Crystal structure of MgK0.5[B6O10](OH)0.5·0.5H2O, poly[dimagnesium potassium bis(hexa­borate) hy­droxide monohydrate]

Qiu, Q.-M.; Song, J.-B.

doi:10.1107/S2056989022008982

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Volume 78| Part 10| October 2022| Pages 1003-1005

https://doi.org/10.1107/S2056989022008982

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Crystal structure of MgK_0.5[B₆O₁₀](OH)_0.5·0.5H₂O, poly[dimagnesium potassium bis(hexaborate) hydroxide monohydrate]

Qi-Ming Qiu ^a ^* and Jian-Biao Song ^b

^aSchool of Science, China University of Geosciences, Beijing 100083, People's Republic of China, and ^bBeijing Chaoyang Foreign Language School, Beijing 100101, People's Republic of China
^*Correspondence e-mail: qiuqiming890521@163.com

Edited by B. Therrien, University of Neuchâtel, Switzerland (Received 31 August 2022; accepted 7 September 2022; online 8 September 2022)

The solvothermal reaction of H₃BO₃, KCF₃SO₃, Mg(CF₃SO₃)₂ and pyridine led to a new alkali- and alkaline-earth-metal borate, MgK_0.5[B₆O₁₀](OH)_0.5·0.5H₂O. Its structure features an intricate three-dimensional framework built from [B₆O₁₃]⁸⁻ clusters, thus resulting in a six-connected achiral net with high symmetry. Each [B₆O₁₃]⁸⁻ building block is composed of three trigonal BO₃ and three tetrahedral BO₄ units, with these BO₄ units being further connected to neighboring BO₃ units, giving rise to an oxoboron cluster of the general formula [B₆O₁₀]²⁻.

Keywords: alkali–earth-metal borate; alkaline-earth-metal borate; solvothermal synthesis; three-dimensional framework; crystal structure.

CCDC reference: 2205808

1. Chemical context

As inorganic materials, borates are an important class of non-linear optical crystals, mainly because they can easily crystallize in non-centrosymmetric space groups and such structures often show a large second-harmonic generation response (Qiu et al., 2021a ; Qui & Yang, 2021a ). The combination of BO₃-trigonal and BO₄-tetrahedral units makes it possible to form a variety of isolated anionic clusters. Extended chains, layers and three-dimensional frameworks can be formed between clusters through the dehydration and condensation of the terminal hydroxyl groups of oxoboron clusters (Wang et al., 2017 ). In addition, negatively charged oxoboron clusters can also combine with a variety of counter-cations, making the structure of borates more complex and diverse. Here, single crystals of MgK_0.5[B₆O₁₀](OH)_0.5·0.5H₂O with alkali- and alkaline-earth metals have been obtained under solvothermal conditions.

2. Structural commentary

The asymmetric unit of the title compound consists of 2 B, 10/3 O, 1/3 Mg, 1/6 K, 1/6 OH, and 1/6 H₂O. The Mg, K, O4, O5 and O6 atoms are located on special positions with occupancy of 1/3 or 1/6, while the remaining B and O atoms are located at general positions with an occupancy of 1. Bond-valence-sum calculations show that Mg, K and B are consistent with the expected oxidation states (Brown & Altermatt, 1985 ; Brese & O'Keeffe, 1991 ). Three BO₄ units are joined together through corner-sharing of the O4 atom and three BO₄ units are connected with three neighboring BO₃ units to form a [B₆O₁₃]⁸⁻ oxoboron cluster (Fig. 1). To the best of our knowledge, this is the first example of a mixed alkali- and alkaline-earth-metal borate crystal with the [B₆O₁₃]⁸⁻ cluster anion. In this cluster, the B—O4 bonds are unique because their bond distances [1.529 (2) Å] are longer than other B—O bonds [1.359 (2)–1.453 (2) Å] in the BO₃ and BO₄ units. Each [B₆O₁₃]⁸⁻ unit is further connected to six other clusters by corner-sharing O atoms, resulting in a three-dimensional framework (Fig. 2).

Figure 1
The asymmetric unit of the [B₆O₁₃]⁸⁻ oxoboron cluster. Displacement ellipsoids are drawn at the 50% probability level.

Figure 2
View of the three-dimensional supramolecular framework along the [100] direction. Color code: BO₃ trigonal, yellow, orange and brown; BO₄ tetrahedral, blue.

3. Supramolecular features

In the title compound, the Mg and K atoms are six-coordinated, with Mg—O and distances in the range 2.332 (1)–2.374 (1) Å and K—O = 2.845 (1) Å. The three-dimensional structure is stabilized by a water cluster formed by O5—H5⋯O5, O5—H5⋯O6 and O6—H6A⋯O2 hydrogen bonds involving the water molecule, hydroxyl group and oxoboron cluster (Table 1). The channels of the compound are filled with ions/molecules (Mg²⁺, K⁺, OH⁻ and H₂O). The title structure is similar to previously reported analogues NH₄NaB₆O₁₀ (Wang et al., 2014 ), K_0.5[B₆O₁₀]·H₂O·1.5H₃O (Qiu & Yang, 2021b ), and NaRb_0.5[B₆O₁₀]·0.5H₃O (Qiu et al., 2021b ), so the simultaneous use of NH₄ and Na or K or Na and Rb or Mg and K cations as templates has no effect on the crystallization of the oxoboron three-dimensional framework. However, after the introduction of Cl (Wu et al., 2011 ) or Br (Al-Ama et al., 2006 ), the new compounds crystallize in the trigonal space group R3m with a large second-harmonic generation response. The introduction of different anions can therefore play a key role in changing the crystalline structure to a non-centrosymmetric system.

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O5—H5⋯O5ⁱ	0.85	1.67	2.42 (3)	145
O6—H6A⋯O2ⁱ	0.85	2.58	3.276 (15)	140
O5—H5⋯O6ⁱ	0.85	1.78	2.484 (19)	139
O5—H5⋯O5ⁱⁱ	0.85	2.30	3.06 (3)	150
Symmetry codes: (i) $[y+{\script{1\over 2}}, -z+{\script{1\over 2}}, -x+1]$ ; (ii) .

4. Database survey

A search of the Cambridge Structural Database (CSD, version 5.43, update June 2022; Groom et al., 2016 ) for the [B₆O₁₃]⁸⁻ oxoboron cluster gave 23 hits. The terminal oxygen atoms of this type of [B₆O_x] unit can be completely deprotonated [B₆O₁₃]⁸⁻, partially protonated [B₆O₁₁(OH)₂]⁶⁻ or completely protonated [B₆O₇(OH)₆]²⁻. Among the above 23 compounds, most of them are inorganic–organic hybrid solids, which contain transition-metal complexes and the [B₆O₇(OH)₆]²⁻ cluster (refcodes: CAFYIV, CAFYOB, Altahan et al., 2021 ; CECWEM, Heller & Schellhaas, 1983 ; EMEHIP, Li et al., 2016 ; HIXNAF, Jamai et al., 2014 ; JOCCUC, JOCDAJ, Altahan et al., 2019a ; JUZLIC, Altahan et al., 2020 ; MEBQUI, MEBRET, Altahan et al., 2017 ; POJVIW, POJVOC, Altahan et al., 2019b ; TAFROI, Natarajan et al., 2003 ; VUVLOP, Jemai et al., 2015 ; BATCUY, Jamai et al., 2022 ; SAZVEY, Xin et al., 2022 ). It is worth noting that this oxoboron cluster contains too many active hydroxyl groups and therefore tends to form isolated structures. In the crystal of [Cd(1,2-dap)]·[B₆O₁₁(OH)₂]·H₂O (1,2-dap = 1,2-diaminopropane, refcode: LOZZUY, Deng et al., 2020 ) and Cd₃[B₆O₉(OH)₂]₂·2NO₃·4H₂O (refcode: ZUXLIQ, He et al., 2020 ), partially protonated [B₆O₁₁(OH)₂]⁶⁻ was successfully extended to layered structures via B—O—B bonds. In the crystal of NaRb_0.5[B₆O₁₀]·0.5H₃O (refcode: UCEXOT, Qiu et al., 2021b), each completely deprotonated [B₆O₁₃]⁸⁻ unit was linked to six nearest neighbors by bridging O atoms, leading to a 3D framework, similar to that of the title compound.

5. Synthesis and crystallization

A mixture of H₃BO₃ (0.618 g, 10 mmol), KCF₃SO₃ (0.188 g, 1 mmol) and Mg(CF₃SO₃)₂ (0.322 g, 1 mmol) was added to pyridine (3.0 mL). After stirring for 20 min, the resulting mixture was sealed in a 25 mL Teflon-lined stainless steel autoclave, heated at 488 K for 9 d, and then slowly cooled to room temperature and colorless block-shaped crystals MgK_0.5[B₆O₁₀](OH)_0.5·0.5H₂O were obtained (yield 56% based on H₃BO₃). Infrared (KBr pallet, cm⁻¹): 3190vs, 1631s, 1360s, 1268m, 1188m, 1134m, 1099m, 964s, 845m, 781m, 741m, 718m, 630w, 564w, 540w, 480w, 455w.

6. Refinement

Crystal data, data collection and structure refinement details are summarized in Table 2. Hydrogen atoms were positioned geometrically (O—H = 0.85 Å) and refined as riding with U_iso(H) 1.2U_eq(O).

Table 2
Experimental details

Crystal data
Chemical formula	Mg₂K[B₆O₁₀]₂(OH)·H₂O
M_r	572.46
Crystal system, space group	Cubic, Pa $[\overline{3}]$
Temperature (K)	296
a (Å)	12.2966 (2)
V (Å³)	1859.32 (9)
Z	4
Radiation type	Mo Kα
μ (mm⁻¹)	0.47
Crystal size (mm)	0.10 × 0.08 × 0.08

Data collection
Diffractometer	Bruker APEXII CCD
Absorption correction	Multi-scan (SADABS; Krause et al., 2015 )
T_min, T_max	0.762, 0.936
No. of measured, independent and observed [I > 2σ(I)] reflections	23808, 952, 828
R_int	0.056
(sin θ/λ)_max (Å⁻¹)	0.714

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.039, 0.116, 1.16
No. of reflections	952
No. of parameters	72
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.66, −0.64
Computer programs: APEX2 and SAINT (Bruker, 2006 ), SHELXT2018/3 (Sheldrick, 2015a ), SHELXL2018/3 (Sheldrick, 2015b ), and SHELXTL (Sheldrick, 2008 ).

Supporting information

CCDC reference: 2205808

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S2056989022008982/tx2057sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S2056989022008982/tx2057Isup2.hkl

checkCIF report

Computing details top

Data collection: APEX2 (Bruker, 2006); cell refinement: SAINT (Bruker, 2006); data reduction: SAINT (Bruker, 2006); program(s) used to solve structure: SHELXT2018/3 (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2018/3 (Sheldrick, 2015b); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Poly[dimagnesium potassium bis(hexaborate) hydroxide monohydrate] top

Crystal data top

MgK_0.5[B₆O₁₀](OH)_0.5·0.5H₂O	Mo Kα radiation, λ = 0.71073 Å
M_r = 572.46	Cell parameters from 5324 reflections
Cubic, Pa3	θ = 2.9–30.3°
a = 12.2966 (2) Å	µ = 0.47 mm⁻¹
V = 1859.32 (9) Å³	T = 296 K
Z = 4	Block, colorless
F(000) = 1128	0.10 × 0.08 × 0.08 mm
D_x = 2.045 Mg m⁻³

Data collection top

Bruker APEXII CCD diffractometer	828 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube, Bruker (Mo) X-ray Source	R_int = 0.056
φ and ω scans	θ_max = 30.5°, θ_min = 3.3°
Absorption correction: multi-scan (SADABS; Krause et al., 2015)	h = −16→17
T_min = 0.762, T_max = 0.936	k = −16→16
23808 measured reflections	l = −16→17
952 independent reflections

Refinement top

Refinement on F²	0 restraints
Least-squares matrix: full	Hydrogen site location: difference Fourier map
R[F² > 2σ(F²)] = 0.039	H-atom parameters constrained
wR(F²) = 0.116	w = 1/[σ²(F_o²) + (0.0658P)² + 0.9552P] where P = (F_o² + 2F_c²)/3
S = 1.16	(Δ/σ)_max < 0.001
952 reflections	Δρ_max = 0.66 e Å⁻³
72 parameters	Δρ_min = −0.64 e Å⁻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.

Refinement. The structure was solved by direct methods and refined by the full-matrix least-squares method on F² using the SHELXL programs (Bruker, 2006; Sheldrick, 2015a). All non-hydrogen atoms in the complex were refined anisotropically.

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Mg	0.33884 (5)	0.33884 (5)	0.33884 (5)	0.0205 (3)
K	0.500000	0.500000	0.500000	0.0257 (3)
O1	0.52065 (8)	0.28854 (8)	0.29782 (8)	0.0110 (3)
O2	0.22982 (9)	0.18931 (8)	0.38027 (8)	0.0118 (3)
O3	0.36386 (8)	0.68000 (8)	0.55091 (8)	0.0113 (3)
O4	0.18887 (7)	0.18887 (7)	0.18887 (7)	0.0057 (3)
O5	0.4745 (13)	0.1216 (14)	0.5078 (12)	0.066 (4)	0.1667
H5	0.504419	0.061354	0.523614	0.099*	0.1667
O6	0.544 (2)	0.0524 (17)	0.5575 (10)	0.080 (6)	0.1667
H6A	0.548070	0.065436	0.625259	0.121*	0.1667
H6B	0.587560	0.097246	0.528419	0.121*	0.1667
B1	0.21526 (12)	0.22026 (12)	0.48534 (12)	0.0084 (3)
B2	0.16682 (11)	0.13303 (11)	0.29771 (11)	0.0067 (3)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mg	0.0205 (3)	0.0205 (3)	0.0205 (3)	0.0007 (2)	0.0007 (2)	0.0007 (2)
K	0.0257 (3)	0.0257 (3)	0.0257 (3)	0.0071 (2)	0.0071 (2)	0.0071 (2)
O1	0.0060 (4)	0.0113 (5)	0.0156 (5)	0.0015 (3)	−0.0031 (3)	−0.0047 (4)
O2	0.0141 (5)	0.0157 (5)	0.0055 (4)	−0.0039 (4)	0.0005 (3)	−0.0023 (3)
O3	0.0138 (5)	0.0134 (5)	0.0066 (4)	0.0060 (4)	−0.0017 (4)	−0.0027 (3)
O4	0.0057 (3)	0.0057 (3)	0.0057 (3)	0.0007 (3)	0.0007 (3)	0.0007 (3)
O5	0.058 (8)	0.074 (11)	0.067 (9)	0.005 (7)	0.011 (7)	−0.018 (8)
O6	0.123 (19)	0.101 (16)	0.017 (5)	0.029 (12)	−0.018 (7)	−0.002 (6)
B1	0.0094 (6)	0.0091 (6)	0.0065 (6)	0.0007 (5)	−0.0008 (5)	−0.0009 (5)
B2	0.0067 (6)	0.0067 (6)	0.0067 (6)	0.0003 (4)	0.0006 (4)	0.0005 (5)

Geometric parameters (Å, º) top

Mg—O2ⁱ	2.3319 (12)	O2—B1	1.3587 (16)
Mg—O2ⁱⁱ	2.3319 (12)	O2—B2	1.4525 (16)
Mg—O2	2.3319 (12)	O3—B1^vii	1.3570 (18)
Mg—O1ⁱ	2.3738 (10)	O3—B2^viii	1.4519 (16)
Mg—O1ⁱⁱ	2.3738 (10)	O4—B2ⁱ	1.5285 (15)
Mg—O1	2.3738 (10)	O4—B2ⁱⁱ	1.5285 (15)
Mg—B1	2.7714 (15)	O4—B2	1.5285 (15)
Mg—B1ⁱ	2.7715 (15)	O5—O6^ix	0.96 (2)
Mg—B1ⁱⁱ	2.7715 (15)	O5—O6^x	1.27 (3)
Mg—K	3.4324 (11)	O5—O6	1.35 (3)
K—O3	2.8450 (10)	O5—H5	0.8500
K—O3ⁱⁱⁱ	2.8450 (10)	O5—H6B	1.4451
K—O3ⁱ	2.8450 (10)	O5—H6A^ix	0.70 (3)
K—O3^iv	2.8450 (10)	O6—O6^ix	1.20 (3)
K—O3^v	2.8450 (10)	O6—O6^xi	1.20 (3)
K—O3ⁱⁱ	2.8450 (10)	O6—H5	0.6476
O1—B1ⁱⁱ	1.3821 (18)	O6—H6A	0.8500
O1—B2^vi	1.4531 (16)	O6—H6B	0.8500

O2ⁱ—Mg—O2ⁱⁱ	81.06 (5)	B1ⁱⁱ—O1—B2^vi	123.77 (11)
O2ⁱ—Mg—O2	81.06 (5)	B1ⁱⁱ—O1—Mg	91.19 (8)
O2ⁱⁱ—Mg—O2	81.06 (5)	B2^vi—O1—Mg	144.28 (8)
O2ⁱ—Mg—O1ⁱ	112.48 (4)	B1—O2—B2	136.70 (11)
O2ⁱⁱ—Mg—O1ⁱ	132.64 (4)	B1—O2—Mg	93.59 (8)
O2—Mg—O1ⁱ	58.46 (3)	B2—O2—Mg	121.98 (8)
O2ⁱ—Mg—O1ⁱⁱ	58.46 (3)	B1^vii—O3—B2^viii	122.23 (11)
O2ⁱⁱ—Mg—O1ⁱⁱ	112.48 (4)	B1^vii—O3—K	125.09 (8)
O2—Mg—O1ⁱⁱ	132.64 (4)	B2^viii—O3—K	110.32 (7)
O1ⁱ—Mg—O1ⁱⁱ	112.97 (3)	B2ⁱ—O4—B2ⁱⁱ	117.97 (4)
O2ⁱ—Mg—O1	132.64 (4)	B2ⁱ—O4—B2	117.97 (4)
O2ⁱⁱ—Mg—O1	58.46 (3)	B2ⁱⁱ—O4—B2	117.97 (4)
O2—Mg—O1	112.48 (4)	O6^ix—O5—O6	59 (2)
O1ⁱ—Mg—O1	112.96 (3)	O6^x—O5—O6	89.1 (19)
O1ⁱⁱ—Mg—O1	112.96 (3)	O6^ix—O5—H5	47.9
O2ⁱ—Mg—B1	93.22 (5)	O6^x—O5—H5	67.1
O2ⁱⁱ—Mg—B1	109.26 (5)	O6—O5—H5	22.1
O2—Mg—B1	29.29 (4)	O6^ix—O5—H6B	94.6
O1ⁱ—Mg—B1	29.91 (4)	O6^x—O5—H6B	104.1
O1ⁱⁱ—Mg—B1	123.25 (4)	O6—O5—H6B	35.2
O1—Mg—B1	121.16 (4)	H5—O5—H6B	50.4
O2ⁱ—Mg—B1ⁱ	29.30 (4)	O5^xi—O6—O6^ix	71 (3)
O2ⁱⁱ—Mg—B1ⁱ	93.22 (5)	O5^xi—O6—O6^xi	77 (3)
O2—Mg—B1ⁱ	109.26 (5)	O6^ix—O6—O6^xi	101 (2)
O1ⁱ—Mg—B1ⁱ	121.16 (4)	O5^xi—O6—O5^xii	114 (2)
O1ⁱⁱ—Mg—B1ⁱ	29.90 (4)	O6^ix—O6—O5^xii	136.9 (16)
O1—Mg—B1ⁱ	123.25 (4)	O6^xi—O6—O5^xii	45.7 (12)
B1—Mg—B1ⁱ	114.20 (3)	O5^xi—O6—O5	107 (3)
O2ⁱ—Mg—B1ⁱⁱ	109.26 (5)	O6^ix—O6—O5	43.9 (9)
O2ⁱⁱ—Mg—B1ⁱⁱ	29.30 (4)	O6^xi—O6—O5	133.5 (16)
O2—Mg—B1ⁱⁱ	93.22 (5)	O5^xii—O6—O5	134.5 (17)
O1ⁱ—Mg—B1ⁱⁱ	123.25 (4)	O5^xi—O6—H5	104.1
O1ⁱⁱ—Mg—B1ⁱⁱ	121.16 (4)	O6^ix—O6—H5	33.1
O1—Mg—B1ⁱⁱ	29.91 (4)	O6^xi—O6—H5	103.9
B1—Mg—B1ⁱⁱ	114.20 (3)	O5^xii—O6—H5	117.5
B1ⁱ—Mg—B1ⁱⁱ	114.20 (3)	O5—O6—H5	29.6
O2ⁱ—Mg—K	131.38 (3)	O5^xi—O6—H6A	44.8
O2ⁱⁱ—Mg—K	131.38 (3)	O6^ix—O6—H6A	101.0
O2—Mg—K	131.38 (3)	O6^xi—O6—H6A	103.2
O1ⁱ—Mg—K	74.30 (3)	O5^xii—O6—H6A	111.4
O1ⁱⁱ—Mg—K	74.30 (3)	O5—O6—H6A	111.4
O1—Mg—K	74.30 (3)	H5—O6—H6A	130.2
B1—Mg—K	104.19 (4)	O5^xi—O6—H6B	149.2
B1ⁱ—Mg—K	104.19 (4)	O6^ix—O6—H6B	122.2
B1ⁱⁱ—Mg—K	104.19 (4)	O6^xi—O6—H6B	122.0
O3—K—O3ⁱⁱⁱ	65.411 (16)	O5^xii—O6—H6B	76.7
O3—K—O3ⁱ	114.589 (16)	O5—O6—H6B	78.5
O3ⁱⁱⁱ—K—O3ⁱ	180.0	H5—O6—H6B	95.3
O3—K—O3^iv	65.410 (16)	H6A—O6—H6B	104.5
O3ⁱⁱⁱ—K—O3^iv	114.590 (15)	O5^xi—O6—H5^xi	58.1 (15)
O3ⁱ—K—O3^iv	65.410 (15)	O6^ix—O6—H5^xi	74 (3)
O3—K—O3ⁱⁱ	114.590 (16)	O6^xi—O6—H5^xi	28.4 (18)
O3ⁱⁱⁱ—K—O3ⁱⁱ	65.410 (15)	O5^xii—O6—H5^xi	74 (3)
O3ⁱ—K—O3ⁱⁱ	114.590 (15)	O5—O6—H5^xi	114 (3)
O3^iv—K—O3ⁱⁱ	180.0	H5—O6—H5^xi	87.3
O3^v—K—O3ⁱⁱ	65.410 (16)	H6A—O6—H5^xi	97.8
O3—K—Mg^v	76.32 (2)	H6B—O6—H5^xi	148.0
O3ⁱⁱⁱ—K—Mg^v	103.68 (2)	O3^xiii—B1—O2	123.87 (12)
O3ⁱ—K—Mg^v	76.32 (2)	O3^xiii—B1—O1ⁱ	122.17 (12)
O3^iv—K—Mg^v	103.68 (2)	O2—B1—O1ⁱ	113.96 (12)
O3^v—K—Mg^v	103.68 (2)	O3^xiii—B1—Mg	166.22 (10)
O3ⁱⁱ—K—Mg^v	76.32 (2)	O2—B1—Mg	57.12 (7)
O3—K—Mg	103.68 (2)	O1ⁱ—B1—Mg	58.91 (7)
O3ⁱⁱⁱ—K—Mg	76.32 (2)	O3^xiv—B2—O2	112.28 (11)
O3ⁱ—K—Mg	103.68 (2)	O3^xiv—B2—O1^xv	109.48 (11)
O3^iv—K—Mg	76.32 (2)	O2—B2—O1^xv	110.35 (11)
O3^v—K—Mg	76.32 (2)	O3^xiv—B2—O4	109.12 (10)
O3ⁱⁱ—K—Mg	103.68 (2)	O2—B2—O4	107.66 (11)
Mg^v—K—Mg	180.000 (17)	O1^xv—B2—O4	107.83 (10)

O6^ix—O5—O6—O5^xi	−36 (3)	B1—O2—B2—O3^xiv	21.1 (2)
O6^x—O5—O6—O5^xi	−94.9 (17)	Mg—O2—B2—O3^xiv	−119.29 (10)
O6^x—O5—O6—O6^ix	−59 (2)	B1—O2—B2—O1^xv	−101.35 (17)
O6^ix—O5—O6—O6^xi	52 (3)	Mg—O2—B2—O1^xv	118.27 (10)
O6^x—O5—O6—O6^xi	−7 (5)	B1—O2—B2—O4	141.21 (14)
O6^ix—O5—O6—O5^xii	117 (3)	Mg—O2—B2—O4	0.84 (12)
O6^x—O5—O6—O5^xii	58 (4)	B2ⁱ—O4—B2—O3^xiv	45.6 (2)
B2—O2—B1—O3^xiii	16.3 (2)	B2ⁱⁱ—O4—B2—O3^xiv	−162.41 (10)
Mg—O2—B1—O3^xiii	163.52 (12)	B2ⁱ—O4—B2—O2	−76.54 (15)
B2—O2—B1—O1ⁱ	−163.39 (13)	B2ⁱⁱ—O4—B2—O2	75.49 (15)
Mg—O2—B1—O1ⁱ	−16.21 (12)	B2ⁱ—O4—B2—O1^xv	164.40 (10)
B2—O2—B1—Mg	−147.18 (17)	B2ⁱⁱ—O4—B2—O1^xv	−43.6 (2)

Symmetry codes: (i) y, z, x; (ii) z, x, y; (iii) −y+1, −z+1, −x+1; (iv) −z+1, −x+1, −y+1; (v) −x+1, −y+1, −z+1; (vi) y+1/2, z, −x+1/2; (vii) −x+1/2, y+1/2, z; (viii) −y+1/2, −z+1, x+1/2; (ix) −y+1/2, z−1/2, x; (x) −z+1, x−1/2, −y+1/2; (xi) z, −x+1/2, y+1/2; (xii) y+1/2, −z+1/2, −x+1; (xiii) −x+1/2, y−1/2, z; (xiv) z−1/2, −x+1/2, −y+1; (xv) −z+1/2, x−1/2, y.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O5—H5···O5^xii	0.85	1.67	2.42 (3)	145
O6—H6A···O2^xii	0.85	2.58	3.276 (15)	140
O6—H5···O6^ix	0.65	0.74	1.20 (3)	119
O6—H5···O6^x	0.65	1.23	1.84 (2)	158
O6—H5···O6^xvi	0.65	1.82	2.19 (3)	118
O6—H5···O5^ix	0.65	1.79	2.34 (3)	143
O6—H5···O5^x	0.65	2.09	2.484 (19)	121
O6—H5···O5	0.65	0.85	1.35 (3)	128
O5—H5···O6^xii	0.85	1.78	2.484 (19)	139
O5—H5···O6^xi	0.85	1.49	2.34 (3)	179
O5—H5···O6^xvi	0.85	1.82	2.30 (2)	114
O5—H5···O5^xii	0.85	1.67	2.42 (3)	145
O5—H5···O5^xi	0.85	1.28	1.88 (3)	122
O5—H5···O5^xvi	0.85	2.30	3.06 (3)	150

Symmetry codes: (ix) −y+1/2, z−1/2, x; (x) −z+1, x−1/2, −y+1/2; (xi) z, −x+1/2, y+1/2; (xii) y+1/2, −z+1/2, −x+1; (xvi) −x+1, −y, −z+1.

Funding information

We gratefully acknowledge support by the Fundamental Research Funds for the Central Universities (grant No. 2–9-2021–008).

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