | 2.14 (3) | 2.897 (3) | 151 (6) |
O11—H11A···Cl3iii | 0.84 (2) | 2.79 (3) | 3.535 (3) | 149 (5) |
O12—H12A···O15ii | 0.84 (1) | 2.13 (4) | 2.826 (3) | 141 (5) |
O12—H12B···Cl3i | 0.84 (1) | 2.36 (2) | 3.200 (2) | 177 (5) |
O1—H1B···Cl3 | 0.84 (1) | 2.15 (2) | 2.986 (2) | 171 (4) |
O15—H15A···O7 | 0.83 (1) | 2.02 (2) | 2.850 (3) | 174 (4) |
O7—H7A···Cl3 | 0.84 (1) | 2.47 (3) | 3.236 (2) | 153 (4) |
O2—H2A···O9xi | 0.84 (2) | 1.83 (2) | 2.663 (3) | 175 (6) |
O2—H2B···O10 | 0.84 (1) | 1.82 (2) | 2.646 (3) | 171 (5) |
O8—H8B···Cl1v | 0.84 (1) | 2.30 (2) | 3.102 (2) | 159 (5) |
O8—H8A···Cl2 | 0.84 (1) | 2.32 (2) | 3.147 (2) | 171 (5) |
O4—H4A···O8 | 0.83 (1) | 1.85 (2) | 2.676 (3) | 173 (5) |
O4—H4B···O12 | 0.84 (1) | 1.78 (2) | 2.605 (3) | 166 (6) |
O5—H5B···O15 | 0.84 (2) | 1.81 (2) | 2.646 (3) | 176 (6) |
O5—H5A···O13 | 0.84 (1) | 1.80 (2) | 2.635 (3) | 175 (4) |
O1—H1A···O9x | 0.84 (1) | 1.84 (2) | 2.671 (3) | 174 (5) |
O3—H3A···O11viii | 0.84 (1) | 1.84 (2) | 2.673 (3) | 174 (6) |
O3—H3B···O7ii | 0.83 (1) | 1.85 (2) | 2.686 (3) | 178 (5) |
O11—H11B···O10 | 0.84 (1) | 2.01 (2) | 2.822 (4) | 163 (4) |
O7—H7B···Cl2x | 0.84 (1) | 2.33 (2) | 3.164 (2) | 177 (4) |
O10—H10B···Cl1iv | 0.84 (1) | 2.37 (2) | 3.172 (2) | 159 (5) |
O15—H15B···Cl1viii | 0.84 (1) | 2.33 (2) | 3.165 (2) | 178 (4) |
O13—H13B···O14 | 0.84 (2) | 1.94 (2) | 2.785 (4) | 177 (5) |
O14—H14B···Cl1 | 0.84 (2) | 2.83 (4) | 3.345 (2) | 122 (4) |
O14—H14B···O11ix | 0.84 (2) | 2.12 (3) | 2.892 (3) | 153 (4) |
O14—H14A···Cl2ix | 0.84 (1) | 2.34 (2) | 3.169 (2) | 170 (5) |
O6—H6A···O8viii | 0.84 (1) | 1.84 (2) | 2.672 (3) | 177 (4) |
O6—H6B···O14viii | 0.84 (1) | 1.82 (2) | 2.656 (3) | 178 (5) |
O13—H13A···Cl2vii | 0.84 (1) | 2.93 (5) | 3.329 (3) | 111 (4) |
O13—H13A···Cl3vi | 0.84 (1) | 2.71 (5) | 3.284 (3) | 127 (5) |
O9—H9A···Cl1v | 0.84 (1) | 2.26 (2) | 3.090 (2) | 172 (5) |
O9—H9B···Cl2 | 0.84 (1) | 2.28 (2) | 3.108 (2) | 171 (6) |
O10—H10A···Cl2 | 0.83 (2) | 2.86 (5) | 3.416 (2) | 126 (5) |
O10—H10A···O13iv | 0.83 (2) | 2.14 (3) | 2.897 (3) | 151 (6) |
O11—H11A···Cl3iii | 0.84 (2) | 2.79 (3) | 3.535 (3) | 149 (5) |
O12—H12A···O15ii | 0.84 (1) | 2.13 (4) | 2.826 (3) | 141 (5) |
O12—H12B···Cl3i | 0.84 (1) | 2.36 (2) | 3.200 (2) | 177 (5) |
O1—H1B···Cl3 | 0.84 (1) | 2.15 (2) | 2.986 (2) | 171 (4) |
O15—H15A···O7 | 0.83 (1) | 2.02 (2) | 2.850 (3) | 174 (4) |
O7—H7A···Cl3 | 0.84 (1) | 2.47 (3) | 3.236 (2) | 153 (4) |
O2—H2A···O9xi | 0.84 (2) | 1.83 (2) | 2.663 (3) | 175 (6) |
O2—H2B···O10 | 0.84 (1) | 1.82 (2) | 2.646 (3) | 171 (5) |
O8—H8B···Cl1v | 0.84 (1) | 2.30 (2) | 3.102 (2) | 159 (5) |
O8—H8A···Cl2 | 0.84 (1) | 2.32 (2) | 3.147 (2) | 171 (5) |
O4—H4A···O8 | 0.83 (1) | 1.85 (2) | 2.676 (3) | 173 (5) |
O4—H4B···O12 | 0.84 (1) | 1.78 (2) | 2.605 (3) | 166 (6) |
O5—H5B···O15 | 0.84 (2) | 1.81 (2) | 2.646 (3) | 176 (6) |
O5—H5A···O13 | 0.84 (1) | 1.80 (2) | 2.635 (3) | 175 (4) |
O1—H1A···O9x | 0.84 (1) | 1.84 (2) | 2.671 (3) | 174 (5) |
O3—H3A···O11viii | 0.84 (1) | 1.84 (2) | 2.673 (3) | 174 (6) |
O3—H3B···O7ii | 0.83 (1) | 1.85 (2) | 2.686 (3) | 178 (5) |
O11—H11B···O10 | 0.84 (1) | 2.01 (2) | 2.822 (4) | 163 (4) |
O7—H7B···Cl2x | 0.84 (1) | 2.33 (2) | 3.164 (2) | 177 (4) |
O10—H10B···Cl1iv | 0.84 (1) | 2.37 (2) | 3.172 (2) | 159 (5) |
O15—H15B···Cl1viii | 0.84 (1) | 2.33 (2) | 3.165 (2) | 178 (4) |
O13—H13B···O14 | 0.84 (2) | 1.94 (2) | 2.785 (4) | 177 (5) |
O14—H14B···Cl1 | 0.84 (2) | 2.83 (4) | 3.345 (2) | 122 (4) |
O14—H14B···O11ix | 0.84 (2) | 2.12 (3) | 2.892 (3) | 153 (4) |
O14—H14A···Cl2ix | 0.84 (1) | 2.34 (2) | 3.169 (2) | 170 (5) |
O6—H6A···O8viii | 0.84 (1) | 1.84 (2) | 2.672 (3) | 177 (4) |
O6—H6B···O14viii | 0.84 (1) | 1.82 (2) | 2.656 (3) | 178 (5) |
O13—H13A···Cl2vii | 0.84 (1) | 2.93 (5) | 3.329 (3) | 111 (4) |
O13—H13A···Cl3vi | 0.84 (1) | 2.71 (5) | 3.284 (3) | 127 (5) |
O9—H9A···Cl1v | 0.84 (1) | 2.26 (2) | 3.090 (2) | 172 (5) |
O9—H9B···Cl2 | 0.84 (1) | 2.28 (2) | 3.108 (2) | 171 (6) |
O10—H10A···Cl2 | 0.83 (2) | 2.86 (5) | 3.416 (2) | 126 (5) |
O10—H10A···O13iv | 0.83 (2) | 2.14 (3) | 2.897 (3) | 151 (6) |
O11—H11A···Cl3iii | 0.84 (2) | 2.79 (3) | 3.535 (3) | 149 (5) |
O12—H12A···O15ii | 0.84 (1) | 2.13 (4) | 2.826 (3) | 141 (5) |
O12—H12B···Cl3i | 0.84 (1) | 2.36 (2) | 3.200 (2) | 177 (5) |
O1—H1B···Cl3 | 0.84 (1) | 2.15 (2) | 2.986 (2) | 171 (4) |
O15—H15A···O7 | 0.83 (1) | 2.02 (2) | 2.850 (3) | 174 (4) |
O7—H7A···Cl3 | 0.84 (1) | 2.47 (3) | 3.236 (2) | 153 (4) |
Symmetry codes: (i) x−1/2, y−1/2, z; (ii) x−1/2, −y+1/2, z−1/2; (iii) x, y+1, z; (iv) x, −y+1, z−1/2; (v) x−1/2, −y+3/2, z−1/2; (vi) x−1/2, y+1/2, z; (vii) x, −y+1, z+1/2; (viii) x, y−1, z; (ix) x, −y+2, z+1/2; (x) x+1/2, −y+1/2, z+1/2; (xi) x+1/2, −y+3/2, z+1/2. |
[Al(H2O)]Br3·9H2O | F(000) = 1072 |
Mr = 536.95 | Dx = 1.860 Mg m−3 |
Monoclinic, Cc | Mo Kα radiation, λ = 0.71073 Å |
a = 19.0122 (13) Å | Cell parameters from 6652 reflections |
b = 6.6568 (6) Å | θ = 2.1–29.6° |
c = 18.2360 (13) Å | µ = 6.41 mm−1 |
β = 123.834 (5)° | T = 120 K |
V = 1917.1 (3) Å3 | 0.33 × 0.22 × 0.10 mm |
Z = 4 |
Stoe IPDS 2 diffractometer | 3992 independent reflections |
Radiation source: sealed X-ray tube | 3320 reflections with I > 2σ(I) |
Detector resolution: 6.67 pixels mm-1 | Rint = 0.082 |
rotation method scans | θmax = 26.5°, θmin = 2.2° |
Absorption correction: integration (Coppens, 1970) | h = −23→23 |
Tmin = 0.208, Tmax = 0.525 | k = −8→8 |
10481 measured reflections | l = −22→22 |
Refinement on F2 | Only H-atom coordinates refined |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.1668P)2 + 5.8293P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.065 | (Δ/σ)max < 0.001 |
wR(F2) = 0.197 | Δρmax = 1.81 e Å−3 |
S = 1.06 | Δρmin = −1.23 e Å−3 |
3602 reflections | Extinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
263 parameters | Extinction coefficient: 0.0035 (8) |
47 restraints | Absolute structure: Classical Flack (1983) method preferred over Parsons (2003) because s.u. is lower |
Hydrogen site location: difference Fourier map | Absolute structure parameter: 0.13 (3) |
[Al(H2O)]Br3·9H2O | V = 1917.1 (3) Å3 |
Mr = 536.95 | Z = 4 |
Monoclinic, Cc | Mo Kα radiation |
a = 19.0122 (13) Å | µ = 6.41 mm−1 |
b = 6.6568 (6) Å | T = 120 K |
c = 18.2360 (13) Å | 0.33 × 0.22 × 0.10 mm |
β = 123.834 (5)° |
Stoe IPDS 2 diffractometer | 3992 independent reflections |
Absorption correction: integration (Coppens, 1970) | 3320 reflections with I > 2σ(I) |
Tmin = 0.208, Tmax = 0.525 | Rint = 0.082 |
10481 measured reflections |
R[F2 > 2σ(F2)] = 0.065 | Only H-atom coordinates refined |
wR(F2) = 0.197 | Δρmax = 1.81 e Å−3 |
S = 1.06 | Δρmin = −1.23 e Å−3 |
3602 reflections | Absolute structure: Classical Flack (1983) method preferred over Parsons (2003) because s.u. is lower |
263 parameters | Absolute structure parameter: 0.13 (3) |
47 restraints |
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. |
x | y | z | Uiso*/Ueq | ||
Br1 | 0.48766 (8) | 0.26066 (18) | 0.23017 (8) | 0.0172 (4) | |
Br2 | 0.79285 (10) | 0.24916 (16) | 0.78526 (10) | 0.0185 (4) | |
Al1 | 0.6431 (3) | 0.7599 (5) | 0.5052 (3) | 0.0121 (8) | |
Br3 | 0.39218 (12) | 0.7164 (2) | 0.47648 (12) | 0.0230 (4) | |
O5 | 0.6023 (5) | 0.6533 (13) | 0.3926 (6) | 0.0141 (17) | |
H5A | 0.558 (6) | 0.68 (2) | 0.344 (5) | 0.017* | |
H5B | 0.629 (9) | 0.564 (17) | 0.385 (10) | 0.017* | |
O3 | 0.6807 (6) | 0.8711 (12) | 0.6161 (6) | 0.0121 (16) | |
H3A | 0.718 (8) | 0.80 (2) | 0.660 (7) | 0.015* | |
H3B | 0.641 (7) | 0.92 (2) | 0.617 (10) | 0.015* | |
O1 | 0.5350 (6) | 0.8810 (12) | 0.4565 (6) | 0.0127 (16) | |
H1A | 0.524 (10) | 1.003 (7) | 0.445 (11) | 0.015* | |
H1B | 0.510 (9) | 0.797 (18) | 0.469 (11) | 0.015* | |
O2 | 0.6064 (6) | 0.5278 (13) | 0.5331 (6) | 0.0139 (18) | |
H2A | 0.571 (8) | 0.47 (2) | 0.487 (6) | 0.017* | |
H2B | 0.610 (10) | 0.50 (2) | 0.580 (5) | 0.017* | |
O4 | 0.7484 (6) | 0.6422 (13) | 0.5511 (6) | 0.0162 (18) | |
H4A | 0.788 (7) | 0.68 (2) | 0.546 (11) | 0.019* | |
H4B | 0.740 (11) | 0.518 (5) | 0.549 (11) | 0.019* | |
O6 | 0.6762 (6) | 0.9946 (13) | 0.4745 (6) | 0.0129 (17) | |
H6A | 0.679 (9) | 0.98 (3) | 0.430 (6) | 0.015* | |
H6B | 0.723 (5) | 1.02 (2) | 0.521 (5) | 0.015* | |
O9 | 0.9989 (7) | 0.2333 (14) | 0.9124 (7) | 0.018 (2) | |
H9A | 1.003 (12) | 0.25 (2) | 0.869 (8) | 0.022* | |
H9B | 0.955 (6) | 0.16 (2) | 0.891 (9) | 0.022* | |
O8 | 0.7835 (8) | 0.2568 (12) | 0.6009 (9) | 0.017 (2) | |
H8A | 0.834 (4) | 0.24 (2) | 0.617 (12) | 0.020* | |
H8B | 0.774 (12) | 0.25 (2) | 0.641 (9) | 0.020* | |
O7 | 0.3185 (8) | 0.7703 (14) | 0.2625 (8) | 0.019 (2) | |
H7A | 0.362 (8) | 0.73 (2) | 0.311 (7) | 0.023* | |
H7B | 0.311 (10) | 0.893 (6) | 0.250 (10) | 0.023* | |
O14 | 0.6798 (7) | 0.0319 (17) | 0.3330 (7) | 0.022 (2) | |
H14A | 0.713 (8) | −0.04 (2) | 0.328 (11) | 0.026* | |
H14B | 0.631 (4) | 0.02 (3) | 0.287 (6) | 0.026* | |
O13 | 0.6963 (7) | 0.4505 (17) | 0.3543 (8) | 0.023 (2) | |
H13A | 0.747 (4) | 0.49 (2) | 0.391 (9) | 0.028* | |
H13B | 0.695 (11) | 0.325 (3) | 0.352 (12) | 0.028* | |
O10 | 0.5897 (6) | 0.4690 (16) | 0.6666 (7) | 0.019 (2) | |
H10A | 0.633 (5) | 0.47 (3) | 0.718 (4) | 0.022* | |
H10B | 0.556 (8) | 0.54 (2) | 0.670 (10) | 0.022* | |
O11 | 0.5698 (7) | 0.0478 (16) | 0.6441 (7) | 0.022 (2) | |
H11A | 0.574 (11) | 0.172 (6) | 0.638 (11) | 0.026* | |
H11B | 0.524 (6) | −0.01 (2) | 0.605 (8) | 0.026* | |
O12 | 0.8827 (8) | 0.7984 (18) | 0.5695 (9) | 0.028 (2) | |
H12A | 0.912 (10) | 0.85 (3) | 0.621 (5) | 0.033* | |
H12B | 0.896 (12) | 0.80 (3) | 0.533 (9) | 0.033* | |
O15 | 0.4616 (8) | 0.7835 (16) | 0.2518 (7) | 0.020 (2) | |
H15B | 0.477 (10) | 0.898 (10) | 0.247 (11) | 0.025* | |
H15A | 0.421 (8) | 0.79 (2) | 0.258 (12) | 0.025* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Br1 | 0.0149 (8) | 0.0166 (7) | 0.0215 (7) | −0.0004 (5) | 0.0109 (6) | −0.0004 (5) |
Br2 | 0.0162 (8) | 0.0161 (7) | 0.0246 (8) | −0.0006 (4) | 0.0122 (7) | −0.0002 (4) |
Al1 | 0.011 (2) | 0.0078 (14) | 0.0190 (19) | −0.0014 (12) | 0.0093 (17) | −0.0022 (12) |
Br3 | 0.0155 (7) | 0.0289 (7) | 0.0231 (7) | −0.0019 (7) | 0.0099 (6) | 0.0077 (8) |
O5 | 0.004 (4) | 0.014 (4) | 0.012 (4) | 0.002 (3) | −0.003 (4) | −0.006 (3) |
O3 | 0.010 (4) | 0.012 (4) | 0.016 (4) | 0.000 (3) | 0.008 (4) | −0.003 (3) |
O1 | 0.008 (4) | 0.009 (4) | 0.017 (4) | 0.000 (3) | 0.004 (3) | 0.001 (3) |
O2 | 0.021 (5) | 0.011 (4) | 0.013 (4) | −0.004 (3) | 0.012 (4) | −0.002 (3) |
O4 | 0.016 (5) | 0.007 (4) | 0.031 (5) | 0.000 (3) | 0.016 (4) | 0.001 (3) |
O6 | 0.012 (4) | 0.013 (4) | 0.010 (4) | −0.004 (3) | 0.004 (4) | −0.004 (3) |
O9 | 0.021 (7) | 0.017 (5) | 0.023 (6) | −0.003 (3) | 0.016 (6) | 0.000 (3) |
O8 | 0.012 (5) | 0.011 (5) | 0.028 (6) | 0.001 (3) | 0.012 (5) | 0.000 (3) |
O7 | 0.018 (6) | 0.010 (4) | 0.027 (6) | −0.003 (4) | 0.011 (5) | −0.003 (4) |
O14 | 0.016 (6) | 0.023 (5) | 0.025 (6) | −0.004 (4) | 0.010 (5) | 0.004 (4) |
O13 | 0.021 (5) | 0.017 (5) | 0.036 (6) | 0.002 (4) | 0.018 (5) | −0.007 (4) |
O10 | 0.013 (5) | 0.021 (5) | 0.022 (5) | 0.003 (4) | 0.010 (4) | 0.000 (4) |
O11 | 0.013 (5) | 0.018 (5) | 0.031 (6) | −0.004 (4) | 0.011 (5) | −0.003 (4) |
O12 | 0.023 (6) | 0.026 (5) | 0.036 (6) | −0.005 (5) | 0.017 (6) | 0.000 (5) |
O15 | 0.020 (6) | 0.015 (4) | 0.021 (5) | −0.004 (4) | 0.008 (5) | −0.006 (4) |
Al1—O4 | 1.859 (11) | Al1—O6 | 1.882 (10) |
Al1—O2 | 1.878 (10) | Al1—O5 | 1.883 (10) |
Al1—O3 | 1.881 (10) | Al1—O1 | 1.906 (10) |
O4—Al1—O2 | 90.0 (4) | O3—Al1—O5 | 178.2 (5) |
O4—Al1—O3 | 90.7 (5) | O6—Al1—O5 | 89.5 (5) |
O2—Al1—O3 | 90.5 (4) | O4—Al1—O1 | 179.2 (5) |
O4—Al1—O6 | 91.7 (5) | O2—Al1—O1 | 90.4 (5) |
O2—Al1—O6 | 178.2 (6) | O3—Al1—O1 | 90.0 (4) |
O3—Al1—O6 | 90.2 (4) | O6—Al1—O1 | 87.9 (4) |
O4—Al1—O5 | 91.1 (4) | O5—Al1—O1 | 88.2 (5) |
O2—Al1—O5 | 89.8 (4) |
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5A···O15 | 0.84 (1) | 1.79 (4) | 2.618 (15) | 169 (15) |
O5—H5B···O13 | 0.84 (1) | 1.83 (6) | 2.625 (14) | 159 (16) |
O3—H3A···O7i | 0.84 (1) | 1.85 (6) | 2.662 (15) | 162 (18) |
O3—H3B···O11ii | 0.84 (1) | 1.87 (4) | 2.701 (14) | 168 (15) |
O1—H1A···O9iii | 0.84 (2) | 1.83 (2) | 2.664 (12) | 177 (15) |
O1—H1B···Br3 | 0.84 (1) | 2.38 (9) | 3.130 (9) | 148 (14) |
O2—H2A···O9iv | 0.84 (1) | 1.84 (5) | 2.653 (14) | 162 (15) |
O2—H2B···O10 | 0.84 (1) | 1.83 (5) | 2.654 (13) | 164 (16) |
O4—H4A···O12 | 0.84 (1) | 1.79 (6) | 2.599 (15) | 161 (17) |
O4—H4B···O8 | 0.84 (1) | 1.93 (10) | 2.679 (12) | 148 (17) |
O6—H6A···O14ii | 0.84 (1) | 1.81 (5) | 2.631 (13) | 164 (17) |
O6—H6B···O8ii | 0.84 (2) | 1.99 (11) | 2.700 (14) | 141 (15) |
O9—H9A···Br1v | 0.84 (1) | 2.39 (4) | 3.210 (11) | 166 (15) |
O9—H9B···Br2 | 0.84 (2) | 2.63 (13) | 3.258 (12) | 133 (15) |
O8—H8A···Br1v | 0.84 (1) | 2.47 (9) | 3.232 (12) | 151 (16) |
O8—H8B···Br2 | 0.84 (1) | 2.46 (6) | 3.267 (13) | 162 (17) |
O7—H7A···Br3 | 0.84 (1) | 2.75 (17) | 3.352 (13) | 130 (19) |
O7—H7B···Br2iii | 0.84 (1) | 2.53 (8) | 3.296 (10) | 152 (14) |
O14—H14A···Br2vi | 0.84 (1) | 2.48 (3) | 3.312 (11) | 170 (15) |
O14—H14B···Br1 | 0.84 (1) | 2.82 (13) | 3.398 (11) | 127 (13) |
O14—H14B···O11vi | 0.84 (1) | 2.22 (11) | 2.916 (16) | 140 (14) |
O13—H13A···Br3vii | 0.84 (2) | 2.91 (14) | 3.468 (12) | 125 (13) |
O13—H13B···O14 | 0.84 (1) | 1.97 (3) | 2.807 (17) | 174 (18) |
O10—H10A···Br2 | 0.84 (2) | 2.95 (13) | 3.526 (11) | 128 (13) |
O10—H10A···O13viii | 0.84 (2) | 2.14 (8) | 2.895 (14) | 150 (14) |
O10—H10B···Br1viii | 0.84 (1) | 2.48 (5) | 3.294 (10) | 162 (14) |
O11—H11A···O10 | 0.84 (2) | 2.03 (7) | 2.828 (17) | 159 (17) |
O11—H11B···Br3ix | 0.84 (1) | 2.94 (5) | 3.757 (11) | 166 (15) |
O12—H12A···Br1i | 0.84 (2) | 3.11 (12) | 3.830 (13) | 145 (17) |
O12—H12A···O15i | 0.84 (2) | 2.21 (15) | 2.837 (17) | 132 (17) |
O12—H12B···Br3x | 0.84 (1) | 2.91 (19) | 3.316 (12) | 112 (16) |
O15—H15B···Br1ii | 0.84 (1) | 2.45 (4) | 3.272 (11) | 165 (14) |
O15—H15A···O7 | 0.84 (1) | 2.01 (4) | 2.835 (16) | 169 (16) |
Symmetry codes: (i) x+1/2, −y+3/2, z+1/2; (ii) x, y+1, z; (iii) x−1/2, −y+3/2, z−1/2; (iv) x−1/2, −y+1/2, z−1/2; (v) x+1/2, −y+1/2, z+1/2; (vi) x, −y, z−1/2; (vii) x+1/2, y−1/2, z; (viii) x, −y+1, z+1/2; (ix) x, y−1, z; (x) x+1/2, y+1/2, z. |
[Al(H2O)6]I3·9H2O | F(000) = 2576 |
Mr = 677.92 | Dx = 2.098 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
a = 37.010 (3) Å | Cell parameters from 17084 reflections |
b = 6.9011 (3) Å | θ = 2.2–32.3° |
c = 18.1054 (16) Å | µ = 4.46 mm−1 |
β = 111.829 (7)° | T = 100 K |
V = 4292.7 (6) Å3 | Needle, colourless |
Z = 8 | 0.64 × 0.41 × 0.14 mm |
Stoe IPDS 2T diffractometer | 4912 independent reflections |
Radiation source: sealed X-ray tube | 4740 reflections with I > 2σ(I) |
Detector resolution: 6.67 pixels mm-1 | Rint = 0.054 |
rotation method scans | θmax = 27.5°, θmin = 3.0° |
Absorption correction: integration (Coppens, 1970) | h = −48→48 |
Tmin = 0.127, Tmax = 0.546 | k = −8→8 |
19548 measured reflections | l = −23→23 |
Refinement on F2 | Hydrogen site location: difference Fourier map |
Least-squares matrix: full | Only H-atom coordinates refined |
R[F2 > 2σ(F2)] = 0.021 | w = 1/[σ2(Fo2) + (0.011P)2 + 5.6496P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.050 | (Δ/σ)max = 0.003 |
S = 1.29 | Δρmax = 0.57 e Å−3 |
4912 reflections | Δρmin = −0.78 e Å−3 |
282 parameters | Extinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
73 restraints | Extinction coefficient: 0.000186 (13) |
[Al(H2O)6]I3·9H2O | V = 4292.7 (6) Å3 |
Mr = 677.92 | Z = 8 |
Monoclinic, C2/c | Mo Kα radiation |
a = 37.010 (3) Å | µ = 4.46 mm−1 |
b = 6.9011 (3) Å | T = 100 K |
c = 18.1054 (16) Å | 0.64 × 0.41 × 0.14 mm |
β = 111.829 (7)° |
Stoe IPDS 2T diffractometer | 4912 independent reflections |
Absorption correction: integration (Coppens, 1970) | 4740 reflections with I > 2σ(I) |
Tmin = 0.127, Tmax = 0.546 | Rint = 0.054 |
19548 measured reflections |
R[F2 > 2σ(F2)] = 0.021 | 73 restraints |
wR(F2) = 0.050 | Only H-atom coordinates refined |
S = 1.29 | Δρmax = 0.57 e Å−3 |
4912 reflections | Δρmin = −0.78 e Å−3 |
282 parameters |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
I1 | 0.87175 (2) | 0.26652 (2) | 0.92474 (2) | 0.01305 (5) | |
I2 | 0.83138 (2) | 0.25004 (2) | 0.25407 (2) | 0.01323 (5) | |
I3 | 0.92893 (6) | 0.9552 (3) | 0.66841 (12) | 0.01703 (18) | 0.631 (4) |
I3A | 0.92810 (11) | 0.9908 (3) | 0.6677 (2) | 0.01703 (18) | 0.369 (4) |
Al1 | 0.0000 | 0.5000 | 0.0000 | 0.0174 (2) | |
Al2 | 0.7500 | 0.2500 | 0.5000 | 0.00893 (18) | |
O2 | 0.76568 (5) | 0.4862 (2) | 0.46782 (10) | 0.0122 (3) | |
H2B | 0.7671 (9) | 0.506 (4) | 0.4234 (10) | 0.015* | |
H2A | 0.7821 (7) | 0.565 (3) | 0.4977 (15) | 0.015* | |
O3 | 0.70199 (5) | 0.3634 (2) | 0.48752 (10) | 0.0127 (3) | |
H3A | 0.6970 (9) | 0.4792 (19) | 0.4734 (17) | 0.015* | |
H3B | 0.6815 (5) | 0.298 (4) | 0.4732 (18) | 0.015* | |
O1 | 0.72985 (5) | 0.1636 (2) | 0.39344 (9) | 0.0129 (3) | |
H1B | 0.7070 (4) | 0.183 (4) | 0.3626 (15) | 0.015* | |
H1A | 0.7427 (7) | 0.093 (4) | 0.3744 (16) | 0.015* | |
O5 | −0.03578 (5) | 0.4144 (3) | 0.04548 (12) | 0.0192 (4) | |
H5B | −0.0572 (5) | 0.363 (4) | 0.0188 (16) | 0.023* | |
H5A | −0.0352 (10) | 0.443 (5) | 0.0907 (10) | 0.023* | |
O6 | 0.02843 (5) | 0.6310 (2) | 0.09473 (12) | 0.0207 (4) | |
H6A | 0.0232 (10) | 0.745 (2) | 0.103 (2) | 0.025* | |
H6B | 0.0467 (7) | 0.587 (5) | 0.1338 (13) | 0.025* | |
O4 | 0.02941 (5) | 0.2739 (3) | 0.03759 (14) | 0.0233 (4) | |
H4A | 0.0231 (10) | 0.196 (4) | 0.0666 (17) | 0.028* | |
H4B | 0.0521 (5) | 0.259 (5) | 0.040 (2) | 0.028* | |
O7 | 0.68230 (5) | 0.7407 (2) | 0.44843 (11) | 0.0153 (4) | |
H7A | 0.6643 (7) | 0.759 (4) | 0.4650 (19) | 0.018* | |
H7B | 0.6753 (9) | 0.754 (4) | 0.3993 (7) | 0.018* | |
O10 | 0.22646 (5) | 0.5559 (3) | 0.16914 (10) | 0.0163 (3) | |
H10B | 0.2417 (7) | 0.514 (4) | 0.2132 (10) | 0.020* | |
H10A | 0.2046 (5) | 0.525 (4) | 0.1690 (19) | 0.020* | |
O9 | 0.77109 (5) | 0.9598 (2) | 0.32594 (11) | 0.0163 (3) | |
H9A | 0.7724 (9) | 0.8383 (15) | 0.3306 (18) | 0.020* | |
H9B | 0.7935 (4) | 0.994 (4) | 0.332 (2) | 0.020* | |
O13 | 0.01541 (5) | 0.0022 (3) | 0.13019 (11) | 0.0189 (3) | |
H13B | −0.0070 (5) | 0.026 (5) | 0.130 (2) | 0.023* | |
H13A | 0.0302 (8) | 0.020 (5) | 0.1775 (8) | 0.023* | |
O12 | 0.89976 (6) | 0.2213 (3) | 0.45738 (15) | 0.0264 (5) | |
H12A | 0.8938 (10) | 0.1048 (19) | 0.456 (2) | 0.032* | |
H12B | 0.8881 (10) | 0.270 (5) | 0.4132 (11) | 0.032* | |
O11 | 0.63937 (5) | 0.1552 (3) | 0.43734 (13) | 0.0250 (4) | |
H11A | 0.6244 (8) | 0.160 (5) | 0.4622 (18) | 0.030* | |
H11B | 0.6291 (10) | 0.203 (5) | 0.3922 (10) | 0.030* | |
O15 | 0.65866 (6) | 0.2571 (2) | 0.29104 (12) | 0.0193 (4) | |
H15A | 0.6516 (10) | 0.211 (4) | 0.2455 (10) | 0.023* | |
H15B | 0.6555 (10) | 0.3753 (18) | 0.2802 (19) | 0.023* | |
O8 | 0.96504 (5) | 0.5549 (3) | 0.18196 (12) | 0.0236 (4) | 0.631 (4) |
H8A | 0.9587 (5) | 0.6689 (15) | 0.1783 (17) | 0.028* | 0.631 (4) |
H8B | 0.9483 (6) | 0.503 (3) | 0.1945 (17) | 0.028* | 0.631 (4) |
O14 | 0.91548 (10) | 0.5147 (5) | 0.2667 (2) | 0.0230 (7) | 0.631 (4) |
H14A | 0.9049 (7) | 0.416 (2) | 0.273 (2) | 0.028* | 0.631 (4) |
H14B | 0.8972 (5) | 0.590 (3) | 0.249 (3) | 0.028* | 0.631 (4) |
O8A | 0.96504 (5) | 0.5549 (3) | 0.18196 (12) | 0.0236 (4) | 0.369 (4) |
H8C | 0.9857 (7) | 0.555 (4) | 0.2200 (18) | 0.028* | 0.369 (4) |
H8D | 0.9587 (5) | 0.6689 (15) | 0.1783 (17) | 0.028* | 0.369 (4) |
O14A | 0.92630 (18) | 0.4377 (9) | 0.2926 (4) | 0.0230 (7) | 0.369 (4) |
H14C | 0.9363 (10) | 0.334 (3) | 0.289 (2) | 0.028* | 0.369 (4) |
H14D | 0.9232 (17) | 0.489 (4) | 0.2501 (12) | 0.028* | 0.369 (4) |
U11 | U22 | U33 | U12 | U13 | U23 | |
I1 | 0.01017 (8) | 0.01519 (8) | 0.01155 (9) | 0.00013 (5) | 0.00147 (6) | 0.00040 (5) |
I2 | 0.01240 (8) | 0.01291 (8) | 0.01465 (10) | −0.00064 (5) | 0.00536 (7) | −0.00047 (5) |
I3 | 0.01726 (12) | 0.0147 (5) | 0.01897 (10) | −0.0036 (4) | 0.00651 (8) | −0.0044 (4) |
I3A | 0.01726 (12) | 0.0147 (5) | 0.01897 (10) | −0.0036 (4) | 0.00651 (8) | −0.0044 (4) |
Al1 | 0.0062 (4) | 0.0111 (4) | 0.0327 (6) | 0.0018 (3) | 0.0045 (4) | 0.0056 (4) |
Al2 | 0.0082 (4) | 0.0104 (4) | 0.0080 (5) | −0.0004 (3) | 0.0028 (4) | −0.0007 (3) |
O2 | 0.0134 (7) | 0.0127 (7) | 0.0110 (8) | −0.0040 (6) | 0.0051 (6) | −0.0006 (6) |
O3 | 0.0090 (7) | 0.0115 (7) | 0.0169 (8) | 0.0000 (6) | 0.0042 (6) | −0.0004 (6) |
O1 | 0.0094 (7) | 0.0169 (8) | 0.0114 (8) | 0.0025 (6) | 0.0029 (6) | −0.0021 (6) |
O5 | 0.0073 (7) | 0.0176 (8) | 0.0299 (10) | −0.0026 (6) | 0.0037 (7) | 0.0030 (7) |
O6 | 0.0099 (7) | 0.0138 (8) | 0.0350 (11) | 0.0021 (6) | 0.0043 (7) | 0.0067 (7) |
O4 | 0.0096 (8) | 0.0162 (8) | 0.0433 (13) | 0.0037 (7) | 0.0089 (8) | 0.0122 (8) |
O7 | 0.0134 (8) | 0.0174 (8) | 0.0141 (9) | 0.0015 (6) | 0.0039 (7) | −0.0006 (6) |
O10 | 0.0126 (7) | 0.0229 (8) | 0.0145 (9) | −0.0018 (7) | 0.0061 (7) | 0.0002 (7) |
O9 | 0.0133 (8) | 0.0162 (8) | 0.0209 (9) | −0.0026 (6) | 0.0081 (7) | −0.0034 (7) |
O13 | 0.0173 (8) | 0.0242 (8) | 0.0152 (9) | 0.0053 (7) | 0.0059 (7) | 0.0031 (7) |
O12 | 0.0123 (8) | 0.0176 (8) | 0.0434 (14) | −0.0027 (7) | 0.0036 (9) | 0.0058 (8) |
O11 | 0.0146 (8) | 0.0227 (9) | 0.0332 (11) | −0.0016 (7) | 0.0035 (8) | 0.0048 (8) |
O15 | 0.0219 (10) | 0.0160 (8) | 0.0173 (10) | 0.0020 (7) | 0.0042 (8) | 0.0006 (6) |
O8 | 0.0160 (8) | 0.0235 (9) | 0.0278 (11) | −0.0022 (7) | 0.0041 (7) | 0.0048 (8) |
O14 | 0.0151 (16) | 0.0258 (19) | 0.031 (2) | −0.0074 (12) | 0.0112 (14) | −0.0085 (13) |
O8A | 0.0160 (8) | 0.0235 (9) | 0.0278 (11) | −0.0022 (7) | 0.0041 (7) | 0.0048 (8) |
O14A | 0.0151 (16) | 0.0258 (19) | 0.031 (2) | −0.0074 (12) | 0.0112 (14) | −0.0085 (13) |
Al1—O6i | 1.877 (2) | Al2—O3ii | 1.8765 (16) |
Al1—O6 | 1.877 (2) | Al2—O3 | 1.8766 (16) |
Al1—O4i | 1.8792 (17) | Al2—O1ii | 1.8879 (16) |
Al1—O4 | 1.8792 (17) | Al2—O1 | 1.8879 (16) |
Al1—O5i | 1.8948 (18) | Al2—O2 | 1.8936 (15) |
Al1—O5 | 1.8950 (18) | Al2—O2ii | 1.8936 (15) |
O6i—Al1—O6 | 180.0 | O3ii—Al2—O3 | 180.00 (10) |
O6i—Al1—O4i | 90.95 (9) | O3ii—Al2—O1ii | 90.69 (7) |
O6—Al1—O4i | 89.05 (9) | O3—Al2—O1ii | 89.31 (7) |
O6i—Al1—O4 | 89.05 (9) | O3ii—Al2—O1 | 89.31 (7) |
O6—Al1—O4 | 90.95 (9) | O3—Al2—O1 | 90.69 (7) |
O4i—Al1—O4 | 180.00 (11) | O1ii—Al2—O1 | 180.0 |
O6i—Al1—O5i | 89.89 (8) | O3ii—Al2—O2 | 90.64 (7) |
O6—Al1—O5i | 90.11 (8) | O3—Al2—O2 | 89.36 (7) |
O4i—Al1—O5i | 89.32 (8) | O1ii—Al2—O2 | 89.57 (7) |
O4—Al1—O5i | 90.68 (8) | O1—Al2—O2 | 90.42 (7) |
O6i—Al1—O5 | 90.11 (8) | O3ii—Al2—O2ii | 89.36 (7) |
O6—Al1—O5 | 89.89 (8) | O3—Al2—O2ii | 90.64 (7) |
O4i—Al1—O5 | 90.68 (8) | O1ii—Al2—O2ii | 90.42 (7) |
O4—Al1—O5 | 89.32 (8) | O1—Al2—O2ii | 89.58 (7) |
O5i—Al1—O5 | 180.00 (5) | O2—Al2—O2ii | 180.0 |
Symmetry codes: (i) −x, −y+1, −z; (ii) −x+3/2, −y+1/2, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O14A—H14D···O8A | 0.82 (1) | 2.36 (4) | 2.976 (6) | 133 (5) |
O14A—H14C···I3Aiii | 0.82 (1) | 3.07 (3) | 3.738 (7) | 140 (3) |
O8A—H8D···I3Aiv | 0.82 (1) | 2.58 (1) | 3.391 (3) | 171 (2) |
O14—H14B···O15v | 0.82 (1) | 2.24 (1) | 3.048 (4) | 170 (3) |
O8—H8B···O14 | 0.82 (1) | 2.09 (2) | 2.808 (4) | 147 (3) |
O8—H8B···I3iii | 0.82 (1) | 3.24 (2) | 3.741 (3) | 122 (2) |
O8—H8A···I3iv | 0.82 (1) | 2.80 (1) | 3.610 (3) | 173 (2) |
O15—H15B···I2v | 0.84 (1) | 2.74 (1) | 3.5496 (17) | 162 (3) |
O15—H15A···I2vi | 0.83 (1) | 3.24 (3) | 3.6429 (17) | 113 (3) |
O15—H15A···I1ii | 0.83 (1) | 2.88 (2) | 3.645 (2) | 154 (3) |
O11—H11B···O15 | 0.83 (1) | 2.48 (3) | 3.070 (3) | 128 (3) |
O11—H11B···I3Avii | 0.83 (1) | 2.90 (3) | 3.505 (4) | 131 (3) |
O11—H11B···I3vii | 0.83 (1) | 3.10 (3) | 3.699 (3) | 131 (3) |
O11—H11A···O12ii | 0.83 (1) | 2.14 (2) | 2.917 (3) | 156 (3) |
O12—H12B···I2 | 0.83 (1) | 2.87 (2) | 3.615 (2) | 151 (3) |
O12—H12B···I1iii | 0.83 (1) | 3.28 (3) | 3.6691 (19) | 112 (3) |
O12—H12A···I1viii | 0.83 (1) | 2.69 (1) | 3.5072 (19) | 170 (3) |
O13—H13A···I3Aix | 0.84 (1) | 2.65 (1) | 3.474 (4) | 169 (3) |
O13—H13A···I3ix | 0.84 (1) | 2.64 (1) | 3.470 (3) | 173 (3) |
O13—H13B···I3Ax | 0.84 (1) | 2.74 (2) | 3.541 (4) | 160 (3) |
O13—H13B···I3x | 0.84 (1) | 2.72 (1) | 3.529 (3) | 163 (3) |
O9—H9B···I2xi | 0.83 (1) | 2.92 (2) | 3.5840 (18) | 138 (3) |
O9—H9B···I1iii | 0.83 (1) | 3.29 (3) | 3.8162 (18) | 124 (2) |
O9—H9A···O10xii | 0.84 (1) | 1.95 (1) | 2.789 (3) | 175 (3) |
O10—H10A···I2xii | 0.84 (1) | 2.95 (2) | 3.6308 (18) | 140 (3) |
O10—H10A···I1ix | 0.84 (1) | 3.06 (3) | 3.6067 (18) | 125 (3) |
O10—H10B···O9xiii | 0.84 (1) | 1.96 (1) | 2.782 (3) | 167 (3) |
O7—H7B···I2v | 0.83 (1) | 2.70 (1) | 3.5103 (19) | 166 (3) |
O7—H7A···I1xiv | 0.84 (1) | 2.78 (2) | 3.5668 (19) | 157 (3) |
O4—H4B···O12xii | 0.83 (1) | 1.78 (1) | 2.614 (3) | 179 (4) |
O4—H4A···O13 | 0.84 (1) | 1.86 (1) | 2.691 (3) | 171 (3) |
O6—H6B···O14Axii | 0.83 (1) | 1.69 (2) | 2.491 (6) | 161 (3) |
O6—H6B···O14xii | 0.83 (1) | 1.89 (1) | 2.716 (4) | 170 (3) |
O6—H6A···O13xi | 0.84 (1) | 1.89 (1) | 2.727 (3) | 175 (4) |
O5—H5A···O8xv | 0.84 (1) | 1.82 (1) | 2.644 (3) | 169 (3) |
O5—H5B···I1xvi | 0.84 (1) | 2.63 (1) | 3.4596 (17) | 169 (3) |
O1—H1A···O9xvii | 0.84 (1) | 1.85 (1) | 2.681 (2) | 174 (3) |
O1—H1B···O15 | 0.83 (1) | 1.85 (1) | 2.676 (3) | 172 (3) |
O3—H3B···O11 | 0.84 (1) | 1.75 (1) | 2.587 (2) | 176 (3) |
O3—H3A···O7 | 0.84 (1) | 1.89 (1) | 2.726 (2) | 174 (3) |
O2—H2A···O7vii | 0.84 (1) | 1.88 (1) | 2.718 (2) | 172 (3) |
O2—H2B···O10xii | 0.84 (1) | 1.81 (1) | 2.646 (2) | 176 (3) |
O14A—H14D···O8A | 0.82 (1) | 2.36 (4) | 2.976 (6) | 133 (5) |
O14A—H14C···I3Aiii | 0.82 (1) | 3.07 (3) | 3.738 (7) | 140 (3) |
O8A—H8D···I3Aiv | 0.82 (1) | 2.58 (1) | 3.391 (3) | 171 (2) |
O14—H14B···O15v | 0.82 (1) | 2.24 (1) | 3.048 (4) | 170 (3) |
O8—H8B···O14 | 0.82 (1) | 2.09 (2) | 2.808 (4) | 147 (3) |
O8—H8B···I3iii | 0.82 (1) | 3.24 (2) | 3.741 (3) | 122 (2) |
O8—H8A···I3iv | 0.82 (1) | 2.80 (1) | 3.610 (3) | 173 (2) |
O15—H15B···I2v | 0.84 (1) | 2.74 (1) | 3.5496 (17) | 162 (3) |
O15—H15A···I2vi | 0.83 (1) | 3.24 (3) | 3.6429 (17) | 113 (3) |
O15—H15A···I1ii | 0.83 (1) | 2.88 (2) | 3.645 (2) | 154 (3) |
O11—H11B···O15 | 0.83 (1) | 2.48 (3) | 3.070 (3) | 128 (3) |
O11—H11B···I3Avii | 0.83 (1) | 2.90 (3) | 3.505 (4) | 131 (3) |
O11—H11B···I3vii | 0.83 (1) | 3.10 (3) | 3.699 (3) | 131 (3) |
O11—H11A···O12ii | 0.83 (1) | 2.14 (2) | 2.917 (3) | 156 (3) |
O12—H12B···I2 | 0.83 (1) | 2.87 (2) | 3.615 (2) | 151 (3) |
O12—H12B···I1iii | 0.83 (1) | 3.28 (3) | 3.6691 (19) | 112 (3) |
O12—H12A···I1viii | 0.83 (1) | 2.69 (1) | 3.5072 (19) | 170 (3) |
O13—H13A···I3Aix | 0.84 (1) | 2.65 (1) | 3.474 (4) | 169 (3) |
O13—H13A···I3ix | 0.84 (1) | 2.64 (1) | 3.470 (3) | 173 (3) |
O13—H13B···I3Ax | 0.84 (1) | 2.74 (2) | 3.541 (4) | 160 (3) |
O13—H13B···I3x | 0.84 (1) | 2.72 (1) | 3.529 (3) | 163 (3) |
O9—H9B···I2xi | 0.83 (1) | 2.92 (2) | 3.5840 (18) | 138 (3) |
O9—H9B···I1iii | 0.83 (1) | 3.29 (3) | 3.8162 (18) | 124 (2) |
O9—H9A···O10xii | 0.84 (1) | 1.95 (1) | 2.789 (3) | 175 (3) |
O10—H10A···I2xii | 0.84 (1) | 2.95 (2) | 3.6308 (18) | 140 (3) |
O10—H10A···I1ix | 0.84 (1) | 3.06 (3) | 3.6067 (18) | 125 (3) |
O10—H10B···O9xiii | 0.84 (1) | 1.96 (1) | 2.782 (3) | 167 (3) |
O7—H7B···I2v | 0.83 (1) | 2.70 (1) | 3.5103 (19) | 166 (3) |
O7—H7A···I1xiv | 0.84 (1) | 2.78 (2) | 3.5668 (19) | 157 (3) |
O4—H4B···O12xii | 0.83 (1) | 1.78 (1) | 2.614 (3) | 179 (4) |
O4—H4A···O13 | 0.84 (1) | 1.86 (1) | 2.691 (3) | 171 (3) |
O6—H6B···O14Axii | 0.83 (1) | 1.69 (2) | 2.491 (6) | 161 (3) |
O6—H6B···O14xii | 0.83 (1) | 1.89 (1) | 2.716 (4) | 170 (3) |
O6—H6A···O13xi | 0.84 (1) | 1.89 (1) | 2.727 (3) | 175 (4) |
O5—H5A···O8xv | 0.84 (1) | 1.82 (1) | 2.644 (3) | 169 (3) |
O5—H5B···I1xvi | 0.84 (1) | 2.63 (1) | 3.4596 (17) | 169 (3) |
O1—H1A···O9xvii | 0.84 (1) | 1.85 (1) | 2.681 (2) | 174 (3) |
O1—H1B···O15 | 0.83 (1) | 1.85 (1) | 2.676 (3) | 172 (3) |
O3—H3B···O11 | 0.84 (1) | 1.75 (1) | 2.587 (2) | 176 (3) |
O3—H3A···O7 | 0.84 (1) | 1.89 (1) | 2.726 (2) | 174 (3) |
O2—H2A···O7vii | 0.84 (1) | 1.88 (1) | 2.718 (2) | 172 (3) |
O2—H2B···O10xii | 0.84 (1) | 1.81 (1) | 2.646 (2) | 176 (3) |
O14A—H14D···O8A | 0.82 (1) | 2.36 (4) | 2.976 (6) | 133 (5) |
O14A—H14C···I3Aiii | 0.82 (1) | 3.07 (3) | 3.738 (7) | 140 (3) |
O8A—H8D···I3Aiv | 0.82 (1) | 2.58 (1) | 3.391 (3) | 171 (2) |
O14—H14B···O15v | 0.82 (1) | 2.24 (1) | 3.048 (4) | 170 (3) |
O8—H8B···O14 | 0.82 (1) | 2.09 (2) | 2.808 (4) | 147 (3) |
O8—H8B···I3iii | 0.82 (1) | 3.24 (2) | 3.741 (3) | 122 (2) |
O8—H8A···I3iv | 0.82 (1) | 2.80 (1) | 3.610 (3) | 173 (2) |
O15—H15B···I2v | 0.84 (1) | 2.74 (1) | 3.5496 (17) | 162 (3) |
O15—H15A···I2vi | 0.83 (1) | 3.24 (3) | 3.6429 (17) | 113 (3) |
O15—H15A···I1ii | 0.83 (1) | 2.88 (2) | 3.645 (2) | 154 (3) |
O11—H11B···O15 | 0.83 (1) | 2.48 (3) | 3.070 (3) | 128 (3) |
O11—H11B···I3Avii | 0.83 (1) | 2.90 (3) | 3.505 (4) | 131 (3) |
O11—H11B···I3vii | 0.83 (1) | 3.10 (3) | 3.699 (3) | 131 (3) |
O11—H11A···O12ii | 0.83 (1) | 2.14 (2) | 2.917 (3) | 156 (3) |
O12—H12B···I2 | 0.83 (1) | 2.87 (2) | 3.615 (2) | 151 (3) |
O12—H12B···I1iii | 0.83 (1) | 3.28 (3) | 3.6691 (19) | 112 (3) |
O12—H12A···I1viii | 0.83 (1) | 2.69 (1) | 3.5072 (19) | 170 (3) |
O13—H13A···I3Aix | 0.84 (1) | 2.65 (1) | 3.474 (4) | 169 (3) |
O13—H13A···I3ix | 0.84 (1) | 2.64 (1) | 3.470 (3) | 173 (3) |
O13—H13B···I3Ax | 0.84 (1) | 2.74 (2) | 3.541 (4) | 160 (3) |
O13—H13B···I3x | 0.84 (1) | 2.72 (1) | 3.529 (3) | 163 (3) |
O9—H9B···I2xi | 0.83 (1) | 2.92 (2) | 3.5840 (18) | 138 (3) |
O9—H9B···I1iii | 0.83 (1) | 3.29 (3) | 3.8162 (18) | 124 (2) |
O9—H9A···O10xii | 0.84 (1) | 1.95 (1) | 2.789 (3) | 175 (3) |
O10—H10A···I2xii | 0.84 (1) | 2.95 (2) | 3.6308 (18) | 140 (3) |
O10—H10A···I1ix | 0.84 (1) | 3.06 (3) | 3.6067 (18) | 125 (3) |
O10—H10B···O9xiii | 0.84 (1) | 1.96 (1) | 2.782 (3) | 167 (3) |
O7—H7B···I2v | 0.83 (1) | 2.70 (1) | 3.5103 (19) | 166 (3) |
O7—H7A···I1xiv | 0.84 (1) | 2.78 (2) | 3.5668 (19) | 157 (3) |
O4—H4B···O12xii | 0.83 (1) | 1.78 (1) | 2.614 (3) | 179 (4) |
O4—H4A···O13 | 0.84 (1) | 1.86 (1) | 2.691 (3) | 171 (3) |
O6—H6B···O14Axii | 0.83 (1) | 1.69 (2) | 2.491 (6) | 161 (3) |
O6—H6B···O14xii | 0.83 (1) | 1.89 (1) | 2.716 (4) | 170 (3) |
O6—H6A···O13xi | 0.84 (1) | 1.89 (1) | 2.727 (3) | 175 (4) |
O5—H5A···O8xv | 0.84 (1) | 1.82 (1) | 2.644 (3) | 169 (3) |
O5—H5B···I1xvi | 0.84 (1) | 2.63 (1) | 3.4596 (17) | 169 (3) |
O1—H1A···O9xvii | 0.84 (1) | 1.85 (1) | 2.681 (2) | 174 (3) |
O1—H1B···O15 | 0.83 (1) | 1.85 (1) | 2.676 (3) | 172 (3) |
O3—H3B···O11 | 0.84 (1) | 1.75 (1) | 2.587 (2) | 176 (3) |
O3—H3A···O7 | 0.84 (1) | 1.89 (1) | 2.726 (2) | 174 (3) |
O2—H2A···O7vii | 0.84 (1) | 1.88 (1) | 2.718 (2) | 172 (3) |
O2—H2B···O10xii | 0.84 (1) | 1.81 (1) | 2.646 (2) | 176 (3) |
O2—H2B···O10xii | 0.84 (1) | 1.81 (1) | 2.646 (2) | 176 (3) |
O2—H2A···O7vii | 0.84 (1) | 1.88 (1) | 2.718 (2) | 172 (3) |
O3—H3A···O7 | 0.84 (1) | 1.89 (1) | 2.726 (2) | 174 (3) |
O3—H3B···O11 | 0.84 (1) | 1.75 (1) | 2.587 (2) | 176 (3) |
O1—H1B···O15 | 0.83 (1) | 1.85 (1) | 2.676 (3) | 172 (3) |
O1—H1A···O9xvii | 0.84 (1) | 1.85 (1) | 2.681 (2) | 174 (3) |
O5—H5B···I1xvi | 0.84 (1) | 2.63 (1) | 3.4596 (17) | 169 (3) |
O5—H5A···O8xv | 0.84 (1) | 1.82 (1) | 2.644 (3) | 169 (3) |
O6—H6A···O13xi | 0.84 (1) | 1.89 (1) | 2.727 (3) | 175 (4) |
O6—H6B···O14xii | 0.83 (1) | 1.89 (1) | 2.716 (4) | 170 (3) |
O6—H6B···O14Axii | 0.83 (1) | 1.69 (2) | 2.491 (6) | 161 (3) |
O4—H4A···O13 | 0.84 (1) | 1.86 (1) | 2.691 (3) | 171 (3) |
O4—H4B···O12xii | 0.83 (1) | 1.78 (1) | 2.614 (3) | 179 (4) |
O7—H7A···I1xiv | 0.84 (1) | 2.78 (2) | 3.5668 (19) | 157 (3) |
O7—H7B···I2v | 0.83 (1) | 2.70 (1) | 3.5103 (19) | 166 (3) |
O10—H10B···O9xiii | 0.84 (1) | 1.96 (1) | 2.782 (3) | 167 (3) |
O10—H10A···I1ix | 0.84 (1) | 3.06 (3) | 3.6067 (18) | 125 (3) |
O10—H10A···I2xii | 0.84 (1) | 2.95 (2) | 3.6308 (18) | 140 (3) |
O9—H9A···O10xii | 0.84 (1) | 1.95 (1) | 2.789 (3) | 175 (3) |
O9—H9B···I1iii | 0.83 (1) | 3.29 (3) | 3.8162 (18) | 124 (2) |
O9—H9B···I2xi | 0.83 (1) | 2.92 (2) | 3.5840 (18) | 138 (3) |
O13—H13B···I3x | 0.84 (1) | 2.72 (1) | 3.529 (3) | 163 (3) |
O13—H13B···I3Ax | 0.84 (1) | 2.74 (2) | 3.541 (4) | 160 (3) |
O13—H13A···I3ix | 0.84 (1) | 2.64 (1) | 3.470 (3) | 173 (3) |
O13—H13A···I3Aix | 0.84 (1) | 2.65 (1) | 3.474 (4) | 169 (3) |
O12—H12A···I1viii | 0.83 (1) | 2.69 (1) | 3.5072 (19) | 170 (3) |
O12—H12B···I1iii | 0.83 (1) | 3.28 (3) | 3.6691 (19) | 112 (3) |
O12—H12B···I2 | 0.83 (1) | 2.87 (2) | 3.615 (2) | 151 (3) |
O11—H11A···O12ii | 0.83 (1) | 2.14 (2) | 2.917 (3) | 156 (3) |
O11—H11B···I3vii | 0.83 (1) | 3.10 (3) | 3.699 (3) | 131 (3) |
O11—H11B···I3Avii | 0.83 (1) | 2.90 (3) | 3.505 (4) | 131 (3) |
O11—H11B···O15 | 0.83 (1) | 2.48 (3) | 3.070 (3) | 128 (3) |
O15—H15A···I1ii | 0.83 (1) | 2.88 (2) | 3.645 (2) | 154 (3) |
O15—H15A···I2vi | 0.83 (1) | 3.24 (3) | 3.6429 (17) | 113 (3) |
O15—H15B···I2v | 0.84 (1) | 2.74 (1) | 3.5496 (17) | 162 (3) |
O8—H8A···I3iv | 0.82 (1) | 2.80 (1) | 3.610 (3) | 173 (2) |
O8—H8B···I3iii | 0.82 (1) | 3.24 (2) | 3.741 (3) | 122 (2) |
O8—H8B···O14 | 0.82 (1) | 2.09 (2) | 2.808 (4) | 147 (3) |
O14—H14B···O15v | 0.82 (1) | 2.24 (1) | 3.048 (4) | 170 (3) |
O8A—H8D···I3Aiv | 0.82 (1) | 2.58 (1) | 3.391 (3) | 171 (2) |
O14A—H14C···I3Aiii | 0.82 (1) | 3.07 (3) | 3.738 (7) | 140 (3) |
O14A—H14D···O8A | 0.82 (1) | 2.36 (4) | 2.976 (6) | 133 (5) |
O2—H2B···O10xii | 0.84 (1) | 1.81 (1) | 2.646 (2) | 176 (3) |
O2—H2A···O7vii | 0.84 (1) | 1.88 (1) | 2.718 (2) | 172 (3) |
O3—H3A···O7 | 0.84 (1) | 1.89 (1) | 2.726 (2) | 174 (3) |
O3—H3B···O11 | 0.84 (1) | 1.75 (1) | 2.587 (2) | 176 (3) |
O1—H1B···O15 | 0.83 (1) | 1.85 (1) | 2.676 (3) | 172 (3) |
O1—H1A···O9xvii | 0.84 (1) | 1.85 (1) | 2.681 (2) | 174 (3) |
O5—H5B···I1xvi | 0.84 (1) | 2.63 (1) | 3.4596 (17) | 169 (3) |
O5—H5A···O8xv | 0.84 (1) | 1.82 (1) | 2.644 (3) | 169 (3) |
O6—H6A···O13xi | 0.84 (1) | 1.89 (1) | 2.727 (3) | 175 (4) |
O6—H6B···O14xii | 0.83 (1) | 1.89 (1) | 2.716 (4) | 170 (3) |
O6—H6B···O14Axii | 0.83 (1) | 1.69 (2) | 2.491 (6) | 161 (3) |
O4—H4A···O13 | 0.84 (1) | 1.86 (1) | 2.691 (3) | 171 (3) |
O4—H4B···O12xii | 0.83 (1) | 1.78 (1) | 2.614 (3) | 179 (4) |
O7—H7A···I1xiv | 0.84 (1) | 2.78 (2) | 3.5668 (19) | 157 (3) |
O7—H7B···I2v | 0.83 (1) | 2.70 (1) | 3.5103 (19) | 166 (3) |
O10—H10B···O9xiii | 0.84 (1) | 1.96 (1) | 2.782 (3) | 167 (3) |
O10—H10A···I1ix | 0.84 (1) | 3.06 (3) | 3.6067 (18) | 125 (3) |
O10—H10A···I2xii | 0.84 (1) | 2.95 (2) | 3.6308 (18) | 140 (3) |
O9—H9A···O10xii | 0.84 (1) | 1.95 (1) | 2.789 (3) | 175 (3) |
O9—H9B···I1iii | 0.83 (1) | 3.29 (3) | 3.8162 (18) | 124 (2) |
O9—H9B···I2xi | 0.83 (1) | 2.92 (2) | 3.5840 (18) | 138 (3) |
O13—H13B···I3x | 0.84 (1) | 2.72 (1) | 3.529 (3) | 163 (3) |
O13—H13B···I3Ax | 0.84 (1) | 2.74 (2) | 3.541 (4) | 160 (3) |
O13—H13A···I3ix | 0.84 (1) | 2.64 (1) | 3.470 (3) | 173 (3) |
O13—H13A···I3Aix | 0.84 (1) | 2.65 (1) | 3.474 (4) | 169 (3) |
O12—H12A···I1viii | 0.83 (1) | 2.69 (1) | 3.5072 (19) | 170 (3) |
O12—H12B···I2 | 0.83 (1) | 2.87 (2) | 3.615 (2) | 151 (3) |
O11—H11A···O12ii | 0.83 (1) | 2.14 (2) | 2.917 (3) | 156 (3) |
O11—H11B···I3vii | 0.83 (1) | 3.10 (3) | 3.699 (3) | 131 (3) |
O11—H11B···I3Avii | 0.83 (1) | 2.90 (3) | 3.505 (4) | 131 (3) |
O11—H11B···O15 | 0.83 (1) | 2.48 (3) | 3.070 (3) | 128 (3) |
O15—H15A···I1ii | 0.83 (1) | 2.88 (2) | 3.645 (2) | 154 (3) |
O15—H15A···I2vi | 0.83 (1) | 3.24 (3) | 3.6429 (17) | 113 (3) |
O15—H15B···I2v | 0.84 (1) | 2.74 (1) | 3.5496 (17) | 162 (3) |
O8—H8A···I3iv | 0.82 (1) | 2.80 (1) | 3.610 (3) | 173 (2) |
O8—H8B···I3iii | 0.82 (1) | 3.24 (2) | 3.741 (3) | 122 (2) |
O8—H8B···O14 | 0.82 (1) | 2.09 (2) | 2.808 (4) | 147 (3) |
O14—H14B···O15v | 0.82 (1) | 2.24 (1) | 3.048 (4) | 170 (3) |
O8A—H8D···I3Aiv | 0.82 (1) | 2.58 (1) | 3.391 (3) | 171 (2) |
O14A—H14C···I3Aiii | 0.82 (1) | 3.07 (3) | 3.738 (7) | 140 (3) |
O14A—H14D···O8A | 0.82 (1) | 2.36 (4) | 2.976 (6) | 133 (5) |
O2—H2B···O10xii | 0.84 (1) | 1.81 (1) | 2.646 (2) | 176 (3) |
O2—H2A···O7vii | 0.84 (1) | 1.88 (1) | 2.718 (2) | 172 (3) |
O3—H3A···O7 | 0.84 (1) | 1.89 (1) | 2.726 (2) | 174 (3) |
O3—H3B···O11 | 0.84 (1) | 1.75 (1) | 2.587 (2) | 176 (3) |
O1—H1B···O15 | 0.83 (1) | 1.85 (1) | 2.676 (3) | 172 (3) |
O1—H1A···O9xvii | 0.84 (1) | 1.85 (1) | 2.681 (2) | 174 (3) |
O5—H5B···I1xvi | 0.84 (1) | 2.63 (1) | 3.4596 (17) | 169 (3) |
O5—H5A···O8xv | 0.84 (1) | 1.82 (1) | 2.644 (3) | 169 (3) |
O6—H6A···O13xi | 0.84 (1) | 1.89 (1) | 2.727 (3) | 175 (4) |
O6—H6B···O14xii | 0.83 (1) | 1.89 (1) | 2.716 (4) | 170 (3) |
O6—H6B···O14Axii | 0.83 (1) | 1.69 (2) | 2.491 (6) | 161 (3) |
O4—H4A···O13 | 0.84 (1) | 1.86 (1) | 2.691 (3) | 171 (3) |
O4—H4B···O12xii | 0.83 (1) | 1.78 (1) | 2.614 (3) | 179 (4) |
O7—H7A···I1xiv | 0.84 (1) | 2.78 (2) | 3.5668 (19) | 157 (3) |
O7—H7B···I2v | 0.83 (1) | 2.70 (1) | 3.5103 (19) | 166 (3) |
O10—H10B···O9xiii | 0.84 (1) | 1.96 (1) | 2.782 (3) | 167 (3) |
O10—H10A···I1ix | 0.84 (1) | 3.06 (3) | 3.6067 (18) | 125 (3) |
O10—H10A···I2xii | 0.84 (1) | 2.95 (2) | 3.6308 (18) | 140 (3) |
O9—H9A···O10xii | 0.84 (1) | 1.95 (1) | 2.789 (3) | 175 (3) |
O9—H9B···I1iii | 0.83 (1) | 3.29 (3) | 3.8162 (18) | 124 (2) |
O9—H9B···I2xi | 0.83 (1) | 2.92 (2) | 3.5840 (18) | 138 (3) |
O13—H13B···I3x | 0.84 (1) | 2.72 (1) | 3.529 (3) | 163 (3) |
O13—H13B···I3Ax | 0.84 (1) | 2.74 (2) | 3.541 (4) | 160 (3) |
O13—H13A···I3ix | 0.84 (1) | 2.64 (1) | 3.470 (3) | 173 (3) |
O13—H13A···I3Aix | 0.84 (1) | 2.65 (1) | 3.474 (4) | 169 (3) |
O12—H12A···I1viii | 0.83 (1) | 2.69 (1) | 3.5072 (19) | 170 (3) |
O12—H12B···I1iii | 0.83 (1) | 3.28 (3) | 3.6691 (19) | 112 (3) |
O12—H12B···I2 | 0.83 (1) | 2.87 (2) | 3.615 (2) | 151 (3) |
O11—H11A···O12ii | 0.83 (1) | 2.14 (2) | 2.917 (3) | 156 (3) |
O11—H11B···I3vii | 0.83 (1) | 3.10 (3) | 3.699 (3) | 131 (3) |
O11—H11B···I3Avii | 0.83 (1) | 2.90 (3) | 3.505 (4) | 131 (3) |
O11—H11B···O15 | 0.83 (1) | 2.48 (3) | 3.070 (3) | 128 (3) |
O15—H15A···I1ii | 0.83 (1) | 2.88 (2) | 3.645 (2) | 154 (3) |
O15—H15A···I2vi | 0.83 (1) | 3.24 (3) | 3.6429 (17) | 113 (3) |
O15—H15B···I2v | 0.84 (1) | 2.74 (1) | 3.5496 (17) | 162 (3) |
O8—H8A···I3iv | 0.82 (1) | 2.80 (1) | 3.610 (3) | 173 (2) |
O8—H8B···I3iii | 0.82 (1) | 3.24 (2) | 3.741 (3) | 122 (2) |
O8—H8B···O14 | 0.82 (1) | 2.09 (2) | 2.808 (4) | 147 (3) |
O14—H14B···O15v | 0.82 (1) | 2.24 (1) | 3.048 (4) | 170 (3) |
O8A—H8D···I3Aiv | 0.82 (1) | 2.58 (1) | 3.391 (3) | 171 (2) |
O14A—H14C···I3Aiii | 0.82 (1) | 3.07 (3) | 3.738 (7) | 140 (3) |
O14A—H14D···O8A | 0.82 (1) | 2.36 (4) | 2.976 (6) | 133 (5) |
O2—H2B···O10xii | 0.84 (1) | 1.81 (1) | 2.646 (2) | 176 (3) |
O2—H2A···O7vii | 0.84 (1) | 1.88 (1) | 2.718 (2) | 172 (3) |
O3—H3A···O7 | 0.84 (1) | 1.89 (1) | 2.726 (2) | 174 (3) |
O3—H3B···O11 | 0.84 (1) | 1.75 (1) | 2.587 (2) | 176 (3) |
O1—H1B···O15 | 0.83 (1) | 1.85 (1) | 2.676 (3) | 172 (3) |
O1—H1A···O9xvii | 0.84 (1) | 1.85 (1) | 2.681 (2) | 174 (3) |
O5—H5B···I1xvi | 0.84 (1) | 2.63 (1) | 3.4596 (17) | 169 (3) |
O5—H5A···O8xv | 0.84 (1) | 1.82 (1) | 2.644 (3) | 169 (3) |
O6—H6A···O13xi | 0.84 (1) | 1.89 (1) | 2.727 (3) | 175 (4) |
O6—H6B···O14xii | 0.83 (1) | 1.89 (1) | 2.716 (4) | 170 (3) |
O6—H6B···O14Axii | 0.83 (1) | 1.69 (2) | 2.491 (6) | 161 (3) |
O4—H4A···O13 | 0.84 (1) | 1.86 (1) | 2.691 (3) | 171 (3) |
O4—H4B···O12xii | 0.83 (1) | 1.78 (1) | 2.614 (3) | 179 (4) |
O7—H7A···I1xiv | 0.84 (1) | 2.78 (2) | 3.5668 (19) | 157 (3) |
O7—H7B···I2v | 0.83 (1) | 2.70 (1) | 3.5103 (19) | 166 (3) |
O10—H10B···O9xiii | 0.84 (1) | 1.96 (1) | 2.782 (3) | 167 (3) |
O10—H10A···I1ix | 0.84 (1) | 3.06 (3) | 3.6067 (18) | 125 (3) |
O10—H10A···I2xii | 0.84 (1) | 2.95 (2) | 3.6308 (18) | 140 (3) |
O9—H9A···O10xii | 0.84 (1) | 1.95 (1) | 2.789 (3) | 175 (3) |
O9—H9B···I1iii | 0.83 (1) | 3.29 (3) | 3.8162 (18) | 124 (2) |
O9—H9B···I2xi | 0.83 (1) | 2.92 (2) | 3.5840 (18) | 138 (3) |
O13—H13B···I3x | 0.84 (1) | 2.72 (1) | 3.529 (3) | 163 (3) |
O13—H13B···I3Ax | 0.84 (1) | 2.74 (2) | 3.541 (4) | 160 (3) |
O13—H13A···I3ix | 0.84 (1) | 2.64 (1) | 3.470 (3) | 173 (3) |
O13—H13A···I3Aix | 0.84 (1) | 2.65 (1) | 3.474 (4) | 169 (3) |
O12—H12A···I1viii | 0.83 (1) | 2.69 (1) | 3.5072 (19) | 170 (3) |
O12—H12B···I1iii | 0.83 (1) | 3.28 (3) | 3.6691 (19) | 112 (3) |
O12—H12B···I2 | 0.83 (1) | 2.87 (2) | 3.615 (2) | 151 (3) |
O11—H11A···O12ii | 0.83 (1) | 2.14 (2) | 2.917 (3) | 156 (3) |
O11—H11B···I3vii | 0.83 (1) | 3.10 (3) | 3.699 (3) | 131 (3) |
O11—H11B···I3Avii | 0.83 (1) | 2.90 (3) | 3.505 (4) | 131 (3) |
O11—H11B···O15 | 0.83 (1) | 2.48 (3) | 3.070 (3) | 128 (3) |
O15—H15A···I1ii | 0.83 (1) | 2.88 (2) | 3.645 (2) | 154 (3) |
O15—H15A···I2vi | 0.83 (1) | 3.24 (3) | 3.6429 (17) | 113 (3) |
O15—H15B···I2v | 0.84 (1) | 2.74 (1) | 3.5496 (17) | 162 (3) |
O8—H8A···I3iv | 0.82 (1) | 2.80 (1) | 3.610 (3) | 173 (2) |
O8—H8B···I3iii | 0.82 (1) | 3.24 (2) | 3.741 (3) | 122 (2) |
O8—H8B···O14 | 0.82 (1) | 2.09 (2) | 2.808 (4) | 147 (3) |
O14—H14B···O15v | 0.82 (1) | 2.24 (1) | 3.048 (4) | 170 (3) |
O8A—H8D···I3Aiv | 0.82 (1) | 2.58 (1) | 3.391 (3) | 171 (2) |
O14A—H14C···I3Aiii | 0.82 (1) | 3.07 (3) | 3.738 (7) | 140 (3) |
O14A—H14D···O8A | 0.82 (1) | 2.36 (4) | 2.976 (6) | 133 (5) |
Symmetry codes: (ii) −x+3/2, −y+1/2, −z+1; (iii) x, −y+1, z−1/2; (iv) x, −y+2, z−1/2; (v) −x+3/2, y+1/2, −z+1/2; (vi) −x+3/2, y−1/2, −z+1/2; (vii) −x+3/2, −y+3/2, −z+1; (viii) x, −y, z−1/2; (ix) −x+1, −y+1, −z+1; (x) x−1, −y+1, z−1/2; (xi) x, y+1, z; (xii) −x+1, y, −z+1/2; (xiii) x−1/2, y−1/2, z; (xiv) −x+3/2, y+1/2, −z+3/2; (xv) x−1, y, z; (xvi) x−1, y, z−1; (xvii) x, y−1, z. |
[Al(H2O)6]I3·11H2O | Z = 4 |
Mr = 713.95 | F(000) = 1368 |
Triclinic, P1 | Dx = 2.054 Mg m−3 |
a = 9.7093 (8) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 15.0164 (14) Å | Cell parameters from 20312 reflections |
c = 17.2792 (15) Å | θ = 1.7–29.6° |
α = 70.293 (7)° | µ = 4.16 mm−1 |
β = 76.888 (7)° | T = 150 K |
γ = 87.591 (7)° | 0.56 × 0.31 × 0.13 mm |
V = 2308.3 (4) Å3 |
Stoe IPDS 2T diffractometer | 9574 independent reflections |
Radiation source: sealed X-ray tube | 8261 reflections with I > 2σ(I) |
Detector resolution: 6.67 pixels mm-1 | Rint = 0.095 |
rotation method scans | θmax = 26.5°, θmin = 2.5° |
Absorption correction: integration (Coppens, 1970) | h = −12→12 |
Tmin = 0.230, Tmax = 0.596 | k = −18→18 |
15854 measured reflections | l = −21→21 |
Refinement on F2 | Hydrogen site location: difference Fourier map |
Least-squares matrix: full | Only H-atom coordinates refined |
R[F2 > 2σ(F2)] = 0.048 | w = 1/[σ2(Fo2) + (0.1145P)2 + 8.7174P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.176 | (Δ/σ)max = 0.001 |
S = 1.12 | Δρmax = 2.58 e Å−3 |
9530 reflections | Δρmin = −1.60 e Å−3 |
592 parameters | Extinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
102 restraints | Extinction coefficient: 0.0014 (2) |
[Al(H2O)6]I3·11H2O | γ = 87.591 (7)° |
Mr = 713.95 | V = 2308.3 (4) Å3 |
Triclinic, P1 | Z = 4 |
a = 9.7093 (8) Å | Mo Kα radiation |
b = 15.0164 (14) Å | µ = 4.16 mm−1 |
c = 17.2792 (15) Å | T = 150 K |
α = 70.293 (7)° | 0.56 × 0.31 × 0.13 mm |
β = 76.888 (7)° |
Stoe IPDS 2T diffractometer | 9574 independent reflections |
Absorption correction: integration (Coppens, 1970) | 8261 reflections with I > 2σ(I) |
Tmin = 0.230, Tmax = 0.596 | Rint = 0.095 |
15854 measured reflections |
R[F2 > 2σ(F2)] = 0.048 | 102 restraints |
wR(F2) = 0.176 | Only H-atom coordinates refined |
S = 1.12 | Δρmax = 2.58 e Å−3 |
9530 reflections | Δρmin = −1.60 e Å−3 |
592 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
I1 | 0.78750 (4) | 0.89364 (3) | 0.62669 (3) | 0.02739 (15) | |
I2 | 0.72066 (4) | 0.61083 (3) | 0.87053 (3) | 0.02754 (15) | |
I3 | 0.66257 (4) | 0.38470 (3) | 0.76529 (2) | 0.02286 (14) | |
I4 | 0.82586 (4) | 0.10995 (3) | 0.73961 (2) | 0.02231 (14) | |
I5 | 0.75344 (4) | 0.71999 (3) | 0.06854 (2) | 0.02345 (14) | |
I6 | 0.76210 (4) | 0.78220 (3) | 0.43189 (2) | 0.02270 (14) | |
Al1 | 0.29512 (16) | 0.91611 (11) | 0.89753 (10) | 0.0158 (3) | |
Al2 | 0.79511 (16) | 0.41626 (11) | 0.40355 (10) | 0.0151 (3) | |
O16 | 0.4663 (5) | 0.8630 (3) | 0.1057 (3) | 0.0235 (9) | |
H16A | 0.491 (7) | 0.8065 (18) | 0.118 (5) | 0.028* | |
H16B | 0.394 (5) | 0.866 (5) | 0.142 (3) | 0.028* | |
O17 | 0.8529 (5) | 0.8297 (3) | 0.2110 (3) | 0.0266 (9) | |
H17B | 0.919 (5) | 0.803 (5) | 0.187 (4) | 0.032* | |
O29 | 0.5734 (5) | 0.2389 (3) | 0.6365 (3) | 0.0252 (9) | |
H29A | 0.513 (6) | 0.268 (5) | 0.661 (4) | 0.030* | |
H29B | 0.645 (5) | 0.234 (6) | 0.658 (5) | 0.030* | |
O13 | 0.0846 (5) | 0.7524 (3) | 0.1288 (3) | 0.0255 (9) | |
H13A | 0.061 (7) | 0.705 (3) | 0.119 (5) | 0.031* | |
H13B | 0.152 (6) | 0.731 (5) | 0.152 (5) | 0.031* | |
O30 | 0.3874 (5) | 0.5562 (4) | 0.7932 (3) | 0.0324 (11) | |
H30A | 0.453 (6) | 0.518 (4) | 0.797 (5) | 0.039* | |
H30B | 0.323 (6) | 0.514 (4) | 0.815 (5) | 0.039* | |
O33 | 0.6312 (4) | 0.5608 (3) | 0.5636 (3) | 0.0221 (8) | |
H33B | 0.650 (7) | 0.536 (5) | 0.611 (2) | 0.027* | |
O23 | 0.4462 (5) | 0.8053 (3) | 0.5778 (3) | 0.0263 (9) | |
H23A | 0.413 (7) | 0.860 (2) | 0.564 (5) | 0.032* | |
O24 | 0.0570 (5) | 0.6903 (3) | 0.9210 (3) | 0.0262 (9) | |
H24A | −0.026 (3) | 0.677 (6) | 0.949 (4) | 0.031* | |
H24B | 0.058 (7) | 0.687 (5) | 0.873 (2) | 0.031* | |
O26 | 0.8625 (4) | 0.9429 (3) | 0.9369 (3) | 0.0216 (8) | |
H26A | 0.828 (8) | 0.889 (2) | 0.968 (4) | 0.026* | |
H26B | 0.822 (7) | 0.962 (5) | 0.897 (3) | 0.026* | |
O31 | 0.7775 (5) | 0.6425 (3) | 0.6533 (3) | 0.0261 (9) | |
H31B | 0.744 (7) | 0.696 (2) | 0.638 (5) | 0.031* | |
O34 | 0.4124 (6) | 0.6538 (4) | 0.0111 (4) | 0.0416 (14) | |
H34A | 0.381 (9) | 0.645 (7) | 0.0626 (16) | 0.050* | |
H34B | 0.491 (5) | 0.630 (6) | −0.001 (6) | 0.050* | |
O25 | 0.7011 (5) | 0.8583 (3) | 0.8524 (3) | 0.0259 (9) | |
H25A | 0.711 (8) | 0.7995 (11) | 0.869 (5) | 0.031* | |
H25B | 0.749 (7) | 0.889 (5) | 0.804 (2) | 0.031* | |
O1 | 0.2690 (4) | 0.7849 (3) | 0.9321 (3) | 0.0224 (8) | |
H1A | 0.323 (6) | 0.745 (4) | 0.957 (4) | 0.027* | |
H1B | 0.192 (4) | 0.771 (5) | 0.923 (4) | 0.027* | |
O2 | 0.4016 (4) | 0.9152 (3) | 0.7929 (2) | 0.0224 (8) | |
H2A | 0.426 (7) | 0.961 (3) | 0.748 (2) | 0.027* | |
H2B | 0.390 (8) | 0.864 (3) | 0.785 (4) | 0.027* | |
O28 | 0.5084 (5) | 0.0488 (3) | 0.6456 (3) | 0.0245 (9) | |
H28A | 0.521 (7) | 0.1051 (19) | 0.642 (5) | 0.029* | |
H28B | 0.592 (3) | 0.035 (5) | 0.628 (5) | 0.029* | |
O21 | 0.1010 (5) | 0.9299 (4) | 0.7055 (3) | 0.0288 (10) | |
H21A | 0.039 (6) | 0.966 (4) | 0.687 (5) | 0.035* | |
H21B | 0.185 (3) | 0.950 (5) | 0.683 (5) | 0.035* | |
O19 | 0.1054 (6) | 0.8446 (4) | 0.4941 (4) | 0.0366 (12) | |
H19A | 0.143 (8) | 0.853 (7) | 0.4432 (17) | 0.044* | |
H19B | 0.032 (6) | 0.876 (6) | 0.493 (5) | 0.044* | |
O27 | 0.9906 (5) | 0.4467 (3) | 0.8367 (3) | 0.0259 (9) | |
H27B | 0.925 (6) | 0.479 (5) | 0.853 (4) | 0.031* | |
H27A | 1.037 (7) | 0.443 (5) | 0.873 (3) | 0.031* | |
O7 | 0.6442 (4) | 0.4985 (3) | 0.3887 (3) | 0.0231 (8) | |
H7B | 0.562 (3) | 0.476 (5) | 0.396 (5) | 0.028* | |
O5 | 0.1842 (4) | 0.9127 (3) | 1.0038 (3) | 0.0247 (8) | |
H5A | 0.183 (8) | 0.858 (2) | 1.039 (3) | 0.030* | |
H5B | 0.173 (8) | 0.958 (3) | 1.023 (4) | 0.030* | |
O4 | 0.3187 (4) | 1.0487 (3) | 0.8648 (3) | 0.0216 (8) | |
H4A | 0.392 (5) | 1.069 (5) | 0.873 (4) | 0.026* | |
H4B | 0.267 (6) | 1.088 (4) | 0.839 (4) | 0.026* | |
O9 | 0.7814 (4) | 0.3825 (3) | 0.3107 (3) | 0.0232 (8) | |
H9A | 0.714 (5) | 0.399 (5) | 0.287 (4) | 0.028* | |
H9B | 0.832 (6) | 0.340 (4) | 0.298 (4) | 0.028* | |
O6 | 0.4632 (4) | 0.9046 (3) | 0.9378 (3) | 0.0224 (8) | |
H6A | 0.527 (6) | 0.877 (5) | 0.914 (4) | 0.027* | |
H6B | 0.466 (7) | 0.888 (5) | 0.9889 (13) | 0.027* | |
O12 | 0.8105 (4) | 0.4511 (3) | 0.4971 (3) | 0.0231 (8) | |
H12A | 0.851 (7) | 0.418 (4) | 0.535 (3) | 0.028* | |
H12B | 0.754 (6) | 0.489 (4) | 0.513 (4) | 0.028* | |
O10 | 0.9451 (4) | 0.3350 (3) | 0.4228 (3) | 0.0234 (8) | |
H10B | 0.925 (7) | 0.2786 (19) | 0.454 (4) | 0.028* | |
H10A | 1.032 (2) | 0.349 (5) | 0.404 (4) | 0.028* | |
O8 | 0.9247 (4) | 0.5165 (3) | 0.3306 (2) | 0.0231 (8) | |
H8A | 0.949 (7) | 0.533 (5) | 0.2776 (8) | 0.028* | |
H8B | 0.960 (7) | 0.552 (4) | 0.350 (4) | 0.028* | |
O11 | 0.6638 (4) | 0.3180 (3) | 0.4738 (3) | 0.0224 (8) | |
H11A | 0.640 (7) | 0.286 (4) | 0.447 (4) | 0.027* | |
H11B | 0.635 (7) | 0.292 (5) | 0.5262 (10) | 0.027* | |
O3 | 0.1295 (4) | 0.9336 (3) | 0.8546 (3) | 0.0223 (8) | |
H3A | 0.123 (7) | 0.929 (5) | 0.808 (2) | 0.027* | |
H3B | 0.057 (4) | 0.950 (5) | 0.883 (4) | 0.027* | |
O15 | 0.0387 (5) | 0.6393 (3) | 0.3866 (3) | 0.0232 (9) | |
H15A | −0.009 (7) | 0.684 (3) | 0.397 (4) | 0.028* | |
H15B | 0.101 (6) | 0.656 (5) | 0.342 (3) | 0.028* | |
O18 | 0.6524 (5) | 0.6752 (3) | 0.2889 (3) | 0.0242 (9) | |
O20 | 0.3308 (5) | −0.0225 (3) | 0.5685 (3) | 0.0300 (10) | |
H20B | 0.312 (9) | 0.019 (4) | 0.526 (3) | 0.036* | |
O32 | 0.1590 (5) | 0.5108 (3) | 0.9291 (3) | 0.0312 (10) | |
H32A | 0.134 (8) | 0.560 (3) | 0.941 (5) | 0.037* | |
H32B | 0.175 (9) | 0.474 (5) | 0.975 (3) | 0.037* | |
O22 | 0.0480 (5) | 0.7345 (4) | 0.7502 (3) | 0.0317 (10) | |
H22A | −0.037 (3) | 0.722 (5) | 0.753 (5) | 0.038* | |
H22B | 0.066 (8) | 0.7932 (13) | 0.730 (5) | 0.038* | |
O14 | 0.4018 (7) | 0.7634 (4) | 0.7544 (3) | 0.0404 (13) | |
H14A | 0.398 (10) | 0.771 (6) | 0.704 (2) | 0.048* | |
H14B | 0.420 (10) | 0.707 (2) | 0.780 (5) | 0.048* | |
H33A | 0.665 (11) | 0.616 (3) | 0.536 (6) | 0.07 (3)* | |
H18A | 0.722 (7) | 0.714 (5) | 0.273 (6) | 0.06 (3)* | |
H18B | 0.646 (12) | 0.671 (8) | 0.243 (3) | 0.08 (4)* | |
H7A | 0.663 (10) | 0.554 (3) | 0.356 (6) | 0.07 (3)* | |
H23B | 0.532 (4) | 0.818 (8) | 0.553 (7) | 0.09 (4)* | |
H20A | 0.374 (10) | 0.007 (6) | 0.590 (6) | 0.07 (4)* | |
H17A | 0.882 (8) | 0.847 (6) | 0.246 (4) | 0.04 (2)* | |
H31A | 0.744 (7) | 0.609 (4) | 0.7036 (15) | 0.015 (15)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
I1 | 0.0337 (2) | 0.0236 (2) | 0.0289 (2) | 0.00832 (17) | −0.01032 (17) | −0.01277 (18) |
I2 | 0.0302 (2) | 0.0265 (2) | 0.0277 (2) | 0.00049 (17) | −0.00491 (17) | −0.01232 (18) |
I3 | 0.0209 (2) | 0.0188 (2) | 0.0270 (2) | 0.00108 (15) | −0.00377 (15) | −0.00643 (16) |
I4 | 0.0215 (2) | 0.0183 (2) | 0.0258 (2) | 0.00172 (14) | −0.00599 (15) | −0.00529 (16) |
I5 | 0.0255 (2) | 0.0197 (2) | 0.0250 (2) | 0.00315 (15) | −0.00369 (15) | −0.00905 (16) |
I6 | 0.0227 (2) | 0.0211 (2) | 0.0238 (2) | 0.00361 (15) | −0.00427 (15) | −0.00791 (16) |
Al1 | 0.0148 (8) | 0.0131 (8) | 0.0199 (8) | 0.0006 (6) | −0.0038 (6) | −0.0061 (6) |
Al2 | 0.0139 (7) | 0.0124 (8) | 0.0178 (8) | −0.0003 (6) | −0.0024 (6) | −0.0042 (6) |
O16 | 0.019 (2) | 0.022 (2) | 0.028 (2) | 0.0010 (16) | −0.0050 (16) | −0.0060 (17) |
O17 | 0.031 (2) | 0.024 (2) | 0.029 (2) | 0.0086 (18) | −0.0138 (19) | −0.0107 (18) |
O29 | 0.022 (2) | 0.027 (2) | 0.027 (2) | 0.0031 (17) | −0.0089 (17) | −0.0089 (18) |
O13 | 0.027 (2) | 0.019 (2) | 0.029 (2) | −0.0008 (17) | −0.0092 (17) | −0.0051 (17) |
O30 | 0.030 (2) | 0.027 (2) | 0.039 (3) | 0.0064 (19) | −0.016 (2) | −0.005 (2) |
O33 | 0.021 (2) | 0.022 (2) | 0.023 (2) | −0.0009 (16) | −0.0052 (16) | −0.0070 (17) |
O23 | 0.025 (2) | 0.023 (2) | 0.030 (2) | −0.0024 (18) | 0.0007 (18) | −0.0122 (19) |
O24 | 0.024 (2) | 0.027 (2) | 0.031 (2) | −0.0003 (18) | −0.0025 (18) | −0.017 (2) |
O26 | 0.020 (2) | 0.020 (2) | 0.022 (2) | −0.0047 (16) | −0.0022 (16) | −0.0048 (16) |
O31 | 0.033 (2) | 0.021 (2) | 0.022 (2) | 0.0063 (18) | −0.0070 (17) | −0.0049 (17) |
O34 | 0.041 (3) | 0.039 (3) | 0.031 (3) | 0.018 (2) | −0.005 (2) | 0.001 (2) |
O25 | 0.024 (2) | 0.025 (2) | 0.025 (2) | 0.0049 (17) | −0.0028 (17) | −0.0050 (18) |
O1 | 0.023 (2) | 0.0149 (18) | 0.029 (2) | 0.0003 (15) | −0.0078 (16) | −0.0059 (16) |
O2 | 0.030 (2) | 0.0151 (18) | 0.0223 (19) | −0.0013 (16) | −0.0043 (16) | −0.0071 (15) |
O28 | 0.022 (2) | 0.0152 (19) | 0.032 (2) | −0.0001 (16) | −0.0023 (17) | −0.0049 (17) |
O21 | 0.026 (2) | 0.034 (3) | 0.030 (2) | 0.0071 (19) | −0.0146 (18) | −0.010 (2) |
O19 | 0.032 (3) | 0.021 (2) | 0.044 (3) | −0.0022 (19) | −0.002 (2) | 0.001 (2) |
O27 | 0.023 (2) | 0.027 (2) | 0.028 (2) | 0.0045 (17) | −0.0045 (17) | −0.0112 (18) |
O7 | 0.0187 (18) | 0.0161 (19) | 0.031 (2) | 0.0025 (15) | −0.0068 (16) | −0.0025 (16) |
O5 | 0.029 (2) | 0.0189 (19) | 0.026 (2) | 0.0039 (16) | −0.0041 (16) | −0.0100 (16) |
O4 | 0.0230 (19) | 0.0117 (17) | 0.030 (2) | −0.0002 (14) | −0.0094 (16) | −0.0043 (15) |
O9 | 0.026 (2) | 0.0210 (19) | 0.027 (2) | 0.0054 (15) | −0.0092 (16) | −0.0115 (16) |
O6 | 0.0216 (19) | 0.022 (2) | 0.026 (2) | 0.0056 (15) | −0.0075 (16) | −0.0097 (16) |
O12 | 0.026 (2) | 0.023 (2) | 0.0238 (19) | 0.0046 (16) | −0.0057 (15) | −0.0119 (16) |
O10 | 0.0237 (19) | 0.0149 (18) | 0.030 (2) | 0.0049 (15) | −0.0074 (16) | −0.0056 (16) |
O8 | 0.029 (2) | 0.0202 (19) | 0.0200 (18) | −0.0014 (16) | −0.0032 (15) | −0.0078 (16) |
O11 | 0.026 (2) | 0.0180 (19) | 0.0226 (19) | −0.0025 (15) | −0.0038 (15) | −0.0063 (16) |
O3 | 0.0209 (19) | 0.025 (2) | 0.025 (2) | 0.0040 (15) | −0.0062 (15) | −0.0132 (17) |
O15 | 0.020 (2) | 0.021 (2) | 0.028 (2) | 0.0000 (16) | −0.0031 (17) | −0.0081 (18) |
O18 | 0.031 (2) | 0.016 (2) | 0.021 (2) | −0.0025 (17) | −0.0045 (17) | −0.0002 (16) |
O20 | 0.035 (2) | 0.022 (2) | 0.029 (2) | 0.0032 (19) | −0.0072 (19) | −0.0041 (18) |
O32 | 0.038 (3) | 0.020 (2) | 0.035 (2) | 0.0053 (19) | −0.008 (2) | −0.0092 (19) |
O22 | 0.028 (2) | 0.030 (2) | 0.044 (3) | 0.0013 (19) | −0.010 (2) | −0.020 (2) |
O14 | 0.065 (4) | 0.023 (2) | 0.034 (3) | 0.001 (2) | −0.001 (2) | −0.016 (2) |
Al1—O1 | 1.866 (4) | Al2—O9 | 1.871 (4) |
Al1—O2 | 1.872 (4) | Al2—O10 | 1.876 (4) |
Al1—O4 | 1.886 (4) | Al2—O11 | 1.877 (4) |
Al1—O5 | 1.891 (4) | Al2—O7 | 1.882 (4) |
Al1—O3 | 1.892 (4) | Al2—O8 | 1.897 (4) |
Al1—O6 | 1.894 (4) | Al2—O12 | 1.897 (4) |
O1—Al1—O2 | 89.31 (19) | O9—Al2—O10 | 91.13 (19) |
O1—Al1—O4 | 178.7 (2) | O9—Al2—O11 | 89.59 (19) |
O2—Al1—O4 | 91.97 (19) | O10—Al2—O11 | 90.60 (19) |
O1—Al1—O5 | 88.71 (19) | O9—Al2—O7 | 91.29 (19) |
O2—Al1—O5 | 177.9 (2) | O10—Al2—O7 | 177.5 (2) |
O4—Al1—O5 | 90.00 (19) | O11—Al2—O7 | 88.98 (18) |
O1—Al1—O3 | 90.82 (19) | O9—Al2—O8 | 89.38 (19) |
O2—Al1—O3 | 89.77 (19) | O10—Al2—O8 | 90.48 (19) |
O4—Al1—O3 | 89.03 (18) | O11—Al2—O8 | 178.52 (19) |
O5—Al1—O3 | 89.43 (19) | O7—Al2—O8 | 89.98 (19) |
O1—Al1—O6 | 91.73 (19) | O9—Al2—O12 | 179.5 (2) |
O2—Al1—O6 | 89.67 (19) | O10—Al2—O12 | 88.70 (19) |
O4—Al1—O6 | 88.43 (19) | O11—Al2—O12 | 90.87 (19) |
O5—Al1—O6 | 91.22 (19) | O7—Al2—O12 | 88.89 (19) |
O3—Al1—O6 | 177.4 (2) | O8—Al2—O12 | 90.16 (19) |
D—H···A | D—H | H···A | D···A | D—H···A |
O31—H31A···I3 | 0.84 (1) | 3.25 (6) | 3.782 (5) | 124 (6) |
O31—H31A···I2 | 0.84 (1) | 2.85 (5) | 3.535 (5) | 141 (6) |
O17—H17A···I6 | 0.84 (1) | 2.98 (7) | 3.542 (5) | 126 (7) |
O17—H17A···I4i | 0.84 (1) | 3.02 (6) | 3.640 (5) | 133 (7) |
O20—H20A···O28 | 0.84 (1) | 2.02 (3) | 2.837 (7) | 166 (10) |
O23—H23B···I6 | 0.84 (1) | 2.86 (8) | 3.588 (5) | 146 (12) |
O7—H7A···O18 | 0.84 (1) | 1.81 (3) | 2.624 (6) | 165 (10) |
O18—H18B···I5 | 0.84 (1) | 2.80 (6) | 3.543 (5) | 149 (9) |
O18—H18B···I3ii | 0.84 (1) | 3.19 (10) | 3.624 (5) | 115 (8) |
O18—H18A···O17 | 0.84 (1) | 2.03 (3) | 2.840 (8) | 163 (9) |
O33—H33A···I6 | 0.84 (1) | 2.60 (2) | 3.434 (4) | 171 (10) |
O14—H14B···O30 | 0.84 (1) | 2.23 (6) | 2.954 (7) | 144 (8) |
O14—H14A···O23 | 0.84 (1) | 2.02 (3) | 2.833 (7) | 163 (9) |
O22—H22B···O21 | 0.84 (1) | 1.98 (2) | 2.809 (7) | 170 (9) |
O22—H22A···I2iii | 0.84 (1) | 2.88 (5) | 3.573 (5) | 141 (6) |
O32—H32B···I2iv | 0.84 (1) | 2.94 (3) | 3.752 (5) | 164 (7) |
O32—H32A···O24 | 0.84 (1) | 2.01 (3) | 2.802 (7) | 156 (7) |
O20—H20B···I1ii | 0.84 (1) | 2.88 (3) | 3.689 (5) | 161 (7) |
O15—H15B···I3ii | 0.84 (1) | 2.79 (4) | 3.540 (5) | 150 (6) |
O15—H15A···I6iii | 0.84 (1) | 2.69 (3) | 3.482 (5) | 159 (7) |
O3—H3B···O26iii | 0.84 (1) | 1.90 (3) | 2.681 (6) | 155 (7) |
O3—H3A···O21 | 0.84 (1) | 1.83 (1) | 2.671 (6) | 174 (7) |
O11—H11B···O29 | 0.84 (1) | 1.77 (1) | 2.609 (6) | 179 (8) |
O11—H11A···O23ii | 0.84 (1) | 1.85 (2) | 2.659 (6) | 162 (7) |
O8—H8B···O15v | 0.84 (1) | 1.89 (1) | 2.725 (6) | 176 (7) |
O8—H8A···O27i | 0.84 (1) | 1.85 (2) | 2.686 (6) | 173 (7) |
O10—H10A···O31i | 0.84 (1) | 1.88 (2) | 2.696 (6) | 164 (8) |
O10—H10B···O19ii | 0.84 (1) | 1.77 (2) | 2.599 (6) | 171 (8) |
O12—H12B···O33 | 0.84 (1) | 1.85 (2) | 2.681 (6) | 172 (7) |
O12—H12A···O15ii | 0.84 (1) | 1.88 (2) | 2.711 (6) | 171 (7) |
O6—H6B···O16vi | 0.84 (1) | 1.93 (1) | 2.762 (6) | 175 (7) |
O6—H6A···O25 | 0.84 (1) | 1.84 (3) | 2.647 (6) | 159 (7) |
O9—H9B···O22ii | 0.84 (1) | 1.85 (2) | 2.675 (6) | 169 (7) |
O9—H9A···O30ii | 0.84 (1) | 1.80 (2) | 2.617 (6) | 163 (7) |
O4—H4B···O17vii | 0.84 (1) | 1.80 (1) | 2.636 (6) | 177 (7) |
O4—H4A···O16vii | 0.84 (1) | 1.92 (2) | 2.747 (6) | 167 (7) |
O5—H5B···O26viii | 0.84 (1) | 1.84 (1) | 2.678 (6) | 176 (8) |
O5—H5A···O13vi | 0.84 (1) | 1.91 (4) | 2.671 (6) | 151 (7) |
O7—H7B···O33ii | 0.84 (1) | 1.88 (2) | 2.707 (6) | 165 (7) |
O27—H27A···O32v | 0.84 (1) | 2.16 (4) | 2.916 (7) | 150 (7) |
O27—H27A···I5i | 0.84 (1) | 3.16 (6) | 3.699 (5) | 124 (6) |
O27—H27B···I2 | 0.84 (1) | 2.78 (2) | 3.608 (5) | 167 (7) |
O19—H19B···I1iii | 0.84 (1) | 2.98 (6) | 3.614 (6) | 134 (7) |
O19—H19A···I4ii | 0.84 (1) | 2.96 (3) | 3.765 (6) | 160 (7) |
O21—H21B···O20ix | 0.84 (1) | 2.08 (5) | 2.773 (7) | 140 (7) |
O21—H21A···I4x | 0.84 (1) | 3.15 (5) | 3.814 (5) | 139 (7) |
O21—H21A···I1iii | 0.84 (1) | 3.22 (7) | 3.734 (5) | 122 (6) |
O28—H28B···I1xi | 0.84 (1) | 2.79 (4) | 3.530 (5) | 147 (6) |
O28—H28A···O29 | 0.84 (1) | 2.06 (1) | 2.893 (6) | 174 (7) |
O2—H2B···O14 | 0.84 (1) | 1.75 (2) | 2.582 (6) | 168 (7) |
O2—H2A···O28ix | 0.84 (1) | 1.84 (2) | 2.668 (6) | 170 (7) |
O1—H1B···O24 | 0.84 (1) | 1.84 (3) | 2.627 (6) | 154 (7) |
O1—H1A···O34vi | 0.84 (1) | 1.71 (2) | 2.549 (7) | 172 (7) |
O25—H25B···I4ix | 0.84 (1) | 3.19 (7) | 3.727 (5) | 124 (7) |
O25—H25B···I1 | 0.84 (1) | 2.98 (6) | 3.655 (5) | 139 (7) |
O25—H25A···I2 | 0.84 (1) | 2.82 (3) | 3.624 (5) | 160 (7) |
O34—H34B···I2xii | 0.84 (1) | 2.85 (5) | 3.587 (6) | 147 (8) |
O34—H34A···I3ii | 0.84 (1) | 2.79 (2) | 3.612 (6) | 168 (8) |
O31—H31B···I6 | 0.84 (1) | 3.31 (7) | 3.726 (4) | 113 (6) |
O31—H31B···I1 | 0.84 (1) | 2.94 (5) | 3.645 (5) | 142 (6) |
O26—H26B···O25 | 0.84 (1) | 2.39 (6) | 2.941 (6) | 124 (6) |
O26—H26B···I4ix | 0.84 (1) | 2.86 (4) | 3.570 (4) | 143 (6) |
O26—H26A···I5vi | 0.84 (1) | 2.56 (1) | 3.401 (4) | 173 (7) |
O24—H24B···O22 | 0.84 (1) | 2.03 (3) | 2.818 (7) | 157 (7) |
O24—H24A···I5xiii | 0.84 (1) | 2.83 (5) | 3.554 (5) | 145 (7) |
O23—H23A···O20ix | 0.84 (1) | 1.93 (3) | 2.744 (7) | 163 (8) |
O33—H33B···O31 | 0.84 (1) | 2.45 (7) | 2.891 (7) | 114 (6) |
O33—H33B···I3 | 0.84 (1) | 2.88 (3) | 3.665 (4) | 156 (7) |
O30—H30B···O32 | 0.84 (1) | 2.22 (7) | 2.753 (7) | 122 (7) |
O30—H30A···I3 | 0.84 (1) | 2.88 (3) | 3.699 (5) | 164 (7) |
O13—H13B···I3ii | 0.84 (1) | 2.74 (2) | 3.562 (5) | 165 (7) |
O13—H13A···O27ii | 0.84 (1) | 2.18 (4) | 2.935 (7) | 149 (6) |
O13—H13A···I5iii | 0.84 (1) | 3.27 (6) | 3.695 (5) | 114 (5) |
O29—H29B···I4 | 0.84 (1) | 2.77 (5) | 3.490 (4) | 145 (7) |
O29—H29A···O18ii | 0.84 (1) | 1.95 (2) | 2.781 (7) | 170 (7) |
O17—H17B···O13v | 0.84 (1) | 1.97 (2) | 2.805 (7) | 174 (7) |
O16—H16B···I4ii | 0.84 (1) | 2.70 (1) | 3.543 (5) | 175 (7) |
O16—H16A···I5 | 0.84 (1) | 2.90 (5) | 3.522 (5) | 133 (6) |
O16—H16A···I3ii | 0.84 (1) | 3.10 (5) | 3.728 (5) | 133 (6) |
O31—H31A···I3 | 0.84 (1) | 3.25 (6) | 3.782 (5) | 124 (6) |
O31—H31A···I2 | 0.84 (1) | 2.85 (5) | 3.535 (5) | 141 (6) |
O17—H17A···I6 | 0.84 (1) | 2.98 (7) | 3.542 (5) | 126 (7) |
O17—H17A···I4i | 0.84 (1) | 3.02 (6) | 3.640 (5) | 133 (7) |
O20—H20A···O28 | 0.84 (1) | 2.02 (3) | 2.837 (7) | 166 (10) |
O23—H23B···I6 | 0.84 (1) | 2.86 (8) | 3.588 (5) | 146 (12) |
O7—H7A···O18 | 0.84 (1) | 1.81 (3) | 2.624 (6) | 165 (10) |
O18—H18B···I5 | 0.84 (1) | 2.80 (6) | 3.543 (5) | 149 (9) |
O18—H18B···I3ii | 0.84 (1) | 3.19 (10) | 3.624 (5) | 115 (8) |
O18—H18A···O17 | 0.84 (1) | 2.03 (3) | 2.840 (8) | 163 (9) |
O33—H33A···I6 | 0.84 (1) | 2.60 (2) | 3.434 (4) | 171 (10) |
O14—H14B···O30 | 0.84 (1) | 2.23 (6) | 2.954 (7) | 144 (8) |
O14—H14A···O23 | 0.84 (1) | 2.02 (3) | 2.833 (7) | 163 (9) |
O22—H22B···O21 | 0.84 (1) | 1.98 (2) | 2.809 (7) | 170 (9) |
O22—H22A···I2iii | 0.84 (1) | 2.88 (5) | 3.573 (5) | 141 (6) |
O32—H32B···I2iv | 0.84 (1) | 2.94 (3) | 3.752 (5) | 164 (7) |
O32—H32A···O24 | 0.84 (1) | 2.01 (3) | 2.802 (7) | 156 (7) |
O20—H20B···I1ii | 0.84 (1) | 2.88 (3) | 3.689 (5) | 161 (7) |
O15—H15B···I3ii | 0.84 (1) | 2.79 (4) | 3.540 (5) | 150 (6) |
O15—H15A···I6iii | 0.84 (1) | 2.69 (3) | 3.482 (5) | 159 (7) |
O3—H3B···O26iii | 0.84 (1) | 1.90 (3) | 2.681 (6) | 155 (7) |
O3—H3A···O21 | 0.84 (1) | 1.83 (1) | 2.671 (6) | 174 (7) |
O11—H11B···O29 | 0.84 (1) | 1.77 (1) | 2.609 (6) | 179 (8) |
O11—H11A···O23ii | 0.84 (1) | 1.85 (2) | 2.659 (6) | 162 (7) |
O8—H8B···O15v | 0.84 (1) | 1.89 (1) | 2.725 (6) | 176 (7) |
O8—H8A···O27i | 0.84 (1) | 1.85 (2) | 2.686 (6) | 173 (7) |
O10—H10A···O31i | 0.84 (1) | 1.88 (2) | 2.696 (6) | 164 (8) |
O10—H10B···O19ii | 0.84 (1) | 1.77 (2) | 2.599 (6) | 171 (8) |
O12—H12B···O33 | 0.84 (1) | 1.85 (2) | 2.681 (6) | 172 (7) |
O12—H12A···O15ii | 0.84 (1) | 1.88 (2) | 2.711 (6) | 171 (7) |
O6—H6B···O16vi | 0.84 (1) | 1.93 (1) | 2.762 (6) | 175 (7) |
O6—H6A···O25 | 0.84 (1) | 1.84 (3) | 2.647 (6) | 159 (7) |
O9—H9B···O22ii | 0.84 (1) | 1.85 (2) | 2.675 (6) | 169 (7) |
O9—H9A···O30ii | 0.84 (1) | 1.80 (2) | 2.617 (6) | 163 (7) |
O4—H4B···O17vii | 0.84 (1) | 1.80 (1) | 2.636 (6) | 177 (7) |
O4—H4A···O16vii | 0.84 (1) | 1.92 (2) | 2.747 (6) | 167 (7) |
O5—H5B···O26viii | 0.84 (1) | 1.84 (1) | 2.678 (6) | 176 (8) |
O5—H5A···O13vi | 0.84 (1) | 1.91 (4) | 2.671 (6) | 151 (7) |
O7—H7B···O33ii | 0.84 (1) | 1.88 (2) | 2.707 (6) | 165 (7) |
O27—H27A···O32v | 0.84 (1) | 2.16 (4) | 2.916 (7) | 150 (7) |
O27—H27A···I5i | 0.84 (1) | 3.16 (6) | 3.699 (5) | 124 (6) |
O27—H27B···I2 | 0.84 (1) | 2.78 (2) | 3.608 (5) | 167 (7) |
O19—H19B···I1iii | 0.84 (1) | 2.98 (6) | 3.614 (6) | 134 (7) |
O19—H19A···I4ii | 0.84 (1) | 2.96 (3) | 3.765 (6) | 160 (7) |
O21—H21B···O20ix | 0.84 (1) | 2.08 (5) | 2.773 (7) | 140 (7) |
O21—H21A···I4x | 0.84 (1) | 3.15 (5) | 3.814 (5) | 139 (7) |
O21—H21A···I1iii | 0.84 (1) | 3.22 (7) | 3.734 (5) | 122 (6) |
O28—H28B···I1xi | 0.84 (1) | 2.79 (4) | 3.530 (5) | 147 (6) |
O28—H28A···O29 | 0.84 (1) | 2.06 (1) | 2.893 (6) | 174 (7) |
O2—H2B···O14 | 0.84 (1) | 1.75 (2) | 2.582 (6) | 168 (7) |
O2—H2A···O28ix | 0.84 (1) | 1.84 (2) | 2.668 (6) | 170 (7) |
O1—H1B···O24 | 0.84 (1) | 1.84 (3) | 2.627 (6) | 154 (7) |
O1—H1A···O34vi | 0.84 (1) | 1.71 (2) | 2.549 (7) | 172 (7) |
O25—H25B···I4ix | 0.84 (1) | 3.19 (7) | 3.727 (5) | 124 (7) |
O25—H25B···I1 | 0.84 (1) | 2.98 (6) | 3.655 (5) | 139 (7) |
O25—H25A···I2 | 0.84 (1) | 2.82 (3) | 3.624 (5) | 160 (7) |
O34—H34B···I2xii | 0.84 (1) | 2.85 (5) | 3.587 (6) | 147 (8) |
O34—H34A···I3ii | 0.84 (1) | 2.79 (2) | 3.612 (6) | 168 (8) |
O31—H31B···I6 | 0.84 (1) | 3.31 (7) | 3.726 (4) | 113 (6) |
O31—H31B···I1 | 0.84 (1) | 2.94 (5) | 3.645 (5) | 142 (6) |
O26—H26B···O25 | 0.84 (1) | 2.39 (6) | 2.941 (6) | 124 (6) |
O26—H26B···I4ix | 0.84 (1) | 2.86 (4) | 3.570 (4) | 143 (6) |
O26—H26A···I5vi | 0.84 (1) | 2.56 (1) | 3.401 (4) | 173 (7) |
O24—H24B···O22 | 0.84 (1) | 2.03 (3) | 2.818 (7) | 157 (7) |
O24—H24A···I5xiii | 0.84 (1) | 2.83 (5) | 3.554 (5) | 145 (7) |
O23—H23A···O20ix | 0.84 (1) | 1.93 (3) | 2.744 (7) | 163 (8) |
O33—H33B···O31 | 0.84 (1) | 2.45 (7) | 2.891 (7) | 114 (6) |
O33—H33B···I3 | 0.84 (1) | 2.88 (3) | 3.665 (4) | 156 (7) |
O30—H30B···O32 | 0.84 (1) | 2.22 (7) | 2.753 (7) | 122 (7) |
O30—H30A···I3 | 0.84 (1) | 2.88 (3) | 3.699 (5) | 164 (7) |
O13—H13B···I3ii | 0.84 (1) | 2.74 (2) | 3.562 (5) | 165 (7) |
O13—H13A···O27ii | 0.84 (1) | 2.18 (4) | 2.935 (7) | 149 (6) |
O13—H13A···I5iii | 0.84 (1) | 3.27 (6) | 3.695 (5) | 114 (5) |
O29—H29B···I4 | 0.84 (1) | 2.77 (5) | 3.490 (4) | 145 (7) |
O29—H29A···O18ii | 0.84 (1) | 1.95 (2) | 2.781 (7) | 170 (7) |
O17—H17B···O13v | 0.84 (1) | 1.97 (2) | 2.805 (7) | 174 (7) |
O16—H16B···I4ii | 0.84 (1) | 2.70 (1) | 3.543 (5) | 175 (7) |
O16—H16A···I5 | 0.84 (1) | 2.90 (5) | 3.522 (5) | 133 (6) |
O16—H16A···I3ii | 0.84 (1) | 3.10 (5) | 3.728 (5) | 133 (6) |
Symmetry codes: (i) −x+2, −y+1, −z+1; (ii) −x+1, −y+1, −z+1; (iii) x−1, y, z; (iv) −x+1, −y+1, −z+2; (v) x+1, y, z; (vi) x, y, z+1; (vii) −x+1, −y+2, −z+1; (viii) −x+1, −y+2, −z+2; (ix) x, y+1, z; (x) x−1, y+1, z; (xi) x, y−1, z; (xii) x, y, z−1; (xiii) x−1, y, z+1. |
[Al(H2O)6]Br3·3H2O | F(000) = 832.0 |
Mr = 428.82 | Dx = 1.974 Mg m−3 |
Orthorhombic, Pnma | Mo Kα radiation, λ = 0.71073 Å |
a = 13.547 (3) Å | Cell parameters from 7014 reflections |
b = 13.494 (4) Å | θ = 2.9–29.0° |
c = 7.892 (2) Å | µ = 8.47 mm−1 |
V = 1442.6 (7) Å3 | T = 100 K |
Z = 4 | 0.02 × 0.01 × 0.01 mm |
Stoe IPDS 2T diffractometer | 1330 independent reflections |
Radiation source: sealed X-ray tube | 999 reflections with I > 2σ(I) |
Detector resolution: 6.67 pixels mm-1 | Rint = 0.056 |
rotation method scans | θmax = 25.0°, θmin = 3.0° |
Absorption correction: integration (Coppens, 1970) | h = −16→16 |
Tmin = 0.035, Tmax = 0.538 | k = −16→16 |
1330 measured reflections | l = −9→9 |
Refinement on F2 | Hydrogen site location: difference Fourier map |
Least-squares matrix: full | Only H-atom coordinates refined |
R[F2 > 2σ(F2)] = 0.059 | w = 1/[σ2(Fo2) + (0.1221P)2 + 4.5641P]
where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.197 | (Δ/σ)max = 0.851 |
S = 1.05 | Δρmax = 1.23 e Å−3 |
2030 reflections | Δρmin = −2.03 e Å−3 |
97 parameters | Extinction correction: SHELXL2012 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
16 restraints | Extinction coefficient: 0.0000 (7) |
[Al(H2O)6]Br3·3H2O | V = 1442.6 (7) Å3 |
Mr = 428.82 | Z = 4 |
Orthorhombic, Pnma | Mo Kα radiation |
a = 13.547 (3) Å | µ = 8.47 mm−1 |
b = 13.494 (4) Å | T = 100 K |
c = 7.892 (2) Å | 0.02 × 0.01 × 0.01 mm |
Stoe IPDS 2T diffractometer | 1330 independent reflections |
Absorption correction: integration (Coppens, 1970) | 999 reflections with I > 2σ(I) |
Tmin = 0.035, Tmax = 0.538 | Rint = 0.056 |
1330 measured reflections |
R[F2 > 2σ(F2)] = 0.059 | 16 restraints |
wR(F2) = 0.197 | Only H-atom coordinates refined |
S = 1.05 | (Δ/σ)max = 0.851 |
2030 reflections | Δρmax = 1.23 e Å−3 |
97 parameters | Δρmin = −2.03 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | ||
Br1 | 0.39785 (8) | 0.2500 | 0.83123 (13) | 0.0311 (3) | |
Br2 | 0.66239 (4) | 0.46591 (7) | 0.99881 (8) | 0.0299 (3) | |
Al1 | 0.5000 | 0.5000 | 0.5000 | 0.0233 (6) | |
O1 | 0.8276 (5) | 0.7500 | 0.0187 (10) | 0.0323 (18) | |
O2 | 0.3898 (3) | 0.4229 (5) | 0.5650 (6) | 0.0280 (11) | |
H2A | 0.394 (5) | 0.383 (5) | 0.647 (7) | 0.034* | |
H2B | 0.333 (3) | 0.449 (6) | 0.558 (11) | 0.034* | |
O3 | 0.4819 (3) | 0.5839 (4) | 0.6890 (6) | 0.0272 (11) | |
H3A | 0.445 (5) | 0.582 (5) | 0.775 (7) | 0.033* | |
H3B | 0.505 (6) | 0.641 (2) | 0.670 (9) | 0.033* | |
O4 | 0.5832 (3) | 0.4173 (4) | 0.6277 (6) | 0.0261 (11) | |
H4A | 0.606 (6) | 0.435 (5) | 0.722 (5) | 0.031* | |
H4B | 0.593 (6) | 0.3572 (19) | 0.607 (9) | 0.031* | |
O5 | 0.4182 (5) | 0.2500 | 0.2373 (10) | 0.0298 (16) | |
H5A | 0.397 (6) | 0.2500 | 0.137 (4) | 0.036* | |
H5B | 0.373 (5) | 0.2500 | 0.310 (8) | 0.036* | |
O6 | 0.7806 (5) | 0.7500 | 0.6754 (11) | 0.0330 (16) | |
H6A | 0.798 (6) | 0.701 (5) | 0.616 (10) | 0.040* | |
H1A | 0.803 (6) | 0.7500 | −0.079 (5) | 0.040* | |
H1B | 0.785 (5) | 0.7500 | 0.096 (8) | 0.040* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Br1 | 0.0298 (5) | 0.0396 (6) | 0.0239 (5) | 0.000 | 0.0040 (4) | 0.000 |
Br2 | 0.0154 (4) | 0.0528 (5) | 0.0215 (4) | 0.0013 (3) | 0.0010 (2) | −0.0009 (3) |
Al1 | 0.0129 (11) | 0.0387 (17) | 0.0183 (12) | −0.0017 (12) | 0.0005 (9) | 0.0017 (12) |
O1 | 0.023 (3) | 0.046 (5) | 0.028 (4) | 0.000 | 0.004 (3) | 0.000 |
O2 | 0.0128 (19) | 0.044 (3) | 0.027 (2) | −0.001 (2) | −0.0024 (17) | 0.007 (2) |
O3 | 0.0182 (19) | 0.040 (3) | 0.023 (2) | −0.004 (2) | 0.0046 (17) | −0.001 (2) |
O4 | 0.017 (2) | 0.038 (3) | 0.023 (2) | 0.002 (2) | −0.0028 (16) | 0.004 (2) |
O5 | 0.026 (3) | 0.036 (4) | 0.027 (3) | 0.000 | 0.001 (3) | 0.000 |
O6 | 0.024 (3) | 0.036 (4) | 0.039 (4) | 0.000 | 0.001 (3) | 0.000 |
Al1—O4i | 1.880 (5) | Al1—O3 | 1.888 (5) |
Al1—O4 | 1.880 (5) | Al1—O2i | 1.891 (5) |
Al1—O3i | 1.888 (5) | Al1—O2 | 1.891 (5) |
O4i—Al1—O4 | 180.0 | O3i—Al1—O2i | 90.8 (2) |
O4i—Al1—O3i | 90.6 (2) | O3—Al1—O2i | 89.2 (2) |
O4—Al1—O3i | 89.4 (2) | O4i—Al1—O2 | 89.9 (2) |
O4i—Al1—O3 | 89.4 (2) | O4—Al1—O2 | 90.1 (2) |
O4—Al1—O3 | 90.6 (2) | O3i—Al1—O2 | 89.2 (2) |
O3i—Al1—O3 | 180.0 | O3—Al1—O2 | 90.8 (2) |
O4i—Al1—O2i | 90.1 (2) | O2i—Al1—O2 | 180.0 |
O4—Al1—O2i | 89.9 (2) |
Symmetry code: (i) −x+1, −y+1, −z+1. |
Experimental details
(AlCl3_15H2O_150K) | (AlBr3_15H2O_120K) | (AlI3_15H2O_100K) | (AlI3_17H2O_150K) | |
Crystal data | ||||
Chemical formula | [Al(H2O)6]Cl3·9H2O | [Al(H2O)]Br3·9H2O | [Al(H2O)6]I3·9H2O | [Al(H2O)6]I3·11H2O |
Mr | 403.57 | 536.95 | 677.92 | 713.95 |
Crystal system, space group | Monoclinic, Cc | Monoclinic, Cc | Monoclinic, C2/c | Triclinic, P1 |
Temperature (K) | 150 | 120 | 100 | 150 |
a, b, c (Å) | 18.6568 (19), 6.5415 (4), 18.0351 (18) | 19.0122 (13), 6.6568 (6), 18.2360 (13) | 37.010 (3), 6.9011 (3), 18.1054 (16) | 9.7093 (8), 15.0164 (14), 17.2792 (15) |
α, β, γ (°) | 90, 124.223 (7), 90 | 90, 123.834 (5), 90 | 90, 111.829 (7), 90 | 70.293 (7), 76.888 (7), 87.591 (7) |
V (Å3) | 1820.0 (3) | 1917.1 (3) | 4292.7 (6) | 2308.3 (4) |
Z | 4 | 4 | 8 | 4 |
Radiation type | Mo Kα | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 0.61 | 6.41 | 4.46 | 4.16 |
Crystal size (mm) | 0.59 × 0.37 × 0.16 | 0.33 × 0.22 × 0.10 | 0.64 × 0.41 × 0.14 | 0.56 × 0.31 × 0.13 |
Data collection | ||||
Diffractometer | Stoe IPDS 2T diffractometer | Stoe IPDS 2 diffractometer | Stoe IPDS 2T diffractometer | Stoe IPDS 2T diffractometer |
Absorption correction | Integration (Coppens, 1970) | Integration (Coppens, 1970) | Integration (Coppens, 1970) | Integration (Coppens, 1970) |
Tmin, Tmax | 0.761, 0.908 | 0.208, 0.525 | 0.127, 0.546 | 0.230, 0.596 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 17267, 4973, 4480 | 10481, 3992, 3320 | 19548, 4912, 4740 | 15854, 9574, 8261 |
Rint | 0.050 | 0.082 | 0.054 | 0.095 |
(sin θ/λ)max (Å−1) | 0.693 | 0.628 | 0.650 | 0.628 |
Refinement | ||||
R[F2 > 2σ(F2)], wR(F2), S | 0.028, 0.074, 1.01 | 0.065, 0.197, 1.06 | 0.021, 0.050, 1.29 | 0.048, 0.176, 1.12 |
No. of reflections | 4973 | 3602 | 4912 | 9530 |
No. of parameters | 292 | 263 | 282 | 592 |
No. of restraints | 47 | 47 | 73 | 102 |
H-atom treatment | All H-atom parameters refined | Only H-atom coordinates refined | Only H-atom coordinates refined | Only H-atom coordinates refined |
(Δ/σ)max | < 0.001 | < 0.001 | 0.003 | 0.001 |
Δρmax, Δρmin (e Å−3) | 0.30, −0.18 | 1.81, −1.23 | 0.57, −0.78 | 2.58, −1.60 |
Absolute structure | Classical Flack (1983) method preferred over Parsons (2003) because s.u. is lower | Classical Flack (1983) method preferred over Parsons (2003) because s.u. is lower | ? | ? |
Absolute structure parameter | 0.67 (6) | 0.13 (3) | ? | ? |
(AlBr3_9H2O_100K) | |
Crystal data | |
Chemical formula | [Al(H2O)6]Br3·3H2O |
Mr | 428.82 |
Crystal system, space group | Orthorhombic, Pnma |
Temperature (K) | 100 |
a, b, c (Å) | 13.547 (3), 13.494 (4), 7.892 (2) |
α, β, γ (°) | 90, 90, 90 |
V (Å3) | 1442.6 (7) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 8.47 |
Crystal size (mm) | 0.02 × 0.01 × 0.01 |
Data collection | |
Diffractometer | Stoe IPDS 2T diffractometer |
Absorption correction | Integration (Coppens, 1970) |
Tmin, Tmax | 0.035, 0.538 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 1330, 1330, 999 |
Rint | 0.056 |
(sin θ/λ)max (Å−1) | 0.594 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.059, 0.197, 1.05 |
No. of reflections | 2030 |
No. of parameters | 97 |
No. of restraints | 16 |
H-atom treatment | Only H-atom coordinates refined |
(Δ/σ)max | 0.851 |
Δρmax, Δρmin (e Å−3) | 1.23, −2.03 |
Absolute structure | ? |
Absolute structure parameter | ? |
Computer programs: X-AREA (Stoe & Cie, 2003), X-RED (Stoe & Cie, 2003), SHELXS97 (Sheldrick, 2008), SHELXL2012 (Sheldrick, 2008).
D—H···A | D—H | H···A | D···A | D—H···A |
O7—H7A···Cl3 | 0.836 (14) | 2.47 (3) | 3.236 (2) | 153 (4) |
O15—H15A···O7 | 0.833 (14) | 2.020 (15) | 2.850 (3) | 174 (4) |
O1—H1B···Cl3 | 0.838 (14) | 2.154 (16) | 2.986 (2) | 171 (4) |
O12—H12B···Cl3i | 0.839 (14) | 2.362 (15) | 3.200 (2) | 177 (5) |
O12—H12A···O15ii | 0.837 (14) | 2.13 (4) | 2.826 (3) | 141 (5) |
O11—H11A···Cl3iii | 0.840 (15) | 2.79 (3) | 3.535 (3) | 149 (5) |
O10—H10A···O13iv | 0.834 (15) | 2.14 (3) | 2.897 (3) | 151 (6) |
O10—H10A···Cl2 | 0.834 (15) | 2.86 (5) | 3.416 (2) | 126 (5) |
O9—H9B···Cl2 | 0.841 (14) | 2.275 (18) | 3.108 (2) | 171 (6) |
O9—H9A···Cl1v | 0.841 (14) | 2.256 (17) | 3.090 (2) | 172 (5) |
O13—H13A···Cl3vi | 0.842 (14) | 2.71 (5) | 3.284 (3) | 127 (5) |
O13—H13A···Cl2vii | 0.842 (14) | 2.93 (5) | 3.329 (3) | 111 (4) |
O6—H6B···O14viii | 0.841 (14) | 1.815 (15) | 2.656 (3) | 178 (5) |
O6—H6A···O8viii | 0.837 (14) | 1.836 (15) | 2.672 (3) | 177 (4) |
O14—H14A···Cl2ix | 0.836 (14) | 2.343 (17) | 3.169 (2) | 170 (5) |
O14—H14B···O11ix | 0.837 (15) | 2.12 (3) | 2.892 (3) | 153 (4) |
O14—H14B···Cl1 | 0.837 (15) | 2.83 (4) | 3.345 (2) | 122 (4) |
O13—H13B···O14 | 0.843 (15) | 1.942 (15) | 2.785 (4) | 177 (5) |
O15—H15B···Cl1viii | 0.840 (14) | 2.326 (15) | 3.165 (2) | 178 (4) |
O10—H10B···Cl1iv | 0.840 (14) | 2.37 (2) | 3.172 (2) | 159 (5) |
O7—H7B···Cl2x | 0.838 (14) | 2.326 (15) | 3.164 (2) | 177 (4) |
O11—H11B···O10 | 0.840 (14) | 2.008 (19) | 2.822 (4) | 163 (4) |
O3—H3B···O7ii | 0.832 (14) | 1.854 (15) | 2.686 (3) | 178 (5) |
O3—H3A···O11viii | 0.840 (14) | 1.837 (16) | 2.673 (3) | 174 (6) |
O1—H1A···O9x | 0.839 (14) | 1.836 (15) | 2.671 (3) | 174 (5) |
O5—H5A···O13 | 0.835 (14) | 1.803 (15) | 2.635 (3) | 175 (4) |
O5—H5B···O15 | 0.839 (15) | 1.808 (15) | 2.646 (3) | 176 (6) |
O4—H4B···O12 | 0.837 (14) | 1.78 (2) | 2.605 (3) | 166 (6) |
O4—H4A···O8 | 0.833 (14) | 1.847 (16) | 2.676 (3) | 173 (5) |
O8—H8A···Cl2 | 0.836 (14) | 2.320 (17) | 3.147 (2) | 171 (5) |
O8—H8B···Cl1v | 0.841 (14) | 2.30 (2) | 3.102 (2) | 159 (5) |
O2—H2B···O10 | 0.837 (14) | 1.815 (16) | 2.646 (3) | 171 (5) |
O2—H2A···O9xi | 0.837 (15) | 1.828 (15) | 2.663 (3) | 175 (6) |
O7—H7A···Cl3 | 0.836 (14) | 2.47 (3) | 3.236 (2) | 153 (4) |
O15—H15A···O7 | 0.833 (14) | 2.020 (15) | 2.850 (3) | 174 (4) |
O1—H1B···Cl3 | 0.838 (14) | 2.154 (16) | 2.986 (2) | 171 (4) |
O12—H12B···Cl3i | 0.839 (14) | 2.362 (15) | 3.200 (2) | 177 (5) |
O12—H12A···O15ii | 0.837 (14) | 2.13 (4) | 2.826 (3) | 141 (5) |
O11—H11A···Cl3iii | 0.840 (15) | 2.79 (3) | 3.535 (3) | 149 (5) |
O10—H10A···O13iv | 0.834 (15) | 2.14 (3) | 2.897 (3) | 151 (6) |
O10—H10A···Cl2 | 0.834 (15) | 2.86 (5) | 3.416 (2) | 126 (5) |
O9—H9B···Cl2 | 0.841 (14) | 2.275 (18) | 3.108 (2) | 171 (6) |
O9—H9A···Cl1v | 0.841 (14) | 2.256 (17) | 3.090 (2) | 172 (5) |
O13—H13A···Cl3vi | 0.842 (14) | 2.71 (5) | 3.284 (3) | 127 (5) |
O13—H13A···Cl2vii | 0.842 (14) | 2.93 (5) | 3.329 (3) | 111 (4) |
O6—H6B···O14viii | 0.841 (14) | 1.815 (15) | 2.656 (3) | 178 (5) |
O6—H6A···O8viii | 0.837 (14) | 1.836 (15) | 2.672 (3) | 177 (4) |
O14—H14A···Cl2ix | 0.836 (14) | 2.343 (17) | 3.169 (2) | 170 (5) |
O14—H14B···O11ix | 0.837 (15) | 2.12 (3) | 2.892 (3) | 153 (4) |
O14—H14B···Cl1 | 0.837 (15) | 2.83 (4) | 3.345 (2) | 122 (4) |
O13—H13B···O14 | 0.843 (15) | 1.942 (15) | 2.785 (4) | 177 (5) |
O15—H15B···Cl1viii | 0.840 (14) | 2.326 (15) | 3.165 (2) | 178 (4) |
O10—H10B···Cl1iv | 0.840 (14) | 2.37 (2) | 3.172 (2) | 159 (5) |
O7—H7B···Cl2x | 0.838 (14) | 2.326 (15) | 3.164 (2) | 177 (4) |
O11—H11B···O10 | 0.840 (14) | 2.008 (19) | 2.822 (4) | 163 (4) |
O3—H3B···O7ii | 0.832 (14) | 1.854 (15) | 2.686 (3) | 178 (5) |
O3—H3A···O11viii | 0.840 (14) | 1.837 (16) | 2.673 (3) | 174 (6) |
O1—H1A···O9x | 0.839 (14) | 1.836 (15) | 2.671 (3) | 174 (5) |
O5—H5A···O13 | 0.835 (14) | 1.803 (15) | 2.635 (3) | 175 (4) |
O5—H5B···O15 | 0.839 (15) | 1.808 (15) | 2.646 (3) | 176 (6) |
O4—H4B···O12 | 0.837 (14) | 1.78 (2) | 2.605 (3) | 166 (6) |
O4—H4A···O8 | 0.833 (14) | 1.847 (16) | 2.676 (3) | 173 (5) |
O8—H8A···Cl2 | 0.836 (14) | 2.320 (17) | 3.147 (2) | 171 (5) |
O8—H8B···Cl1v | 0.841 (14) | 2.30 (2) | 3.102 (2) | 159 (5) |
O2—H2B···O10 | 0.837 (14) | 1.815 (16) | 2.646 (3) | 171 (5) |
O2—H2A···O9xi | 0.837 (15) | 1.828 (15) | 2.663 (3) | 175 (6) |
O7—H7A···Cl3 | 0.836 (14) | 2.47 (3) | 3.236 (2) | 153 (4) |
O15—H15A···O7 | 0.833 (14) | 2.020 (15) | 2.850 (3) | 174 (4) |
O1—H1B···Cl3 | 0.838 (14) | 2.154 (16) | 2.986 (2) | 171 (4) |
O12—H12B···Cl3i | 0.839 (14) | 2.362 (15) | 3.200 (2) | 177 (5) |
O12—H12A···O15ii | 0.837 (14) | 2.13 (4) | 2.826 (3) | 141 (5) |
O11—H11A···Cl3iii | 0.840 (15) | 2.79 (3) | 3.535 (3) | 149 (5) |
O10—H10A···O13iv | 0.834 (15) | 2.14 (3) | 2.897 (3) | 151 (6) |
O10—H10A···Cl2 | 0.834 (15) | 2.86 (5) | 3.416 (2) | 126 (5) |
O9—H9B···Cl2 | 0.841 (14) | 2.275 (18) | 3.108 (2) | 171 (6) |
O9—H9A···Cl1v | 0.841 (14) | 2.256 (17) | 3.090 (2) | 172 (5) |
O13—H13A···Cl3vi | 0.842 (14) | 2.71 (5) | 3.284 (3) | 127 (5) |
O13—H13A···Cl2vii | 0.842 (14) | 2.93 (5) | 3.329 (3) | 111 (4) |
O6—H6B···O14viii | 0.841 (14) | 1.815 (15) | 2.656 (3) | 178 (5) |
O6—H6A···O8viii | 0.837 (14) | 1.836 (15) | 2.672 (3) | 177 (4) |
O14—H14A···Cl2ix | 0.836 (14) | 2.343 (17) | 3.169 (2) | 170 (5) |
O14—H14B···O11ix | 0.837 (15) | 2.12 (3) | 2.892 (3) | 153 (4) |
O14—H14B···Cl1 | 0.837 (15) | 2.83 (4) | 3.345 (2) | 122 (4) |
O13—H13B···O14 | 0.843 (15) | 1.942 (15) | 2.785 (4) | 177 (5) |
O15—H15B···Cl1viii | 0.840 (14) | 2.326 (15) | 3.165 (2) | 178 (4) |
O10—H10B···Cl1iv | 0.840 (14) | 2.37 (2) | 3.172 (2) | 159 (5) |
O7—H7B···Cl2x | 0.838 (14) | 2.326 (15) | 3.164 (2) | 177 (4) |
O11—H11B···O10 | 0.840 (14) | 2.008 (19) | 2.822 (4) | 163 (4) |
O3—H3B···O7ii | 0.832 (14) | 1.854 (15) | 2.686 (3) | 178 (5) |
O3—H3A···O11viii | 0.840 (14) | 1.837 (16) | 2.673 (3) | 174 (6) |
O1—H1A···O9x | 0.839 (14) | 1.836 (15) | 2.671 (3) | 174 (5) |
O5—H5A···O13 | 0.835 (14) | 1.803 (15) | 2.635 (3) | 175 (4) |
O5—H5B···O15 | 0.839 (15) | 1.808 (15) | 2.646 (3) | 176 (6) |
O4—H4B···O12 | 0.837 (14) | 1.78 (2) | 2.605 (3) | 166 (6) |
O4—H4A···O8 | 0.833 (14) | 1.847 (16) | 2.676 (3) | 173 (5) |
O8—H8A···Cl2 | 0.836 (14) | 2.320 (17) | 3.147 (2) | 171 (5) |
O8—H8B···Cl1v | 0.841 (14) | 2.30 (2) | 3.102 (2) | 159 (5) |
O2—H2B···O10 | 0.837 (14) | 1.815 (16) | 2.646 (3) | 171 (5) |
O2—H2A···O9xi | 0.837 (15) | 1.828 (15) | 2.663 (3) | 175 (6) |
O7—H7A···Cl3 | 0.836 (14) | 2.47 (3) | 3.236 (2) | 153 (4) |
O15—H15A···O7 | 0.833 (14) | 2.020 (15) | 2.850 (3) | 174 (4) |
O1—H1B···Cl3 | 0.838 (14) | 2.154 (16) | 2.986 (2) | 171 (4) |
O12—H12B···Cl3i | 0.839 (14) | 2.362 (15) | 3.200 (2) | 177 (5) |
O12—H12A···O15ii | 0.837 (14) | 2.13 (4) | 2.826 (3) | 141 (5) |
O11—H11A···Cl3iii | 0.840 (15) | 2.79 (3) | 3.535 (3) | 149 (5) |
O10—H10A···O13iv | 0.834 (15) | 2.14 (3) | 2.897 (3) | 151 (6) |
O10—H10A···Cl2 | 0.834 (15) | 2.86 (5) | 3.416 (2) | 126 (5) |
O9—H9B···Cl2 | 0.841 (14) | 2.275 (18) | 3.108 (2) | 171 (6) |
O9—H9A···Cl1v | 0.841 (14) | 2.256 (17) | 3.090 (2) | 172 (5) |
O13—H13A···Cl3vi | 0.842 (14) | 2.71 (5) | 3.284 (3) | 127 (5) |
O13—H13A···Cl2vii | 0.842 (14) | 2.93 (5) | 3.329 (3) | 111 (4) |
O6—H6B···O14viii | 0.841 (14) | 1.815 (15) | 2.656 (3) | 178 (5) |
O6—H6A···O8viii | 0.837 (14) | 1.836 (15) | 2.672 (3) | 177 (4) |
O14—H14A···Cl2ix | 0.836 (14) | 2.343 (17) | 3.169 (2) | 170 (5) |
O14—H14B···O11ix | 0.837 (15) | 2.12 (3) | 2.892 (3) | 153 (4) |
O14—H14B···Cl1 | 0.837 (15) | 2.83 (4) | 3.345 (2) | 122 (4) |
O13—H13B···O14 | 0.843 (15) | 1.942 (15) | 2.785 (4) | 177 (5) |
O15—H15B···Cl1viii | 0.840 (14) | 2.326 (15) | 3.165 (2) | 178 (4) |
O10—H10B···Cl1iv | 0.840 (14) | 2.37 (2) | 3.172 (2) | 159 (5) |
O7—H7B···Cl2x | 0.838 (14) | 2.326 (15) | 3.164 (2) | 177 (4) |
O11—H11B···O10 | 0.840 (14) | 2.008 (19) | 2.822 (4) | 163 (4) |
O3—H3B···O7ii | 0.832 (14) | 1.854 (15) | 2.686 (3) | 178 (5) |
O3—H3A···O11viii | 0.840 (14) | 1.837 (16) | 2.673 (3) | 174 (6) |
O1—H1A···O9x | 0.839 (14) | 1.836 (15) | 2.671 (3) | 174 (5) |
O5—H5A···O13 | 0.835 (14) | 1.803 (15) | 2.635 (3) | 175 (4) |
O5—H5B···O15 | 0.839 (15) | 1.808 (15) | 2.646 (3) | 176 (6) |
O4—H4B···O12 | 0.837 (14) | 1.78 (2) | 2.605 (3) | 166 (6) |
O4—H4A···O8 | 0.833 (14) | 1.847 (16) | 2.676 (3) | 173 (5) |
O8—H8A···Cl2 | 0.836 (14) | 2.320 (17) | 3.147 (2) | 171 (5) |
O8—H8B···Cl1v | 0.841 (14) | 2.30 (2) | 3.102 (2) | 159 (5) |
O2—H2B···O10 | 0.837 (14) | 1.815 (16) | 2.646 (3) | 171 (5) |
O2—H2A···O9xi | 0.837 (15) | 1.828 (15) | 2.663 (3) | 175 (6) |
O7—H7A···Cl3 | 0.836 (14) | 2.47 (3) | 3.236 (2) | 153 (4) |
O15—H15A···O7 | 0.833 (14) | 2.020 (15) | 2.850 (3) | 174 (4) |
O1—H1B···Cl3 | 0.838 (14) | 2.154 (16) | 2.986 (2) | 171 (4) |
O12—H12B···Cl3i | 0.839 (14) | 2.362 (15) | 3.200 (2) | 177 (5) |
O12—H12A···O15ii | 0.837 (14) | 2.13 (4) | 2.826 (3) | 141 (5) |
O11—H11A···Cl3iii | 0.840 (15) | 2.79 (3) | 3.535 (3) | 149 (5) |
O10—H10A···O13iv | 0.834 (15) | 2.14 (3) | 2.897 (3) | 151 (6) |
O10—H10A···Cl2 | 0.834 (15) | 2.86 (5) | 3.416 (2) | 126 (5) |
O9—H9B···Cl2 | 0.841 (14) | 2.275 (18) | 3.108 (2) | 171 (6) |
O9—H9A···Cl1v | 0.841 (14) | 2.256 (17) | 3.090 (2) | 172 (5) |
O13—H13A···Cl3vi | 0.842 (14) | 2.71 (5) | 3.284 (3) | 127 (5) |
O13—H13A···Cl2vii | 0.842 (14) | 2.93 (5) | 3.329 (3) | 111 (4) |
O6—H6B···O14viii | 0.841 (14) | 1.815 (15) | 2.656 (3) | 178 (5) |
O6—H6A···O8viii | 0.837 (14) | 1.836 (15) | 2.672 (3) | 177 (4) |
O14—H14A···Cl2ix | 0.836 (14) | 2.343 (17) | 3.169 (2) | 170 (5) |
O14—H14B···O11ix | 0.837 (15) | 2.12 (3) | 2.892 (3) | 153 (4) |
O14—H14B···Cl1 | 0.837 (15) | 2.83 (4) | 3.345 (2) | 122 (4) |
O13—H13B···O14 | 0.843 (15) | 1.942 (15) | 2.785 (4) | 177 (5) |
O15—H15B···Cl1viii | 0.840 (14) | 2.326 (15) | 3.165 (2) | 178 (4) |
O10—H10B···Cl1iv | 0.840 (14) | 2.37 (2) | 3.172 (2) | 159 (5) |
O7—H7B···Cl2x | 0.838 (14) | 2.326 (15) | 3.164 (2) | 177 (4) |
O11—H11B···O10 | 0.840 (14) | 2.008 (19) | 2.822 (4) | 163 (4) |
O3—H3B···O7ii | 0.832 (14) | 1.854 (15) | 2.686 (3) | 178 (5) |
O3—H3A···O11viii | 0.840 (14) | 1.837 (16) | 2.673 (3) | 174 (6) |
O1—H1A···O9x | 0.839 (14) | 1.836 (15) | 2.671 (3) | 174 (5) |
O5—H5A···O13 | 0.835 (14) | 1.803 (15) | 2.635 (3) | 175 (4) |
O5—H5B···O15 | 0.839 (15) | 1.808 (15) | 2.646 (3) | 176 (6) |
O4—H4B···O12 | 0.837 (14) | 1.78 (2) | 2.605 (3) | 166 (6) |
O4—H4A···O8 | 0.833 (14) | 1.847 (16) | 2.676 (3) | 173 (5) |
O8—H8A···Cl2 | 0.836 (14) | 2.320 (17) | 3.147 (2) | 171 (5) |
O8—H8B···Cl1v | 0.841 (14) | 2.30 (2) | 3.102 (2) | 159 (5) |
O2—H2B···O10 | 0.837 (14) | 1.815 (16) | 2.646 (3) | 171 (5) |
O2—H2A···O9xi | 0.837 (15) | 1.828 (15) | 2.663 (3) | 175 (6) |
O2—H2A···O9xi | 0.837 (15) | 1.828 (15) | 2.663 (3) | 175 (6) |
O2—H2B···O10 | 0.837 (14) | 1.815 (16) | 2.646 (3) | 171 (5) |
O8—H8B···Cl1v | 0.841 (14) | 2.30 (2) | 3.102 (2) | 159 (5) |
O8—H8A···Cl2 | 0.836 (14) | 2.320 (17) | 3.147 (2) | 171 (5) |
O4—H4A···O8 | 0.833 (14) | 1.847 (16) | 2.676 (3) | 173 (5) |
O4—H4B···O12 | 0.837 (14) | 1.78 (2) | 2.605 (3) | 166 (6) |
O5—H5B···O15 | 0.839 (15) | 1.808 (15) | 2.646 (3) | 176 (6) |
O5—H5A···O13 | 0.835 (14) | 1.803 (15) | 2.635 (3) | 175 (4) |
O1—H1A···O9x | 0.839 (14) | 1.836 (15) | 2.671 (3) | 174 (5) |
O3—H3A···O11viii | 0.840 (14) | 1.837 (16) | 2.673 (3) | 174 (6) |
O3—H3B···O7ii | 0.832 (14) | 1.854 (15) | 2.686 (3) | 178 (5) |
O11—H11B···O10 | 0.840 (14) | 2.008 (19) | 2.822 (4) | 163 (4) |
O7—H7B···Cl2x | 0.838 (14) | 2.326 (15) | 3.164 (2) | 177 (4) |
O10—H10B···Cl1iv | 0.840 (14) | 2.37 (2) | 3.172 (2) | 159 (5) |
O15—H15B···Cl1viii | 0.840 (14) | 2.326 (15) | 3.165 (2) | 178 (4) |
O13—H13B···O14 | 0.843 (15) | 1.942 (15) | 2.785 (4) | 177 (5) |
O14—H14B···Cl1 | 0.837 (15) | 2.83 (4) | 3.345 (2) | 122 (4) |
O14—H14B···O11ix | 0.837 (15) | 2.12 (3) | 2.892 (3) | 153 (4) |
O14—H14A···Cl2ix | 0.836 (14) | 2.343 (17) | 3.169 (2) | 170 (5) |
O6—H6A···O8viii | 0.837 (14) | 1.836 (15) | 2.672 (3) | 177 (4) |
O6—H6B···O14viii | 0.841 (14) | 1.815 (15) | 2.656 (3) | 178 (5) |
O13—H13A···Cl2vii | 0.842 (14) | 2.93 (5) | 3.329 (3) | 111 (4) |
O13—H13A···Cl3vi | 0.842 (14) | 2.71 (5) | 3.284 (3) | 127 (5) |
O9—H9A···Cl1v | 0.841 (14) | 2.256 (17) | 3.090 (2) | 172 (5) |
O9—H9B···Cl2 | 0.841 (14) | 2.275 (18) | 3.108 (2) | 171 (6) |
O10—H10A···Cl2 | 0.834 (15) | 2.86 (5) | 3.416 (2) | 126 (5) |
O10—H10A···O13iv | 0.834 (15) | 2.14 (3) | 2.897 (3) | 151 (6) |
O11—H11A···Cl3iii | 0.840 (15) | 2.79 (3) | 3.535 (3) | 149 (5) |
O12—H12A···O15ii | 0.837 (14) | 2.13 (4) | 2.826 (3) | 141 (5) |
O12—H12B···Cl3i | 0.839 (14) | 2.362 (15) | 3.200 (2) | 177 (5) |
O1—H1B···Cl3 | 0.838 (14) | 2.154 (16) | 2.986 (2) | 171 (4) |
O15—H15A···O7 | 0.833 (14) | 2.020 (15) | 2.850 (3) | 174 (4) |
O7—H7A···Cl3 | 0.836 (14) | 2.47 (3) | 3.236 (2) | 153 (4) |
O2—H2A···O9xi | 0.837 (15) | 1.828 (15) | 2.663 (3) | 175 (6) |
O2—H2B···O10 | 0.837 (14) | 1.815 (16) | 2.646 (3) | 171 (5) |
O8—H8B···Cl1v | 0.841 (14) | 2.30 (2) | 3.102 (2) | 159 (5) |
O8—H8A···Cl2 | 0.836 (14) | 2.320 (17) | 3.147 (2) | 171 (5) |
O4—H4A···O8 | 0.833 (14) | 1.847 (16) | 2.676 (3) | 173 (5) |
O4—H4B···O12 | 0.837 (14) | 1.78 (2) | 2.605 (3) | 166 (6) |
O5—H5B···O15 | 0.839 (15) | 1.808 (15) | 2.646 (3) | 176 (6) |
O5—H5A···O13 | 0.835 (14) | 1.803 (15) | 2.635 (3) | 175 (4) |
O1—H1A···O9x | 0.839 (14) | 1.836 (15) | 2.671 (3) | 174 (5) |
O3—H3A···O11viii | 0.840 (14) | 1.837 (16) | 2.673 (3) | 174 (6) |
O3—H3B···O7ii | 0.832 (14) | 1.854 (15) | 2.686 (3) | 178 (5) |
O11—H11B···O10 | 0.840 (14) | 2.008 (19) | 2.822 (4) | 163 (4) |
O7—H7B···Cl2x | 0.838 (14) | 2.326 (15) | 3.164 (2) | 177 (4) |
O10—H10B···Cl1iv | 0.840 (14) | 2.37 (2) | 3.172 (2) | 159 (5) |
O15—H15B···Cl1viii | 0.840 (14) | 2.326 (15) | 3.165 (2) | 178 (4) |
O13—H13B···O14 | 0.843 (15) | 1.942 (15) | 2.785 (4) | 177 (5) |
O14—H14B···Cl1 | 0.837 (15) | 2.83 (4) | 3.345 (2) | 122 (4) |
O14—H14B···O11ix | 0.837 (15) | 2.12 (3) | 2.892 (3) | 153 (4) |
O14—H14A···Cl2ix | 0.836 (14) | 2.343 (17) | 3.169 (2) | 170 (5) |
O6—H6A···O8viii | 0.837 (14) | 1.836 (15) | 2.672 (3) | 177 (4) |
O6—H6B···O14viii | 0.841 (14) | 1.815 (15) | 2.656 (3) | 178 (5) |
O13—H13A···Cl2vii | 0.842 (14) | 2.93 (5) | 3.329 (3) | 111 (4) |
O13—H13A···Cl3vi | 0.842 (14) | 2.71 (5) | 3.284 (3) | 127 (5) |
O9—H9A···Cl1v | 0.841 (14) | 2.256 (17) | 3.090 (2) | 172 (5) |
O9—H9B···Cl2 | 0.841 (14) | 2.275 (18) | 3.108 (2) | 171 (6) |
O10—H10A···Cl2 | 0.834 (15) | 2.86 (5) | 3.416 (2) | 126 (5) |
O10—H10A···O13iv | 0.834 (15) | 2.14 (3) | 2.897 (3) | 151 (6) |
O11—H11A···Cl3iii | 0.840 (15) | 2.79 (3) | 3.535 (3) | 149 (5) |
O12—H12A···O15ii | 0.837 (14) | 2.13 (4) | 2.826 (3) | 141 (5) |
O12—H12B···Cl3i | 0.839 (14) | 2.362 (15) | 3.200 (2) | 177 (5) |
O1—H1B···Cl3 | 0.838 (14) | 2.154 (16) | 2.986 (2) | 171 (4) |
O15—H15A···O7 | 0.833 (14) | 2.020 (15) | 2.850 (3) | 174 (4) |
O7—H7A···Cl3 | 0.836 (14) | 2.47 (3) | 3.236 (2) | 153 (4) |
O2—H2A···O9xi | 0.837 (15) | 1.828 (15) | 2.663 (3) | 175 (6) |
O2—H2B···O10 | 0.837 (14) | 1.815 (16) | 2.646 (3) | 171 (5) |
O8—H8B···Cl1v | 0.841 (14) | 2.30 (2) | 3.102 (2) | 159 (5) |
O8—H8A···Cl2 | 0.836 (14) | 2.320 (17) | 3.147 (2) | 171 (5) |
O4—H4A···O8 | 0.833 (14) | 1.847 (16) | 2.676 (3) | 173 (5) |
O4—H4B···O12 | 0.837 (14) | 1.78 (2) | 2.605 (3) | 166 (6) |
O5—H5B···O15 | 0.839 (15) | 1.808 (15) | 2.646 (3) | 176 (6) |
O5—H5A···O13 | 0.835 (14) | 1.803 (15) | 2.635 (3) | 175 (4) |
O1—H1A···O9x | 0.839 (14) | 1.836 (15) | 2.671 (3) | 174 (5) |
O3—H3A···O11viii | 0.840 (14) | 1.837 (16) | 2.673 (3) | 174 (6) |
O3—H3B···O7ii | 0.832 (14) | 1.854 (15) | 2.686 (3) | 178 (5) |
O11—H11B···O10 | 0.840 (14) | 2.008 (19) | 2.822 (4) | 163 (4) |
O7—H7B···Cl2x | 0.838 (14) | 2.326 (15) | 3.164 (2) | 177 (4) |
O10—H10B···Cl1iv | 0.840 (14) | 2.37 (2) | 3.172 (2) | 159 (5) |
O15—H15B···Cl1viii | 0.840 (14) | 2.326 (15) | 3.165 (2) | 178 (4) |
O13—H13B···O14 | 0.843 (15) | 1.942 (15) | 2.785 (4) | 177 (5) |
O14—H14B···Cl1 | 0.837 (15) | 2.83 (4) | 3.345 (2) | 122 (4) |
O14—H14B···O11ix | 0.837 (15) | 2.12 (3) | 2.892 (3) | 153 (4) |
O14—H14A···Cl2ix | 0.836 (14) | 2.343 (17) | 3.169 (2) | 170 (5) |
O6—H6A···O8viii | 0.837 (14) | 1.836 (15) | 2.672 (3) | 177 (4) |
O6—H6B···O14viii | 0.841 (14) | 1.815 (15) | 2.656 (3) | 178 (5) |
O13—H13A···Cl2vii | 0.842 (14) | 2.93 (5) | 3.329 (3) | 111 (4) |
O13—H13A···Cl3vi | 0.842 (14) | 2.71 (5) | 3.284 (3) | 127 (5) |
O9—H9A···Cl1v | 0.841 (14) | 2.256 (17) | 3.090 (2) | 172 (5) |
O9—H9B···Cl2 | 0.841 (14) | 2.275 (18) | 3.108 (2) | 171 (6) |
O10—H10A···Cl2 | 0.834 (15) | 2.86 (5) | 3.416 (2) | 126 (5) |
O10—H10A···O13iv | 0.834 (15) | 2.14 (3) | 2.897 (3) | 151 (6) |
O11—H11A···Cl3iii | 0.840 (15) | 2.79 (3) | 3.535 (3) | 149 (5) |
O12—H12A···O15ii | 0.837 (14) | 2.13 (4) | 2.826 (3) | 141 (5) |
O12—H12B···Cl3i | 0.839 (14) | 2.362 (15) | 3.200 (2) | 177 (5) |
O1—H1B···Cl3 | 0.838 (14) | 2.154 (16) | 2.986 (2) | 171 (4) |
O15—H15A···O7 | 0.833 (14) | 2.020 (15) | 2.850 (3) | 174 (4) |
O7—H7A···Cl3 | 0.836 (14) | 2.47 (3) | 3.236 (2) | 153 (4) |
Symmetry codes: (i) x−1/2, y−1/2, z; (ii) x−1/2, −y+1/2, z−1/2; (iii) x, y+1, z; (iv) x, −y+1, z−1/2; (v) x−1/2, −y+3/2, z−1/2; (vi) x−1/2, y+1/2, z; (vii) x, −y+1, z+1/2; (viii) x, y−1, z; (ix) x, −y+2, z+1/2; (x) x+1/2, −y+1/2, z+1/2; (xi) x+1/2, −y+3/2, z+1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5A···O15 | 0.839 (14) | 1.79 (4) | 2.618 (15) | 169 (15) |
O5—H5B···O13 | 0.839 (14) | 1.83 (6) | 2.625 (14) | 159 (16) |
O3—H3A···O7i | 0.840 (14) | 1.85 (6) | 2.662 (15) | 162 (18) |
O3—H3B···O11ii | 0.839 (14) | 1.87 (4) | 2.701 (14) | 168 (15) |
O1—H1A···O9iii | 0.839 (15) | 1.83 (2) | 2.664 (12) | 177 (15) |
O1—H1B···Br3 | 0.840 (14) | 2.38 (9) | 3.130 (9) | 148 (14) |
O2—H2A···O9iv | 0.840 (14) | 1.84 (5) | 2.653 (14) | 162 (15) |
O2—H2B···O10 | 0.841 (14) | 1.83 (5) | 2.654 (13) | 164 (16) |
O4—H4A···O12 | 0.840 (14) | 1.79 (6) | 2.599 (15) | 161 (17) |
O4—H4B···O8 | 0.839 (14) | 1.93 (10) | 2.679 (12) | 148 (17) |
O6—H6A···O14ii | 0.841 (14) | 1.81 (5) | 2.631 (13) | 164 (17) |
O6—H6B···O8ii | 0.839 (15) | 1.99 (11) | 2.700 (14) | 141 (15) |
O9—H9A···Br1v | 0.841 (14) | 2.39 (4) | 3.210 (11) | 166 (15) |
O9—H9B···Br2 | 0.841 (15) | 2.63 (13) | 3.258 (12) | 133 (15) |
O8—H8A···Br1v | 0.841 (14) | 2.47 (9) | 3.232 (12) | 151 (16) |
O8—H8B···Br2 | 0.840 (14) | 2.46 (6) | 3.267 (13) | 162 (17) |
O7—H7A···Br3 | 0.840 (14) | 2.75 (17) | 3.352 (13) | 130 (19) |
O7—H7B···Br2iii | 0.839 (14) | 2.53 (8) | 3.296 (10) | 152 (14) |
O14—H14A···Br2vi | 0.841 (14) | 2.48 (3) | 3.312 (11) | 170 (15) |
O14—H14B···Br1 | 0.839 (14) | 2.82 (13) | 3.398 (11) | 127 (13) |
O14—H14B···O11vi | 0.839 (14) | 2.22 (11) | 2.916 (16) | 140 (14) |
O13—H13A···Br3vii | 0.840 (15) | 2.91 (14) | 3.468 (12) | 125 (13) |
O13—H13B···O14 | 0.840 (14) | 1.97 (3) | 2.807 (17) | 174 (18) |
O10—H10A···Br2 | 0.840 (15) | 2.95 (13) | 3.526 (11) | 128 (13) |
O10—H10A···O13viii | 0.840 (15) | 2.14 (8) | 2.895 (14) | 150 (14) |
O10—H10B···Br1viii | 0.841 (14) | 2.48 (5) | 3.294 (10) | 162 (14) |
O11—H11A···O10 | 0.840 (15) | 2.03 (7) | 2.828 (17) | 159 (17) |
O11—H11B···Br3ix | 0.839 (14) | 2.94 (5) | 3.757 (11) | 166 (15) |
O12—H12A···Br1i | 0.840 (15) | 3.11 (12) | 3.830 (13) | 145 (17) |
O12—H12A···O15i | 0.840 (15) | 2.21 (15) | 2.837 (17) | 132 (17) |
O12—H12B···Br3x | 0.839 (14) | 2.91 (19) | 3.316 (12) | 112 (16) |
O15—H15B···Br1ii | 0.841 (14) | 2.45 (4) | 3.272 (11) | 165 (14) |
O15—H15A···O7 | 0.840 (14) | 2.01 (4) | 2.835 (16) | 169 (16) |
Symmetry codes: (i) x+1/2, −y+3/2, z+1/2; (ii) x, y+1, z; (iii) x−1/2, −y+3/2, z−1/2; (iv) x−1/2, −y+1/2, z−1/2; (v) x+1/2, −y+1/2, z+1/2; (vi) x, −y, z−1/2; (vii) x+1/2, y−1/2, z; (viii) x, −y+1, z+1/2; (ix) x, y−1, z; (x) x+1/2, y+1/2, z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O14A—H14D···O8A | 0.817 (10) | 2.36 (4) | 2.976 (6) | 133 (5) |
O14A—H14C···I3Ai | 0.817 (10) | 3.07 (3) | 3.738 (7) | 140 (3) |
O8A—H8D···I3Aii | 0.817 (10) | 2.582 (11) | 3.391 (3) | 170.7 (19) |
O14—H14B···O15iii | 0.817 (10) | 2.240 (12) | 3.048 (4) | 170 (3) |
O8—H8B···O14 | 0.817 (10) | 2.089 (19) | 2.808 (4) | 147 (3) |
O8—H8B···I3i | 0.817 (10) | 3.24 (2) | 3.741 (3) | 122 (2) |
O8—H8A···I3ii | 0.817 (10) | 2.797 (11) | 3.610 (3) | 173 (2) |
O15—H15B···I2iii | 0.837 (10) | 2.744 (14) | 3.5496 (17) | 162 (3) |
O15—H15A···I2iv | 0.831 (10) | 3.24 (3) | 3.6429 (17) | 113 (3) |
O15—H15A···I1v | 0.831 (10) | 2.879 (17) | 3.645 (2) | 154 (3) |
O11—H11B···O15 | 0.832 (10) | 2.48 (3) | 3.070 (3) | 128 (3) |
O11—H11B···I3Avi | 0.832 (10) | 2.90 (3) | 3.505 (4) | 131 (3) |
O11—H11B···I3vi | 0.832 (10) | 3.10 (3) | 3.699 (3) | 131 (3) |
O11—H11A···O12v | 0.834 (10) | 2.136 (18) | 2.917 (3) | 156 (3) |
O12—H12B···I2 | 0.827 (10) | 2.87 (2) | 3.615 (2) | 151 (3) |
O12—H12B···I1i | 0.827 (10) | 3.28 (3) | 3.6691 (19) | 112 (3) |
O12—H12A···I1vii | 0.832 (10) | 2.685 (12) | 3.5072 (19) | 170 (3) |
O13—H13A···I3Aviii | 0.837 (10) | 2.651 (13) | 3.474 (4) | 169 (3) |
O13—H13A···I3viii | 0.837 (10) | 2.639 (11) | 3.470 (3) | 173 (3) |
O13—H13B···I3Aix | 0.841 (10) | 2.738 (15) | 3.541 (4) | 160 (3) |
O13—H13B···I3ix | 0.841 (10) | 2.716 (14) | 3.529 (3) | 163 (3) |
O9—H9B···I2x | 0.832 (10) | 2.92 (2) | 3.5840 (18) | 138 (3) |
O9—H9B···I1i | 0.832 (10) | 3.29 (3) | 3.8162 (18) | 124 (2) |
O9—H9A···O10xi | 0.842 (10) | 1.950 (11) | 2.789 (3) | 175 (3) |
O10—H10A···I2xi | 0.836 (10) | 2.95 (2) | 3.6308 (18) | 140 (3) |
O10—H10A···I1viii | 0.836 (10) | 3.06 (3) | 3.6067 (18) | 125 (3) |
O10—H10B···O9xii | 0.838 (10) | 1.959 (12) | 2.782 (3) | 167 (3) |
O7—H7B···I2iii | 0.834 (10) | 2.695 (13) | 3.5103 (19) | 166 (3) |
O7—H7A···I1xiii | 0.837 (10) | 2.783 (16) | 3.5668 (19) | 157 (3) |
O4—H4B···O12xi | 0.834 (10) | 1.780 (10) | 2.614 (3) | 179 (4) |
O4—H4A···O13 | 0.843 (10) | 1.855 (12) | 2.691 (3) | 171 (3) |
O6—H6B···O14Axi | 0.833 (10) | 1.687 (15) | 2.491 (6) | 161 (3) |
O6—H6B···O14xi | 0.833 (10) | 1.892 (12) | 2.716 (4) | 170 (3) |
O6—H6A···O13x | 0.837 (10) | 1.893 (11) | 2.727 (3) | 175 (4) |
O5—H5A···O8xiv | 0.836 (10) | 1.820 (12) | 2.644 (3) | 169 (3) |
O5—H5B···I1xv | 0.839 (10) | 2.631 (12) | 3.4596 (17) | 169 (3) |
O1—H1A···O9xvi | 0.839 (10) | 1.846 (11) | 2.681 (2) | 174 (3) |
O1—H1B···O15 | 0.832 (10) | 1.850 (11) | 2.676 (3) | 172 (3) |
O3—H3B···O11 | 0.839 (10) | 1.750 (10) | 2.587 (2) | 176 (3) |
O3—H3A···O7 | 0.838 (10) | 1.891 (11) | 2.726 (2) | 174 (3) |
O2—H2A···O7vi | 0.843 (10) | 1.880 (11) | 2.718 (2) | 172 (3) |
O2—H2B···O10xi | 0.837 (10) | 1.811 (10) | 2.646 (2) | 176 (3) |
O14A—H14D···O8A | 0.817 (10) | 2.36 (4) | 2.976 (6) | 133 (5) |
O14A—H14C···I3Ai | 0.817 (10) | 3.07 (3) | 3.738 (7) | 140 (3) |
O8A—H8D···I3Aii | 0.817 (10) | 2.582 (11) | 3.391 (3) | 170.7 (19) |
O14—H14B···O15iii | 0.817 (10) | 2.240 (12) | 3.048 (4) | 170 (3) |
O8—H8B···O14 | 0.817 (10) | 2.089 (19) | 2.808 (4) | 147 (3) |
O8—H8B···I3i | 0.817 (10) | 3.24 (2) | 3.741 (3) | 122 (2) |
O8—H8A···I3ii | 0.817 (10) | 2.797 (11) | 3.610 (3) | 173 (2) |
O15—H15B···I2iii | 0.837 (10) | 2.744 (14) | 3.5496 (17) | 162 (3) |
O15—H15A···I2iv | 0.831 (10) | 3.24 (3) | 3.6429 (17) | 113 (3) |
O15—H15A···I1v | 0.831 (10) | 2.879 (17) | 3.645 (2) | 154 (3) |
O11—H11B···O15 | 0.832 (10) | 2.48 (3) | 3.070 (3) | 128 (3) |
O11—H11B···I3Avi | 0.832 (10) | 2.90 (3) | 3.505 (4) | 131 (3) |
O11—H11B···I3vi | 0.832 (10) | 3.10 (3) | 3.699 (3) | 131 (3) |
O11—H11A···O12v | 0.834 (10) | 2.136 (18) | 2.917 (3) | 156 (3) |
O12—H12B···I2 | 0.827 (10) | 2.87 (2) | 3.615 (2) | 151 (3) |
O12—H12B···I1i | 0.827 (10) | 3.28 (3) | 3.6691 (19) | 112 (3) |
O12—H12A···I1vii | 0.832 (10) | 2.685 (12) | 3.5072 (19) | 170 (3) |
O13—H13A···I3Aviii | 0.837 (10) | 2.651 (13) | 3.474 (4) | 169 (3) |
O13—H13A···I3viii | 0.837 (10) | 2.639 (11) | 3.470 (3) | 173 (3) |
O13—H13B···I3Aix | 0.841 (10) | 2.738 (15) | 3.541 (4) | 160 (3) |
O13—H13B···I3ix | 0.841 (10) | 2.716 (14) | 3.529 (3) | 163 (3) |
O9—H9B···I2x | 0.832 (10) | 2.92 (2) | 3.5840 (18) | 138 (3) |
O9—H9B···I1i | 0.832 (10) | 3.29 (3) | 3.8162 (18) | 124 (2) |
O9—H9A···O10xi | 0.842 (10) | 1.950 (11) | 2.789 (3) | 175 (3) |
O10—H10A···I2xi | 0.836 (10) | 2.95 (2) | 3.6308 (18) | 140 (3) |
O10—H10A···I1viii | 0.836 (10) | 3.06 (3) | 3.6067 (18) | 125 (3) |
O10—H10B···O9xii | 0.838 (10) | 1.959 (12) | 2.782 (3) | 167 (3) |
O7—H7B···I2iii | 0.834 (10) | 2.695 (13) | 3.5103 (19) | 166 (3) |
O7—H7A···I1xiii | 0.837 (10) | 2.783 (16) | 3.5668 (19) | 157 (3) |
O4—H4B···O12xi | 0.834 (10) | 1.780 (10) | 2.614 (3) | 179 (4) |
O4—H4A···O13 | 0.843 (10) | 1.855 (12) | 2.691 (3) | 171 (3) |
O6—H6B···O14Axi | 0.833 (10) | 1.687 (15) | 2.491 (6) | 161 (3) |
O6—H6B···O14xi | 0.833 (10) | 1.892 (12) | 2.716 (4) | 170 (3) |
O6—H6A···O13x | 0.837 (10) | 1.893 (11) | 2.727 (3) | 175 (4) |
O5—H5A···O8xiv | 0.836 (10) | 1.820 (12) | 2.644 (3) | 169 (3) |
O5—H5B···I1xv | 0.839 (10) | 2.631 (12) | 3.4596 (17) | 169 (3) |
O1—H1A···O9xvi | 0.839 (10) | 1.846 (11) | 2.681 (2) | 174 (3) |
O1—H1B···O15 | 0.832 (10) | 1.850 (11) | 2.676 (3) | 172 (3) |
O3—H3B···O11 | 0.839 (10) | 1.750 (10) | 2.587 (2) | 176 (3) |
O3—H3A···O7 | 0.838 (10) | 1.891 (11) | 2.726 (2) | 174 (3) |
O2—H2A···O7vi | 0.843 (10) | 1.880 (11) | 2.718 (2) | 172 (3) |
O2—H2B···O10xi | 0.837 (10) | 1.811 (10) | 2.646 (2) | 176 (3) |
O14A—H14D···O8A | 0.817 (10) | 2.36 (4) | 2.976 (6) | 133 (5) |
O14A—H14C···I3Ai | 0.817 (10) | 3.07 (3) | 3.738 (7) | 140 (3) |
O8A—H8D···I3Aii | 0.817 (10) | 2.582 (11) | 3.391 (3) | 170.7 (19) |
O14—H14B···O15iii | 0.817 (10) | 2.240 (12) | 3.048 (4) | 170 (3) |
O8—H8B···O14 | 0.817 (10) | 2.089 (19) | 2.808 (4) | 147 (3) |
O8—H8B···I3i | 0.817 (10) | 3.24 (2) | 3.741 (3) | 122 (2) |
O8—H8A···I3ii | 0.817 (10) | 2.797 (11) | 3.610 (3) | 173 (2) |
O15—H15B···I2iii | 0.837 (10) | 2.744 (14) | 3.5496 (17) | 162 (3) |
O15—H15A···I2iv | 0.831 (10) | 3.24 (3) | 3.6429 (17) | 113 (3) |
O15—H15A···I1v | 0.831 (10) | 2.879 (17) | 3.645 (2) | 154 (3) |
O11—H11B···O15 | 0.832 (10) | 2.48 (3) | 3.070 (3) | 128 (3) |
O11—H11B···I3Avi | 0.832 (10) | 2.90 (3) | 3.505 (4) | 131 (3) |
O11—H11B···I3vi | 0.832 (10) | 3.10 (3) | 3.699 (3) | 131 (3) |
O11—H11A···O12v | 0.834 (10) | 2.136 (18) | 2.917 (3) | 156 (3) |
O12—H12B···I2 | 0.827 (10) | 2.87 (2) | 3.615 (2) | 151 (3) |
O12—H12B···I1i | 0.827 (10) | 3.28 (3) | 3.6691 (19) | 112 (3) |
O12—H12A···I1vii | 0.832 (10) | 2.685 (12) | 3.5072 (19) | 170 (3) |
O13—H13A···I3Aviii | 0.837 (10) | 2.651 (13) | 3.474 (4) | 169 (3) |
O13—H13A···I3viii | 0.837 (10) | 2.639 (11) | 3.470 (3) | 173 (3) |
O13—H13B···I3Aix | 0.841 (10) | 2.738 (15) | 3.541 (4) | 160 (3) |
O13—H13B···I3ix | 0.841 (10) | 2.716 (14) | 3.529 (3) | 163 (3) |
O9—H9B···I2x | 0.832 (10) | 2.92 (2) | 3.5840 (18) | 138 (3) |
O9—H9B···I1i | 0.832 (10) | 3.29 (3) | 3.8162 (18) | 124 (2) |
O9—H9A···O10xi | 0.842 (10) | 1.950 (11) | 2.789 (3) | 175 (3) |
O10—H10A···I2xi | 0.836 (10) | 2.95 (2) | 3.6308 (18) | 140 (3) |
O10—H10A···I1viii | 0.836 (10) | 3.06 (3) | 3.6067 (18) | 125 (3) |
O10—H10B···O9xii | 0.838 (10) | 1.959 (12) | 2.782 (3) | 167 (3) |
O7—H7B···I2iii | 0.834 (10) | 2.695 (13) | 3.5103 (19) | 166 (3) |
O7—H7A···I1xiii | 0.837 (10) | 2.783 (16) | 3.5668 (19) | 157 (3) |
O4—H4B···O12xi | 0.834 (10) | 1.780 (10) | 2.614 (3) | 179 (4) |
O4—H4A···O13 | 0.843 (10) | 1.855 (12) | 2.691 (3) | 171 (3) |
O6—H6B···O14Axi | 0.833 (10) | 1.687 (15) | 2.491 (6) | 161 (3) |
O6—H6B···O14xi | 0.833 (10) | 1.892 (12) | 2.716 (4) | 170 (3) |
O6—H6A···O13x | 0.837 (10) | 1.893 (11) | 2.727 (3) | 175 (4) |
O5—H5A···O8xiv | 0.836 (10) | 1.820 (12) | 2.644 (3) | 169 (3) |
O5—H5B···I1xv | 0.839 (10) | 2.631 (12) | 3.4596 (17) | 169 (3) |
O1—H1A···O9xvi | 0.839 (10) | 1.846 (11) | 2.681 (2) | 174 (3) |
O1—H1B···O15 | 0.832 (10) | 1.850 (11) | 2.676 (3) | 172 (3) |
O3—H3B···O11 | 0.839 (10) | 1.750 (10) | 2.587 (2) | 176 (3) |
O3—H3A···O7 | 0.838 (10) | 1.891 (11) | 2.726 (2) | 174 (3) |
O2—H2A···O7vi | 0.843 (10) | 1.880 (11) | 2.718 (2) | 172 (3) |
O2—H2B···O10xi | 0.837 (10) | 1.811 (10) | 2.646 (2) | 176 (3) |
O2—H2B···O10xi | 0.837 (10) | 1.811 (10) | 2.646 (2) | 176 (3) |
O2—H2A···O7vi | 0.843 (10) | 1.880 (11) | 2.718 (2) | 172 (3) |
O3—H3A···O7 | 0.838 (10) | 1.891 (11) | 2.726 (2) | 174 (3) |
O3—H3B···O11 | 0.839 (10) | 1.750 (10) | 2.587 (2) | 176 (3) |
O1—H1B···O15 | 0.832 (10) | 1.850 (11) | 2.676 (3) | 172 (3) |
O1—H1A···O9xvi | 0.839 (10) | 1.846 (11) | 2.681 (2) | 174 (3) |
O5—H5B···I1xv | 0.839 (10) | 2.631 (12) | 3.4596 (17) | 169 (3) |
O5—H5A···O8xiv | 0.836 (10) | 1.820 (12) | 2.644 (3) | 169 (3) |
O6—H6A···O13x | 0.837 (10) | 1.893 (11) | 2.727 (3) | 175 (4) |
O6—H6B···O14xi | 0.833 (10) | 1.892 (12) | 2.716 (4) | 170 (3) |
O6—H6B···O14Axi | 0.833 (10) | 1.687 (15) | 2.491 (6) | 161 (3) |
O4—H4A···O13 | 0.843 (10) | 1.855 (12) | 2.691 (3) | 171 (3) |
O4—H4B···O12xi | 0.834 (10) | 1.780 (10) | 2.614 (3) | 179 (4) |
O7—H7A···I1xiii | 0.837 (10) | 2.783 (16) | 3.5668 (19) | 157 (3) |
O7—H7B···I2iii | 0.834 (10) | 2.695 (13) | 3.5103 (19) | 166 (3) |
O10—H10B···O9xii | 0.838 (10) | 1.959 (12) | 2.782 (3) | 167 (3) |
O10—H10A···I1viii | 0.836 (10) | 3.06 (3) | 3.6067 (18) | 125 (3) |
O10—H10A···I2xi | 0.836 (10) | 2.95 (2) | 3.6308 (18) | 140 (3) |
O9—H9A···O10xi | 0.842 (10) | 1.950 (11) | 2.789 (3) | 175 (3) |
O9—H9B···I1i | 0.832 (10) | 3.29 (3) | 3.8162 (18) | 124 (2) |
O9—H9B···I2x | 0.832 (10) | 2.92 (2) | 3.5840 (18) | 138 (3) |
O13—H13B···I3ix | 0.841 (10) | 2.716 (14) | 3.529 (3) | 163 (3) |
O13—H13B···I3Aix | 0.841 (10) | 2.738 (15) | 3.541 (4) | 160 (3) |
O13—H13A···I3viii | 0.837 (10) | 2.639 (11) | 3.470 (3) | 173 (3) |
O13—H13A···I3Aviii | 0.837 (10) | 2.651 (13) | 3.474 (4) | 169 (3) |
O12—H12A···I1vii | 0.832 (10) | 2.685 (12) | 3.5072 (19) | 170 (3) |
O12—H12B···I1i | 0.827 (10) | 3.28 (3) | 3.6691 (19) | 112 (3) |
O12—H12B···I2 | 0.827 (10) | 2.87 (2) | 3.615 (2) | 151 (3) |
O11—H11A···O12v | 0.834 (10) | 2.136 (18) | 2.917 (3) | 156 (3) |
O11—H11B···I3vi | 0.832 (10) | 3.10 (3) | 3.699 (3) | 131 (3) |
O11—H11B···I3Avi | 0.832 (10) | 2.90 (3) | 3.505 (4) | 131 (3) |
O11—H11B···O15 | 0.832 (10) | 2.48 (3) | 3.070 (3) | 128 (3) |
O15—H15A···I1v | 0.831 (10) | 2.879 (17) | 3.645 (2) | 154 (3) |
O15—H15A···I2iv | 0.831 (10) | 3.24 (3) | 3.6429 (17) | 113 (3) |
O15—H15B···I2iii | 0.837 (10) | 2.744 (14) | 3.5496 (17) | 162 (3) |
O8—H8A···I3ii | 0.817 (10) | 2.797 (11) | 3.610 (3) | 173 (2) |
O8—H8B···I3i | 0.817 (10) | 3.24 (2) | 3.741 (3) | 122 (2) |
O8—H8B···O14 | 0.817 (10) | 2.089 (19) | 2.808 (4) | 147 (3) |
O14—H14B···O15iii | 0.817 (10) | 2.240 (12) | 3.048 (4) | 170 (3) |
O8A—H8D···I3Aii | 0.817 (10) | 2.582 (11) | 3.391 (3) | 170.7 (19) |
O14A—H14C···I3Ai | 0.817 (10) | 3.07 (3) | 3.738 (7) | 140 (3) |
O14A—H14D···O8A | 0.817 (10) | 2.36 (4) | 2.976 (6) | 133 (5) |
O2—H2B···O10xi | 0.837 (10) | 1.811 (10) | 2.646 (2) | 176 (3) |
O2—H2A···O7vi | 0.843 (10) | 1.880 (11) | 2.718 (2) | 172 (3) |
O3—H3A···O7 | 0.838 (10) | 1.891 (11) | 2.726 (2) | 174 (3) |
O3—H3B···O11 | 0.839 (10) | 1.750 (10) | 2.587 (2) | 176 (3) |
O1—H1B···O15 | 0.832 (10) | 1.850 (11) | 2.676 (3) | 172 (3) |
O1—H1A···O9xvi | 0.839 (10) | 1.846 (11) | 2.681 (2) | 174 (3) |
O5—H5B···I1xv | 0.839 (10) | 2.631 (12) | 3.4596 (17) | 169 (3) |
O5—H5A···O8xiv | 0.836 (10) | 1.820 (12) | 2.644 (3) | 169 (3) |
O6—H6A···O13x | 0.837 (10) | 1.893 (11) | 2.727 (3) | 175 (4) |
O6—H6B···O14xi | 0.833 (10) | 1.892 (12) | 2.716 (4) | 170 (3) |
O6—H6B···O14Axi | 0.833 (10) | 1.687 (15) | 2.491 (6) | 161 (3) |
O4—H4A···O13 | 0.843 (10) | 1.855 (12) | 2.691 (3) | 171 (3) |
O4—H4B···O12xi | 0.834 (10) | 1.780 (10) | 2.614 (3) | 179 (4) |
O7—H7A···I1xiii | 0.837 (10) | 2.783 (16) | 3.5668 (19) | 157 (3) |
O7—H7B···I2iii | 0.834 (10) | 2.695 (13) | 3.5103 (19) | 166 (3) |
O10—H10B···O9xii | 0.838 (10) | 1.959 (12) | 2.782 (3) | 167 (3) |
O10—H10A···I1viii | 0.836 (10) | 3.06 (3) | 3.6067 (18) | 125 (3) |
O10—H10A···I2xi | 0.836 (10) | 2.95 (2) | 3.6308 (18) | 140 (3) |
O9—H9A···O10xi | 0.842 (10) | 1.950 (11) | 2.789 (3) | 175 (3) |
O9—H9B···I1i | 0.832 (10) | 3.29 (3) | 3.8162 (18) | 124 (2) |
O9—H9B···I2x | 0.832 (10) | 2.92 (2) | 3.5840 (18) | 138 (3) |
O13—H13B···I3ix | 0.841 (10) | 2.716 (14) | 3.529 (3) | 163 (3) |
O13—H13B···I3Aix | 0.841 (10) | 2.738 (15) | 3.541 (4) | 160 (3) |
O13—H13A···I3viii | 0.837 (10) | 2.639 (11) | 3.470 (3) | 173 (3) |
O13—H13A···I3Aviii | 0.837 (10) | 2.651 (13) | 3.474 (4) | 169 (3) |
O12—H12A···I1vii | 0.832 (10) | 2.685 (12) | 3.5072 (19) | 170 (3) |
O12—H12B···I2 | 0.827 (10) | 2.87 (2) | 3.615 (2) | 151 (3) |
O11—H11A···O12v | 0.834 (10) | 2.136 (18) | 2.917 (3) | 156 (3) |
O11—H11B···I3vi | 0.832 (10) | 3.10 (3) | 3.699 (3) | 131 (3) |
O11—H11B···I3Avi | 0.832 (10) | 2.90 (3) | 3.505 (4) | 131 (3) |
O11—H11B···O15 | 0.832 (10) | 2.48 (3) | 3.070 (3) | 128 (3) |
O15—H15A···I1v | 0.831 (10) | 2.879 (17) | 3.645 (2) | 154 (3) |
O15—H15A···I2iv | 0.831 (10) | 3.24 (3) | 3.6429 (17) | 113 (3) |
O15—H15B···I2iii | 0.837 (10) | 2.744 (14) | 3.5496 (17) | 162 (3) |
O8—H8A···I3ii | 0.817 (10) | 2.797 (11) | 3.610 (3) | 173 (2) |
O8—H8B···I3i | 0.817 (10) | 3.24 (2) | 3.741 (3) | 122 (2) |
O8—H8B···O14 | 0.817 (10) | 2.089 (19) | 2.808 (4) | 147 (3) |
O14—H14B···O15iii | 0.817 (10) | 2.240 (12) | 3.048 (4) | 170 (3) |
O8A—H8D···I3Aii | 0.817 (10) | 2.582 (11) | 3.391 (3) | 170.7 (19) |
O14A—H14C···I3Ai | 0.817 (10) | 3.07 (3) | 3.738 (7) | 140 (3) |
O14A—H14D···O8A | 0.817 (10) | 2.36 (4) | 2.976 (6) | 133 (5) |
O2—H2B···O10xi | 0.837 (10) | 1.811 (10) | 2.646 (2) | 176 (3) |
O2—H2A···O7vi | 0.843 (10) | 1.880 (11) | 2.718 (2) | 172 (3) |
O3—H3A···O7 | 0.838 (10) | 1.891 (11) | 2.726 (2) | 174 (3) |
O3—H3B···O11 | 0.839 (10) | 1.750 (10) | 2.587 (2) | 176 (3) |
O1—H1B···O15 | 0.832 (10) | 1.850 (11) | 2.676 (3) | 172 (3) |
O1—H1A···O9xvi | 0.839 (10) | 1.846 (11) | 2.681 (2) | 174 (3) |
O5—H5B···I1xv | 0.839 (10) | 2.631 (12) | 3.4596 (17) | 169 (3) |
O5—H5A···O8xiv | 0.836 (10) | 1.820 (12) | 2.644 (3) | 169 (3) |
O6—H6A···O13x | 0.837 (10) | 1.893 (11) | 2.727 (3) | 175 (4) |
O6—H6B···O14xi | 0.833 (10) | 1.892 (12) | 2.716 (4) | 170 (3) |
O6—H6B···O14Axi | 0.833 (10) | 1.687 (15) | 2.491 (6) | 161 (3) |
O4—H4A···O13 | 0.843 (10) | 1.855 (12) | 2.691 (3) | 171 (3) |
O4—H4B···O12xi | 0.834 (10) | 1.780 (10) | 2.614 (3) | 179 (4) |
O7—H7A···I1xiii | 0.837 (10) | 2.783 (16) | 3.5668 (19) | 157 (3) |
O7—H7B···I2iii | 0.834 (10) | 2.695 (13) | 3.5103 (19) | 166 (3) |
O10—H10B···O9xii | 0.838 (10) | 1.959 (12) | 2.782 (3) | 167 (3) |
O10—H10A···I1viii | 0.836 (10) | 3.06 (3) | 3.6067 (18) | 125 (3) |
O10—H10A···I2xi | 0.836 (10) | 2.95 (2) | 3.6308 (18) | 140 (3) |
O9—H9A···O10xi | 0.842 (10) | 1.950 (11) | 2.789 (3) | 175 (3) |
O9—H9B···I1i | 0.832 (10) | 3.29 (3) | 3.8162 (18) | 124 (2) |
O9—H9B···I2x | 0.832 (10) | 2.92 (2) | 3.5840 (18) | 138 (3) |
O13—H13B···I3ix | 0.841 (10) | 2.716 (14) | 3.529 (3) | 163 (3) |
O13—H13B···I3Aix | 0.841 (10) | 2.738 (15) | 3.541 (4) | 160 (3) |
O13—H13A···I3viii | 0.837 (10) | 2.639 (11) | 3.470 (3) | 173 (3) |
O13—H13A···I3Aviii | 0.837 (10) | 2.651 (13) | 3.474 (4) | 169 (3) |
O12—H12A···I1vii | 0.832 (10) | 2.685 (12) | 3.5072 (19) | 170 (3) |
O12—H12B···I1i | 0.827 (10) | 3.28 (3) | 3.6691 (19) | 112 (3) |
O12—H12B···I2 | 0.827 (10) | 2.87 (2) | 3.615 (2) | 151 (3) |
O11—H11A···O12v | 0.834 (10) | 2.136 (18) | 2.917 (3) | 156 (3) |
O11—H11B···I3vi | 0.832 (10) | 3.10 (3) | 3.699 (3) | 131 (3) |
O11—H11B···I3Avi | 0.832 (10) | 2.90 (3) | 3.505 (4) | 131 (3) |
O11—H11B···O15 | 0.832 (10) | 2.48 (3) | 3.070 (3) | 128 (3) |
O15—H15A···I1v | 0.831 (10) | 2.879 (17) | 3.645 (2) | 154 (3) |
O15—H15A···I2iv | 0.831 (10) | 3.24 (3) | 3.6429 (17) | 113 (3) |
O15—H15B···I2iii | 0.837 (10) | 2.744 (14) | 3.5496 (17) | 162 (3) |
O8—H8A···I3ii | 0.817 (10) | 2.797 (11) | 3.610 (3) | 173 (2) |
O8—H8B···I3i | 0.817 (10) | 3.24 (2) | 3.741 (3) | 122 (2) |
O8—H8B···O14 | 0.817 (10) | 2.089 (19) | 2.808 (4) | 147 (3) |
O14—H14B···O15iii | 0.817 (10) | 2.240 (12) | 3.048 (4) | 170 (3) |
O8A—H8D···I3Aii | 0.817 (10) | 2.582 (11) | 3.391 (3) | 170.7 (19) |
O14A—H14C···I3Ai | 0.817 (10) | 3.07 (3) | 3.738 (7) | 140 (3) |
O14A—H14D···O8A | 0.817 (10) | 2.36 (4) | 2.976 (6) | 133 (5) |
O2—H2B···O10xi | 0.837 (10) | 1.811 (10) | 2.646 (2) | 176 (3) |
O2—H2A···O7vi | 0.843 (10) | 1.880 (11) | 2.718 (2) | 172 (3) |
O3—H3A···O7 | 0.838 (10) | 1.891 (11) | 2.726 (2) | 174 (3) |
O3—H3B···O11 | 0.839 (10) | 1.750 (10) | 2.587 (2) | 176 (3) |
O1—H1B···O15 | 0.832 (10) | 1.850 (11) | 2.676 (3) | 172 (3) |
O1—H1A···O9xvi | 0.839 (10) | 1.846 (11) | 2.681 (2) | 174 (3) |
O5—H5B···I1xv | 0.839 (10) | 2.631 (12) | 3.4596 (17) | 169 (3) |
O5—H5A···O8xiv | 0.836 (10) | 1.820 (12) | 2.644 (3) | 169 (3) |
O6—H6A···O13x | 0.837 (10) | 1.893 (11) | 2.727 (3) | 175 (4) |
O6—H6B···O14xi | 0.833 (10) | 1.892 (12) | 2.716 (4) | 170 (3) |
O6—H6B···O14Axi | 0.833 (10) | 1.687 (15) | 2.491 (6) | 161 (3) |
O4—H4A···O13 | 0.843 (10) | 1.855 (12) | 2.691 (3) | 171 (3) |
O4—H4B···O12xi | 0.834 (10) | 1.780 (10) | 2.614 (3) | 179 (4) |
O7—H7A···I1xiii | 0.837 (10) | 2.783 (16) | 3.5668 (19) | 157 (3) |
O7—H7B···I2iii | 0.834 (10) | 2.695 (13) | 3.5103 (19) | 166 (3) |
O10—H10B···O9xii | 0.838 (10) | 1.959 (12) | 2.782 (3) | 167 (3) |
O10—H10A···I1viii | 0.836 (10) | 3.06 (3) | 3.6067 (18) | 125 (3) |
O10—H10A···I2xi | 0.836 (10) | 2.95 (2) | 3.6308 (18) | 140 (3) |
O9—H9A···O10xi | 0.842 (10) | 1.950 (11) | 2.789 (3) | 175 (3) |
O9—H9B···I1i | 0.832 (10) | 3.29 (3) | 3.8162 (18) | 124 (2) |
O9—H9B···I2x | 0.832 (10) | 2.92 (2) | 3.5840 (18) | 138 (3) |
O13—H13B···I3ix | 0.841 (10) | 2.716 (14) | 3.529 (3) | 163 (3) |
O13—H13B···I3Aix | 0.841 (10) | 2.738 (15) | 3.541 (4) | 160 (3) |
O13—H13A···I3viii | 0.837 (10) | 2.639 (11) | 3.470 (3) | 173 (3) |
O13—H13A···I3Aviii | 0.837 (10) | 2.651 (13) | 3.474 (4) | 169 (3) |
O12—H12A···I1vii | 0.832 (10) | 2.685 (12) | 3.5072 (19) | 170 (3) |
O12—H12B···I1i | 0.827 (10) | 3.28 (3) | 3.6691 (19) | 112 (3) |
O12—H12B···I2 | 0.827 (10) | 2.87 (2) | 3.615 (2) | 151 (3) |
O11—H11A···O12v | 0.834 (10) | 2.136 (18) | 2.917 (3) | 156 (3) |
O11—H11B···I3vi | 0.832 (10) | 3.10 (3) | 3.699 (3) | 131 (3) |
O11—H11B···I3Avi | 0.832 (10) | 2.90 (3) | 3.505 (4) | 131 (3) |
O11—H11B···O15 | 0.832 (10) | 2.48 (3) | 3.070 (3) | 128 (3) |
O15—H15A···I1v | 0.831 (10) | 2.879 (17) | 3.645 (2) | 154 (3) |
O15—H15A···I2iv | 0.831 (10) | 3.24 (3) | 3.6429 (17) | 113 (3) |
O15—H15B···I2iii | 0.837 (10) | 2.744 (14) | 3.5496 (17) | 162 (3) |
O8—H8A···I3ii | 0.817 (10) | 2.797 (11) | 3.610 (3) | 173 (2) |
O8—H8B···I3i | 0.817 (10) | 3.24 (2) | 3.741 (3) | 122 (2) |
O8—H8B···O14 | 0.817 (10) | 2.089 (19) | 2.808 (4) | 147 (3) |
O14—H14B···O15iii | 0.817 (10) | 2.240 (12) | 3.048 (4) | 170 (3) |
O8A—H8D···I3Aii | 0.817 (10) | 2.582 (11) | 3.391 (3) | 170.7 (19) |
O14A—H14C···I3Ai | 0.817 (10) | 3.07 (3) | 3.738 (7) | 140 (3) |
O14A—H14D···O8A | 0.817 (10) | 2.36 (4) | 2.976 (6) | 133 (5) |
Symmetry codes: (i) x, −y+1, z−1/2; (ii) x, −y+2, z−1/2; (iii) −x+3/2, y+1/2, −z+1/2; (iv) −x+3/2, y−1/2, −z+1/2; (v) −x+3/2, −y+1/2, −z+1; (vi) −x+3/2, −y+3/2, −z+1; (vii) x, −y, z−1/2; (viii) −x+1, −y+1, −z+1; (ix) x−1, −y+1, z−1/2; (x) x, y+1, z; (xi) −x+1, y, −z+1/2; (xii) x−1/2, y−1/2, z; (xiii) −x+3/2, y+1/2, −z+3/2; (xiv) x−1, y, z; (xv) x−1, y, z−1; (xvi) x, y−1, z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O31—H31A···I3 | 0.838 (10) | 3.25 (6) | 3.782 (5) | 124 (6) |
O31—H31A···I2 | 0.838 (10) | 2.85 (5) | 3.535 (5) | 141 (6) |
O17—H17A···I6 | 0.842 (10) | 2.98 (7) | 3.542 (5) | 126 (7) |
O17—H17A···I4i | 0.842 (10) | 3.02 (6) | 3.640 (5) | 133 (7) |
O20—H20A···O28 | 0.840 (10) | 2.02 (3) | 2.837 (7) | 166 (10) |
O23—H23B···I6 | 0.842 (10) | 2.86 (8) | 3.588 (5) | 146 (12) |
O7—H7A···O18 | 0.840 (10) | 1.81 (3) | 2.624 (6) | 165 (10) |
O18—H18B···I5 | 0.840 (10) | 2.80 (6) | 3.543 (5) | 149 (9) |
O18—H18B···I3ii | 0.840 (10) | 3.19 (10) | 3.624 (5) | 115 (8) |
O18—H18A···O17 | 0.841 (10) | 2.03 (3) | 2.840 (8) | 163 (9) |
O33—H33A···I6 | 0.839 (10) | 2.601 (19) | 3.434 (4) | 171 (10) |
O14—H14B···O30 | 0.840 (10) | 2.23 (6) | 2.954 (7) | 144 (8) |
O14—H14A···O23 | 0.841 (10) | 2.02 (3) | 2.833 (7) | 163 (9) |
O22—H22B···O21 | 0.841 (10) | 1.98 (2) | 2.809 (7) | 170 (9) |
O22—H22A···I2iii | 0.841 (10) | 2.88 (5) | 3.573 (5) | 141 (6) |
O32—H32B···I2iv | 0.840 (10) | 2.94 (3) | 3.752 (5) | 164 (7) |
O32—H32A···O24 | 0.842 (10) | 2.01 (3) | 2.802 (7) | 156 (7) |
O20—H20B···I1ii | 0.840 (10) | 2.88 (3) | 3.689 (5) | 161 (7) |
O15—H15B···I3ii | 0.839 (10) | 2.79 (4) | 3.540 (5) | 150 (6) |
O15—H15A···I6iii | 0.840 (10) | 2.69 (3) | 3.482 (5) | 159 (7) |
O3—H3B···O26iii | 0.839 (10) | 1.90 (3) | 2.681 (6) | 155 (7) |
O3—H3A···O21 | 0.840 (10) | 1.834 (14) | 2.671 (6) | 174 (7) |
O11—H11B···O29 | 0.840 (10) | 1.768 (12) | 2.609 (6) | 179 (8) |
O11—H11A···O23ii | 0.841 (10) | 1.85 (2) | 2.659 (6) | 162 (7) |
O8—H8B···O15v | 0.841 (10) | 1.885 (13) | 2.725 (6) | 176 (7) |
O8—H8A···O27i | 0.842 (10) | 1.849 (15) | 2.686 (6) | 173 (7) |
O10—H10A···O31i | 0.841 (10) | 1.88 (2) | 2.696 (6) | 164 (8) |
O10—H10B···O19ii | 0.841 (10) | 1.766 (17) | 2.599 (6) | 171 (8) |
O12—H12B···O33 | 0.842 (10) | 1.845 (15) | 2.681 (6) | 172 (7) |
O12—H12A···O15ii | 0.842 (10) | 1.877 (17) | 2.711 (6) | 171 (7) |
O6—H6B···O16vi | 0.839 (10) | 1.925 (14) | 2.762 (6) | 175 (7) |
O6—H6A···O25 | 0.840 (10) | 1.84 (3) | 2.647 (6) | 159 (7) |
O9—H9B···O22ii | 0.840 (10) | 1.846 (19) | 2.675 (6) | 169 (7) |
O9—H9A···O30ii | 0.841 (10) | 1.80 (2) | 2.617 (6) | 163 (7) |
O4—H4B···O17vii | 0.839 (10) | 1.797 (13) | 2.636 (6) | 177 (7) |
O4—H4A···O16vii | 0.841 (10) | 1.92 (2) | 2.747 (6) | 167 (7) |
O5—H5B···O26viii | 0.841 (10) | 1.838 (13) | 2.678 (6) | 176 (8) |
O5—H5A···O13vi | 0.839 (10) | 1.91 (4) | 2.671 (6) | 151 (7) |
O7—H7B···O33ii | 0.844 (10) | 1.88 (2) | 2.707 (6) | 165 (7) |
O27—H27A···O32v | 0.838 (10) | 2.16 (4) | 2.916 (7) | 150 (7) |
O27—H27A···I5i | 0.838 (10) | 3.16 (6) | 3.699 (5) | 124 (6) |
O27—H27B···I2 | 0.841 (10) | 2.783 (19) | 3.608 (5) | 167 (7) |
O19—H19B···I1iii | 0.841 (10) | 2.98 (6) | 3.614 (6) | 134 (7) |
O19—H19A···I4ii | 0.842 (10) | 2.96 (3) | 3.765 (6) | 160 (7) |
O21—H21B···O20ix | 0.839 (10) | 2.08 (5) | 2.773 (7) | 140 (7) |
O21—H21A···I4x | 0.838 (10) | 3.15 (5) | 3.814 (5) | 139 (7) |
O21—H21A···I1iii | 0.838 (10) | 3.22 (7) | 3.734 (5) | 122 (6) |
O28—H28B···I1xi | 0.841 (10) | 2.79 (4) | 3.530 (5) | 147 (6) |
O28—H28A···O29 | 0.839 (10) | 2.058 (14) | 2.893 (6) | 174 (7) |
O2—H2B···O14 | 0.842 (10) | 1.75 (2) | 2.582 (6) | 168 (7) |
O2—H2A···O28ix | 0.842 (10) | 1.835 (17) | 2.668 (6) | 170 (7) |
O1—H1B···O24 | 0.840 (10) | 1.84 (3) | 2.627 (6) | 154 (7) |
O1—H1A···O34vi | 0.841 (10) | 1.713 (16) | 2.549 (7) | 172 (7) |
O25—H25B···I4ix | 0.840 (10) | 3.19 (7) | 3.727 (5) | 124 (7) |
O25—H25B···I1 | 0.840 (10) | 2.98 (6) | 3.655 (5) | 139 (7) |
O25—H25A···I2 | 0.840 (10) | 2.82 (3) | 3.624 (5) | 160 (7) |
O34—H34B···I2xii | 0.839 (10) | 2.85 (5) | 3.587 (6) | 147 (8) |
O34—H34A···I3ii | 0.839 (10) | 2.79 (2) | 3.612 (6) | 168 (8) |
O31—H31B···I6 | 0.839 (10) | 3.31 (7) | 3.726 (4) | 113 (6) |
O31—H31B···I1 | 0.839 (10) | 2.94 (5) | 3.645 (5) | 142 (6) |
O26—H26B···O25 | 0.840 (10) | 2.39 (6) | 2.941 (6) | 124 (6) |
O26—H26B···I4ix | 0.840 (10) | 2.86 (4) | 3.570 (4) | 143 (6) |
O26—H26A···I5vi | 0.842 (10) | 2.563 (14) | 3.401 (4) | 173 (7) |
O24—H24B···O22 | 0.839 (10) | 2.03 (3) | 2.818 (7) | 157 (7) |
O24—H24A···I5xiii | 0.840 (10) | 2.83 (5) | 3.554 (5) | 145 (7) |
O23—H23A···O20ix | 0.841 (10) | 1.93 (3) | 2.744 (7) | 163 (8) |
O33—H33B···O31 | 0.838 (10) | 2.45 (7) | 2.891 (7) | 114 (6) |
O33—H33B···I3 | 0.838 (10) | 2.88 (3) | 3.665 (4) | 156 (7) |
O30—H30B···O32 | 0.838 (10) | 2.22 (7) | 2.753 (7) | 122 (7) |
O30—H30A···I3 | 0.840 (10) | 2.88 (3) | 3.699 (5) | 164 (7) |
O13—H13B···I3ii | 0.840 (10) | 2.74 (2) | 3.562 (5) | 165 (7) |
O13—H13A···O27ii | 0.840 (10) | 2.18 (4) | 2.935 (7) | 149 (6) |
O13—H13A···I5iii | 0.840 (10) | 3.27 (6) | 3.695 (5) | 114 (5) |
O29—H29B···I4 | 0.840 (10) | 2.77 (5) | 3.490 (4) | 145 (7) |
O29—H29A···O18ii | 0.841 (10) | 1.949 (18) | 2.781 (7) | 170 (7) |
O17—H17B···O13v | 0.842 (10) | 1.966 (15) | 2.805 (7) | 174 (7) |
O16—H16B···I4ii | 0.843 (10) | 2.702 (13) | 3.543 (5) | 175 (7) |
O16—H16A···I5 | 0.841 (10) | 2.90 (5) | 3.522 (5) | 133 (6) |
O16—H16A···I3ii | 0.841 (10) | 3.10 (5) | 3.728 (5) | 133 (6) |
O31—H31A···I3 | 0.838 (10) | 3.25 (6) | 3.782 (5) | 124 (6) |
O31—H31A···I2 | 0.838 (10) | 2.85 (5) | 3.535 (5) | 141 (6) |
O17—H17A···I6 | 0.842 (10) | 2.98 (7) | 3.542 (5) | 126 (7) |
O17—H17A···I4i | 0.842 (10) | 3.02 (6) | 3.640 (5) | 133 (7) |
O20—H20A···O28 | 0.840 (10) | 2.02 (3) | 2.837 (7) | 166 (10) |
O23—H23B···I6 | 0.842 (10) | 2.86 (8) | 3.588 (5) | 146 (12) |
O7—H7A···O18 | 0.840 (10) | 1.81 (3) | 2.624 (6) | 165 (10) |
O18—H18B···I5 | 0.840 (10) | 2.80 (6) | 3.543 (5) | 149 (9) |
O18—H18B···I3ii | 0.840 (10) | 3.19 (10) | 3.624 (5) | 115 (8) |
O18—H18A···O17 | 0.841 (10) | 2.03 (3) | 2.840 (8) | 163 (9) |
O33—H33A···I6 | 0.839 (10) | 2.601 (19) | 3.434 (4) | 171 (10) |
O14—H14B···O30 | 0.840 (10) | 2.23 (6) | 2.954 (7) | 144 (8) |
O14—H14A···O23 | 0.841 (10) | 2.02 (3) | 2.833 (7) | 163 (9) |
O22—H22B···O21 | 0.841 (10) | 1.98 (2) | 2.809 (7) | 170 (9) |
O22—H22A···I2iii | 0.841 (10) | 2.88 (5) | 3.573 (5) | 141 (6) |
O32—H32B···I2iv | 0.840 (10) | 2.94 (3) | 3.752 (5) | 164 (7) |
O32—H32A···O24 | 0.842 (10) | 2.01 (3) | 2.802 (7) | 156 (7) |
O20—H20B···I1ii | 0.840 (10) | 2.88 (3) | 3.689 (5) | 161 (7) |
O15—H15B···I3ii | 0.839 (10) | 2.79 (4) | 3.540 (5) | 150 (6) |
O15—H15A···I6iii | 0.840 (10) | 2.69 (3) | 3.482 (5) | 159 (7) |
O3—H3B···O26iii | 0.839 (10) | 1.90 (3) | 2.681 (6) | 155 (7) |
O3—H3A···O21 | 0.840 (10) | 1.834 (14) | 2.671 (6) | 174 (7) |
O11—H11B···O29 | 0.840 (10) | 1.768 (12) | 2.609 (6) | 179 (8) |
O11—H11A···O23ii | 0.841 (10) | 1.85 (2) | 2.659 (6) | 162 (7) |
O8—H8B···O15v | 0.841 (10) | 1.885 (13) | 2.725 (6) | 176 (7) |
O8—H8A···O27i | 0.842 (10) | 1.849 (15) | 2.686 (6) | 173 (7) |
O10—H10A···O31i | 0.841 (10) | 1.88 (2) | 2.696 (6) | 164 (8) |
O10—H10B···O19ii | 0.841 (10) | 1.766 (17) | 2.599 (6) | 171 (8) |
O12—H12B···O33 | 0.842 (10) | 1.845 (15) | 2.681 (6) | 172 (7) |
O12—H12A···O15ii | 0.842 (10) | 1.877 (17) | 2.711 (6) | 171 (7) |
O6—H6B···O16vi | 0.839 (10) | 1.925 (14) | 2.762 (6) | 175 (7) |
O6—H6A···O25 | 0.840 (10) | 1.84 (3) | 2.647 (6) | 159 (7) |
O9—H9B···O22ii | 0.840 (10) | 1.846 (19) | 2.675 (6) | 169 (7) |
O9—H9A···O30ii | 0.841 (10) | 1.80 (2) | 2.617 (6) | 163 (7) |
O4—H4B···O17vii | 0.839 (10) | 1.797 (13) | 2.636 (6) | 177 (7) |
O4—H4A···O16vii | 0.841 (10) | 1.92 (2) | 2.747 (6) | 167 (7) |
O5—H5B···O26viii | 0.841 (10) | 1.838 (13) | 2.678 (6) | 176 (8) |
O5—H5A···O13vi | 0.839 (10) | 1.91 (4) | 2.671 (6) | 151 (7) |
O7—H7B···O33ii | 0.844 (10) | 1.88 (2) | 2.707 (6) | 165 (7) |
O27—H27A···O32v | 0.838 (10) | 2.16 (4) | 2.916 (7) | 150 (7) |
O27—H27A···I5i | 0.838 (10) | 3.16 (6) | 3.699 (5) | 124 (6) |
O27—H27B···I2 | 0.841 (10) | 2.783 (19) | 3.608 (5) | 167 (7) |
O19—H19B···I1iii | 0.841 (10) | 2.98 (6) | 3.614 (6) | 134 (7) |
O19—H19A···I4ii | 0.842 (10) | 2.96 (3) | 3.765 (6) | 160 (7) |
O21—H21B···O20ix | 0.839 (10) | 2.08 (5) | 2.773 (7) | 140 (7) |
O21—H21A···I4x | 0.838 (10) | 3.15 (5) | 3.814 (5) | 139 (7) |
O21—H21A···I1iii | 0.838 (10) | 3.22 (7) | 3.734 (5) | 122 (6) |
O28—H28B···I1xi | 0.841 (10) | 2.79 (4) | 3.530 (5) | 147 (6) |
O28—H28A···O29 | 0.839 (10) | 2.058 (14) | 2.893 (6) | 174 (7) |
O2—H2B···O14 | 0.842 (10) | 1.75 (2) | 2.582 (6) | 168 (7) |
O2—H2A···O28ix | 0.842 (10) | 1.835 (17) | 2.668 (6) | 170 (7) |
O1—H1B···O24 | 0.840 (10) | 1.84 (3) | 2.627 (6) | 154 (7) |
O1—H1A···O34vi | 0.841 (10) | 1.713 (16) | 2.549 (7) | 172 (7) |
O25—H25B···I4ix | 0.840 (10) | 3.19 (7) | 3.727 (5) | 124 (7) |
O25—H25B···I1 | 0.840 (10) | 2.98 (6) | 3.655 (5) | 139 (7) |
O25—H25A···I2 | 0.840 (10) | 2.82 (3) | 3.624 (5) | 160 (7) |
O34—H34B···I2xii | 0.839 (10) | 2.85 (5) | 3.587 (6) | 147 (8) |
O34—H34A···I3ii | 0.839 (10) | 2.79 (2) | 3.612 (6) | 168 (8) |
O31—H31B···I6 | 0.839 (10) | 3.31 (7) | 3.726 (4) | 113 (6) |
O31—H31B···I1 | 0.839 (10) | 2.94 (5) | 3.645 (5) | 142 (6) |
O26—H26B···O25 | 0.840 (10) | 2.39 (6) | 2.941 (6) | 124 (6) |
O26—H26B···I4ix | 0.840 (10) | 2.86 (4) | 3.570 (4) | 143 (6) |
O26—H26A···I5vi | 0.842 (10) | 2.563 (14) | 3.401 (4) | 173 (7) |
O24—H24B···O22 | 0.839 (10) | 2.03 (3) | 2.818 (7) | 157 (7) |
O24—H24A···I5xiii | 0.840 (10) | 2.83 (5) | 3.554 (5) | 145 (7) |
O23—H23A···O20ix | 0.841 (10) | 1.93 (3) | 2.744 (7) | 163 (8) |
O33—H33B···O31 | 0.838 (10) | 2.45 (7) | 2.891 (7) | 114 (6) |
O33—H33B···I3 | 0.838 (10) | 2.88 (3) | 3.665 (4) | 156 (7) |
O30—H30B···O32 | 0.838 (10) | 2.22 (7) | 2.753 (7) | 122 (7) |
O30—H30A···I3 | 0.840 (10) | 2.88 (3) | 3.699 (5) | 164 (7) |
O13—H13B···I3ii | 0.840 (10) | 2.74 (2) | 3.562 (5) | 165 (7) |
O13—H13A···O27ii | 0.840 (10) | 2.18 (4) | 2.935 (7) | 149 (6) |
O13—H13A···I5iii | 0.840 (10) | 3.27 (6) | 3.695 (5) | 114 (5) |
O29—H29B···I4 | 0.840 (10) | 2.77 (5) | 3.490 (4) | 145 (7) |
O29—H29A···O18ii | 0.841 (10) | 1.949 (18) | 2.781 (7) | 170 (7) |
O17—H17B···O13v | 0.842 (10) | 1.966 (15) | 2.805 (7) | 174 (7) |
O16—H16B···I4ii | 0.843 (10) | 2.702 (13) | 3.543 (5) | 175 (7) |
O16—H16A···I5 | 0.841 (10) | 2.90 (5) | 3.522 (5) | 133 (6) |
O16—H16A···I3ii | 0.841 (10) | 3.10 (5) | 3.728 (5) | 133 (6) |
Symmetry codes: (i) −x+2, −y+1, −z+1; (ii) −x+1, −y+1, −z+1; (iii) x−1, y, z; (iv) −x+1, −y+1, −z+2; (v) x+1, y, z; (vi) x, y, z+1; (vii) −x+1, −y+2, −z+1; (viii) −x+1, −y+2, −z+2; (ix) x, y+1, z; (x) x−1, y+1, z; (xi) x, y−1, z; (xii) x, y, z−1; (xiii) x−1, y, z+1. |
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