Crystal structures of the alkali aluminoboracites A4B4Al3O12Cl (A = Li, Na)

Yoshino, S.; Arima, H.; Ishijima, M.; Kajihara, K.

doi:10.1107/S2056989024000501

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Volume 80| Part 2| February 2024| Pages 169-173

https://doi.org/10.1107/S2056989024000501

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Crystal structures of the alkali aluminoboracites A₄B₄Al₃O₁₂Cl (A = Li, Na)

Sho Yoshino,^a Hidechika Arima,^a Masanao Ishijima ^a and Koichi Kajihara ^a ^*

^aDepartment of Applied Chemistry for Environment, Graduate School of Urban Environmental Sciences, Tokyo Metropolitan University, 1-1 Minami-Osawa, Hachoji, Tokyo 192-0397, Japan
^*Correspondence e-mail: kkaji@tmu.ac.jp

Edited by M. Weil, Vienna University of Technology, Austria (Received 13 November 2023; accepted 13 January 2024; online 26 January 2024)

Single crystals of alkali aluminoboracites, A₄B₄Al₃O₁₂Cl (A = Li, Na), were grown using the self-flux method, and their isotypic cubic crystal structures were determined by single-crystal X-ray diffraction. Na₄B₄Al₃O₁₂Cl is the first reported sodium boracite, and its lattice parameter [13.5904 (1) Å] is the largest among the boracites consisting of a cation–oxygen framework reported so far. For both crystals, structure models refined in the cubic space group F $[\overline{4}]$ 3c, which assume that all cubic octant subcells in the unit cell are equivalent, converged with R1 factors of ∼0.03. However, the presence of weak hhl reflections with odd h and l values indicates that refinements in the space group F23, which presume a checkerboard-like ordering of two types of subcells with slightly different atomic positions, are more appropriate.

Keywords: alkali aluminoboracite; self-flux method; weak structure ordering; isotypism; crystal structure.

CCDC references: 2325537; 2325536; 2325535; 2325534

1. Chemical context

Boracite is originally known as a mineral with the formula Mg₃B₇O₁₃Cl. The name boracite also refers to borate compounds with the general formula M₃B₇O₁₃X, consisting of a negatively charged B–O framework, extraframework divalent cations M, such as Mg²⁺, Cr²⁺, Mn²⁺, Fe²⁺, Co²⁺, Ni²⁺, Cu²⁺, Zn²⁺ and Cd²⁺, and extraframework anions X, such as Cl⁻, Br⁻, I⁻ and S²⁻ (Schmid, 1965 ; Nelmes, 1974 ). The extraframework cations can also be an alkali ion, but only lithium variants Li_4–xB₇O_12+x/2X, Li₄B_7–3xAl_3xO₁₂X and Li₄B_7–3xGa_3xO₁₂Cl (X = Cl, Br; x = 0–1) have been reported to date (Levasseur et al., 1971 ; Réau et al., 1976 ; Jeitschko et al., 1977 ; Calès et al., 1977 ; Sorokin, 2015 ; Tezuka et al., 2017 ; Kajihara et al., 2017 ; Katsumata et al., 2022 ). The latter two compounds (Kajihara et al., 2017; Katsumata et al., 2022) are the first examples of boracites containing framework cations other than B³⁺ ions. The lithium boracites are lithium-ion conducting, and their dc Li⁺ ion conductivity can be increased to ∼10⁻⁵ S cm⁻¹ at room temperature in glass-ceramics consisting mainly of Li₄B₄M₃O₁₂Cl (M = Al, Ga; Kajihara et al., 2017). In addition, Li₄B₄Al₃O₁₂Cl is stable in contact with Li metal and is water-resistant; solid-state cells consisting of an Li₄B₄Al₃O₁₂Cl-based glass-ceramic solid electrolyte, an LiCoO₂-based composite cathode containing an ionic liquid and an Li–Au alloy anode worked successfully (Saito et al., 2021 ). More recently, a thioboracite, Li₆B₇S₁₃I, a sulfide variant of lithium boracite with room-temperature Li⁺ ion conductivity of ∼5 × 10⁻⁴ S cm⁻¹ has been reported (Kaup et al., 2021 ). However, single crystals of Li₄B₄Al₃O₁₂Cl have not yet been grown, and the preliminary crystal structure analysis of Li₄B₄Al₃O₁₂Cl (Kajihara et al., 2017; Katsumata et al., 2022) was incomplete. In addition, boracites containing alkali ions other than Li⁺ have not been reported. Furthermore, a rhombohedral distortion of the unit cell of single-crystalline Li₄B₇O₁₂Cl was experimentally observed at room temperature (Jeitschko et al., 1977) and was recently theoretically confirmed (Li & Holzwarth, 2022 ), raising the question whether similar unit-cell distortions occur in other alkali boracites.

In the present study, we report the growth of single crystals of A₄B₄Al₃O₁₂Cl (A = Li, Na) using the self-flux method and their structural characterization by single-crystal X-ray diffraction (XRD).

2. Structural commentary

The crystallites of Li₄B₄Al₃O₁₂Cl exhibit complete extinction under cross-polarized light, supporting cubic symmetry. Hence, the unit cell of Li₄B₄Al₃O₁₂Cl is not distorted. At first, the crystal structure was refined in the noncentrosymmetric cubic space group F $[\overline{4}]$ 3c following the model from the Rietveld refinement of powder X-ray diffraction data (Kajihara et al., 2017; Katsumata et al., 2022). The occupancy (g) of Cl1 converged to the upper bound [g(Cl1) = 1] and was fixed at this value. The reliability factor R1 converged to 0.031, and the refinement results agreed well with those derived from the powder samples (Kajihara et al., 2017; Katsumata et al., 2022). The unit cell of Li₄B₄Al₃O₁₂Cl can be divided into eight equivalent cubic subcells, each containing one Cl1 at the cube centre. The Cl1 site is surrounded by six sites with multiplicity 24 (Wyckoff letter c) and four sites with multiplicity 32 (Wyckoff letter e) containing four Li atoms in total, and the resulting ClLi₄ moiety is embedded in a negatively charged framework consisting of alternating corner-shared bridges of planar BO₃ triangles and AlO₄ tetrahedra. The occupancy of Li1 is close to 1, whereas that of Li2 is ∼ $[1 \over 4]$ . The lattice parameter of Li₄B₄Al₃O₁₂Cl [a = 12.9839 (1) Å] is similar to that of the polycrystalline sample obtained by solid-state synthesis [a = 12.9687 (1) Å; Katsumata et al., 2022] but larger than that crystallized from glass-ceramics [a = 12.9149 (5) Å; Kajihara et al., 2017], probably because of an incomplete uptake of Al in crystals obtained from glass-ceramics.

Similar to Li₄B₄Al₃O₁₂Cl, the crystallites of Na₄B₄Al₃O₁₂Cl exhibit complete cross-polarized extinction. Refinement in the space group F $[\overline{4}]$ 3c resulted in a reliability factor R1 of 0.022, and the results indicate that Na₄B₄Al₃O₁₂Cl is isostructural with Li₄B₄Al₃O₁₂Cl, except that Na1 is located at the 48 g site and displaced from the 24 c site at the midpoint between neighbouring Cl1 atoms. The lattice parameter of Na₄B₄Al₃O₁₂Cl [a = 13.5904 (1) Å] is the largest among known cubic boracites, apart from the sulfide variant Li₆B₇S₁₃I [a = 15.245 (2) Å; Kaup et al., 2021]. The occupancy of Cl1 is less than 1 (∼0.92), possibly because of its higher growth temperature compared to that of Li₄B₄Al₃O₁₂Cl. The equivalent isotropic displacement parameters (U_eq) of extraframework species [Cl1, 0.0350 (9) Å²; Na1, 0.0422 (14) Å²; Na2, 0.017 (2) Å²] of Na₄B₄Al₃O₁₂Cl are notably smaller than those of Li₄B₄Al₃O₁₂Cl [Cl1, 0.0787 (15) Å²; Li1, 0.066 (6) Å²; Li2, 0.028 (11) Å²], despite that the species in the framework (B1, Al1 and O1) are similar or even larger in Na₄B₄Al₃O₁₂Cl. These observations suggest that replacing Li with Na increases the packing density at the extraframework sites and suppresses the thermal motion of the atoms located therein.

The convergence of the structure refinements of Li₄B₄Al₃O₁₂Cl and Na₄B₄Al₃O₁₂Cl in the space group F $[\overline{4}]$ 3c was satisfactory (R1 ≃ 0.03). However, these crystals both exhibit weak hhl reflections with odd h and l, which violate the extinction conditions in space group F $[\overline{4}]$ 3c, as listed in Table 1. The noncentrosymmetric cubic space groups compatible with the observed reflection condition (hhl: h + l = 2n) are F23, F432 and F $[\overline{4}]$ 3m. Among them, only the structure analyses in the space group F23 were successful. The conversion of the space group from F $[\overline{4}]$ 3c to F23 is accompanied by the splitting of atoms except for Al1. This conversion also splits Li1 at the 24 c site of F $[\overline{4}]$ 3c into Li1 and Li2 at the 24 g site of F23. The occupancies of A1 and A2 (A = Li, Na) converged to the upper bound [g(A1) = g(A2) = 0.5] both in Li₄B₄Al₃O₁₂Cl and Na₄B₄Al₃O₁₂Cl, and were fixed at this value. The slightly larger R1 factors in F23 compared to F $[\overline{4}]$ 3c are due to an increased number of measured reflections partially with low intensities.

Table 1
Summary of the observed hhl reflections in Li₄B₄Al₃O₁₂Cl and Na₄B₄Al₃O₁₂Cl

	Li₄B₄Al₃O₁₂Cl		Na₄B₄Al₃O₁₂Cl
	<I/σ(I)>	Number of reflections	<I/σ(I)>	Number of reflections
No conditions	14.35	325	12.14	340
h even	30.24	153	24.96	165
h odd	0.21	172	0.04	175
l even	30.24	153	24.96	165
l odd	0.21	172	0.04	175
h + l even	14.35	325	12.14	340
h + l odd	0.00	0	0.00	0

Fig. 1 summarizes the schematic illustrations of two adjacent cubic octant subcells of the unit cells of Li₄B₄Al₃O₁₂Cl and Na₄B₄Al₃O₁₂Cl, along with their asymmetric units derived from the analyses in the space group F23. In the space group F $[\overline{4}]$ 3c, the eight subcells in a unit cell are equivalent. In contrast, in the space group F23, they are classified into two types of subcells stacked alternately in three dimensions. Nevertheless, the atomic displacements associated with the conversion of the space group from F $[\overline{4}]$ 3c to F23 are small, and the structures solved in these two space groups are very similar, apart from the splitting of Li1 in space group F $[\overline{4}]$ 3c into Li1 and Li2 in space group F23. Such subcell ordering is also observed in the lithium-rich boracite Li₅B₇O_12.5Cl (space group F23) (Vlasse et al., 1981 ; Tezuka et al., 2017; Li & Holzwarth, 2022); in Li₅B₇O_12.5Cl, the chemical compositions of adjacent subcells differ notably as a result of the incorporation of excess Li and O and the resulting partial conversion of BO₃ triangles to BO₄ tetrahedra, as well as the ordering of Li. In contrast, in the title compounds Li₄B₄Al₃O₁₂Cl and Na₄B₄Al₃O₁₂Cl, such a distinct structural ordering associated with a compositional change is not observed, as the conversion of BO₃ triangles to BO₄ tetrahedra is unlikely even under alkali-rich conditions.

Figure 1
Schematic illustrations of two neighbouring cubic octant subcells in the unit cell of Li₄B₄Al₃O₁₂Cl in the space groups F $[\overline{4}]$ 3c (top left) and F23 (middle left), those of Na₄B₄Al₃O₁₂Cl in the space groups F $[\overline{4}]$ 3c (top right) and F23 (middle right), and asymmetric units with displacement ellipsoids at the 50% probability level of Li₄B₄Al₃O₁₂Cl (bottom left) and Na₄B₄Al₃O₁₂Cl (bottom right) in the space group F23. Red, large green, small green and yellow spheres denote O, Cl, Li and Na atoms, respectively. Green triangles and gray tetrahedra denote BO₃ and AlO₄ units, respectively. The forefront Al atoms located at z = 0.5 are not shown for clarity. In the middle and bottom figures, red and pale-red spheres denote O1 and O2 atoms, respectively.

Table 2 lists selected atomic distances and angles. The B—O and Al—O distances are similar between Li₄B₄Al₃O₁₂Cl and Na₄B₄Al₃O₁₂Cl. In contrast, the B—O—Al angles in Na₄B₄Al₃O₁₂Cl are larger than those in Li₄B₄Al₃O₁₂Cl by ∼10°. This widening in the B—O—Al angles is responsible for the expansion of the unit cell in Na₄B₄Al₃O₁₂Cl. The increase in A—O (A = Li, Na) distances from Li₄B₄Al₃O₁₂Cl and Na₄B₄Al₃O₁₂Cl amounts to ∼0.2–0.3 Å, and is consistent with the difference in the ionic radii between Li and Na with the same coordination numbers (1.13–0.73 Å = 0.40 Å for fourfold corrdination and 1.16–0.90 Å = 0.26 Å for sixfold coordination; Shannon, 1976 ). In contrast, the increase in A—Cl distances is notably smaller (∼0.05 Å) or even negative, indicating an increase in the packing density of extraframework A and Cl. This observation is consistent with the smaller atomic displacement parameters of extraframework A and Cl in Na₄B₄Al₃O₁₂Cl compared to Li₄B₄Al₃O₁₂Cl (see above).

Table 2
Selected bond lengths and angles (Å, °) in A₄B₄Al₃O₁₂Cl crystal structures

Space group F $[\overline{4}]$ 3c			Space group F23
	A = Li	A = Na		A = Li	A = Na
A1—O1	2.0828 (17)	2.2588 (16)	A1—O1	2.053 (3)	2.2585 (18)
A1—O1ⁱ	2.0828 (17)	2.446 (2)	A1—O2ⁱⁱ	2.143 (16)	2.452 (3)
			A2—O2ⁱⁱⁱ	2.056 (4)	2.2602 (18)
			A2—O1^iv	2.132 (16)	2.442 (3)
A1—Cl1	3.2460 (1)	2.936 (4)	A1—Cl1	2.98 (6)	2.925 (6)
			A2—Cl2	3.03 (6)	2.948 (6)
A2—O1^v	2.22 (3)	2.484 (5)	A3—O2^vi	2.23 (3)	2.488 (6)
A2—O1^vii	2.828 (8)	2.913 (2)	A3—O1^vii	2.824 (8)	2.912 (2)
			A4—O1^viii	2.23 (3)	2.480 (6)
			A4—O2^ix	2.826 (8)	2.914 (2)
A2—Cl1	2.57 (5)	2.605 (9)	A3—Cl1	2.55 (6)	2.599 (10)
			A4—Cl2	2.55 (5)	2.612 (10)
B1—O1	1.3700 (16)	1.3693 (15)	B1—O1	1.3693 (17)	1.3684 (16)
			B2—O2^x	1.3702 (17)	1.3684 (16)
Al1—O1^xi	1.7533 (17)	1.7506 (16)	Al1—O1^xi	1.754 (2)	1.7495 (18)
			Al1—O2^xii	1.754 (2)	1.7522 (18)

B1—O1—Al1^xiii	118.97 (12)	128.59 (12)	B1—O1—Al1^xiii	119.05 (13)	128.62 (14)
			B2^xiv—O2—Al1^vii	118.94 (13)	128.66 (14)
Symmetry code(s): (i) −x, −z + $[{1\over 2}]$ , y; (ii) −x, y, −z + 1; (iii) x + $[{1\over 2}]$ , −y + 1, −z + $[{3\over 2}]$ ; (iv) −x + $[{1\over 2}]$ , −y + 1, z + $[{1\over 2}]$ ; (v) −y + $[{1\over 2}]$ , x + $[{1\over 2}]$ , −z + $[{1\over 2}]$ ; (vi) −z + 1, x + $[{1\over 2}]$ , −y + $[{1\over 2}]$ ; (vii) z, −x + $[{1\over 2}]$ , −y + $[{1\over 2}]$ ; (viii) x + 1, −y + 1, −z + 1; (ix) −x + 1, y + $[{1\over 2}]$ , −z + $[{3\over 2}]$ ; (x) z, x + $[{1\over 2}]$ , y + $[{1\over 2}]$ ; (xi) z, x, y; (xii) −y + $[{1\over 2}]$ , z − $[{1\over 2}]$ , −x; (xiii) y, z, x; (xiv) x − $[{1\over 2}]$ , y − $[{1\over 2}]$ , z.

3. Synthesis and crystallization

Li₂CO₃ (Fujifilm Wako Chemicals, 99%), Na₂CO₃ (Fujifilm Wako Chemicals, 99%), B₂O₃ (Kojundo Chemical Laboratory, 99.9%), γ-Al₂O₃ (Kojundo Chemical Laboratory, 99.99%), LiCl (Kanto Chemical, 99.9%) and NaCl (Kojundo Chemical Laboratory, 99.9%) were mixed in an A₂CO₃:B₂O₃:γ-Al₂O₃:ACl (A = Li, Na) molar ratio of 3:4:3:14, with a B₂O₃ content of 10 mmol. LiCl (melting point: 878 K) and NaCl (melting point: 1074 K), acting as self-fluxes, were added in excess. The mixture of sample 1 (A = Li) or 2 (A = Na) was placed in a platinum crucible covered by an alumina crucible, heated to 1073 K for 3 h (sample 1) or 1123 K for 4 h (sample 2), maintained for 5 h, cooled at a rate of 3 K h⁻¹ for 50 h, and then cooled to room temperature in the furnace by turning off the power.

The resulting mixtures were washed with water to leach out water-soluble components. The residues were characterized by powder X-ray diffraction (SmartLab diffractometer, Rigaku) using Cu Kα radiation. The main impurity phases in the residues of samples 1 and 2 were Li₂BAlO₄ (space group P2₁/c) and LiAl₅O₈ (space group P4₁32), and Na₂Al₂B₄O₇ (space group P $[\overline{3}]$ 1c), respectively. Single-crystal particles with cubic symmetry were selected using an optical microscope (BH2, Olympus), showing complete light extinction under crossed polarizers.

4. Refinement

Crystal data, data collection and structure refinement details are summarized in Table 3. The crystal structures of Li₄B₄Al₃O₁₂Cl and Na₄B₄Al₃O₁₂Cl were solved both in the space groups F $[\overline{4}]$ 3c and F23 using the same hkl file. In the refinements in the space group F23, all reflections were used. In the refinements in the space group F $[\overline{4}]$ 3c, reflections that violate the extinction conditions (885 in Li₄B₄Al₃O₁₂Cl and 1010 in Na₄B₄Al₃O₁₂Cl) were rejected by SHELXL (Sheldrick, 2015b ), but few rejected reflections had intensities with I/σ(I) > 3 (3 in Li₄B₄Al₃O₁₂Cl and 4 in Na₄B₄Al₃O₁₂Cl). To maintain charge neutrality, the occupancies, g, of A (A = Li, Na) and Cl were refined under the restraint that the total number of A in the unit cell was larger by 24 than that of Cl [e.g. 24g(Li1) + 32g(Li2) − 8g(Cl1) = 24 for Li₄B₄Al₃O₁₂Cl solved in F $[\overline{4}]$ 3c], while permitting possible Cl deficiency. The summary of reflections was derived by the program SpaceGroup in WinGX (Farrugia, 2012 ).

Table 3
Experimental details

	Li₄B₄Al₃O₁₂Cl in F $[\overline{4}]$ 3c	Li₄B₄Al₃O₁₂Cl in F23	Na_3.92B₄Al₃O₁₂Cl_0.92 in F $[\overline{4}]$ 3c	Na_3.92B₄Al₃O₁₂Cl_0.92 in F23
Crystal data
Chemical formula	Li₄B₄Al₃O₁₂Cl	Li₄B₄Al₃O₁₂Cl	Na_3.92B₄Al₃O₁₂Cl_0.92	Na_3.92B₄Al₃O₁₂Cl_0.92
M_r	379.39	379.39	438.91	438.91
Crystal system, space group	Cubic, F $[\overline{4}]$ 3c	Cubic, F23	Cubic, F $[\overline{4}]$ 3c	Cubic, F23
Temperature (K)	297	297	294	294
a (Å)	12.9839 (1)	12.9839 (1)	13.5904 (1)	13.5904 (1)
V (Å³)	2188.85 (5)	2188.85 (5)	2510.13 (6)	2510.13 (6)
Z	8	8	8	8
Radiation type	Cu Kα	Cu Kα	Cu Kα	Cu Kα
μ (mm⁻¹)	6.12	6.12	6.78	6.78
Crystal size (mm)	0.11 × 0.10 × 0.06	0.11 × 0.10 × 0.06	0.08 × 0.06 × 0.04	0.08 × 0.06 × 0.04

Data collection
Diffractometer	Bruker D8 goniometer	Bruker D8 goniometer	Bruker D8 goniometer	Bruker D8 goniometer
Absorption correction	Multi-scan (SADABS; Krause et al., 2015 )	Multi-scan (SADABS; Krause et al., 2015)	Multi-scan (SADABS; Krause et al., 2015)	Multi-scan (SADABS; Krause et al., 2015)
T_min, T_max	0.62, 0.75	0.62, 0.75	0.66, 0.75	0.66, 0.75
No. of measured, independent and observed [I > 2σ(I)] reflections	3843, 193, 191	4728, 389, 317	4504, 218, 216	5514, 437, 355
R_int	0.023	0.024	0.027	0.028
(sin θ/λ)_max (Å⁻¹)	0.621	0.621	0.624	0.624

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.031, 0.075, 1.16	0.032, 0.081, 1.17	0.022, 0.055, 1.20	0.024, 0.066, 1.12
No. of reflections	193	389	218	437
No. of parameters	23	50	27	52
No. of restraints	1	1	1	1
Δρ_max, Δρ_min (e Å⁻³)	0.20, −0.63	0.20, −0.91	0.15, −0.45	0.17, −0.58
Absolute structure	Flack x determined using 80 quotients [(I⁺) − (I⁻)]/[(I⁺) + (I⁻)] (Parsons et al., 2013 )	Flack x determined using 132 quotients [(I⁺) − (I⁻)]/[(I⁺) + (I⁻)] (Parsons et al., 2013).	Flack x determined using 89 quotients [(I⁺) − (I⁻)]/[(I⁺) + (I⁻)] (Parsons et al., 2013)	Flack x determined using 142 quotients [(I⁺) − (I⁻)]/[(I⁺) + (I⁻)] (Parsons et al., 2013).
Absolute structure parameter	−0.03 (3)	−0.03 (2)	0.01 (3)	0.01 (2)
Computer programs: BIS (Bruker, 2021 ), SAINT (Bruker, 2019 ), SHELXTL (Sheldrick, 2015a ), SHELXL (Sheldrick, 2015b), ShelXle (Hübschle et al., 2011 ), VESTA (Momma & Izumi, 2011 ) and publCIF (Westrip, 2010 ).

Supporting information

CCDC references: 2325537; 2325536; 2325535; 2325534

Crystal structure: contains datablocks kjh0818yoshinoL14_0m_a, kjh0818yoshinoL14_0m_a_1, kjh230804yoshinoN4_0m_a, kjh230804yoshinoN4_0m_a_1, global. DOI: https://doi.org/10.1107/S2056989024000501/wm5704sup1.cif

Structure factors: contains datablock kjh0818yoshinoL14_0m_a. DOI: https://doi.org/10.1107/S2056989024000501/wm5704kjh0818yoshinoL14_0m_asup2.hkl

Structure factors: contains datablock kjh0818yoshinoL14_0m_a_1. DOI: https://doi.org/10.1107/S2056989024000501/wm5704kjh0818yoshinoL14_0m_a_1sup3.hkl

Structure factors: contains datablock kjh230804yoshinoN4_0m_a. DOI: https://doi.org/10.1107/S2056989024000501/wm5704kjh230804yoshinoN4_0m_asup4.hkl

Structure factors: contains datablock kjh230804yoshinoN4_0m_a_1. DOI: https://doi.org/10.1107/S2056989024000501/wm5704kjh230804yoshinoN4_0m_a_1sup5.hkl

checkCIF report

Computing details top

Lithium aluminoboracite (kjh0818yoshinoL14_0m_a) top

Crystal data top

Li₄B₄Al₃O₁₂Cl	Cu Kα radiation, λ = 1.54178 Å
M_r = 379.39	Cell parameters from 2808 reflections
Cubic, F43c	θ = 6.8–73.2°
a = 12.9839 (1) Å	µ = 6.12 mm⁻¹
V = 2188.85 (5) Å³	T = 297 K
Z = 8	Plate, colorless
F(000) = 1472	0.11 × 0.10 × 0.06 mm
D_x = 2.303 Mg m⁻³

Data collection top

Bruker D8 goniometer diffractometer	193 independent reflections
Radiation source: sealed tube	191 reflections with I > 2σ(I)
Detector resolution: 7.3910 pixels mm^-1	R_int = 0.023
ω scans	θ_max = 73.2°, θ_min = 6.8°
Absorption correction: multi-scan (SADABS; Krause et al., 2015)	h = −15→12
T_min = 0.62, T_max = 0.75	k = −15→16
3843 measured reflections	l = −16→15

Refinement top

Refinement on F²	1 restraint
Least-squares matrix: full	w = 1/[σ²(F_o²) + (0.0536P)² + 3.2978P] where P = (F_o² + 2F_c²)/3
R[F² > 2σ(F²)] = 0.031	(Δ/σ)_max < 0.001
wR(F²) = 0.075	Δρ_max = 0.20 e Å⁻³
S = 1.16	Δρ_min = −0.63 e Å⁻³
193 reflections	Absolute structure: Flack x determined using 80 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons et al., 2013)
23 parameters	Absolute structure parameter: −0.03 (3)

Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Li1	0.000000	0.250000	0.250000	0.066 (6)	0.991 (13)
Li2	0.364 (2)	0.364 (2)	0.364 (2)	0.028 (11)	0.256 (10)
B1	0.1057 (3)	0.1057 (3)	0.1057 (3)	0.0114 (10)
Al1	0.250000	0.000000	0.000000	0.0118 (6)
O1	0.02786 (13)	0.11000 (13)	0.17680 (15)	0.0166 (6)
Cl1	0.250000	0.250000	0.250000	0.0787 (15)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Li1	0.156 (18)	0.021 (4)	0.021 (4)	0.000	0.000	0.000
Li2	0.028 (11)	0.028 (11)	0.028 (11)	0.000 (9)	0.000 (9)	0.000 (9)
B1	0.0114 (10)	0.0114 (10)	0.0114 (10)	−0.0014 (14)	−0.0014 (14)	−0.0014 (14)
Al1	0.0115 (8)	0.0120 (6)	0.0120 (6)	0.000	0.000	0.000
O1	0.0185 (11)	0.0154 (10)	0.0158 (9)	0.0048 (7)	0.0067 (10)	0.0044 (9)
Cl1	0.0787 (15)	0.0787 (15)	0.0787 (15)	0.000	0.000	0.000

Geometric parameters (Å, º) top

Li1—O1	2.0828 (17)	Li2—O1^xiii	2.22 (3)
Li1—O1ⁱ	2.0828 (17)	Li2—Cl1	2.57 (5)
Li1—O1ⁱⁱ	2.0828 (17)	Li2—O1^ix	2.828 (8)
Li1—O1ⁱⁱⁱ	2.0828 (17)	Li2—O1^xiv	2.828 (8)
Li1—Li2^iv	2.740 (13)	Li2—O1^vi	2.828 (8)
Li1—Li2^v	2.740 (13)	Li2—Al1^xv	2.90 (2)
Li1—Li2^vi	2.740 (13)	Li2—Al1^xvi	2.90 (2)
Li1—Li2^vii	2.740 (13)	B1—O1^x	1.3700 (16)
Li1—Cl1	3.2460 (1)	B1—O1^xvii	1.3700 (16)
Li1—Al1^viii	3.2460 (1)	B1—O1	1.3700 (16)
Li1—Al1^ix	3.2460 (1)	Al1—O1^xviii	1.7533 (17)
Li1—Al1^x	3.2460 (1)	Al1—O1^xix	1.7533 (17)
Li2—O1^xi	2.22 (3)	Al1—O1^xvii	1.7533 (17)
Li2—O1^xii	2.22 (3)	Al1—O1^xx	1.7533 (17)

O1—Li1—O1ⁱ	160.00 (10)	O1^ix—Li2—O1^vi	118.0 (5)
O1—Li1—O1ⁱⁱ	91.729 (17)	O1^xiv—Li2—O1^vi	118.0 (5)
O1ⁱ—Li1—O1ⁱⁱ	91.729 (17)	O1^xi—Li2—Al1^xv	69.0 (7)
O1—Li1—O1ⁱⁱⁱ	91.729 (17)	O1^xii—Li2—Al1^xv	37.1 (3)
O1ⁱ—Li1—O1ⁱⁱⁱ	91.729 (17)	O1^xiii—Li2—Al1^xv	123 (2)
O1ⁱⁱ—Li1—O1ⁱⁱⁱ	160.00 (10)	Cl1—Li2—Al1^xv	114.0 (9)
O1—Li1—Li2^iv	52.6 (10)	Li1^xiv—Li2—Al1^xv	171 (2)
O1ⁱ—Li1—Li2^iv	146.2 (9)	Li1^ix—Li2—Al1^xv	70.20 (14)
O1ⁱⁱ—Li1—Li2^iv	70.29 (8)	Li1^vi—Li2—Al1^xv	70.20 (14)
O1ⁱⁱⁱ—Li1—Li2^iv	96.5 (4)	O1^ix—Li2—Al1^xv	106.4 (4)
O1—Li1—Li2^v	96.5 (4)	O1^xiv—Li2—Al1^xv	134.8 (7)
O1ⁱ—Li1—Li2^v	70.29 (8)	O1^vi—Li2—Al1^xv	35.62 (12)
O1ⁱⁱ—Li1—Li2^v	52.6 (10)	O1^xi—Li2—Al1^xvi	123 (2)
O1ⁱⁱⁱ—Li1—Li2^v	146.2 (9)	O1^xii—Li2—Al1^xvi	69.0 (7)
Li2^iv—Li1—Li2^v	114.4 (12)	O1^xiii—Li2—Al1^xvi	37.1 (3)
O1—Li1—Li2^vi	70.29 (8)	Cl1—Li2—Al1^xvi	114.0 (9)
O1ⁱ—Li1—Li2^vi	96.5 (4)	Li1^xiv—Li2—Al1^xvi	70.20 (14)
O1ⁱⁱ—Li1—Li2^vi	146.2 (9)	Li1^ix—Li2—Al1^xvi	70.20 (14)
O1ⁱⁱⁱ—Li1—Li2^vi	52.6 (10)	Li1^vi—Li2—Al1^xvi	171 (2)
Li2^iv—Li1—Li2^vi	114.4 (12)	O1^ix—Li2—Al1^xvi	35.62 (12)
Li2^v—Li1—Li2^vi	100 (2)	O1^xiv—Li2—Al1^xvi	106.4 (4)
O1—Li1—Li2^vii	146.2 (9)	O1^vi—Li2—Al1^xvi	134.8 (7)
O1ⁱ—Li1—Li2^vii	52.6 (10)	Al1^xv—Li2—Al1^xvi	104.6 (11)
O1ⁱⁱ—Li1—Li2^vii	96.5 (4)	O1^x—B1—O1^xvii	119.981 (12)
O1ⁱⁱⁱ—Li1—Li2^vii	70.29 (8)	O1^x—B1—O1	119.980 (12)
Li2^iv—Li1—Li2^vii	100 (2)	O1^xvii—B1—O1	119.982 (12)
Li2^v—Li1—Li2^vii	114.4 (12)	O1^xviii—Al1—O1^xix	107.09 (6)
Li2^vi—Li1—Li2^vii	114.4 (12)	O1^xviii—Al1—O1^xvii	114.35 (13)
O1—Li1—Cl1	80.00 (5)	O1^xix—Al1—O1^xvii	107.09 (6)
O1ⁱ—Li1—Cl1	80.00 (5)	O1^xviii—Al1—O1^xx	107.09 (6)
O1ⁱⁱ—Li1—Cl1	100.00 (5)	O1^xix—Al1—O1^xx	114.35 (13)
O1ⁱⁱⁱ—Li1—Cl1	100.00 (5)	O1^xvii—Al1—O1^xx	107.09 (6)
Li2^iv—Li1—Cl1	130.0 (11)	O1^xviii—Al1—Li2ⁱ	153.8 (2)
Li2^v—Li1—Cl1	50.0 (11)	O1^xix—Al1—Li2ⁱ	49.7 (3)
Li2^vi—Li1—Cl1	50.0 (11)	O1^xvii—Al1—Li2ⁱ	69.9 (9)
Li2^vii—Li1—Cl1	130.0 (11)	O1^xx—Al1—Li2ⁱ	95.3 (7)
O1—Li1—Al1^viii	150.78 (5)	O1^xviii—Al1—Li2^xxi	69.9 (9)
O1ⁱ—Li1—Al1^viii	29.22 (5)	O1^xix—Al1—Li2^xxi	95.3 (7)
O1ⁱⁱ—Li1—Al1^viii	62.85 (5)	O1^xvii—Al1—Li2^xxi	153.8 (2)
O1ⁱⁱⁱ—Li1—Al1^viii	117.15 (5)	O1^xx—Al1—Li2^xxi	49.7 (3)
Li2^iv—Li1—Al1^viii	122.8 (6)	Li2ⁱ—Al1—Li2^xxi	118.5 (19)
Li2^v—Li1—Al1^viii	57.2 (6)	O1^xviii—Al1—Li2^xxii	95.3 (7)
Li2^vi—Li1—Al1^viii	122.8 (6)	O1^xix—Al1—Li2^xxii	153.8 (2)
Li2^vii—Li1—Al1^viii	57.2 (6)	O1^xvii—Al1—Li2^xxii	49.7 (3)
Cl1—Li1—Al1^viii	90.0	O1^xx—Al1—Li2^xxii	69.9 (9)
O1—Li1—Al1^ix	117.15 (5)	Li2ⁱ—Al1—Li2^xxii	105.2 (9)
O1ⁱ—Li1—Al1^ix	62.85 (5)	Li2^xxi—Al1—Li2^xxii	105.2 (9)
O1ⁱⁱ—Li1—Al1^ix	150.78 (5)	O1^xviii—Al1—Li2^xxiii	49.7 (3)
O1ⁱⁱⁱ—Li1—Al1^ix	29.22 (5)	O1^xix—Al1—Li2^xxiii	69.9 (9)
Li2^iv—Li1—Al1^ix	122.8 (6)	O1^xvii—Al1—Li2^xxiii	95.3 (7)
Li2^v—Li1—Al1^ix	122.8 (6)	O1^xx—Al1—Li2^xxiii	153.8 (2)
Li2^vi—Li1—Al1^ix	57.2 (6)	Li2ⁱ—Al1—Li2^xxiii	105.2 (9)
Li2^vii—Li1—Al1^ix	57.2 (6)	Li2^xxi—Al1—Li2^xxiii	105.2 (9)
Cl1—Li1—Al1^ix	90.0	Li2^xxii—Al1—Li2^xxiii	118.5 (19)
Al1^viii—Li1—Al1^ix	90.0	O1^xviii—Al1—Li1^xxiv	78.09 (5)
O1—Li1—Al1^x	29.22 (5)	O1^xix—Al1—Li1^xxiv	144.55 (6)
O1ⁱ—Li1—Al1^x	150.78 (5)	O1^xvii—Al1—Li1^xxiv	101.91 (5)
O1ⁱⁱ—Li1—Al1^x	117.15 (5)	O1^xx—Al1—Li1^xxiv	35.45 (6)
O1ⁱⁱⁱ—Li1—Al1^x	62.85 (5)	Li2ⁱ—Al1—Li1^xxiv	127.4 (4)
Li2^iv—Li1—Al1^x	57.2 (6)	Li2^xxi—Al1—Li1^xxiv	52.6 (4)
Li2^v—Li1—Al1^x	122.8 (6)	Li2^xxii—Al1—Li1^xxiv	52.6 (4)
Li2^vi—Li1—Al1^x	57.2 (6)	Li2^xxiii—Al1—Li1^xxiv	127.4 (4)
Li2^vii—Li1—Al1^x	122.8 (6)	O1^xviii—Al1—Li1^x	101.91 (5)
Cl1—Li1—Al1^x	90.0	O1^xix—Al1—Li1^x	35.45 (6)
Al1^viii—Li1—Al1^x	180.0	O1^xvii—Al1—Li1^x	78.09 (5)
Al1^ix—Li1—Al1^x	90.0	O1^xx—Al1—Li1^x	144.55 (6)
O1^xi—Li2—O1^xii	97.0 (15)	Li2ⁱ—Al1—Li1^x	52.6 (4)
O1^xi—Li2—O1^xiii	97.0 (15)	Li2^xxi—Al1—Li1^x	127.4 (4)
O1^xii—Li2—O1^xiii	97.0 (15)	Li2^xxii—Al1—Li1^x	127.4 (4)
O1^xi—Li2—Cl1	120.1 (12)	Li2^xxiii—Al1—Li1^x	52.6 (4)
O1^xii—Li2—Cl1	120.1 (12)	Li1^xxiv—Al1—Li1^x	180.0
O1^xiii—Li2—Cl1	120.1 (12)	O1^xviii—Al1—Li1^xvii	144.55 (6)
O1^xi—Li2—Li1^xiv	107.0 (3)	O1^xix—Al1—Li1^xvii	101.91 (5)
O1^xii—Li2—Li1^xiv	139.1 (8)	O1^xvii—Al1—Li1^xvii	35.45 (6)
O1^xiii—Li2—Li1^xiv	48.29 (9)	O1^xx—Al1—Li1^xvii	78.09 (5)
Cl1—Li2—Li1^xiv	75.3 (11)	Li2ⁱ—Al1—Li1^xvii	52.6 (4)
O1^xi—Li2—Li1^ix	139.1 (8)	Li2^xxi—Al1—Li1^xvii	127.4 (4)
O1^xii—Li2—Li1^ix	48.29 (9)	Li2^xxii—Al1—Li1^xvii	52.6 (4)
O1^xiii—Li2—Li1^ix	107.0 (3)	Li2^xxiii—Al1—Li1^xvii	127.4 (4)
Cl1—Li2—Li1^ix	75.3 (11)	Li1^xxiv—Al1—Li1^xvii	90.0
Li1^xiv—Li2—Li1^ix	113.8 (9)	Li1^x—Al1—Li1^xvii	90.0
O1^xi—Li2—Li1^vi	48.29 (9)	O1^xviii—Al1—Li1^xviii	35.45 (6)
O1^xii—Li2—Li1^vi	107.0 (3)	O1^xix—Al1—Li1^xviii	78.09 (5)
O1^xiii—Li2—Li1^vi	139.1 (8)	O1^xvii—Al1—Li1^xviii	144.55 (6)
Cl1—Li2—Li1^vi	75.3 (11)	O1^xx—Al1—Li1^xviii	101.91 (5)
Li1^xiv—Li2—Li1^vi	113.8 (9)	Li2ⁱ—Al1—Li1^xviii	127.4 (4)
Li1^ix—Li2—Li1^vi	113.8 (9)	Li2^xxi—Al1—Li1^xviii	52.6 (4)
O1^xi—Li2—O1^ix	158 (2)	Li2^xxii—Al1—Li1^xviii	127.4 (4)
O1^xii—Li2—O1^ix	71.54 (19)	Li2^xxiii—Al1—Li1^xviii	52.6 (4)
O1^xiii—Li2—O1^ix	66.73 (16)	Li1^xxiv—Al1—Li1^xviii	90.0
Cl1—Li2—O1^ix	81.8 (11)	Li1^x—Al1—Li1^xviii	90.0
Li1^xiv—Li2—O1^ix	74.1 (3)	Li1^xvii—Al1—Li1^xviii	180.0
Li1^ix—Li2—O1^ix	43.90 (17)	B1—O1—Al1^x	118.97 (12)
Li1^vi—Li2—O1^ix	152.3 (17)	B1—O1—Li1	118.1 (2)
O1^xi—Li2—O1^xiv	66.73 (16)	Al1^x—O1—Li1	115.33 (9)
O1^xii—Li2—O1^xiv	158 (2)	B1—O1—Li2^iv	123.5 (10)
O1^xiii—Li2—O1^xiv	71.54 (19)	Al1^x—O1—Li2^iv	93.18 (8)
Cl1—Li2—O1^xiv	81.8 (11)	Li1—O1—Li2^iv	79.2 (11)
Li1^xiv—Li2—O1^xiv	43.90 (17)	Li2—Cl1—Li2ⁱ	109.471 (6)
Li1^ix—Li2—O1^xiv	152.3 (17)	Li2—Cl1—Li2^vi	109.471 (1)
Li1^vi—Li2—O1^xiv	74.1 (3)	Li2ⁱ—Cl1—Li2^vi	109.5
O1^ix—Li2—O1^xiv	118.0 (5)	Li2—Cl1—Li2^v	109.471 (3)
O1^xi—Li2—O1^vi	71.54 (19)	Li2ⁱ—Cl1—Li2^v	109.471 (1)
O1^xii—Li2—O1^vi	66.73 (16)	Li2^vi—Cl1—Li2^v	109.471 (1)
O1^xiii—Li2—O1^vi	158 (2)	Li2—Cl1—Li1	125.264 (1)
Cl1—Li2—O1^vi	81.8 (11)	Li2ⁱ—Cl1—Li1	125.264 (1)
Li1^xiv—Li2—O1^vi	152.3 (17)	Li2^vi—Cl1—Li1	54.736 (1)
Li1^ix—Li2—O1^vi	74.1 (3)	Li2^v—Cl1—Li1	54.736 (1)
Li1^vi—Li2—O1^vi	43.90 (17)

Symmetry codes: (i) x, −y+1/2, −z+1/2; (ii) −x, −z+1/2, y; (iii) −x, z, −y+1/2; (iv) y−1/2, −x+1/2, −z+1/2; (v) −x+1/2, y, −z+1/2; (vi) −x+1/2, −y+1/2, z; (vii) y−1/2, x, z; (viii) −y, z+1/2, −x+1/2; (ix) z, −x+1/2, −y+1/2; (x) y, z, x; (xi) x+1/2, −z+1/2, −y+1/2; (xii) −y+1/2, x+1/2, −z+1/2; (xiii) −z+1/2, −y+1/2, x+1/2; (xiv) −y+1/2, z, −x+1/2; (xv) y+1/2, z+1/2, x; (xvi) x, y+1/2, z+1/2; (xvii) z, x, y; (xviii) z, −x, −y; (xix) −z+1/2, y, −x; (xx) −z+1/2, −y, x; (xxi) x, y−1/2, z−1/2; (xxii) −y+1/2, x−1/2, −z+1/2; (xxiii) −y+1/2, −x+1/2, z−1/2; (xxiv) −y+1/2, z−1/2, −x.

Lithium aluminoboracite (kjh0818yoshinoL14_0m_a_1) top

Crystal data top

Li₄B₄Al₃O₁₂Cl	Cu Kα radiation, λ = 1.54178 Å
M_r = 379.39	Cell parameters from 2808 reflections
Cubic, F23	θ = 6.8–73.2°
a = 12.9839 (1) Å	µ = 6.12 mm⁻¹
V = 2188.85 (5) Å³	T = 297 K
Z = 8	Plate, colorless
F(000) = 1472	0.11 × 0.10 × 0.06 mm
D_x = 2.303 Mg m⁻³

Data collection top

Bruker D8 goniometer diffractometer	389 independent reflections
Radiation source: sealed tube	317 reflections with I > 2σ(I)
Detector resolution: 7.3910 pixels mm^-1	R_int = 0.024
ω scans	θ_max = 73.2°, θ_min = 5.9°
Absorption correction: multi-scan (SADABS; Krause et al., 2015)	h = −15→12
T_min = 0.62, T_max = 0.75	k = −15→16
4728 measured reflections	l = −16→15

Refinement top

Refinement on F²	1 restraint
Least-squares matrix: full	w = 1/[σ²(F_o²) + (0.0537P)² + 1.5774P] where P = (F_o² + 2F_c²)/3
R[F² > 2σ(F²)] = 0.032	(Δ/σ)_max = 0.003
wR(F²) = 0.081	Δρ_max = 0.20 e Å⁻³
S = 1.17	Δρ_min = −0.91 e Å⁻³
389 reflections	Absolute structure: Flack x determined using 132 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons et al., 2013).
50 parameters	Absolute structure parameter: −0.03 (2)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Li1	0.020 (4)	0.250000	0.250000	0.047 (13)	0.5
Li2	0.517 (5)	0.750000	0.750000	0.050 (15)	0.5
Li3	0.363 (3)	0.363 (3)	0.363 (3)	0.020 (12)	0.205 (14)
Li4	0.864 (2)	0.864 (2)	0.864 (2)	0.035 (12)	0.295 (14)
B1	0.1060 (3)	0.1060 (3)	0.1060 (3)	0.0112 (10)
B2	0.6057 (3)	0.6057 (3)	0.6057 (3)	0.0119 (10)
Al1	0.24997 (11)	0.000000	0.000000	0.0118 (5)
O1	0.02797 (13)	0.11005 (14)	0.17683 (14)	0.0170 (5)
O2	0.02784 (13)	0.17681 (14)	0.61004 (14)	0.0171 (5)
Cl1	0.250000	0.250000	0.250000	0.0774 (16)
Cl2	0.750000	0.750000	0.750000	0.0786 (16)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Li1	0.08 (3)	0.015 (11)	0.040 (17)	0.000	0.000	−0.012 (14)
Li2	0.11 (5)	0.031 (14)	0.010 (11)	0.000	0.000	−0.008 (13)
Li3	0.020 (12)	0.020 (12)	0.020 (12)	−0.004 (10)	−0.004 (10)	−0.004 (10)
Li4	0.035 (12)	0.035 (12)	0.035 (12)	0.000 (10)	0.000 (10)	0.000 (10)
B1	0.0112 (10)	0.0112 (10)	0.0112 (10)	−0.0005 (15)	−0.0005 (15)	−0.0005 (15)
B2	0.0119 (10)	0.0119 (10)	0.0119 (10)	−0.0001 (15)	−0.0001 (15)	−0.0001 (15)
Al1	0.0115 (6)	0.0119 (6)	0.0120 (6)	0.000	0.000	0.0003 (4)
O1	0.0185 (10)	0.0161 (9)	0.0164 (10)	0.0050 (6)	0.0069 (9)	0.0048 (9)
O2	0.0196 (11)	0.0164 (10)	0.0154 (9)	0.0071 (9)	0.0050 (6)	0.0048 (9)
Cl1	0.0774 (16)	0.0774 (16)	0.0774 (16)	0.000	0.000	0.000
Cl2	0.0786 (16)	0.0786 (16)	0.0786 (16)	0.000	0.000	0.000

Geometric parameters (Å, º) top

Li1—Li2ⁱ	0.48 (10)	Li3—O2^xxiii	2.23 (3)
Li1—O1ⁱⁱ	2.053 (3)	Li3—O2^xxiv	2.23 (3)
Li1—O1	2.053 (3)	Li3—Cl1	2.55 (6)
Li1—O2ⁱⁱⁱ	2.143 (16)	Li3—O1^xxv	2.824 (8)
Li1—O2^iv	2.143 (16)	Li3—O1^xxvi	2.824 (8)
Li1—Li3^v	2.57 (4)	Li3—O1^vi	2.824 (8)
Li1—Li3^vi	2.57 (4)	Li4—O1^xxvii	2.23 (3)
Li1—Li4^vii	2.91 (4)	Li4—O1^xxviii	2.23 (3)
Li1—Li4^viii	2.91 (4)	Li4—O1^xxix	2.23 (3)
Li1—Cl1	2.98 (6)	Li4—Cl2	2.55 (5)
Li1—Al1^ix	3.256 (5)	Li4—O2^xxx	2.826 (8)
Li1—Al1^x	3.256 (5)	Li4—O2^xxxi	2.826 (8)
Li2—O2^xi	2.056 (4)	Li4—O2^xxxii	2.826 (8)
Li2—O2^xii	2.056 (4)	Li4—Al1^xxxiii	2.91 (2)
Li2—O1^xiii	2.132 (16)	Li4—Al1^xxxiv	2.91 (2)
Li2—O1^xiv	2.132 (16)	B1—O1	1.3693 (17)
Li2—Li4^xv	2.60 (4)	B1—O1^ix	1.3693 (17)
Li2—Li4^xvi	2.60 (4)	B1—O1^x	1.3693 (17)
Li2—Li3^xvii	2.88 (4)	B2—O2^xxxv	1.3702 (17)
Li2—Li3^xviii	2.88 (4)	B2—O2^xii	1.3702 (17)
Li2—Cl2	3.03 (6)	B2—O2^xxxvi	1.3702 (17)
Li2—Al1^xix	3.253 (4)	Al1—O1^xxxvii	1.754 (2)
Li2—Al1^xx	3.253 (4)	Al1—O2^xxxviii	1.754 (2)
Li2—Al1^xxi	3.253 (4)	Al1—O1^x	1.754 (2)
Li3—O2^xxii	2.23 (3)	Al1—O2^xxxix	1.754 (2)

Li2ⁱ—Li1—O1ⁱⁱ	92.8 (16)	Li2^xvi—Li4—Li2^xliii	110.8 (14)
Li2ⁱ—Li1—O1	92.8 (16)	Li2^xlii—Li4—Li2^xliii	110.9 (14)
O1ⁱⁱ—Li1—O1	174 (3)	O1^xxvii—Li4—O2^xxx	157 (2)
Li2ⁱ—Li1—O2ⁱⁱⁱ	73.1 (14)	O1^xxviii—Li4—O2^xxx	71.5 (2)
O1ⁱⁱ—Li1—O2ⁱⁱⁱ	90.8 (4)	O1^xxix—Li4—O2^xxx	66.70 (16)
O1—Li1—O2ⁱⁱⁱ	90.8 (4)	Cl2—Li4—O2^xxx	82.1 (11)
Li2ⁱ—Li1—O2^iv	73.1 (14)	Li2^xvi—Li4—O2^xxx	44.3 (2)
O1ⁱⁱ—Li1—O2^iv	90.8 (4)	Li2^xlii—Li4—O2^xxx	74.0 (4)
O1—Li1—O2^iv	90.8 (4)	Li2^xliii—Li4—O2^xxx	150 (2)
O2ⁱⁱⁱ—Li1—O2^iv	146 (3)	O1^xxvii—Li4—O2^xxxi	66.70 (16)
Li2ⁱ—Li1—Li3^v	126.0 (15)	O1^xxviii—Li4—O2^xxxi	157 (2)
O1ⁱⁱ—Li1—Li3^v	74.3 (8)	O1^xxix—Li4—O2^xxxi	71.5 (2)
O1—Li1—Li3^v	102.3 (12)	Cl2—Li4—O2^xxxi	82.1 (11)
O2ⁱⁱⁱ—Li1—Li3^v	55.4 (12)	Li2^xvi—Li4—O2^xxxi	150 (2)
O2^iv—Li1—Li3^v	155 (2)	Li2^xlii—Li4—O2^xxxi	44.3 (2)
Li2ⁱ—Li1—Li3^vi	126.0 (15)	Li2^xliii—Li4—O2^xxxi	74.0 (4)
O1ⁱⁱ—Li1—Li3^vi	102.3 (12)	O2^xxx—Li4—O2^xxxi	118.2 (5)
O1—Li1—Li3^vi	74.3 (8)	O1^xxvii—Li4—O2^xxxii	71.5 (2)
O2ⁱⁱⁱ—Li1—Li3^vi	155 (2)	O1^xxviii—Li4—O2^xxxii	66.70 (16)
O2^iv—Li1—Li3^vi	55.4 (12)	O1^xxix—Li4—O2^xxxii	157 (2)
Li3^v—Li1—Li3^vi	108 (3)	Cl2—Li4—O2^xxxii	82.1 (11)
Li2ⁱ—Li1—Li4^vii	45.7 (13)	Li2^xvi—Li4—O2^xxxii	74.0 (4)
O1ⁱⁱ—Li1—Li4^vii	136 (2)	Li2^xlii—Li4—O2^xxxii	150 (2)
O1—Li1—Li4^vii	49.6 (13)	Li2^xliii—Li4—O2^xxxii	44.3 (2)
O2ⁱⁱⁱ—Li1—Li4^vii	65.9 (10)	O2^xxx—Li4—O2^xxxii	118.2 (5)
O2^iv—Li1—Li4^vii	90.1 (14)	O2^xxxi—Li4—O2^xxxii	118.2 (5)
Li3^v—Li1—Li4^vii	114.3 (10)	O1^xxvii—Li4—Al1^xxxiii	68.7 (7)
Li3^vi—Li1—Li4^vii	114.3 (10)	O1^xxviii—Li4—Al1^xxxiii	37.0 (3)
Li2ⁱ—Li1—Li4^viii	45.7 (13)	O1^xxix—Li4—Al1^xxxiii	122 (2)
O1ⁱⁱ—Li1—Li4^viii	49.6 (13)	Cl2—Li4—Al1^xxxiii	114.3 (9)
O1—Li1—Li4^viii	136 (2)	Li2^xvi—Li4—Al1^xxxiii	72.2 (6)
O2ⁱⁱⁱ—Li1—Li4^viii	90.1 (14)	Li2^xlii—Li4—Al1^xxxiii	174 (2)
O2^iv—Li1—Li4^viii	65.9 (10)	Li2^xliii—Li4—Al1^xxxiii	72.2 (6)
Li3^v—Li1—Li4^viii	114.3 (10)	O2^xxx—Li4—Al1^xxxiii	106.3 (4)
Li3^vi—Li1—Li4^viii	114.3 (10)	O2^xxxi—Li4—Al1^xxxiii	134.6 (7)
Li4^vii—Li1—Li4^viii	91 (3)	O2^xxxii—Li4—Al1^xxxiii	35.59 (12)
Li2ⁱ—Li1—Cl1	180.0	O1^xxvii—Li4—Al1^xxxiv	37.0 (3)
O1ⁱⁱ—Li1—Cl1	87.2 (16)	O1^xxviii—Li4—Al1^xxxiv	122 (2)
O1—Li1—Cl1	87.2 (16)	O1^xxix—Li4—Al1^xxxiv	68.7 (7)
O2ⁱⁱⁱ—Li1—Cl1	106.9 (14)	Cl2—Li4—Al1^xxxiv	114.3 (9)
O2^iv—Li1—Cl1	106.9 (14)	Li2^xvi—Li4—Al1^xxxiv	174 (2)
Li3^v—Li1—Cl1	54.0 (15)	Li2^xlii—Li4—Al1^xxxiv	72.2 (6)
Li3^vi—Li1—Cl1	54.0 (15)	Li2^xliii—Li4—Al1^xxxiv	72.2 (6)
Li4^vii—Li1—Cl1	134.3 (13)	O2^xxx—Li4—Al1^xxxiv	134.6 (7)
Li4^viii—Li1—Cl1	134.3 (13)	O2^xxxi—Li4—Al1^xxxiv	35.59 (12)
Li2ⁱ—Li1—Al1^ix	85.4 (10)	O2^xxxii—Li4—Al1^xxxiv	106.3 (4)
O1ⁱⁱ—Li1—Al1^ix	152.41 (19)	Al1^xxxiii—Li4—Al1^xxxiv	104.3 (11)
O1—Li1—Al1^ix	28.56 (17)	O1—B1—O1^ix	119.972 (15)
O2ⁱⁱⁱ—Li1—Al1^ix	114.7 (7)	O1—B1—O1^x	119.972 (15)
O2^iv—Li1—Al1^ix	62.3 (2)	O1^ix—B1—O1^x	119.972 (15)
Li3^v—Li1—Al1^ix	128.1 (12)	O2^xxxv—B2—O2^xii	119.982 (12)
Li3^vi—Li1—Al1^ix	58.5 (7)	O2^xxxv—B2—O2^xxxvi	119.982 (13)
Li4^vii—Li1—Al1^ix	55.9 (7)	O2^xii—B2—O2^xxxvi	119.982 (12)
Li4^viii—Li1—Al1^ix	116.6 (14)	O1^xxxvii—Al1—O2^xxxviii	107.12 (9)
Cl1—Li1—Al1^ix	94.6 (10)	O1^xxxvii—Al1—O1^x	114.42 (15)
Li2ⁱ—Li1—Al1^x	85.4 (10)	O2^xxxviii—Al1—O1^x	107.03 (8)
O1ⁱⁱ—Li1—Al1^x	117.73 (11)	O1^xxxvii—Al1—O2^xxxix	107.03 (8)
O1—Li1—Al1^x	62.78 (10)	O2^xxxviii—Al1—O2^xxxix	114.35 (15)
O2ⁱⁱⁱ—Li1—Al1^x	29.72 (10)	O1^x—Al1—O2^xxxix	107.12 (9)
O2^iv—Li1—Al1^x	145.3 (15)	O1^xxxvii—Al1—Li4^xliv	95.5 (7)
Li3^v—Li1—Al1^x	58.5 (7)	O2^xxxviii—Al1—Li4^xliv	153.8 (2)
Li3^vi—Li1—Al1^x	128.1 (12)	O1^x—Al1—Li4^xliv	49.8 (3)
Li4^vii—Li1—Al1^x	55.9 (7)	O2^xxxix—Al1—Li4^xliv	69.7 (8)
Li4^viii—Li1—Al1^x	116.6 (14)	O1^xxxvii—Al1—Li4^xlv	49.8 (3)
Cl1—Li1—Al1^x	94.6 (10)	O2^xxxviii—Al1—Li4^xlv	69.7 (8)
Al1^ix—Li1—Al1^x	89.62 (17)	O1^x—Al1—Li4^xlv	95.5 (7)
O2^xi—Li2—O2^xii	172 (3)	O2^xxxix—Al1—Li4^xlv	153.8 (2)
O2^xi—Li2—O1^xiii	91.1 (4)	Li4^xliv—Al1—Li4^xlv	119.1 (19)
O2^xii—Li2—O1^xiii	91.1 (4)	O1^xxxvii—Al1—Li3ⁱⁱ	153.8 (2)
O2^xi—Li2—O1^xiv	91.1 (4)	O2^xxxviii—Al1—Li3ⁱⁱ	49.8 (3)
O2^xii—Li2—O1^xiv	91.1 (4)	O1^x—Al1—Li3ⁱⁱ	69.5 (9)
O1^xiii—Li2—O1^xiv	148 (3)	O2^xxxix—Al1—Li3ⁱⁱ	95.6 (7)
O2^xi—Li2—Li4^xv	101.4 (13)	Li4^xliv—Al1—Li3ⁱⁱ	104.9 (7)
O2^xii—Li2—Li4^xv	73.7 (9)	Li4^xlv—Al1—Li3ⁱⁱ	104.9 (7)
O1^xiii—Li2—Li4^xv	154 (2)	O1^xxxvii—Al1—Li3^xli	69.5 (9)
O1^xiv—Li2—Li4^xv	55.1 (12)	O2^xxxviii—Al1—Li3^xli	95.6 (7)
O2^xi—Li2—Li4^xvi	73.7 (9)	O1^x—Al1—Li3^xli	153.8 (2)
O2^xii—Li2—Li4^xvi	101.4 (13)	O2^xxxix—Al1—Li3^xli	49.8 (3)
O1^xiii—Li2—Li4^xvi	55.1 (12)	Li4^xliv—Al1—Li3^xli	104.9 (7)
O1^xiv—Li2—Li4^xvi	154 (2)	Li4^xlv—Al1—Li3^xli	104.9 (7)
Li4^xv—Li2—Li4^xvi	107 (3)	Li3ⁱⁱ—Al1—Li3^xli	119 (2)
O2^xi—Li2—Li3^xvii	137 (2)	O1^xxxvii—Al1—Li2^xlvi	37.0 (5)
O2^xii—Li2—Li3^xvii	50.2 (14)	O2^xxxviii—Al1—Li2^xlvi	74.9 (9)
O1^xiii—Li2—Li3^xvii	66.6 (10)	O1^x—Al1—Li2^xlvi	143.0 (5)
O1^xiv—Li2—Li3^xvii	91.1 (15)	O2^xxxix—Al1—Li2^xlvi	105.1 (9)
Li4^xv—Li2—Li3^xvii	114.4 (10)	Li4^xliv—Al1—Li2^xlvi	130.5 (9)
Li4^xvi—Li2—Li3^xvii	114.4 (10)	Li4^xlv—Al1—Li2^xlvi	49.5 (9)
O2^xi—Li2—Li3^xviii	50.2 (13)	Li3ⁱⁱ—Al1—Li2^xlvi	124.6 (9)
O2^xii—Li2—Li3^xviii	137 (2)	Li3^xli—Al1—Li2^xlvi	55.4 (9)
O1^xiii—Li2—Li3^xviii	91.1 (15)	O1^xxxvii—Al1—Li2^xlvii	98.7 (9)
O1^xiv—Li2—Li3^xviii	66.6 (10)	O2^xxxviii—Al1—Li2^xlvii	34.2 (3)
Li4^xv—Li2—Li3^xviii	114.4 (10)	O1^x—Al1—Li2^xlvii	81.3 (9)
Li4^xvi—Li2—Li3^xviii	114.4 (10)	O2^xxxix—Al1—Li2^xlvii	145.8 (3)
Li3^xvii—Li2—Li3^xviii	92 (3)	Li4^xliv—Al1—Li2^xlvii	130.5 (9)
O2^xi—Li2—Cl2	86.0 (17)	Li4^xlv—Al1—Li2^xlvii	49.5 (9)
O2^xii—Li2—Cl2	86.0 (17)	Li3ⁱⁱ—Al1—Li2^xlvii	55.4 (9)
O1^xiii—Li2—Cl2	105.9 (15)	Li3^xli—Al1—Li2^xlvii	124.6 (9)
O1^xiv—Li2—Cl2	105.9 (15)	Li2^xlvi—Al1—Li2^xlvii	82 (2)
Li4^xv—Li2—Cl2	53.3 (15)	O1^xxxvii—Al1—Li2^xlviii	81.3 (9)
Li4^xvi—Li2—Cl2	53.3 (15)	O2^xxxviii—Al1—Li2^xlviii	145.8 (3)
Li3^xvii—Li2—Cl2	133.8 (13)	O1^x—Al1—Li2^xlviii	98.7 (9)
Li3^xviii—Li2—Cl2	133.8 (13)	O2^xxxix—Al1—Li2^xlviii	34.2 (3)
O2^xi—Li2—Al1^xix	117.76 (6)	Li4^xliv—Al1—Li2^xlviii	49.5 (9)
O2^xii—Li2—Al1^xix	62.84 (9)	Li4^xlv—Al1—Li2^xlviii	130.5 (9)
O1^xiii—Li2—Al1^xix	29.66 (11)	Li3ⁱⁱ—Al1—Li2^xlviii	124.6 (9)
O1^xiv—Li2—Al1^xix	146.3 (15)	Li3^xli—Al1—Li2^xlviii	55.4 (9)
Li4^xv—Li2—Al1^xix	127.3 (13)	Li2^xlvi—Al1—Li2^xlviii	98 (2)
Li4^xvi—Li2—Al1^xix	58.3 (7)	Li2^xlvii—Al1—Li2^xlviii	179.99 (5)
Li3^xvii—Li2—Al1^xix	56.2 (7)	O1^xxxvii—Al1—Li2^xlix	143.0 (5)
Li3^xviii—Li2—Al1^xix	117.5 (15)	O2^xxxviii—Al1—Li2^xlix	105.1 (9)
Cl2—Li2—Al1^xix	93.9 (10)	O1^x—Al1—Li2^xlix	37.0 (5)
O2^xi—Li2—Al1^xx	152.45 (6)	O2^xxxix—Al1—Li2^xlix	74.9 (9)
O2^xii—Li2—Al1^xx	28.68 (17)	Li4^xliv—Al1—Li2^xlix	49.5 (9)
O1^xiii—Li2—Al1^xx	115.2 (7)	Li4^xlv—Al1—Li2^xlix	130.5 (9)
O1^xiv—Li2—Al1^xx	62.41 (19)	Li3ⁱⁱ—Al1—Li2^xlix	55.4 (9)
Li4^xv—Li2—Al1^xx	58.3 (7)	Li3^xli—Al1—Li2^xlix	124.6 (9)
Li4^xvi—Li2—Al1^xx	127.3 (13)	Li2^xlvi—Al1—Li2^xlix	180.0 (17)
Li3^xvii—Li2—Al1^xx	56.2 (7)	Li2^xlvii—Al1—Li2^xlix	98 (2)
Li3^xviii—Li2—Al1^xx	117.5 (15)	Li2^xlviii—Al1—Li2^xlix	82 (2)
Cl2—Li2—Al1^xx	93.9 (10)	B1—O1—Al1^ix	119.05 (13)
Al1^xix—Li2—Al1^xx	89.75 (15)	B1—O1—Li1	112.4 (12)
O2^xi—Li2—Al1^xxi	28.68 (17)	Al1^ix—O1—Li1	117.4 (4)
O2^xii—Li2—Al1^xxi	152.45 (6)	B1—O1—Li2ⁱ	122.3 (12)
O1^xiii—Li2—Al1^xxi	62.41 (19)	Al1^ix—O1—Li2ⁱ	113.4 (6)
O1^xiv—Li2—Al1^xxi	115.2 (7)	Li1—O1—Li2ⁱ	13 (3)
Li4^xv—Li2—Al1^xxi	127.3 (13)	B1—O1—Li4^vii	123.9 (9)
Li4^xvi—Li2—Al1^xxi	58.3 (7)	Al1^ix—O1—Li4^vii	93.12 (8)
Li3^xvii—Li2—Al1^xxi	117.5 (15)	Li1—O1—Li4^vii	85.7 (19)
Li3^xviii—Li2—Al1^xxi	56.2 (7)	Li2ⁱ—O1—Li4^vii	73.2 (19)
Cl2—Li2—Al1^xxi	93.9 (10)	B1—O1—Li3^vi	102.2 (9)
Al1^xix—Li2—Al1^xxi	89.73 (15)	Al1^ix—O1—Li3^vi	74.9 (10)
Al1^xx—Li2—Al1^xxi	172 (2)	Li1—O1—Li3^vi	61.3 (10)
O2^xxii—Li3—O2^xxiii	96.4 (16)	Li2ⁱ—O1—Li3^vi	69.5 (10)
O2^xxii—Li3—O2^xxiv	96.4 (16)	Li4^vii—O1—Li3^vi	131.5 (12)
O2^xxiii—Li3—O2^xxiv	96.4 (16)	B1—O1—Li3	75.8 (3)
O2^xxii—Li3—Cl1	120.6 (12)	Al1^ix—O1—Li3	112.35 (10)
O2^xxiii—Li3—Cl1	120.6 (12)	Li1—O1—Li3	50.3 (16)
O2^xxiv—Li3—Cl1	120.6 (12)	Li2ⁱ—O1—Li3	63.2 (15)
O2^xxii—Li3—Li1^vi	108.9 (5)	Li4^vii—O1—Li3	135.3 (9)
O2^xxiii—Li3—Li1^vi	140.8 (8)	Li3^vi—O1—Li3	38.8 (10)
O2^xxiv—Li3—Li1^vi	52.5 (10)	B2^l—O2—Al1^xxvi	118.94 (13)
Cl1—Li3—Li1^vi	71.3 (15)	B2^l—O2—Li2^l	113.5 (13)
O2^xxii—Li3—Li1^xxvi	52.4 (10)	Al1^xxvi—O2—Li2^l	117.1 (5)
O2^xxiii—Li3—Li1^xxvi	108.9 (5)	B2^l—O2—Li1^li	123.2 (11)
O2^xxiv—Li3—Li1^xxvi	140.8 (8)	Al1^xxvi—O2—Li1^li	113.0 (5)
Cl1—Li3—Li1^xxvi	71.3 (15)	Li2^l—O2—Li1^li	13 (3)
Li1^vi—Li3—Li1^xxvi	110.2 (15)	B2^l—O2—Li3^lii	123.8 (10)
O2^xxii—Li3—Li1^xxv	140.8 (8)	Al1^xxvi—O2—Li3^lii	93.19 (8)
O2^xxiii—Li3—Li1^xxv	52.4 (10)	Li2^l—O2—Li3^lii	85 (2)
O2^xxiv—Li3—Li1^xxv	108.9 (5)	Li1^li—O2—Li3^lii	72.1 (18)
Cl1—Li3—Li1^xxv	71.3 (15)	B2^l—O2—Li4^liii	102.4 (9)
Li1^vi—Li3—Li1^xxv	110.2 (15)	Al1^xxvi—O2—Li4^liii	74.7 (10)
Li1^xxvi—Li3—Li1^xxv	110.2 (15)	Li2^l—O2—Li4^liii	62.0 (11)
O2^xxii—Li3—O1^xxv	157 (2)	Li1^li—O2—Li4^liii	70.2 (10)
O2^xxiii—Li3—O1^xxv	71.5 (2)	Li3^lii—O2—Li4^liii	131.4 (12)
O2^xxiv—Li3—O1^xxv	66.68 (17)	B2^l—O2—Li4	82.6 (3)
Cl1—Li3—O1^xxv	82.2 (11)	Al1^xxvi—O2—Li4	90.33 (9)
Li1^vi—Li3—O1^xxv	74.0 (4)	Li2^l—O2—Li4	64.2 (14)
Li1^xxvi—Li3—O1^xxv	149 (2)	Li1^li—O2—Li4	75.6 (13)
Li1^xxv—Li3—O1^xxv	44.4 (3)	Li3^lii—O2—Li4	146.2 (12)
O2^xxii—Li3—O1^xxvi	71.5 (2)	Li4^liii—O2—Li4	21.0 (10)
O2^xxiii—Li3—O1^xxvi	66.68 (17)	Li3—Cl1—Li3ⁱⁱ	109.468 (7)
O2^xxiv—Li3—O1^xxvi	157 (2)	Li3—Cl1—Li3^v	109.473 (3)
Cl1—Li3—O1^xxvi	82.2 (11)	Li3ⁱⁱ—Cl1—Li3^v	109.473 (1)
Li1^vi—Li3—O1^xxvi	149 (2)	Li3—Cl1—Li3^vi	109.473 (1)
Li1^xxvi—Li3—O1^xxvi	44.4 (3)	Li3ⁱⁱ—Cl1—Li3^vi	109.5
Li1^xxv—Li3—O1^xxvi	73.9 (4)	Li3^v—Cl1—Li3^vi	109.468 (2)
O1^xxv—Li3—O1^xxvi	118.2 (5)	Li3—Cl1—Li1	125.266 (1)
O2^xxii—Li3—O1^vi	66.68 (17)	Li3ⁱⁱ—Cl1—Li1	125.266 (4)
O2^xxiii—Li3—O1^vi	157 (2)	Li3^v—Cl1—Li1	54.734 (1)
O2^xxiv—Li3—O1^vi	71.5 (2)	Li3^vi—Cl1—Li1	54.734 (2)
Cl1—Li3—O1^vi	82.2 (11)	Li3—Cl1—Li1^xxvi	54.736 (2)
Li1^vi—Li3—O1^vi	44.4 (3)	Li3ⁱⁱ—Cl1—Li1^xxvi	125.264 (3)
Li1^xxvi—Li3—O1^vi	73.9 (4)	Li3^v—Cl1—Li1^xxvi	54.736 (2)
Li1^xxv—Li3—O1^vi	149 (2)	Li3^vi—Cl1—Li1^xxvi	125.264 (2)
O1^xxv—Li3—O1^vi	118.2 (5)	Li1—Cl1—Li1^xxvi	90.000 (3)
O1^xxvi—Li3—O1^vi	118.2 (5)	Li3—Cl1—Li1^ix	125.264 (5)
O2^xxii—Li3—Li2^xl	45.2 (8)	Li3ⁱⁱ—Cl1—Li1^ix	54.736 (1)
O2^xxiii—Li3—Li2^xl	105.2 (6)	Li3^v—Cl1—Li1^ix	54.736 (2)
O2^xxiv—Li3—Li2^xl	137.0 (11)	Li3^vi—Cl1—Li1^ix	125.264 (4)
Cl1—Li3—Li2^xl	79.1 (13)	Li1—Cl1—Li1^ix	90.000 (3)
Li1^vi—Li3—Li2^xl	113.8 (9)	Li1^xxvi—Cl1—Li1^ix	90.0
Li1^xxvi—Li3—Li2^xl	7.8 (17)	Li3—Cl1—Li1^xxv	54.736 (2)
Li1^xxv—Li3—Li2^xl	113.8 (9)	Li3ⁱⁱ—Cl1—Li1^xxv	125.264 (1)
O1^xxv—Li3—Li2^xl	155.6 (18)	Li3^v—Cl1—Li1^xxv	125.264 (2)
O1^xxvi—Li3—Li2^xl	43.86 (15)	Li3^vi—Cl1—Li1^xxv	54.736 (2)
O1^vi—Li3—Li2^xl	74.5 (3)	Li1—Cl1—Li1^xxv	90.000 (3)
O2^xxii—Li3—Li2^xli	105.2 (6)	Li1^xxvi—Cl1—Li1^xxv	90.0
O2^xxiii—Li3—Li2^xli	137.0 (11)	Li1^ix—Cl1—Li1^xxv	180.0
O2^xxiv—Li3—Li2^xli	45.2 (8)	Li3—Cl1—Li1^x	125.264 (1)
Cl1—Li3—Li2^xli	79.1 (13)	Li3ⁱⁱ—Cl1—Li1^x	54.736 (1)
Li1^vi—Li3—Li2^xli	7.8 (17)	Li3^v—Cl1—Li1^x	125.264 (4)
Li1^xxvi—Li3—Li2^xli	113.8 (9)	Li3^vi—Cl1—Li1^x	54.736 (1)
Li1^xxv—Li3—Li2^xli	113.8 (9)	Li1—Cl1—Li1^x	90.000 (4)
O1^xxv—Li3—Li2^xli	74.5 (3)	Li1^xxvi—Cl1—Li1^x	180.0
O1^xxvi—Li3—Li2^xli	155.6 (18)	Li1^ix—Cl1—Li1^x	90.000 (2)
O1^vi—Li3—Li2^xli	43.86 (15)	Li1^xxv—Cl1—Li1^x	90.0
Li2^xl—Li3—Li2^xli	116.5 (8)	Li3—Cl1—Li1^vi	54.734 (2)
O1^xxvii—Li4—O1^xxviii	96.6 (15)	Li3ⁱⁱ—Cl1—Li1^vi	54.734 (3)
O1^xxvii—Li4—O1^xxix	96.6 (15)	Li3^v—Cl1—Li1^vi	125.266 (2)
O1^xxviii—Li4—O1^xxix	96.6 (15)	Li3^vi—Cl1—Li1^vi	125.266 (1)
O1^xxvii—Li4—Cl2	120.5 (12)	Li1—Cl1—Li1^vi	180.0
O1^xxviii—Li4—Cl2	120.5 (12)	Li1^xxvi—Cl1—Li1^vi	90.000 (5)
O1^xxix—Li4—Cl2	120.5 (12)	Li1^ix—Cl1—Li1^vi	90.0
O1^xxvii—Li4—Li2^xvi	140.6 (8)	Li1^xxv—Cl1—Li1^vi	90.000 (4)
O1^xxviii—Li4—Li2^xvi	51.7 (10)	Li1^x—Cl1—Li1^vi	90.000 (1)
O1^xxix—Li4—Li2^xvi	108.6 (5)	Li4—Cl2—Li4^liv	109.474 (11)
Cl2—Li4—Li2^xvi	71.9 (15)	Li4—Cl2—Li4^xvi	109.470 (2)
O1^xxvii—Li4—Li2^xlii	108.6 (5)	Li4^liv—Cl2—Li4^xvi	109.470 (3)
O1^xxviii—Li4—Li2^xlii	140.6 (8)	Li4—Cl2—Li4^xv	109.470 (6)
O1^xxix—Li4—Li2^xlii	51.7 (10)	Li4^liv—Cl2—Li4^xv	109.5
Cl2—Li4—Li2^xlii	71.9 (15)	Li4^xvi—Cl2—Li4^xv	109.474 (7)
Li2^xvi—Li4—Li2^xlii	110.8 (14)	Li4—Cl2—Li2	125.263 (4)
O1^xxvii—Li4—Li2^xliii	51.7 (10)	Li4^liv—Cl2—Li2	125.263 (12)
O1^xxviii—Li4—Li2^xliii	108.6 (5)	Li4^xvi—Cl2—Li2	54.737 (7)
O1^xxix—Li4—Li2^xliii	140.6 (8)	Li4^xv—Cl2—Li2	54.737 (6)
Cl2—Li4—Li2^xliii	71.9 (15)

Symmetry codes: (i) −x+1/2, −y+1, z−1/2; (ii) x, −y+1/2, −z+1/2; (iii) −x, −y+1/2, z−1/2; (iv) −x, y, −z+1; (v) −x+1/2, y, −z+1/2; (vi) −x+1/2, −y+1/2, z; (vii) x−1, −y+1, −z+1; (viii) x−1, y−1/2, z−1/2; (ix) y, z, x; (x) z, x, y; (xi) x+1/2, −y+1, −z+3/2; (xii) x+1/2, y+1/2, z; (xiii) −x+1/2, y+1/2, −z+1; (xiv) −x+1/2, −y+1, z+1/2; (xv) −x+3/2, y, −z+3/2; (xvi) −x+3/2, −y+3/2, z; (xvii) x, −y+1, −z+1; (xviii) x, y+1/2, z+1/2; (xix) −y+1/2, z+1/2, −x+1; (xx) z+1/2, −x+1, −y+1/2; (xxi) z+1/2, x+1/2, y+1; (xxii) −z+1, x+1/2, −y+1/2; (xxiii) −y+1/2, −z+1, x+1/2; (xxiv) x+1/2, −y+1/2, −z+1; (xxv) −y+1/2, z, −x+1/2; (xxvi) z, −x+1/2, −y+1/2; (xxvii) −z+1, x+1, −y+1; (xxviii) x+1, −y+1, −z+1; (xxix) −y+1, −z+1, x+1; (xxx) −x+1, y+1/2, −z+3/2; (xxxi) y+1/2, −z+3/2, −x+1; (xxxii) −z+3/2, −x+1, y+1/2; (xxxiii) −y+1, z+1, −x+1; (xxxiv) −x+1, −y+1, z+1; (xxxv) y+1/2, z, x+1/2; (xxxvi) z, x+1/2, y+1/2; (xxxvii) z, −x, −y; (xxxviii) −y+1/2, z−1/2, −x; (xxxix) −y+1/2, −z+1/2, x; (xl) z−1/2, x, y−1/2; (xli) x, y−1/2, z−1/2; (xlii) −y+3/2, z, −x+3/2; (xliii) z, −x+3/2, −y+3/2; (xliv) −x+1, y−1, −z+1; (xlv) −x+1, −y+1, z−1; (xlvi) z−1/2, x−1/2, y−1; (xlvii) −y+1, z−1/2, −x+1/2; (xlviii) y−1/2, z−1, x−1/2; (xlix) z−1/2, −x+1/2, −y+1; (l) x−1/2, y−1/2, z; (li) −x, −y+1/2, z+1/2; (lii) x−1/2, −y+1/2, −z+1; (liii) −x+1, y−1/2, −z+3/2; (liv) x, −y+3/2, −z+3/2.

Sodium aluminoboracite (kjh230804yoshinoN4_0m_a) top

Crystal data top

Na_3.92B₄Al₃O₁₂Cl_0.92	Cu Kα radiation, λ = 1.54178 Å
M_r = 438.91	Cell parameters from 3423 reflections
Cubic, F43c	θ = 4.6–74.3°
a = 13.5904 (1) Å	µ = 6.78 mm⁻¹
V = 2510.13 (6) Å³	T = 294 K
Z = 8	Plate, colorless
F(000) = 1728	0.08 × 0.06 × 0.04 mm
D_x = 2.323 Mg m⁻³

Data collection top

Bruker D8 goniometer diffractometer	218 independent reflections
Radiation source: sealed tube	216 reflections with I > 2σ(I)
Detector resolution: 7.3910 pixels mm^-1	R_int = 0.027
ω scans	θ_max = 74.3°, θ_min = 6.5°
Absorption correction: multi-scan (SADABS; Krause et al., 2015)	h = −16→16
T_min = 0.66, T_max = 0.75	k = −16→16
4504 measured reflections	l = −16→14

Refinement top

Refinement on F²	1 restraint
Least-squares matrix: full	w = 1/[σ²(F_o²) + (0.0311P)² + 4.0293P] where P = (F_o² + 2F_c²)/3
R[F² > 2σ(F²)] = 0.022	(Δ/σ)_max < 0.001
wR(F²) = 0.055	Δρ_max = 0.15 e Å⁻³
S = 1.20	Δρ_min = −0.45 e Å⁻³
218 reflections	Absolute structure: Flack x determined using 89 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons et al., 2013)
27 parameters	Absolute structure parameter: 0.01 (3)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Na1	0.0340 (3)	0.250000	0.250000	0.0422 (14)	0.499 (4)
Na2	0.3606 (4)	0.3606 (4)	0.3606 (4)	0.017 (2)	0.231 (6)
B1	0.1039 (2)	0.1039 (2)	0.1039 (2)	0.0143 (9)
Al1	0.250000	0.000000	0.000000	0.0095 (4)
O1	0.03513 (13)	0.10047 (12)	0.17745 (12)	0.0176 (5)
Cl1	0.250000	0.250000	0.250000	0.0350 (9)	0.920 (10)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Na1	0.096 (4)	0.0127 (18)	0.0182 (19)	0.000	0.000	−0.0066 (17)
Na2	0.017 (2)	0.017 (2)	0.017 (2)	−0.0006 (18)	−0.0006 (18)	−0.0006 (18)
B1	0.0143 (9)	0.0143 (9)	0.0143 (9)	0.0015 (12)	0.0015 (12)	0.0015 (12)
Al1	0.0096 (6)	0.0095 (5)	0.0095 (5)	0.000	0.000	0.000
O1	0.0189 (9)	0.0149 (8)	0.0188 (8)	0.0060 (6)	0.0102 (8)	0.0061 (7)
Cl1	0.0350 (9)	0.0350 (9)	0.0350 (9)	0.000	0.000	0.000

Geometric parameters (Å, º) top

Na1—Na1ⁱ	0.923 (8)	Na2—O1^x	2.484 (5)
Na1—O1ⁱⁱ	2.2588 (16)	Na2—Cl1	2.605 (9)
Na1—O1	2.2588 (16)	Na2—O1^xi	2.913 (2)
Na1—O1ⁱⁱⁱ	2.446 (2)	Na2—O1^v	2.913 (2)
Na1—O1ⁱ	2.446 (2)	Na2—O1^xii	2.913 (2)
Na1—Na2^iv	2.564 (4)	Na2—Al1^xiii	3.072 (4)
Na1—Na2^v	2.564 (4)	Na2—Al1^xiv	3.072 (4)
Na1—Cl1	2.936 (4)	B1—O1^xv	1.3692 (15)
Na1—B1ⁱⁱ	2.965 (3)	B1—O1^xvi	1.3692 (15)
Na1—B1	2.965 (3)	B1—O1	1.3693 (15)
Na1—Na2^vi	3.174 (3)	Al1—O1^xvii	1.7506 (16)
Na1—Na2^vii	3.174 (3)	Al1—O1^xviii	1.7506 (16)
Na2—O1^viii	2.484 (5)	Al1—O1^xvi	1.7506 (16)
Na2—O1^ix	2.484 (5)	Al1—O1^xix	1.7506 (16)

Na1ⁱ—Na1—O1ⁱⁱ	90.40 (11)	O1—B1—Na1	46.75 (14)
Na1ⁱ—Na1—O1	90.40 (11)	O1^xv—B1—Na1^xv	46.75 (14)
O1ⁱⁱ—Na1—O1	179.2 (2)	O1^xvi—B1—Na1^xv	87.53 (15)
Na1ⁱ—Na1—O1ⁱⁱⁱ	67.42 (9)	O1—B1—Na1^xv	135.5 (3)
O1ⁱⁱ—Na1—O1ⁱⁱⁱ	90.15 (4)	Na1—B1—Na1^xv	88.88 (15)
O1—Na1—O1ⁱⁱⁱ	90.15 (4)	O1^xv—B1—Na1^xvi	135.5 (3)
Na1ⁱ—Na1—O1ⁱ	67.42 (9)	O1^xvi—B1—Na1^xvi	46.75 (14)
O1ⁱⁱ—Na1—O1ⁱ	90.15 (4)	O1—B1—Na1^xvi	87.53 (15)
O1—Na1—O1ⁱ	90.15 (4)	Na1—B1—Na1^xvi	88.88 (15)
O1ⁱⁱⁱ—Na1—O1ⁱ	134.84 (18)	Na1^xv—B1—Na1^xvi	88.88 (15)
Na1ⁱ—Na1—Na2^iv	124.0 (2)	O1^xvii—Al1—O1^xviii	108.49 (6)
O1ⁱⁱ—Na1—Na2^iv	74.01 (7)	O1^xvii—Al1—O1^xvi	111.44 (11)
O1—Na1—Na2^iv	105.53 (9)	O1^xviii—Al1—O1^xvi	108.49 (6)
O1ⁱⁱⁱ—Na1—Na2^iv	59.39 (18)	O1^xvii—Al1—O1^xix	108.49 (6)
O1ⁱ—Na1—Na2^iv	159.73 (13)	O1^xviii—Al1—O1^xix	111.44 (11)
Na1ⁱ—Na1—Na2^v	124.0 (2)	O1^xvi—Al1—O1^xix	108.49 (6)
O1ⁱⁱ—Na1—Na2^v	105.53 (9)	O1^xvii—Al1—Na2ⁱⁱ	157.64 (7)
O1—Na1—Na2^v	74.01 (7)	O1^xviii—Al1—Na2ⁱⁱ	53.95 (9)
O1ⁱⁱⁱ—Na1—Na2^v	159.73 (13)	O1^xvi—Al1—Na2ⁱⁱ	68.08 (15)
O1ⁱ—Na1—Na2^v	59.39 (18)	O1^xix—Al1—Na2ⁱⁱ	92.12 (11)
Na2^iv—Na1—Na2^v	112.1 (4)	O1^xvii—Al1—Na2^xx	68.08 (15)
Na1ⁱ—Na1—Cl1	180.0	O1^xviii—Al1—Na2^xx	92.12 (11)
O1ⁱⁱ—Na1—Cl1	89.60 (11)	O1^xvi—Al1—Na2^xx	157.64 (7)
O1—Na1—Cl1	89.60 (11)	O1^xix—Al1—Na2^xx	53.95 (9)
O1ⁱⁱⁱ—Na1—Cl1	112.58 (9)	Na2ⁱⁱ—Al1—Na2^xx	121.4 (3)
O1ⁱ—Na1—Cl1	112.58 (9)	O1^xvii—Al1—Na2^xxi	92.12 (11)
Na2^iv—Na1—Cl1	56.0 (2)	O1^xviii—Al1—Na2^xxi	157.64 (7)
Na2^v—Na1—Cl1	56.0 (2)	O1^xvi—Al1—Na2^xxi	53.95 (9)
Na1ⁱ—Na1—B1ⁱⁱ	108.69 (11)	O1^xix—Al1—Na2^xxi	68.08 (15)
O1ⁱⁱ—Na1—B1ⁱⁱ	26.20 (7)	Na2ⁱⁱ—Al1—Na2^xxi	103.87 (13)
O1—Na1—B1ⁱⁱ	153.23 (14)	Na2^xx—Al1—Na2^xxi	103.87 (13)
O1ⁱⁱⁱ—Na1—B1ⁱⁱ	114.17 (5)	O1^xvii—Al1—Na2^xxii	53.95 (9)
O1ⁱ—Na1—B1ⁱⁱ	80.59 (6)	O1^xviii—Al1—Na2^xxii	68.08 (15)
Na2^iv—Na1—B1ⁱⁱ	79.69 (9)	O1^xvi—Al1—Na2^xxii	92.12 (11)
Na2^v—Na1—B1ⁱⁱ	79.69 (9)	O1^xix—Al1—Na2^xxii	157.64 (7)
Cl1—Na1—B1ⁱⁱ	71.31 (11)	Na2ⁱⁱ—Al1—Na2^xxii	103.87 (13)
Na1ⁱ—Na1—B1	108.68 (11)	Na2^xx—Al1—Na2^xxii	103.87 (13)
O1ⁱⁱ—Na1—B1	153.23 (14)	Na2^xxi—Al1—Na2^xxii	121.4 (3)
O1—Na1—B1	26.20 (7)	O1^xvii—Al1—Na1^xxiii	67.96 (7)
O1ⁱⁱⁱ—Na1—B1	80.59 (6)	O1^xviii—Al1—Na1^xxiii	137.41 (6)
O1ⁱ—Na1—B1	114.17 (5)	O1^xvi—Al1—Na1^xxiii	112.04 (7)
Na2^iv—Na1—B1	79.69 (9)	O1^xix—Al1—Na1^xxiii	42.59 (6)
Na2^v—Na1—B1	79.69 (9)	Na2ⁱⁱ—Al1—Na1^xxiii	133.95 (9)
Cl1—Na1—B1	71.32 (11)	Na2^xx—Al1—Na1^xxiii	46.05 (9)
B1ⁱⁱ—Na1—B1	142.6 (2)	Na2^xxi—Al1—Na1^xxiii	58.13 (7)
Na1ⁱ—Na1—Na2^vi	42.07 (17)	Na2^xxii—Al1—Na1^xxiii	121.87 (7)
O1ⁱⁱ—Na1—Na2^vi	129.7 (2)	O1^xvii—Al1—Na1^xvii	35.94 (5)
O1—Na1—Na2^vi	51.10 (16)	O1^xviii—Al1—Na1^xvii	80.49 (8)
O1ⁱⁱⁱ—Na1—Na2^vi	60.81 (7)	O1^xvi—Al1—Na1^xvii	144.06 (5)
O1ⁱ—Na1—Na2^vi	85.28 (12)	O1^xix—Al1—Na1^xvii	99.51 (8)
Na2^iv—Na1—Na2^vi	114.50 (19)	Na2ⁱⁱ—Al1—Na1^xvii	133.95 (9)
Na2^v—Na1—Na2^vi	114.50 (19)	Na2^xx—Al1—Na1^xvii	46.05 (9)
Cl1—Na1—Na2^vi	137.93 (17)	Na2^xxi—Al1—Na1^xvii	121.87 (7)
B1ⁱⁱ—Na1—Na2^vi	150.8 (2)	Na2^xxii—Al1—Na1^xvii	58.13 (7)
B1—Na1—Na2^vi	66.6 (2)	Na1^xxiii—Al1—Na1^xvii	74.52 (12)
Na1ⁱ—Na1—Na2^vii	42.07 (17)	O1^xvii—Al1—Na1^xvi	144.06 (5)
O1ⁱⁱ—Na1—Na2^vii	51.10 (16)	O1^xviii—Al1—Na1^xvi	99.51 (8)
O1—Na1—Na2^vii	129.7 (2)	O1^xvi—Al1—Na1^xvi	35.94 (5)
O1ⁱⁱⁱ—Na1—Na2^vii	85.28 (12)	O1^xix—Al1—Na1^xvi	80.49 (8)
O1ⁱ—Na1—Na2^vii	60.81 (7)	Na2ⁱⁱ—Al1—Na1^xvi	46.05 (9)
Na2^iv—Na1—Na2^vii	114.50 (19)	Na2^xx—Al1—Na1^xvi	133.95 (9)
Na2^v—Na1—Na2^vii	114.50 (19)	Na2^xxi—Al1—Na1^xvi	58.13 (7)
Cl1—Na1—Na2^vii	137.93 (17)	Na2^xxii—Al1—Na1^xvi	121.87 (7)
B1ⁱⁱ—Na1—Na2^vii	66.6 (2)	Na1^xxiii—Al1—Na1^xvi	105.48 (12)
B1—Na1—Na2^vii	150.8 (2)	Na1^xvii—Al1—Na1^xvi	180.00 (12)
Na2^vi—Na1—Na2^vii	84.1 (3)	O1^xvii—Al1—Na1^xv	112.04 (7)
O1^viii—Na2—O1^ix	92.3 (2)	O1^xviii—Al1—Na1^xv	42.59 (6)
O1^viii—Na2—O1^x	92.3 (2)	O1^xvi—Al1—Na1^xv	67.96 (7)
O1^ix—Na2—O1^x	92.3 (2)	O1^xix—Al1—Na1^xv	137.41 (6)
O1^viii—Na2—Na1^xi	108.59 (7)	Na2ⁱⁱ—Al1—Na1^xv	46.05 (9)
O1^ix—Na2—Na1^xi	143.23 (13)	Na2^xx—Al1—Na1^xv	133.95 (9)
O1^x—Na2—Na1^xi	57.95 (8)	Na2^xxi—Al1—Na1^xv	121.87 (7)
O1^viii—Na2—Na1^xii	57.95 (8)	Na2^xxii—Al1—Na1^xv	58.13 (7)
O1^ix—Na2—Na1^xii	108.59 (7)	Na1^xxiii—Al1—Na1^xv	180.0
O1^x—Na2—Na1^xii	143.23 (13)	Na1^xvii—Al1—Na1^xv	105.48 (12)
Na1^xi—Na2—Na1^xii	108.1 (2)	Na1^xvi—Al1—Na1^xv	74.52 (12)
O1^viii—Na2—Na1^v	143.23 (13)	B1—O1—Al1^xv	128.59 (12)
O1^ix—Na2—Na1^v	57.95 (8)	B1—O1—Na1	107.1 (2)
O1^x—Na2—Na1^v	108.59 (7)	Al1^xv—O1—Na1	117.00 (8)
Na1^xi—Na2—Na1^v	108.1 (2)	B1—O1—Na1ⁱ	121.89 (16)
Na1^xii—Na2—Na1^v	108.1 (2)	Al1^xv—O1—Na1ⁱ	108.44 (8)
O1^viii—Na2—Cl1	123.62 (17)	Na1—O1—Na1ⁱ	22.18 (18)
O1^ix—Na2—Cl1	123.62 (17)	B1—O1—Na2^vi	119.5 (2)
O1^x—Na2—Cl1	123.62 (17)	Al1^xv—O1—Na2^vi	91.32 (7)
Na1^xi—Na2—Cl1	69.2 (2)	Na1—O1—Na2^vi	83.85 (18)
Na1^xii—Na2—Cl1	69.2 (2)	Na1ⁱ—O1—Na2^vi	62.66 (18)
Na1^v—Na2—Cl1	69.2 (2)	B1—O1—Na2^v	106.6 (3)
O1^viii—Na2—O1^xi	62.95 (7)	Al1^xv—O1—Na2^v	78.04 (18)
O1^ix—Na2—O1^xi	151.5 (3)	Na1—O1—Na2^v	57.80 (10)
O1^x—Na2—O1^xi	75.84 (7)	Na1ⁱ—O1—Na2^v	72.03 (7)
Na1^xi—Na2—O1^xi	48.20 (5)	Na2^vi—O1—Na2^v	127.14 (10)
Na1^xii—Na2—O1^xi	71.49 (6)	Na2ⁱⁱ—Cl1—Na2^iv	109.5
Na1^v—Na2—O1^xi	150.4 (3)	Na2ⁱⁱ—Cl1—Na2^v	109.5
Cl1—Na2—O1^xi	83.80 (18)	Na2^iv—Cl1—Na2^v	109.5
O1^viii—Na2—O1^v	151.5 (3)	Na2ⁱⁱ—Cl1—Na2	109.471 (1)
O1^ix—Na2—O1^v	75.84 (7)	Na2^iv—Cl1—Na2	109.471 (1)
O1^x—Na2—O1^v	62.95 (7)	Na2^v—Cl1—Na2	109.5
Na1^xi—Na2—O1^v	71.49 (6)	Na2ⁱⁱ—Cl1—Na1	125.3
Na1^xii—Na2—O1^v	150.4 (3)	Na2^iv—Cl1—Na1	54.7
Na1^v—Na2—O1^v	48.20 (5)	Na2^v—Cl1—Na1	54.7
Cl1—Na2—O1^v	83.80 (18)	Na2—Cl1—Na1	125.3
O1^xi—Na2—O1^v	118.85 (6)	Na2ⁱⁱ—Cl1—Na1^xi	125.3
O1^viii—Na2—O1^xii	75.84 (7)	Na2^iv—Cl1—Na1^xi	54.7
O1^ix—Na2—O1^xii	62.95 (7)	Na2^v—Cl1—Na1^xi	125.3
O1^x—Na2—O1^xii	151.5 (3)	Na2—Cl1—Na1^xi	54.7
Na1^xi—Na2—O1^xii	150.4 (3)	Na1—Cl1—Na1^xi	90.0
Na1^xii—Na2—O1^xii	48.20 (5)	Na2ⁱⁱ—Cl1—Na1^xv	54.7
Na1^v—Na2—O1^xii	71.49 (6)	Na2^iv—Cl1—Na1^xv	54.7
Cl1—Na2—O1^xii	83.80 (18)	Na2^v—Cl1—Na1^xv	125.3
O1^xi—Na2—O1^xii	118.85 (6)	Na2—Cl1—Na1^xv	125.3
O1^v—Na2—O1^xii	118.85 (6)	Na1—Cl1—Na1^xv	90.0
O1^viii—Na2—Al1^xiii	117.7 (3)	Na1^xi—Cl1—Na1^xv	90.0
O1^ix—Na2—Al1^xiii	69.15 (13)	Na2ⁱⁱ—Cl1—Na1^xii	125.3
O1^x—Na2—Al1^xiii	34.73 (6)	Na2^iv—Cl1—Na1^xii	125.3
Na1^xi—Na2—Al1^xiii	74.34 (5)	Na2^v—Cl1—Na1^xii	54.7
Na1^xii—Na2—Al1^xiii	175.4 (3)	Na2—Cl1—Na1^xii	54.7
Na1^v—Na2—Al1^xiii	74.34 (5)	Na1—Cl1—Na1^xii	90.0
Cl1—Na2—Al1^xiii	115.42 (15)	Na1^xi—Cl1—Na1^xii	90.0
O1^xi—Na2—Al1^xiii	108.42 (8)	Na1^xv—Cl1—Na1^xii	180.0
O1^v—Na2—Al1^xiii	33.89 (4)	Na2ⁱⁱ—Cl1—Na1^v	54.7
O1^xii—Na2—Al1^xiii	130.79 (12)	Na2^iv—Cl1—Na1^v	125.3
O1^viii—Na2—Al1^xiv	69.15 (13)	Na2^v—Cl1—Na1^v	125.3
O1^ix—Na2—Al1^xiv	34.73 (6)	Na2—Cl1—Na1^v	54.7
O1^x—Na2—Al1^xiv	117.7 (3)	Na1—Cl1—Na1^v	180.0
Na1^xi—Na2—Al1^xiv	175.4 (3)	Na1^xi—Cl1—Na1^v	90.0
Na1^xii—Na2—Al1^xiv	74.34 (5)	Na1^xv—Cl1—Na1^v	90.0
Na1^v—Na2—Al1^xiv	74.34 (5)	Na1^xii—Cl1—Na1^v	90.0
Cl1—Na2—Al1^xiv	115.42 (15)	Na2ⁱⁱ—Cl1—Na1^xvi	54.7
O1^xi—Na2—Al1^xiv	130.79 (12)	Na2^iv—Cl1—Na1^xvi	125.3
O1^v—Na2—Al1^xiv	108.42 (8)	Na2^v—Cl1—Na1^xvi	54.7
O1^xii—Na2—Al1^xiv	33.89 (4)	Na2—Cl1—Na1^xvi	125.3
Al1^xiii—Na2—Al1^xiv	102.92 (18)	Na1—Cl1—Na1^xvi	90.0
O1^xv—B1—O1^xvi	119.993 (7)	Na1^xi—Cl1—Na1^xvi	180.0
O1^xv—B1—O1	119.993 (7)	Na1^xv—Cl1—Na1^xvi	90.0
O1^xvi—B1—O1	119.993 (7)	Na1^xii—Cl1—Na1^xvi	90.0
O1^xv—B1—Na1	87.53 (15)	Na1^v—Cl1—Na1^xvi	90.0
O1^xvi—B1—Na1	135.5 (3)

Symmetry codes: (i) −x, z, −y+1/2; (ii) x, −y+1/2, −z+1/2; (iii) −x, −z+1/2, y; (iv) −x+1/2, y, −z+1/2; (v) −x+1/2, −y+1/2, z; (vi) y−1/2, −x+1/2, −z+1/2; (vii) y−1/2, x, z; (viii) −z+1/2, −y+1/2, x+1/2; (ix) x+1/2, −z+1/2, −y+1/2; (x) −y+1/2, x+1/2, −z+1/2; (xi) z, −x+1/2, −y+1/2; (xii) −y+1/2, z, −x+1/2; (xiii) y+1/2, z+1/2, x; (xiv) z+1/2, x, y+1/2; (xv) y, z, x; (xvi) z, x, y; (xvii) z, −x, −y; (xviii) −z+1/2, y, −x; (xix) −z+1/2, −y, x; (xx) x, y−1/2, z−1/2; (xxi) −y+1/2, x−1/2, −z+1/2; (xxii) −y+1/2, −x+1/2, z−1/2; (xxiii) −y+1/2, z−1/2, −x.

Sodium aluminoboracite (kjh230804yoshinoN4_0m_a_1) top

Crystal data top

Na_3.92B₄Al₃O₁₂Cl_0.92	Cu Kα radiation, λ = 1.54178 Å
M_r = 438.91	Cell parameters from 3423 reflections
Cubic, F23	θ = 4.6–74.3°
a = 13.5904 (1) Å	µ = 6.78 mm⁻¹
V = 2510.13 (6) Å³	T = 294 K
Z = 8	Plate, colorless
F(000) = 1728	0.08 × 0.06 × 0.04 mm
D_x = 2.323 Mg m⁻³

Data collection top

Bruker D8 goniometer diffractometer	437 independent reflections
Radiation source: sealed tube	355 reflections with I > 2σ(I)
Detector resolution: 7.3910 pixels mm^-1	R_int = 0.028
ω scans	θ_max = 74.3°, θ_min = 5.6°
Absorption correction: multi-scan (SADABS; Krause et al., 2015)	h = −16→16
T_min = 0.66, T_max = 0.75	k = −16→16
5514 measured reflections	l = −16→14

Refinement top

Refinement on F²	1 restraint
Least-squares matrix: full	w = 1/[σ²(F_o²) + (0.0396P)² + 2.0455P] where P = (F_o² + 2F_c²)/3
R[F² > 2σ(F²)] = 0.024	(Δ/σ)_max = 0.006
wR(F²) = 0.066	Δρ_max = 0.17 e Å⁻³
S = 1.12	Δρ_min = −0.58 e Å⁻³
437 reflections	Absolute structure: Flack x determined using 142 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons et al., 2013).
52 parameters	Absolute structure parameter: 0.01 (2)

Special details top

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Na1	0.0348 (5)	0.250000	0.250000	0.0429 (12)	0.5
Na2	0.5331 (5)	0.750000	0.750000	0.0430 (12)	0.5
Na3	0.3604 (4)	0.3604 (4)	0.3604 (4)	0.015 (2)	0.226 (7)
Na4	0.8610 (4)	0.8610 (4)	0.8610 (4)	0.020 (2)	0.235 (7)
B1	0.1039 (3)	0.1039 (3)	0.1039 (3)	0.0149 (10)
B2	0.6039 (3)	0.6039 (3)	0.6039 (3)	0.0138 (10)
Al1	0.25008 (10)	0.000000	0.000000	0.0099 (3)
O1	0.03517 (13)	0.10051 (12)	0.17740 (13)	0.0181 (5)
O2	0.03517 (13)	0.17741 (13)	0.60039 (12)	0.0182 (5)
Cl1	0.250000	0.250000	0.250000	0.0359 (9)	0.921 (9)
Cl2	0.750000	0.750000	0.750000	0.0350 (9)	0.921 (9)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Na1	0.092 (4)	0.0156 (18)	0.0210 (19)	0.000	0.000	−0.0062 (17)
Na2	0.100 (4)	0.0169 (18)	0.0118 (17)	0.000	0.000	−0.0067 (16)
Na3	0.015 (2)	0.015 (2)	0.015 (2)	−0.0008 (19)	−0.0008 (19)	−0.0008 (19)
Na4	0.020 (2)	0.020 (2)	0.020 (2)	−0.002 (2)	−0.002 (2)	−0.002 (2)
B1	0.0149 (10)	0.0149 (10)	0.0149 (10)	0.0013 (13)	0.0013 (13)	0.0013 (13)
B2	0.0138 (10)	0.0138 (10)	0.0138 (10)	0.0030 (13)	0.0030 (13)	0.0030 (13)
Al1	0.0100 (5)	0.0099 (5)	0.0099 (5)	0.000	0.000	−0.0001 (4)
O1	0.0192 (9)	0.0153 (8)	0.0198 (10)	0.0061 (7)	0.0107 (8)	0.0059 (8)
O2	0.0194 (9)	0.0196 (10)	0.0156 (8)	0.0105 (8)	0.0056 (7)	0.0070 (8)
Cl1	0.0359 (9)	0.0359 (9)	0.0359 (9)	0.000	0.000	0.000
Cl2	0.0350 (9)	0.0350 (9)	0.0350 (9)	0.000	0.000	0.000

Geometric parameters (Å, º) top

Na1—Na2ⁱ	0.922 (6)	Na3—Cl1	2.599 (10)
Na1—O1ⁱⁱ	2.2585 (18)	Na3—O1^xxi	2.912 (2)
Na1—O1	2.2585 (18)	Na3—O1^xxii	2.912 (2)
Na1—O2ⁱⁱⁱ	2.452 (3)	Na3—O1^vi	2.912 (2)
Na1—O2^iv	2.452 (3)	Na3—Al1^xvii	3.074 (4)
Na1—Na3^v	2.556 (5)	Na3—Al1^xxiii	3.074 (4)
Na1—Na3^vi	2.556 (5)	Na4—O1^xxiv	2.480 (6)
Na1—Cl1	2.925 (6)	Na4—O1^xxv	2.480 (6)
Na1—B1ⁱⁱ	2.961 (4)	Na4—O1^xxvi	2.480 (6)
Na1—B1	2.961 (4)	Na4—Cl2	2.612 (10)
Na1—Na4^vii	3.182 (5)	Na4—O2^xxvii	2.914 (2)
Na1—Na4^viii	3.182 (5)	Na4—O2^xxviii	2.914 (2)
Na2—O2^ix	2.2602 (18)	Na4—O2^xxix	2.914 (2)
Na2—O2^x	2.2602 (18)	Na4—Al1^xxx	3.069 (4)
Na2—O1^xi	2.442 (3)	Na4—Al1^xxxi	3.069 (4)
Na2—O1^xii	2.442 (3)	B1—O1^xxxii	1.3684 (16)
Na2—Na4^xiii	2.573 (5)	B1—O1^xxxiii	1.3684 (16)
Na2—Na4^xiv	2.573 (5)	B1—O1	1.3684 (16)
Na2—Cl2	2.948 (6)	B2—O2^xxxiv	1.3685 (16)
Na2—B2^xv	2.969 (4)	B2—O2^xxxv	1.3684 (16)
Na2—B2	2.969 (4)	B2—O2^x	1.3684 (16)
Na2—Na3^xvi	3.164 (5)	Al1—O2^xxxvi	1.7495 (18)
Na2—Na3^xvii	3.164 (5)	Al1—O2^xxxvii	1.7495 (18)
Na3—O2^xviii	2.488 (6)	Al1—O1^xxxviii	1.7522 (18)
Na3—O2^xix	2.488 (6)	Al1—O1^xxxii	1.7522 (18)
Na3—O2^xx	2.488 (6)

Na2ⁱ—Na1—O1ⁱⁱ	90.14 (17)	Cl2—Na4—O2^xxix	83.7 (2)
Na2ⁱ—Na1—O1	90.14 (17)	O2^xxvii—Na4—O2^xxix	118.80 (8)
O1ⁱⁱ—Na1—O1	179.7 (3)	O2^xxviii—Na4—O2^xxix	118.80 (8)
Na2ⁱ—Na1—O2ⁱⁱⁱ	67.19 (14)	O1^xxiv—Na4—Al1^xxx	118.0 (4)
O1ⁱⁱ—Na1—O2ⁱⁱⁱ	90.07 (9)	O1^xxv—Na4—Al1^xxx	69.23 (15)
O1—Na1—O2ⁱⁱⁱ	90.04 (9)	O1^xxvi—Na4—Al1^xxx	34.80 (7)
Na2ⁱ—Na1—O2^iv	67.19 (14)	Na2^xxxix—Na4—Al1^xxx	74.23 (8)
O1ⁱⁱ—Na1—O2^iv	90.04 (9)	Na2^xiv—Na4—Al1^xxx	74.23 (8)
O1—Na1—O2^iv	90.07 (9)	Na2^xl—Na4—Al1^xxx	175.4 (4)
O2ⁱⁱⁱ—Na1—O2^iv	134.4 (3)	Cl2—Na4—Al1^xxx	115.28 (18)
Na2ⁱ—Na1—Na3^v	123.9 (3)	O2^xxvii—Na4—Al1^xxx	33.88 (5)
O1ⁱⁱ—Na1—Na3^v	74.16 (9)	O2^xxviii—Na4—Al1^xxx	130.86 (15)
O1—Na1—Na3^v	105.68 (13)	O2^xxix—Na4—Al1^xxx	108.51 (9)
O2ⁱⁱⁱ—Na1—Na3^v	59.5 (2)	O1^xxiv—Na4—Al1^xxxi	34.80 (7)
O2^iv—Na1—Na3^v	159.92 (19)	O1^xxv—Na4—Al1^xxxi	118.0 (4)
Na2ⁱ—Na1—Na3^vi	123.9 (3)	O1^xxvi—Na4—Al1^xxxi	69.23 (15)
O1ⁱⁱ—Na1—Na3^vi	105.68 (13)	Na2^xxxix—Na4—Al1^xxxi	175.4 (4)
O1—Na1—Na3^vi	74.16 (9)	Na2^xiv—Na4—Al1^xxxi	74.23 (8)
O2ⁱⁱⁱ—Na1—Na3^vi	159.92 (19)	Na2^xl—Na4—Al1^xxxi	74.23 (8)
O2^iv—Na1—Na3^vi	59.5 (2)	Cl2—Na4—Al1^xxxi	115.28 (18)
Na3^v—Na1—Na3^vi	112.2 (5)	O2^xxvii—Na4—Al1^xxxi	130.86 (15)
Na2ⁱ—Na1—Cl1	180.0	O2^xxviii—Na4—Al1^xxxi	108.51 (9)
O1ⁱⁱ—Na1—Cl1	89.86 (17)	O2^xxix—Na4—Al1^xxxi	33.88 (5)
O1—Na1—Cl1	89.86 (17)	Al1^xxx—Na4—Al1^xxxi	103.1 (2)
O2ⁱⁱⁱ—Na1—Cl1	112.81 (14)	O1^xxxii—B1—O1^xxxiii	119.995 (7)
O2^iv—Na1—Cl1	112.81 (14)	O1^xxxii—B1—O1	119.995 (7)
Na3^v—Na1—Cl1	56.1 (3)	O1^xxxiii—B1—O1	119.992 (7)
Na3^vi—Na1—Cl1	56.1 (3)	O1^xxxii—B1—Na1^xxxii	46.89 (18)
Na2ⁱ—Na1—B1ⁱⁱ	108.51 (15)	O1^xxxiii—B1—Na1^xxxii	135.4 (3)
O1ⁱⁱ—Na1—B1ⁱⁱ	26.25 (9)	O1—B1—Na1^xxxii	87.58 (17)
O1—Na1—B1ⁱⁱ	153.5 (2)	O1^xxxii—B1—Na1^xxxiii	87.58 (17)
O2ⁱⁱⁱ—Na1—B1ⁱⁱ	114.16 (5)	O1^xxxiii—B1—Na1^xxxiii	46.89 (18)
O2^iv—Na1—B1ⁱⁱ	80.61 (6)	O1—B1—Na1^xxxiii	135.4 (3)
Na3^v—Na1—B1ⁱⁱ	79.81 (13)	Na1^xxxii—B1—Na1^xxxiii	88.6 (2)
Na3^vi—Na1—B1ⁱⁱ	79.81 (13)	O1^xxxii—B1—Na1	135.4 (3)
Cl1—Na1—B1ⁱⁱ	71.49 (15)	O1^xxxiii—B1—Na1	87.58 (17)
Na2ⁱ—Na1—B1	108.51 (15)	O1—B1—Na1	46.89 (18)
O1ⁱⁱ—Na1—B1	153.5 (2)	Na1^xxxii—B1—Na1	88.6 (2)
O1—Na1—B1	26.25 (9)	Na1^xxxiii—B1—Na1	88.6 (2)
O2ⁱⁱⁱ—Na1—B1	80.61 (6)	O2^xxxiv—B2—O2^xxxv	119.993 (8)
O2^iv—Na1—B1	114.16 (5)	O2^xxxiv—B2—O2^x	119.994 (8)
Na3^v—Na1—B1	79.81 (13)	O2^xxxv—B2—O2^x	119.995 (8)
Na3^vi—Na1—B1	79.81 (13)	O2^xxxiv—B2—Na2	135.7 (3)
Cl1—Na1—B1	71.49 (15)	O2^xxxv—B2—Na2	87.51 (17)
B1ⁱⁱ—Na1—B1	143.0 (3)	O2^x—B2—Na2	46.65 (18)
Na2ⁱ—Na1—Na4^vii	42.1 (2)	O2^xxxiv—B2—Na2^xxxiii	46.65 (18)
O1ⁱⁱ—Na1—Na4^vii	129.4 (3)	O2^xxxv—B2—Na2^xxxiii	135.7 (3)
O1—Na1—Na4^vii	50.85 (19)	O2^x—B2—Na2^xxxiii	87.51 (17)
O2ⁱⁱⁱ—Na1—Na4^vii	60.65 (11)	Na2—B2—Na2^xxxiii	89.2 (2)
O2^iv—Na1—Na4^vii	85.09 (18)	O2^xxxiv—B2—Na2^xxxii	87.51 (17)
Na3^v—Na1—Na4^vii	114.45 (17)	O2^xxxv—B2—Na2^xxxii	46.65 (18)
Na3^vi—Na1—Na4^vii	114.45 (17)	O2^x—B2—Na2^xxxii	135.7 (3)
Cl1—Na1—Na4^vii	137.9 (2)	Na2—B2—Na2^xxxii	89.2 (2)
B1ⁱⁱ—Na1—Na4^vii	150.6 (3)	Na2^xxxiii—B2—Na2^xxxii	89.2 (2)
B1—Na1—Na4^vii	66.4 (2)	O2^xxxvi—Al1—O2^xxxvii	111.44 (14)
Na2ⁱ—Na1—Na4^viii	42.1 (2)	O2^xxxvi—Al1—O1^xxxviii	108.50 (8)
O1ⁱⁱ—Na1—Na4^viii	50.85 (19)	O2^xxxvii—Al1—O1^xxxviii	108.53 (8)
O1—Na1—Na4^viii	129.4 (3)	O2^xxxvi—Al1—O1^xxxii	108.53 (8)
O2ⁱⁱⁱ—Na1—Na4^viii	85.09 (18)	O2^xxxvii—Al1—O1^xxxii	108.50 (8)
O2^iv—Na1—Na4^viii	60.65 (11)	O1^xxxviii—Al1—O1^xxxii	111.37 (14)
Na3^v—Na1—Na4^viii	114.45 (17)	O2^xxxvi—Al1—Na4^xli	157.72 (8)
Na3^vi—Na1—Na4^viii	114.45 (17)	O2^xxxvii—Al1—Na4^xli	68.19 (18)
Cl1—Na1—Na4^viii	137.9 (2)	O1^xxxviii—Al1—Na4^xli	92.00 (14)
B1ⁱⁱ—Na1—Na4^viii	66.4 (2)	O1^xxxii—Al1—Na4^xli	53.90 (9)
B1—Na1—Na4^viii	150.6 (3)	O2^xxxvi—Al1—Na4^xlii	68.19 (18)
Na4^vii—Na1—Na4^viii	84.1 (4)	O2^xxxvii—Al1—Na4^xlii	157.72 (8)
Na1^xii—Na2—O2^ix	90.71 (17)	O1^xxxviii—Al1—Na4^xlii	53.90 (9)
Na1^xii—Na2—O2^x	90.71 (17)	O1^xxxii—Al1—Na4^xlii	92.00 (14)
O2^ix—Na2—O2^x	178.6 (3)	Na4^xli—Al1—Na4^xlii	121.1 (4)
Na1^xii—Na2—O1^xi	67.66 (14)	O2^xxxvi—Al1—Na3ⁱⁱ	54.03 (9)
O2^ix—Na2—O1^xi	90.25 (9)	O2^xxxvii—Al1—Na3ⁱⁱ	92.18 (13)
O2^x—Na2—O1^xi	90.29 (9)	O1^xxxviii—Al1—Na3ⁱⁱ	157.61 (8)
Na1^xii—Na2—O1^xii	67.66 (15)	O1^xxxii—Al1—Na3ⁱⁱ	67.99 (17)
O2^ix—Na2—O1^xii	90.29 (9)	Na4^xli—Al1—Na3ⁱⁱ	103.88 (11)
O2^x—Na2—O1^xii	90.25 (9)	Na4^xlii—Al1—Na3ⁱⁱ	103.88 (11)
O1^xi—Na2—O1^xii	135.3 (3)	O2^xxxvi—Al1—Na3^xliii	92.18 (13)
Na1^xii—Na2—Na4^xiii	124.0 (3)	O2^xxxvii—Al1—Na3^xliii	54.03 (9)
O2^ix—Na2—Na4^xiii	105.33 (14)	O1^xxxviii—Al1—Na3^xliii	67.99 (17)
O2^x—Na2—Na4^xiii	73.84 (9)	O1^xxxii—Al1—Na3^xliii	157.61 (8)
O1^xi—Na2—Na4^xiii	159.6 (2)	Na4^xli—Al1—Na3^xliii	103.88 (11)
O1^xii—Na2—Na4^xiii	59.2 (2)	Na4^xlii—Al1—Na3^xliii	103.88 (11)
Na1^xii—Na2—Na4^xiv	124.0 (3)	Na3ⁱⁱ—Al1—Na3^xliii	121.6 (4)
O2^ix—Na2—Na4^xiv	73.84 (9)	O2^xxxvi—Al1—Na2^xliv	68.10 (10)
O2^x—Na2—Na4^xiv	105.33 (14)	O2^xxxvii—Al1—Na2^xliv	111.93 (11)
O1^xi—Na2—Na4^xiv	59.2 (2)	O1^xxxviii—Al1—Na2^xliv	42.50 (8)
O1^xii—Na2—Na4^xiv	159.6 (2)	O1^xxxii—Al1—Na2^xliv	137.46 (9)
Na4^xiii—Na2—Na4^xiv	111.9 (5)	Na4^xli—Al1—Na2^xliv	133.72 (12)
Na1^xii—Na2—Cl2	180.0	Na4^xlii—Al1—Na2^xliv	46.26 (12)
O2^ix—Na2—Cl2	89.29 (17)	Na3ⁱⁱ—Al1—Na2^xliv	122.08 (10)
O2^x—Na2—Cl2	89.29 (17)	Na3^xliii—Al1—Na2^xliv	57.94 (10)
O1^xi—Na2—Cl2	112.34 (14)	O2^xxxvi—Al1—Na2^xlv	36.03 (6)
O1^xii—Na2—Cl2	112.34 (14)	O2^xxxvii—Al1—Na2^xlv	144.01 (8)
Na4^xiii—Na2—Cl2	56.0 (3)	O1^xxxviii—Al1—Na2^xlv	99.67 (11)
Na4^xiv—Na2—Cl2	56.0 (3)	O1^xxxii—Al1—Na2^xlv	80.31 (10)
Na1^xii—Na2—B2^xv	108.90 (15)	Na4^xli—Al1—Na2^xlv	133.72 (12)
O2^ix—Na2—B2^xv	26.12 (9)	Na4^xlii—Al1—Na2^xlv	46.26 (12)
O2^x—Na2—B2^xv	152.8 (2)	Na3ⁱⁱ—Al1—Na2^xlv	57.94 (10)
O1^xi—Na2—B2^xv	114.17 (5)	Na3^xliii—Al1—Na2^xlv	122.08 (10)
O1^xii—Na2—B2^xv	80.61 (6)	Na2^xliv—Al1—Na2^xlv	74.9 (2)
Na4^xiii—Na2—B2^xv	79.56 (13)	O2^xxxvi—Al1—Na2^xlvi	144.01 (8)
Na4^xiv—Na2—B2^xv	79.56 (13)	O2^xxxvii—Al1—Na2^xlvi	36.03 (6)
Cl2—Na2—B2^xv	71.10 (15)	O1^xxxviii—Al1—Na2^xlvi	80.31 (10)
Na1^xii—Na2—B2	108.90 (15)	O1^xxxii—Al1—Na2^xlvi	99.67 (11)
O2^ix—Na2—B2	152.9 (2)	Na4^xli—Al1—Na2^xlvi	46.26 (12)
O2^x—Na2—B2	26.12 (9)	Na4^xlii—Al1—Na2^xlvi	133.72 (12)
O1^xi—Na2—B2	80.61 (6)	Na3ⁱⁱ—Al1—Na2^xlvi	122.08 (10)
O1^xii—Na2—B2	114.17 (5)	Na3^xliii—Al1—Na2^xlvi	57.94 (10)
Na4^xiii—Na2—B2	79.56 (13)	Na2^xliv—Al1—Na2^xlvi	105.1 (2)
Na4^xiv—Na2—B2	79.56 (13)	Na2^xlv—Al1—Na2^xlvi	179.96 (4)
Cl2—Na2—B2	71.10 (15)	O2^xxxvi—Al1—Na2^xlvii	111.93 (11)
B2^xv—Na2—B2	142.2 (3)	O2^xxxvii—Al1—Na2^xlvii	68.10 (10)
Na1^xii—Na2—Na3^xvi	42.1 (2)	O1^xxxviii—Al1—Na2^xlvii	137.46 (9)
O2^ix—Na2—Na3^xvi	130.0 (3)	O1^xxxii—Al1—Na2^xlvii	42.50 (8)
O2^x—Na2—Na3^xvi	51.37 (19)	Na4^xli—Al1—Na2^xlvii	46.26 (12)
O1^xi—Na2—Na3^xvi	61.00 (11)	Na4^xlii—Al1—Na2^xlvii	133.72 (12)
O1^xii—Na2—Na3^xvi	85.47 (18)	Na3ⁱⁱ—Al1—Na2^xlvii	57.94 (10)
Na4^xiii—Na2—Na3^xvi	114.53 (18)	Na3^xliii—Al1—Na2^xlvii	122.08 (10)
Na4^xiv—Na2—Na3^xvi	114.53 (18)	Na2^xliv—Al1—Na2^xlvii	179.96 (12)
Cl2—Na2—Na3^xvi	137.9 (2)	Na2^xlv—Al1—Na2^xlvii	105.1 (2)
B2^xv—Na2—Na3^xvi	151.0 (3)	Na2^xlvi—Al1—Na2^xlvii	74.9 (2)
B2—Na2—Na3^xvi	66.8 (2)	B1—O1—Al1^xxxiii	128.62 (14)
Na1^xii—Na2—Na3^xvii	42.1 (2)	B1—O1—Na1	106.9 (3)
O2^ix—Na2—Na3^xvii	51.37 (18)	Al1^xxxiii—O1—Na1	117.02 (10)
O2^x—Na2—Na3^xvii	130.0 (3)	B1—O1—Na2ⁱ	121.75 (19)
O1^xi—Na2—Na3^xvii	85.47 (18)	Al1^xxxiii—O1—Na2ⁱ	108.49 (10)
O1^xii—Na2—Na3^xvii	61.00 (11)	Na1—O1—Na2ⁱ	22.20 (14)
Na4^xiii—Na2—Na3^xvii	114.53 (18)	B1—O1—Na4^vii	119.4 (2)
Na4^xiv—Na2—Na3^xvii	114.53 (18)	Al1^xxxiii—O1—Na4^vii	91.30 (7)
Cl2—Na2—Na3^xvii	137.9 (2)	Na1—O1—Na4^vii	84.2 (2)
B2^xv—Na2—Na3^xvii	66.8 (2)	Na2ⁱ—O1—Na4^vii	63.0 (2)
B2—Na2—Na3^xvii	151.0 (3)	B1—O1—Na3^vi	106.5 (3)
Na3^xvi—Na2—Na3^xvii	84.2 (4)	Al1^xxxiii—O1—Na3^vi	78.1 (2)
O2^xviii—Na3—O2^xix	92.1 (3)	Na1—O1—Na3^vi	57.59 (12)
O2^xviii—Na3—O2^xx	92.1 (3)	Na2ⁱ—O1—Na3^vi	71.84 (11)
O2^xix—Na3—O2^xx	92.1 (3)	Na4^vii—O1—Na3^vi	127.3 (2)
O2^xviii—Na3—Na1^vi	143.25 (16)	B2^xlviii—O2—Al1^xxii	128.66 (14)
O2^xix—Na3—Na1^vi	108.65 (10)	B2^xlviii—O2—Na2^xlviii	107.2 (3)
O2^xx—Na3—Na1^vi	58.15 (12)	Al1^xxii—O2—Na2^xlviii	116.89 (10)
O2^xviii—Na3—Na1^xxi	58.15 (12)	B2^xlviii—O2—Na1^xlix	121.99 (19)
O2^xix—Na3—Na1^xxi	143.26 (16)	Al1^xxii—O2—Na1^xlix	108.31 (10)
O2^xx—Na3—Na1^xxi	108.65 (10)	Na2^xlviii—O2—Na1^xlix	22.10 (14)
Na1^vi—Na3—Na1^xxi	108.1 (3)	B2^xlviii—O2—Na3^l	119.5 (2)
O2^xviii—Na3—Na1^xxii	108.65 (10)	Al1^xxii—O2—Na3^l	91.29 (7)
O2^xix—Na3—Na1^xxii	58.15 (12)	Na2^xlviii—O2—Na3^l	83.4 (2)
O2^xx—Na3—Na1^xxii	143.25 (16)	Na1^xlix—O2—Na3^l	62.3 (2)
Na1^vi—Na3—Na1^xxii	108.1 (3)	B2^xlviii—O2—Na4^li	106.8 (3)
Na1^xxi—Na3—Na1^xxii	108.1 (3)	Al1^xxii—O2—Na4^li	77.9 (2)
O2^xviii—Na3—Cl1	123.8 (2)	Na2^xlviii—O2—Na4^li	58.00 (12)
O2^xix—Na3—Cl1	123.8 (2)	Na1^xlix—O2—Na4^li	72.17 (10)
O2^xx—Na3—Cl1	123.8 (2)	Na3^l—O2—Na4^li	126.9 (2)
Na1^vi—Na3—Cl1	69.1 (3)	Na3—Cl1—Na3ⁱⁱ	109.472 (1)
Na1^xxi—Na3—Cl1	69.1 (3)	Na3—Cl1—Na3^v	109.5
Na1^xxii—Na3—Cl1	69.1 (3)	Na3ⁱⁱ—Cl1—Na3^v	109.5
O2^xviii—Na3—O1^xxi	75.84 (8)	Na3—Cl1—Na3^vi	109.5
O2^xix—Na3—O1^xxi	151.3 (4)	Na3ⁱⁱ—Cl1—Na3^vi	109.5
O2^xx—Na3—O1^xxi	62.94 (6)	Na3^v—Cl1—Na3^vi	109.5
Na1^vi—Na3—O1^xxi	71.52 (7)	Na3—Cl1—Na1^vi	54.7
Na1^xxi—Na3—O1^xxi	48.25 (5)	Na3ⁱⁱ—Cl1—Na1^vi	54.736 (1)
Na1^xxii—Na3—O1^xxi	150.4 (4)	Na3^v—Cl1—Na1^vi	125.3
Cl1—Na3—O1^xxi	83.9 (2)	Na3^vi—Cl1—Na1^vi	125.3
O2^xviii—Na3—O1^xxii	62.94 (6)	Na3—Cl1—Na1^xxii	54.7
O2^xix—Na3—O1^xxii	75.84 (8)	Na3ⁱⁱ—Cl1—Na1^xxii	125.3
O2^xx—Na3—O1^xxii	151.3 (4)	Na3^v—Cl1—Na1^xxii	54.7
Na1^vi—Na3—O1^xxii	150.4 (4)	Na3^vi—Cl1—Na1^xxii	125.3
Na1^xxi—Na3—O1^xxii	71.53 (7)	Na1^vi—Cl1—Na1^xxii	90.0
Na1^xxii—Na3—O1^xxii	48.25 (5)	Na3—Cl1—Na1^xxxiii	125.3
Cl1—Na3—O1^xxii	83.9 (2)	Na3ⁱⁱ—Cl1—Na1^xxxiii	54.7
O1^xxi—Na3—O1^xxii	118.89 (7)	Na3^v—Cl1—Na1^xxxiii	54.7
O2^xviii—Na3—O1^vi	151.3 (4)	Na3^vi—Cl1—Na1^xxxiii	125.3
O2^xix—Na3—O1^vi	62.94 (6)	Na1^vi—Cl1—Na1^xxxiii	90.0
O2^xx—Na3—O1^vi	75.84 (8)	Na1^xxii—Cl1—Na1^xxxiii	90.0
Na1^vi—Na3—O1^vi	48.25 (5)	Na3—Cl1—Na1^xxi	54.7
Na1^xxi—Na3—O1^vi	150.4 (4)	Na3ⁱⁱ—Cl1—Na1^xxi	125.3
Na1^xxii—Na3—O1^vi	71.52 (7)	Na3^v—Cl1—Na1^xxi	125.3
Cl1—Na3—O1^vi	83.9 (2)	Na3^vi—Cl1—Na1^xxi	54.7
O1^xxi—Na3—O1^vi	118.88 (7)	Na1^vi—Cl1—Na1^xxi	90.0
O1^xxii—Na3—O1^vi	118.88 (7)	Na1^xxii—Cl1—Na1^xxi	90.0
O2^xviii—Na3—Al1^xvii	34.68 (7)	Na1^xxxiii—Cl1—Na1^xxi	180.0
O2^xix—Na3—Al1^xvii	69.06 (15)	Na3—Cl1—Na1^xxxii	125.3
O2^xx—Na3—Al1^xvii	117.4 (4)	Na3ⁱⁱ—Cl1—Na1^xxxii	54.7
Na1^vi—Na3—Al1^xvii	175.3 (4)	Na3^v—Cl1—Na1^xxxii	125.3
Na1^xxi—Na3—Al1^xvii	74.45 (8)	Na3^vi—Cl1—Na1^xxxii	54.7
Na1^xxii—Na3—Al1^xvii	74.45 (8)	Na1^vi—Cl1—Na1^xxxii	90.0
Cl1—Na3—Al1^xvii	115.54 (18)	Na1^xxii—Cl1—Na1^xxxii	180.0
O1^xxi—Na3—Al1^xvii	108.38 (9)	Na1^xxxiii—Cl1—Na1^xxxii	90.0
O1^xxii—Na3—Al1^xvii	33.91 (5)	Na1^xxi—Cl1—Na1^xxxii	90.0
O1^vi—Na3—Al1^xvii	130.71 (15)	Na3—Cl1—Na1	125.3
O2^xviii—Na3—Al1^xxiii	117.4 (4)	Na3ⁱⁱ—Cl1—Na1	125.264 (1)
O2^xix—Na3—Al1^xxiii	34.68 (7)	Na3^v—Cl1—Na1	54.7
O2^xx—Na3—Al1^xxiii	69.06 (15)	Na3^vi—Cl1—Na1	54.7
Na1^vi—Na3—Al1^xxiii	74.45 (8)	Na1^vi—Cl1—Na1	180.0
Na1^xxi—Na3—Al1^xxiii	175.3 (4)	Na1^xxii—Cl1—Na1	90.0
Na1^xxii—Na3—Al1^xxiii	74.45 (8)	Na1^xxxiii—Cl1—Na1	90.0
Cl1—Na3—Al1^xxiii	115.54 (18)	Na1^xxi—Cl1—Na1	90.0
O1^xxi—Na3—Al1^xxiii	130.71 (14)	Na1^xxxii—Cl1—Na1	90.0
O1^xxii—Na3—Al1^xxiii	108.38 (10)	Na4^xiv—Cl2—Na4^xv	109.472 (1)
O1^vi—Na3—Al1^xxiii	33.91 (5)	Na4^xiv—Cl2—Na4^xiii	109.470 (1)
Al1^xvii—Na3—Al1^xxiii	102.8 (2)	Na4^xv—Cl2—Na4^xiii	109.472 (1)
O1^xxiv—Na4—O1^xxv	92.5 (3)	Na4^xiv—Cl2—Na4	109.5
O1^xxiv—Na4—O1^xxvi	92.5 (3)	Na4^xv—Cl2—Na4	109.470 (2)
O1^xxv—Na4—O1^xxvi	92.5 (3)	Na4^xiii—Cl2—Na4	109.472 (1)
O1^xxiv—Na4—Na2^xxxix	143.20 (16)	Na4^xiv—Cl2—Na2^xxxii	54.7
O1^xxv—Na4—Na2^xxxix	57.75 (12)	Na4^xv—Cl2—Na2^xxxii	54.7
O1^xxvi—Na4—Na2^xxxix	108.55 (10)	Na4^xiii—Cl2—Na2^xxxii	125.264 (2)
O1^xxiv—Na4—Na2^xiv	108.55 (10)	Na4—Cl2—Na2^xxxii	125.3
O1^xxv—Na4—Na2^xiv	143.20 (16)	Na4^xiv—Cl2—Na2^xxxix	125.3
O1^xxvi—Na4—Na2^xiv	57.75 (12)	Na4^xv—Cl2—Na2^xxxix	125.264 (1)
Na2^xxxix—Na4—Na2^xiv	108.2 (3)	Na4^xiii—Cl2—Na2^xxxix	54.736 (1)
O1^xxiv—Na4—Na2^xl	57.75 (12)	Na4—Cl2—Na2^xxxix	54.7
O1^xxv—Na4—Na2^xl	108.55 (10)	Na2^xxxii—Cl2—Na2^xxxix	180.0
O1^xxvi—Na4—Na2^xl	143.20 (16)	Na4^xiv—Cl2—Na2^xxxiii	125.264 (1)
Na2^xxxix—Na4—Na2^xl	108.2 (3)	Na4^xv—Cl2—Na2^xxxiii	54.736 (1)
Na2^xiv—Na4—Na2^xl	108.2 (3)	Na4^xiii—Cl2—Na2^xxxiii	54.7
O1^xxiv—Na4—Cl2	123.5 (2)	Na4—Cl2—Na2^xxxiii	125.264 (1)
O1^xxv—Na4—Cl2	123.5 (2)	Na2^xxxii—Cl2—Na2^xxxiii	90.0
O1^xxvi—Na4—Cl2	123.5 (2)	Na2^xxxix—Cl2—Na2^xxxiii	90.0
Na2^xxxix—Na4—Cl2	69.3 (3)	Na4^xiv—Cl2—Na2^xl	54.736 (1)
Na2^xiv—Na4—Cl2	69.3 (3)	Na4^xv—Cl2—Na2^xl	125.3
Na2^xl—Na4—Cl2	69.3 (3)	Na4^xiii—Cl2—Na2^xl	125.264 (1)
O1^xxiv—Na4—O2^xxvii	151.8 (4)	Na4—Cl2—Na2^xl	54.736 (1)
O1^xxv—Na4—O2^xxvii	75.89 (8)	Na2^xxxii—Cl2—Na2^xl	90.0
O1^xxvi—Na4—O2^xxvii	62.98 (6)	Na2^xxxix—Cl2—Na2^xl	90.0
Na2^xxxix—Na4—O2^xxvii	48.16 (5)	Na2^xxxiii—Cl2—Na2^xl	180.0
Na2^xiv—Na4—O2^xxvii	71.42 (7)	Na4^xiv—Cl2—Na2	54.735 (1)
Na2^xl—Na4—O2^xxvii	150.3 (4)	Na4^xv—Cl2—Na2	125.265 (1)
Cl2—Na4—O2^xxvii	83.7 (2)	Na4^xiii—Cl2—Na2	54.735 (1)
O1^xxiv—Na4—O2^xxviii	75.89 (8)	Na4—Cl2—Na2	125.3
O1^xxv—Na4—O2^xxviii	62.98 (6)	Na2^xxxii—Cl2—Na2	90.000 (2)
O1^xxvi—Na4—O2^xxviii	151.8 (4)	Na2^xxxix—Cl2—Na2	90.0
Na2^xxxix—Na4—O2^xxviii	71.42 (7)	Na2^xxxiii—Cl2—Na2	90.000 (1)
Na2^xiv—Na4—O2^xxviii	150.3 (4)	Na2^xl—Cl2—Na2	90.0
Na2^xl—Na4—O2^xxviii	48.16 (5)	Na4^xiv—Cl2—Na2^xiv	125.3
Cl2—Na4—O2^xxviii	83.7 (2)	Na4^xv—Cl2—Na2^xiv	54.735 (1)
O2^xxvii—Na4—O2^xxviii	118.80 (8)	Na4^xiii—Cl2—Na2^xiv	125.265 (1)
O1^xxiv—Na4—O2^xxix	62.98 (6)	Na4—Cl2—Na2^xiv	54.735 (1)
O1^xxv—Na4—O2^xxix	151.8 (4)	Na2^xxxii—Cl2—Na2^xiv	90.0
O1^xxvi—Na4—O2^xxix	75.89 (8)	Na2^xxxix—Cl2—Na2^xiv	90.000 (2)
Na2^xxxix—Na4—O2^xxix	150.3 (4)	Na2^xxxiii—Cl2—Na2^xiv	90.0
Na2^xiv—Na4—O2^xxix	48.16 (5)	Na2^xl—Cl2—Na2^xiv	90.000 (1)
Na2^xl—Na4—O2^xxix	71.42 (7)	Na2—Cl2—Na2^xiv	180.0

Symmetry codes: (i) −x+1/2, −y+1, z−1/2; (ii) x, −y+1/2, −z+1/2; (iii) −x, −y+1/2, z−1/2; (iv) −x, y, −z+1; (v) −x+1/2, y, −z+1/2; (vi) −x+1/2, −y+1/2, z; (vii) x−1, −y+1, −z+1; (viii) x−1, y−1/2, z−1/2; (ix) x+1/2, −y+1, −z+3/2; (x) x+1/2, y+1/2, z; (xi) −x+1/2, y+1/2, −z+1; (xii) −x+1/2, −y+1, z+1/2; (xiii) −x+3/2, y, −z+3/2; (xiv) −x+3/2, −y+3/2, z; (xv) x, −y+3/2, −z+3/2; (xvi) x, −y+1, −z+1; (xvii) x, y+1/2, z+1/2; (xviii) −y+1/2, −z+1, x+1/2; (xix) −z+1, x+1/2, −y+1/2; (xx) x+1/2, −y+1/2, −z+1; (xxi) −y+1/2, z, −x+1/2; (xxii) z, −x+1/2, −y+1/2; (xxiii) y+1/2, z+1/2, x; (xxiv) −y+1, −z+1, x+1; (xxv) −z+1, x+1, −y+1; (xxvi) x+1, −y+1, −z+1; (xxvii) −z+3/2, −x+1, y+1/2; (xxviii) y+1/2, −z+3/2, −x+1; (xxix) −x+1, y+1/2, −z+3/2; (xxx) −y+1, z+1, −x+1; (xxxi) z+1, −x+1, −y+1; (xxxii) z, x, y; (xxxiii) y, z, x; (xxxiv) y+1/2, z, x+1/2; (xxxv) z, x+1/2, y+1/2; (xxxvi) −y+1/2, z−1/2, −x; (xxxvii) −y+1/2, −z+1/2, x; (xxxviii) z, −x, −y; (xxxix) z, −x+3/2, −y+3/2; (xl) −y+3/2, z, −x+3/2; (xli) −x+1, y−1, −z+1; (xlii) −x+1, −y+1, z−1; (xliii) x, y−1/2, z−1/2; (xliv) z−1/2, x−1/2, y−1; (xlv) −y+1, z−1/2, −x+1/2; (xlvi) y−1/2, z−1, x−1/2; (xlvii) z−1/2, −x+1/2, −y+1; (xlviii) x−1/2, y−1/2, z; (xlix) −x, −y+1/2, z+1/2; (l) x−1/2, −y+1/2, −z+1; (li) −x+1, y−1/2, −z+3/2.

Summary of the observed hhl reflections in Li₄B₄Al₃O₁₂Cl and Na₄B₄Al₃O₁₂Cl top

	Li₄B₄Al₃O₁₂Cl		Na₄B₄Al₃O₁₂Cl
	<I/σ(I)>	Number of reflections	<I/σ(I)>	Number of reflections
No conditions	14.35	325	12.14	340
h even	30.24	153	24.96	165
h odd	0.21	172	0.04	175
l even	30.24	153	24.96	165
l odd	0.21	172	0.04	175
h + l even	14.35	325	12.14	340
h + l odd	0.00	0	0.00	0

Selected bond lengths and angles (Å, °) in A₄B₄Al₃O₁₂Cl crystal structures top

Space group F43c			Space group F23
	A = Li	A = Na		A = Li	A = Na
A1—O1	2.0828 (17)	2.2588 (16)	A1—O1	2.053 (3)	2.2585 (18)
A1—O1ⁱ	2.0828 (17)	2.446 (2)	A1—O2ⁱⁱ	2.143 (16)	2.452 (3)
			A2—O2ⁱⁱⁱ	2.056 (4)	2.2602 (18)
			A2—O1^iv	2.132 (16)	2.442 (3)
A1—Cl1	3.2460 (1)	2.936 (4)	A1—Cl1	2.98 (6)	2.925 (6)
			A2—Cl2	3.03 (6)	2.948 (6)
A2—O1^v	2.22 (3)	2.484 (5)	A3—O2^vi	2.23 (3)	2.488 (6)
A2—O1^vii	2.828 (8)	2.913 (2)	A3—O1^vii	2.824 (8)	2.912 (2)
			A4—O1^viii	2.23 (3)	2.480 (6)
			A4—O2^ix	2.826 (8)	2.914 (2)
A2—Cl1	2.57 (5)	2.605 (9)	A3—Cl1	2.55 (6)	2.599 (10)
			A4—Cl2	2.55 (5)	2.612 (10)
B1—O1	1.3700 (16)	1.3693 (15)	B1—O1	1.3693 (17)	1.3684 (16)
			B2—O2^x	1.3702 (17)	1.3684 (16)
Al1—O1^xi	1.7533 (17)	1.7506 (16)	Al1—O1^xi	1.754 (2)	1.7495 (18)
			Al1—O2^xii	1.754 (2)	1.7522 (18)

B1—O1—Al1^xiii	118.97 (12)	128.59 (12)	B1—O1—Al1^xiii	119.05 (13)	128.62 (14)
			B2^xiv—O2—Al1^vii	118.94 (13)	128.66 (14)

Symmetry code(s): (i) -x, -z+1/2, y; (ii) -x, y, -z+1; (iii) x+1/2, -y+1, -z+3/2; (iv) -x+1/2, -y+1, z+1/2; (v) -y+1/2, x+1/2, -z+1/2; (vi) -z+1, x+1/2, -y+1/2; (vii) z, -x+1/2, -y+1/2; (viii) x+1, -y+1, -z+1; (ix) -x+1, y+1/2, -z+3/2; (x) z, x+1/2, y+1/2; (xi) z, x, y; (xii) -y+1/2, z-1/2, -x; (xiii) y, z, x; (xiv) x-1/2, y-1/2, z.

Funding information

Funding for this research was provided by: Japan Society for the Promotion of Science (grant No. 19H00828).

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