Synthesis and crystal structure of NaRbB5O8(OH)·H2O

Zhang, X.-Y.; Xiao, H.-L.; Zhou, X.-L.; Zou, M.-J.; Cheng, J.-W.; Wen, Y.-H.

doi:10.1107/S2056989026007140

research communications

CRYSTALLOGRAPHIC
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ISSN: 2056-9890

Volume 82| Part 8| August 2026| Pages 942-945

https://doi.org/10.1107/S2056989026007140

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Synthesis and crystal structure of NaRbB₅O₈(OH)·H₂O

Xin-Yue Zhang,^a Hui-Lin Xiao,^a Xiao-Liang Zhou,^a Mei-Jun Zou,^a Jian-Wen Cheng ^a and Yi-Hang Wen ^a ^*

^aKey Laboratory of the Ministry of Education for Advanced Catalysis Materials, Institute of Physical Chemistry, Zhejiang Normal University, Jinhua, Zhejiang 321004, People's Republic of China
^*Correspondence e-mail: [email protected]

Edited by S. P. Kelley, University of Missouri-Columbia, USA (Received 9 April 2026; accepted 10 July 2026; online 21 July 2026)

A new mixed alkali-metal borate, poly[[sodium rubidium [hydroxidoocta-μ-oxidopentaborate] monohydrate], NaRbB₅O₈(OH)·H₂O, has been synthesized via a surfactant-thermal method using H₃BO₃, Rb₂CO₃, Na₂SiO₃·9H₂O, ethanediamine and poly(ethylene glycol)-400 as starting materials. It features a layered boron-oxide framework constructed from pentaborate [B₅O₁₀(OH)]⁶⁻ building units. Adjacent single layers are interconnected to form double layers through hydrogen-bonding interactions. Na⁺, Rb⁺ cations and H₂O molecules are located in the voids of the framework.

Keywords: alkali-metal borate; pentaborate unit; surfactant-thermal synthesis; hydrogen bond; crystal structure.

CCDC reference: 2543102

1. Chemical context

Crystalline metal borates are widely recognized as promising non-linear optical materials in the ultraviolet region (Zhang et al., 2026 ; Li et al., 2023a ,b ,c ; Lu et al., 2024 ; Tian et al., 2013 ; Chen et al., 2024a , 2025 ; Wang et al., 2017 , 2025 ; Wei et al., 2016 ; Yu et al., 2017 ; Zhao et al., 2025 , 2026 ; Zou et al., 2026a ). Boron can adopt either three- or four-coordinate geometries with oxygen atoms. Corner-sharing oxygen linkages between planar BO₃ triangles and tetrahedral BO₄ units enable the construction of various polyborate anions (Mutailipu et al., 2021 ), including [B₃O₃(OH)₄]⁻, [B₄O₅(OH)₄]²⁻, [B₇O₁₂(OH)₁₄]⁷⁻, and [B₁₂O₁₈(OH)₆]⁶⁻ (Lin et al., 2011 ; Huang et al., 2019 ; Chen et al., 2024c ). Pentaborate units typically serve as fundamental building blocks. Various arrangements of BO₃ triangles, BO₄ tetrahedra, as well as [B₅O_n] (n= 10–12, 14) and hydroxylated [B₅O_n(OH)_m] units, have been observed (Wei et al., 2014 ; Ding et al., 2018 ). These pentaborate anions are further interconnected to construct chains, layers, and three-dimensional frameworks with rich structural diversity (Li et al., 2024 ; Shi et al., 2019 ; Zhao et al., 2022 , 2024 ; Chen et al., 2024b ). In such crystal structures, alkali and alkaline-earth metal cations reside in interstitial voids to balance the overall charge of the polyborate anionic frameworks.

Borosilicates are new types of non-linear optical materials that combine different anionic groups (Ou et al., 2025 ). Our initial synthetic strategy was aimed at the exploration of new borosilicate crystals. However, the targeted borosilicate phase was not obtained under the applied synthetic conditions, and a pure borate compound was ultimately isolated instead. Herein, we report the synthesis and single-crystal structural characterization of a new mixed alkali-metal pentaborate, NaRbB₅O₈(OH)·H₂O, (I).

2. Structural commentary

The title compound crystallizes in the triclinic space group P $[\overline{1}]$ . The asymmetric unit of (I) consists of five boron atoms, ten oxygen atoms, three hydrogen atoms, one Na⁺ cation and one Rb⁺ cation. As shown in Fig. 1, the fundamental building block of (I) is the [B₅O₁₀(OH)]⁶⁻ unit, which is composed of two [BO₃] triangles, two [BO₄] tetrahedra and one [BO₂(OH)] group. The B—O bond lengths fall in the range 1.344 (3)–1.506 (3) Å (Table 1). Each [B₅O₁₀(OH)]⁶⁻ unit links to four adjacent equivalents, generating a two-dimensional layered structure containing nine-membered ring windows in the ab plane (Fig. 2).

Table 1
Selected bond lengths (Å)

Rb1—O8ⁱ	2.8044 (18)	B1—O2	1.365 (3)
Rb1—O6ⁱⁱ	2.8777 (18)	B1—O1	1.386 (4)
Rb1—O4	2.9174 (17)	B2—O4	1.420 (3)
Rb1—O7ⁱⁱ	2.9197 (17)	B2—O6^vii	1.474 (3)
Rb1—O4ⁱ	2.9691 (17)	B2—O9^viii	1.495 (3)
Rb1—O5	3.0402 (19)	B2—O2	1.504 (3)
Rb1—O9ⁱⁱ	3.0659 (19)	B3—O4	1.438 (3)
Rb1—O5ⁱⁱⁱ	3.0669 (17)	B3—O7	1.469 (3)
Rb1—O7	3.1981 (19)	B3—O5	1.493 (3)
Na1—O3	2.320 (2)	B3—O3	1.506 (3)
Na1—O10	2.328 (2)	B4—O5	1.344 (3)
Na1—O6	2.372 (2)	B4—O6	1.364 (3)
Na1—O10^iv	2.408 (3)	B4—O8^ix	1.392 (3)
Na1—O2^v	2.470 (2)	B5—O7	1.356 (3)
Na1—O1^vi	2.773 (3)	B5—O9	1.359 (3)
B1—O3	1.348 (4)	B5—O8	1.383 (3)
Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) ; (vii) ; (viii) ; (ix) .

Figure 1
Structure of (I)

with displacement ellipsoids drawn at the 50% probability level. [Symmetry codes: (vii) x, y − 1, z; (viii) x − 1, y, z].

Figure 2
Two-dimensional layered structure of (I)

in the ab plane.

Adjacent single layers are connected into double layers through O—H⋯O hydrogen-bonding interactions between the hydroxyl group (O1) and oxygen atom (O2) of the [B₅O₁₀(OH)]⁶⁻ units. Hydrogen-bonding interactions also exist between the water molecule (O10) and hydroxyl group (O1) in the anionic framework. The corresponding O⋯O hydrogen-bond distances range from 2.869 (3) to 2.916 (3) Å (Table 2). Its hydrogen-bonding interactions are highly analogous to those of the isotypic protonated borate NaKB₅O₈(OH)·H₂O (Li et al., 2024). These hydrogen-bonded double layers further stack parallel to one another along the c axis. Na⁺ ions and water molecules reside in the interlayer voids within the double layers, whereas Rb⁺ ions occupy the voids between adjacent double layers. The Na⁺ and Rb⁺ ions are six- and nine-coordinated, respectively, with Na—O distances of 2.320 (2)–2.773 (3) Å and Rb—O distances of 2.8044 (18)–3.1981 (19) Å (Table 1). These cations occupy the voids of the framework to maintain overall charge balance (Fig. 3).

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1⋯O2^x	0.82	2.11	2.869 (3)	155
O10—H10B⋯O1^iv	0.84	2.16	2.916 (3)	151
Symmetry codes: (iv) ; (x) .

Figure 3
View of the three-dimensional packing structure of (I)

along the b axis.

3. Database survey

An online search of the Inorganic Crystal Structure Database (ICSD, version 5.6.0, updated January 2026, Zagorac et al., 2019 ) for alkali-metal compounds incorporating the [B₅O₁₀(OH)]⁶⁻ moiety returned seven hits: NaKB₅O₈(OH)·H₂O (triclinic, P $[\overline{1}]$ space group; Li et al., 2024), LiRbB₅O₈(OH)·H₂O (monoclinic, P2₁/n space group; Shi et al., 2019), K₂B₅O₈(OH)·2H₂O (orthorhombic, Pna2₁ space group; Shi et al., 2019), Rb₂B₅O₈(OH) (orthorhombic, Pca2₁ space group; Qiu et al., 2021 ), LiCsB₅O₈(OH)·H₂O (monoclinic, P2₁/c space group; Chen et al., 2017 ), LiKB₅O₈(OH)·1.5H₂O (orthorhombic, C222₁ space group; Li et al., 2019 ), and Na₂B₅O₈(OH)·2H₂O (orthorhombic, Pna2₁ space group; Wang et al., 2009 ). In addition, we have recently reported another pentaborate, NaCsB₅O₈(OH)·H₂O (orthorhombic, Pbca space group; Zou et al., 2026b ). Compound (I) is isostructural with NaKB₅O₈(OH)·H₂O, and they share the same space group and similar cell parameters. The other seven reported compounds share similar layered structural features and the common [B₅O₁₀(OH)]⁶⁻ building unit. Differences in alkali metal cations and space groups lead to the structural uniqueness of compound (I).

4. Synthesis and crystallization

A mixture of H₃BO₃ (0.6183 g, 10 mmol), Rb₂CO₃ (0.2308 g, 1 mmol), Na₂SiO₃·9H₂O (0.2842 g, 1 mmol), ethanediamine (1 ml), and poly(ethylene glycol)-400 (4 ml) was sealed in a 30 ml Teflon-lined bomb at 453 K for 6 days and then cooled to room temperature over 6 hours. Colorless crystals of (I) were obtained by filtration, washed with distilled water, and dried in air.

5. Refinement

Crystal data, data collection and structure refinement details are summarized in Table 3. H atoms bonded to O atoms were positioned geometrically and refined using a riding model [O_hydroxyl—H = 0.82 Å and O_water—H = 0.84 Å, U_iso(H) = 1.2 U_eq(O)].

Table 3
Experimental details

Crystal data
Chemical formula	NaRbB₅O₈(OH)·H₂O
M_r	325.53
Crystal system, space group	Triclinic, P $[\overline{1}]$
Temperature (K)	287
a, b, c (Å)	6.6580 (4), 6.6744 (4), 11.5322 (6)
α, β, γ (°)	79.094 (2), 77.508 (2), 60.492 (2)
V (Å³)	433.37 (4)
Z	2
Radiation type	Mo Kα
μ (mm⁻¹)	5.80
Crystal size (mm)	0.13 × 0.12 × 0.10

Data collection
Diffractometer	Bruker APEXII area detector
Absorption correction	Empirical (using intensity measurements) (SADABS; Krause et al., 2015 )
T_min, T_max	0.48, 0.56
No. of measured, independent and observed [I > 2σ(I)] reflections	9111, 1985, 1863
R_int	0.035
(sin θ/λ)_max (Å⁻¹)	0.649

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.026, 0.065, 1.08
No. of reflections	1985
No. of parameters	155
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.87, −0.42
Computer programs: APEX2 and SAINT (Bruker, 2014 ), SHELXT (Sheldrick, 2015a ), SHELXL2014/7 (Sheldrick, 2015b ) and OLEX2 (Dolomanov et al., 2009 ).

Supporting information

CCDC reference: 2543102

Crystal structure: contains datablocks I, new. DOI: https://doi.org/10.1107/S2056989026007140/ev2027sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S2056989026007140/ev2027Isup3.hkl

checkCIF report

Computing details top

Poly[[sodium rubidium [hydroxidoocta-µ-oxidopentaborate] monohydrate] top

Crystal data top

NaRbB₅O₈(OH)·H₂O	Z = 2
M_r = 325.53	F(000) = 312
Triclinic, P1	D_x = 2.495 Mg m⁻³
a = 6.6580 (4) Å	Mo Kα radiation, λ = 0.71073 Å
b = 6.6744 (4) Å	Cell parameters from 5543 reflections
c = 11.5322 (6) Å	θ = 3.5–27.5°
α = 79.094 (2)°	µ = 5.80 mm⁻¹
β = 77.508 (2)°	T = 287 K
γ = 60.492 (2)°	Block, clear colourless
V = 433.37 (4) Å³	0.13 × 0.12 × 0.10 mm

Data collection top

Bruker APEXII area detector diffractometer	1863 reflections with I > 2σ(I)
ω scans	R_int = 0.035
Absorption correction: empirical (using intensity measurements) (SADABS; Krause et al., 2015)	θ_max = 27.5°, θ_min = 3.5°
T_min = 0.48, T_max = 0.56	h = −8→8
9111 measured reflections	k = −8→8
1985 independent reflections	l = −14→14

Refinement top

Refinement on F²	Hydrogen site location: mixed
Least-squares matrix: full	H-atom parameters constrained
R[F² > 2σ(F²)] = 0.026	w = 1/[σ²(F_o²) + (0.0306P)² + 0.5265P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.065	(Δ/σ)_max < 0.001
S = 1.08	Δρ_max = 0.87 e Å⁻³
1985 reflections	Δρ_min = −0.42 e Å⁻³
155 parameters	Extinction correction: SHELXL2014/7 (Sheldrick 2015b), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.005 (2)

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
Rb1	−0.15536 (4)	0.31899 (4)	0.42548 (2)	0.01816 (11)
Na1	−0.1957 (2)	0.6023 (2)	0.90050 (11)	0.0262 (3)
B1	−0.3018 (5)	0.1647 (5)	0.9121 (3)	0.0167 (6)
B2	−0.3654 (5)	0.0470 (5)	0.7382 (3)	0.0126 (5)
B3	−0.1935 (5)	0.3118 (4)	0.7072 (2)	0.0111 (5)
B4	−0.4410 (5)	0.7519 (5)	0.6765 (3)	0.0133 (5)
B5	0.2491 (5)	0.1475 (5)	0.6798 (3)	0.0147 (5)
O1	−0.3247 (4)	0.1631 (4)	1.03462 (18)	0.0266 (5)
H1	−0.3758	0.0744	1.0684	0.040*
O2	−0.3634 (3)	0.0278 (3)	0.87005 (16)	0.0172 (4)
O3	−0.2273 (3)	0.3071 (3)	0.84093 (16)	0.0182 (4)
O4	−0.2045 (3)	0.1225 (3)	0.67186 (15)	0.0118 (3)
O5	−0.3820 (3)	0.5345 (3)	0.66024 (17)	0.0152 (4)
O6	−0.2980 (3)	0.8115 (3)	0.71344 (16)	0.0136 (4)
O7	0.0306 (3)	0.3107 (3)	0.66079 (17)	0.0156 (4)
O8	0.3356 (3)	−0.0786 (3)	0.6563 (2)	0.0228 (4)
O9	0.3882 (3)	0.2091 (3)	0.71832 (18)	0.0182 (4)
O10	0.1852 (4)	0.5348 (4)	0.8910 (2)	0.0294 (5)
H10A	0.2601	0.4538	0.8343	0.044*
H10B	0.2258	0.6376	0.8853	0.044*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Rb1	0.01984 (15)	0.01750 (15)	0.02004 (15)	−0.01100 (11)	−0.00189 (9)	−0.00294 (9)
Na1	0.0329 (6)	0.0231 (6)	0.0287 (6)	−0.0154 (5)	−0.0134 (5)	0.0009 (5)
B1	0.0189 (14)	0.0152 (13)	0.0169 (14)	−0.0080 (11)	−0.0038 (11)	−0.0020 (11)
B2	0.0103 (12)	0.0104 (12)	0.0178 (14)	−0.0050 (10)	−0.0016 (10)	−0.0032 (10)
B3	0.0115 (12)	0.0082 (11)	0.0152 (13)	−0.0055 (10)	−0.0022 (10)	−0.0017 (10)
B4	0.0115 (12)	0.0122 (12)	0.0154 (13)	−0.0046 (10)	−0.0017 (10)	−0.0026 (10)
B5	0.0139 (13)	0.0120 (12)	0.0173 (14)	−0.0053 (11)	−0.0024 (10)	−0.0022 (10)
O1	0.0438 (13)	0.0338 (12)	0.0146 (9)	−0.0283 (10)	−0.0024 (9)	−0.0025 (8)
O2	0.0234 (9)	0.0200 (9)	0.0151 (9)	−0.0161 (8)	−0.0012 (7)	−0.0016 (7)
O3	0.0284 (10)	0.0197 (9)	0.0151 (9)	−0.0173 (8)	−0.0033 (8)	−0.0034 (7)
O4	0.0125 (8)	0.0102 (8)	0.0147 (8)	−0.0068 (7)	−0.0012 (6)	−0.0023 (6)
O5	0.0119 (8)	0.0094 (8)	0.0261 (10)	−0.0039 (7)	−0.0071 (7)	−0.0037 (7)
O6	0.0113 (8)	0.0086 (8)	0.0217 (9)	−0.0039 (7)	−0.0049 (7)	−0.0024 (7)
O7	0.0093 (8)	0.0107 (8)	0.0274 (10)	−0.0052 (7)	−0.0034 (7)	−0.0006 (7)
O8	0.0148 (9)	0.0124 (9)	0.0439 (13)	−0.0032 (7)	−0.0137 (8)	−0.0074 (8)
O9	0.0120 (9)	0.0107 (8)	0.0321 (11)	−0.0028 (7)	−0.0057 (7)	−0.0072 (7)
O10	0.0274 (11)	0.0318 (12)	0.0292 (12)	−0.0139 (9)	−0.0003 (9)	−0.0078 (9)

Geometric parameters (Å, º) top

Rb1—O8ⁱ	2.8044 (18)	B2—Rb1ⁱ	3.482 (3)
Rb1—O6ⁱⁱ	2.8777 (18)	B3—O4	1.438 (3)
Rb1—O4	2.9174 (17)	B3—O7	1.469 (3)
Rb1—O7ⁱⁱ	2.9197 (17)	B3—O5	1.493 (3)
Rb1—O4ⁱ	2.9691 (17)	B3—O3	1.506 (3)
Rb1—O5	3.0402 (19)	B4—O5	1.344 (3)
Rb1—O9ⁱⁱ	3.0659 (19)	B4—O6	1.364 (3)
Rb1—O5ⁱⁱⁱ	3.0669 (17)	B4—O8^ix	1.392 (3)
Rb1—B3	3.197 (3)	B4—Rb1ⁱⁱⁱ	3.415 (3)
Rb1—O7	3.1981 (19)	B4—Rb1ⁱⁱ	3.703 (3)
Rb1—B5ⁱⁱ	3.323 (3)	B5—O7	1.356 (3)
Rb1—B4ⁱⁱⁱ	3.415 (3)	B5—O9	1.359 (3)
Na1—O3	2.320 (2)	B5—O8	1.383 (3)
Na1—O10	2.328 (2)	B5—Rb1ⁱⁱ	3.323 (3)
Na1—O6	2.372 (2)	O1—Na1^vi	2.773 (3)
Na1—O10^iv	2.408 (3)	O1—H1	0.8200
Na1—O2^v	2.470 (2)	O2—Na1^vii	2.470 (2)
Na1—O1^vi	2.773 (3)	O4—Rb1ⁱ	2.9691 (17)
Na1—B2^v	3.017 (3)	O5—Rb1ⁱⁱⁱ	3.0669 (17)
Na1—B4	3.095 (3)	O6—B2^v	1.474 (3)
Na1—Na1^iv	3.438 (2)	O6—Rb1ⁱⁱ	2.8778 (18)
Na1—Rb1ⁱⁱ	4.0661 (13)	O7—Rb1ⁱⁱ	2.9197 (17)
Na1—H10A	2.6638	O8—B4^x	1.393 (3)
B1—O3	1.348 (4)	O8—Rb1ⁱ	2.8043 (18)
B1—O2	1.365 (3)	O9—B2^xi	1.495 (3)
B1—O1	1.386 (4)	O9—Rb1ⁱⁱ	3.0659 (19)
B2—O4	1.420 (3)	O10—Na1^iv	2.408 (3)
B2—O6^vii	1.474 (3)	O10—Rb1ⁱⁱ	3.618 (2)
B2—O9^viii	1.495 (3)	O10—H10A	0.8343
B2—O2	1.504 (3)	O10—H10B	0.8397
B2—Na1^vii	3.017 (3)

O8ⁱ—Rb1—O6ⁱⁱ	105.39 (5)	Na1^iv—Na1—Rb1ⁱⁱ	106.24 (5)
O8ⁱ—Rb1—O4	93.14 (6)	O3—Na1—H10A	99.4
O6ⁱⁱ—Rb1—O4	120.87 (5)	O10—Na1—H10A	17.6
O8ⁱ—Rb1—O7ⁱⁱ	139.14 (6)	O6—Na1—H10A	94.4
O6ⁱⁱ—Rb1—O7ⁱⁱ	63.54 (5)	O10^iv—Na1—H10A	97.8
O4—Rb1—O7ⁱⁱ	126.94 (5)	O2^v—Na1—H10A	103.5
O8ⁱ—Rb1—O4ⁱ	65.68 (5)	O1^vi—Na1—H10A	169.4
O6ⁱⁱ—Rb1—O4ⁱ	48.12 (5)	B2^v—Na1—H10A	97.7
O4—Rb1—O4ⁱ	96.20 (4)	B4—Na1—H10A	109.6
O7ⁱⁱ—Rb1—O4ⁱ	111.32 (5)	Na1^iv—Na1—H10A	56.6
O8ⁱ—Rb1—O5	119.37 (6)	Rb1ⁱⁱ—Na1—H10A	50.7
O6ⁱⁱ—Rb1—O5	132.86 (5)	O3—B1—O2	123.4 (2)
O4—Rb1—O5	47.21 (5)	O3—B1—O1	118.3 (2)
O7ⁱⁱ—Rb1—O5	88.93 (5)	O2—B1—O1	118.2 (2)
O4ⁱ—Rb1—O5	141.35 (5)	O4—B2—O6^vii	111.0 (2)
O8ⁱ—Rb1—O9ⁱⁱ	100.57 (5)	O4—B2—O9^viii	113.1 (2)
O6ⁱⁱ—Rb1—O9ⁱⁱ	94.20 (5)	O6^vii—B2—O9^viii	110.6 (2)
O4—Rb1—O9ⁱⁱ	137.30 (5)	O4—B2—O2	111.0 (2)
O7ⁱⁱ—Rb1—O9ⁱⁱ	46.02 (5)	O6^vii—B2—O2	104.7 (2)
O4ⁱ—Rb1—O9ⁱⁱ	126.34 (5)	O9^viii—B2—O2	106.1 (2)
O5—Rb1—O9ⁱⁱ	91.62 (5)	O4—B2—Na1^vii	120.06 (16)
O8ⁱ—Rb1—O5ⁱⁱⁱ	46.44 (5)	O6^vii—B2—Na1^vii	50.58 (11)
O6ⁱⁱ—Rb1—O5ⁱⁱⁱ	128.56 (5)	O9^viii—B2—Na1^vii	126.80 (17)
O4—Rb1—O5ⁱⁱⁱ	104.92 (5)	O2—B2—Na1^vii	54.58 (11)
O7ⁱⁱ—Rb1—O5ⁱⁱⁱ	107.34 (5)	O4—B2—Rb1ⁱ	57.43 (11)
O4ⁱ—Rb1—O5ⁱⁱⁱ	108.89 (5)	O6^vii—B2—Rb1ⁱ	54.13 (11)
O5—Rb1—O5ⁱⁱⁱ	94.80 (5)	O9^viii—B2—Rb1ⁱ	137.87 (17)
O9ⁱⁱ—Rb1—O5ⁱⁱⁱ	61.34 (5)	O2—B2—Rb1ⁱ	115.65 (15)
O8ⁱ—Rb1—B3	118.10 (7)	Na1^vii—B2—Rb1ⁱ	77.10 (6)
O6ⁱⁱ—Rb1—B3	117.20 (6)	O4—B3—O7	112.4 (2)
O4—Rb1—B3	26.71 (6)	O4—B3—O5	109.14 (19)
O7ⁱⁱ—Rb1—B3	100.64 (6)	O7—B3—O5	107.95 (19)
O4ⁱ—Rb1—B3	113.99 (6)	O4—B3—O3	111.7 (2)
O5—Rb1—B3	27.55 (6)	O7—B3—O3	107.32 (19)
O9ⁱⁱ—Rb1—B3	117.66 (6)	O5—B3—O3	108.17 (19)
O5ⁱⁱⁱ—Rb1—B3	114.24 (6)	O4—B3—Rb1	65.75 (12)
O8ⁱ—Rb1—O7	138.07 (5)	O7—B3—Rb1	76.77 (13)
O6ⁱⁱ—Rb1—O7	91.65 (5)	O5—B3—Rb1	70.37 (12)
O4—Rb1—O7	46.24 (4)	O3—B3—Rb1	175.90 (16)
O7ⁱⁱ—Rb1—O7	82.76 (5)	O5—B4—O6	123.9 (2)
O4ⁱ—Rb1—O7	103.24 (5)	O5—B4—O8^ix	116.5 (2)
O5—Rb1—O7	45.07 (4)	O6—B4—O8^ix	119.6 (2)
O9ⁱⁱ—Rb1—O7	116.34 (5)	O5—B4—Na1	93.79 (16)
O5ⁱⁱⁱ—Rb1—O7	139.24 (5)	O6—B4—Na1	46.49 (12)
B3—Rb1—O7	26.56 (6)	O8^ix—B4—Na1	131.13 (18)
O8ⁱ—Rb1—B5ⁱⁱ	124.32 (6)	O5—B4—Rb1ⁱⁱⁱ	63.74 (13)
O6ⁱⁱ—Rb1—B5ⁱⁱ	83.61 (6)	O6—B4—Rb1ⁱⁱⁱ	172.23 (18)
O4—Rb1—B5ⁱⁱ	129.51 (6)	O8^ix—B4—Rb1ⁱⁱⁱ	52.91 (12)
O7ⁱⁱ—Rb1—B5ⁱⁱ	23.98 (6)	Na1—B4—Rb1ⁱⁱⁱ	138.69 (10)
O4ⁱ—Rb1—B5ⁱⁱ	127.99 (6)	O5—B4—Rb1ⁱⁱ	94.43 (15)
O5—Rb1—B5ⁱⁱ	83.11 (6)	O6—B4—Rb1ⁱⁱ	43.80 (12)
O9ⁱⁱ—Rb1—B5ⁱⁱ	24.12 (6)	O8^ix—B4—Rb1ⁱⁱ	135.22 (17)
O5ⁱⁱⁱ—Rb1—B5ⁱⁱ	84.63 (6)	Na1—B4—Rb1ⁱⁱ	72.86 (6)
B3—Rb1—B5ⁱⁱ	103.94 (7)	Rb1ⁱⁱⁱ—B4—Rb1ⁱⁱ	138.55 (9)
O7—Rb1—B5ⁱⁱ	95.01 (6)	O7—B5—O9	119.4 (2)
O8ⁱ—Rb1—B4ⁱⁱⁱ	23.33 (6)	O7—B5—O8	121.0 (2)
O6ⁱⁱ—Rb1—B4ⁱⁱⁱ	119.67 (6)	O9—B5—O8	119.5 (2)
O4—Rb1—B4ⁱⁱⁱ	99.01 (6)	O7—B5—Rb1ⁱⁱ	61.07 (13)
O7ⁱⁱ—Rb1—B4ⁱⁱⁱ	125.52 (6)	O9—B5—Rb1ⁱⁱ	67.26 (14)
O4ⁱ—Rb1—B4ⁱⁱⁱ	87.64 (6)	O8—B5—Rb1ⁱⁱ	147.58 (19)
O5—Rb1—B4ⁱⁱⁱ	107.45 (6)	B1—O1—Na1^vi	102.67 (17)
O9ⁱⁱ—Rb1—B4ⁱⁱⁱ	81.07 (6)	B1—O1—H1	109.5
O5ⁱⁱⁱ—Rb1—B4ⁱⁱⁱ	23.13 (6)	Na1^vi—O1—H1	68.7
B3—Rb1—B4ⁱⁱⁱ	117.84 (7)	B1—O2—B2	118.9 (2)
O7—Rb1—B4ⁱⁱⁱ	143.96 (6)	B1—O2—Na1^vii	128.30 (17)
B5ⁱⁱ—Rb1—B4ⁱⁱⁱ	105.15 (7)	B2—O2—Na1^vii	95.68 (14)
O3—Na1—O10	114.72 (9)	B1—O3—B3	120.6 (2)
O3—Na1—O6	87.80 (7)	B1—O3—Na1	126.20 (17)
O10—Na1—O6	102.94 (8)	B3—O3—Na1	112.48 (14)
O3—Na1—O10^iv	97.54 (8)	B2—O4—B3	120.1 (2)
O10—Na1—O10^iv	86.93 (9)	B2—O4—Rb1	132.21 (15)
O6—Na1—O10^iv	165.69 (9)	B3—O4—Rb1	87.55 (13)
O3—Na1—O2^v	139.94 (8)	B2—O4—Rb1ⁱ	98.80 (13)
O10—Na1—O2^v	94.71 (8)	B3—O4—Rb1ⁱ	133.22 (14)
O6—Na1—O2^v	58.24 (6)	Rb1—O4—Rb1ⁱ	83.80 (4)
O10^iv—Na1—O2^v	111.23 (8)	B4—O5—B3	129.0 (2)
O3—Na1—O1^vi	90.30 (8)	B4—O5—Rb1	124.85 (16)
O10—Na1—O1^vi	154.55 (9)	B3—O5—Rb1	82.08 (13)
O6—Na1—O1^vi	81.58 (7)	B4—O5—Rb1ⁱⁱⁱ	93.13 (14)
O10^iv—Na1—O1^vi	85.11 (8)	B3—O5—Rb1ⁱⁱⁱ	135.15 (14)
O2^v—Na1—O1^vi	66.05 (7)	Rb1—O5—Rb1ⁱⁱⁱ	85.20 (5)
O3—Na1—B2^v	115.13 (8)	B4—O6—B2^v	124.4 (2)
O10—Na1—B2^v	97.70 (9)	B4—O6—Na1	108.88 (16)
O6—Na1—B2^v	28.69 (7)	B2^v—O6—Na1	100.73 (14)
O10^iv—Na1—B2^v	140.75 (9)	B4—O6—Rb1ⁱⁱ	117.06 (15)
O2^v—Na1—B2^v	29.74 (7)	B2^v—O6—Rb1ⁱⁱ	101.35 (13)
O1^vi—Na1—B2^v	74.11 (7)	Na1—O6—Rb1ⁱⁱ	101.09 (6)
O3—Na1—B4	66.83 (7)	B5—O7—B3	129.6 (2)
O10—Na1—B4	122.57 (9)	B5—O7—Rb1ⁱⁱ	94.94 (15)
O6—Na1—B4	24.64 (7)	B3—O7—Rb1ⁱⁱ	132.55 (14)
O10^iv—Na1—B4	150.00 (9)	B5—O7—Rb1	119.02 (16)
O2^v—Na1—B4	74.63 (7)	B3—O7—Rb1	76.67 (13)
O1^vi—Na1—B4	70.18 (7)	Rb1ⁱⁱ—O7—Rb1	97.24 (5)
B2^v—Na1—B4	48.48 (8)	B5—O8—B4^x	121.5 (2)
O3—Na1—Na1^iv	112.03 (7)	B5—O8—Rb1ⁱ	134.67 (16)
O10—Na1—Na1^iv	44.38 (6)	B4^x—O8—Rb1ⁱ	103.76 (15)
O6—Na1—Na1^iv	146.14 (8)	B5—O9—B2^xi	124.3 (2)
O10^iv—Na1—Na1^iv	42.55 (6)	B5—O9—Rb1ⁱⁱ	88.62 (15)
O2^v—Na1—Na1^iv	108.01 (7)	B2^xi—O9—Rb1ⁱⁱ	133.40 (15)
O1^vi—Na1—Na1^iv	123.50 (7)	Na1—O10—Na1^iv	93.07 (9)
B2^v—Na1—Na1^iv	129.28 (8)	Na1—O10—Rb1ⁱⁱ	83.25 (7)
B4—Na1—Na1^iv	166.20 (8)	Na1^iv—O10—Rb1ⁱⁱ	172.67 (9)
O3—Na1—Rb1ⁱⁱ	90.67 (6)	Na1—O10—H10A	104.6
O10—Na1—Rb1ⁱⁱ	62.09 (6)	Na1^iv—O10—H10A	125.6
O6—Na1—Rb1ⁱⁱ	43.99 (5)	Rb1ⁱⁱ—O10—H10A	50.0
O10^iv—Na1—Rb1ⁱⁱ	148.42 (7)	Na1—O10—H10B	125.3
O2^v—Na1—Rb1ⁱⁱ	79.34 (5)	Na1^iv—O10—H10B	101.5
O1^vi—Na1—Rb1ⁱⁱ	125.46 (6)	Rb1ⁱⁱ—O10—H10B	85.8
B2^v—Na1—Rb1ⁱⁱ	56.58 (6)	H10A—O10—H10B	108.3
B4—Na1—Rb1ⁱⁱ	60.48 (6)

O3—B1—O1—Na1^vi	106.2 (2)	Rb1ⁱⁱⁱ—B4—O5—Rb1	86.33 (13)
O2—B1—O1—Na1^vi	−71.6 (3)	Rb1ⁱⁱ—B4—O5—Rb1	−56.82 (15)
O3—B1—O2—B2	−4.5 (4)	O6—B4—O5—Rb1ⁱⁱⁱ	−178.1 (2)
O1—B1—O2—B2	173.2 (2)	O8^ix—B4—O5—Rb1ⁱⁱⁱ	3.4 (2)
O3—B1—O2—Na1^vii	121.0 (2)	Na1—B4—O5—Rb1ⁱⁱⁱ	143.78 (7)
O1—B1—O2—Na1^vii	−61.3 (3)	Rb1ⁱⁱ—B4—O5—Rb1ⁱⁱⁱ	−143.15 (6)
O4—B2—O2—B1	27.4 (3)	O4—B3—O5—B4	176.8 (2)
O6^vii—B2—O2—B1	147.2 (2)	O7—B3—O5—B4	−60.8 (3)
O9^viii—B2—O2—B1	−95.9 (3)	O3—B3—O5—B4	55.0 (3)
Na1^vii—B2—O2—B1	140.1 (2)	Rb1—B3—O5—B4	−129.0 (2)
Rb1ⁱ—B2—O2—B1	90.3 (2)	O4—B3—O5—Rb1	−54.17 (17)
O4—B2—O2—Na1^vii	−112.69 (17)	O7—B3—O5—Rb1	68.22 (16)
O6^vii—B2—O2—Na1^vii	7.12 (18)	O3—B3—O5—Rb1	−175.95 (17)
O9^viii—B2—O2—Na1^vii	124.07 (16)	O4—B3—O5—Rb1ⁱⁱⁱ	20.8 (3)
Rb1ⁱ—B2—O2—Na1^vii	−49.79 (13)	O7—B3—O5—Rb1ⁱⁱⁱ	143.17 (16)
O2—B1—O3—B3	−3.8 (4)	O3—B3—O5—Rb1ⁱⁱⁱ	−101.0 (2)
O1—B1—O3—B3	178.5 (2)	Rb1—B3—O5—Rb1ⁱⁱⁱ	74.95 (16)
O2—B1—O3—Na1	165.68 (19)	O5—B4—O6—B2^v	−176.3 (2)
O1—B1—O3—Na1	−12.0 (4)	O8^ix—B4—O6—B2^v	2.1 (4)
O4—B3—O3—B1	−11.5 (3)	Na1—B4—O6—B2^v	−118.2 (3)
O7—B3—O3—B1	−135.1 (2)	Rb1ⁱⁱ—B4—O6—B2^v	128.1 (3)
O5—B3—O3—B1	108.7 (2)	O5—B4—O6—Na1	−58.2 (3)
O4—B3—O3—Na1	177.71 (15)	O8^ix—B4—O6—Na1	120.3 (2)
O7—B3—O3—Na1	54.1 (2)	Rb1ⁱⁱ—B4—O6—Na1	−113.76 (15)
O5—B3—O3—Na1	−62.1 (2)	O5—B4—O6—Rb1ⁱⁱ	55.6 (3)
O6^vii—B2—O4—B3	−161.2 (2)	O8^ix—B4—O6—Rb1ⁱⁱ	−126.0 (2)
O9^viii—B2—O4—B3	73.8 (3)	Na1—B4—O6—Rb1ⁱⁱ	113.76 (15)
O2—B2—O4—B3	−45.2 (3)	O9—B5—O7—B3	−127.1 (3)
Na1^vii—B2—O4—B3	−105.5 (2)	O8—B5—O7—B3	55.3 (4)
Rb1ⁱ—B2—O4—B3	−153.0 (2)	Rb1ⁱⁱ—B5—O7—B3	−162.2 (3)
O6^vii—B2—O4—Rb1	81.4 (2)	O9—B5—O7—Rb1ⁱⁱ	35.1 (3)
O9^viii—B2—O4—Rb1	−43.6 (3)	O8—B5—O7—Rb1ⁱⁱ	−142.5 (2)
O2—B2—O4—Rb1	−162.63 (13)	O9—B5—O7—Rb1	136.2 (2)
Na1^vii—B2—O4—Rb1	137.07 (12)	O8—B5—O7—Rb1	−41.4 (3)
Rb1ⁱ—B2—O4—Rb1	89.59 (15)	Rb1ⁱⁱ—B5—O7—Rb1	101.11 (12)
O6^vii—B2—O4—Rb1ⁱ	−8.2 (2)	O4—B3—O7—B5	−60.4 (3)
O9^viii—B2—O4—Rb1ⁱ	−133.16 (18)	O5—B3—O7—B5	179.2 (2)
O2—B2—O4—Rb1ⁱ	107.78 (17)	O3—B3—O7—B5	62.8 (3)
Na1^vii—B2—O4—Rb1ⁱ	47.47 (16)	Rb1—B3—O7—B5	−116.8 (2)
O7—B3—O4—B2	158.4 (2)	O4—B3—O7—Rb1ⁱⁱ	144.03 (15)
O5—B3—O4—B2	−81.9 (3)	O5—B3—O7—Rb1ⁱⁱ	23.6 (3)
O3—B3—O4—B2	37.6 (3)	O3—B3—O7—Rb1ⁱⁱ	−92.7 (2)
Rb1—B3—O4—B2	−138.8 (2)	Rb1—B3—O7—Rb1ⁱⁱ	87.61 (16)
O7—B3—O4—Rb1	−62.82 (18)	O4—B3—O7—Rb1	56.42 (17)
O5—B3—O4—Rb1	56.89 (17)	O5—B3—O7—Rb1	−63.97 (16)
O3—B3—O4—Rb1	176.48 (17)	O3—B3—O7—Rb1	179.65 (17)
O7—B3—O4—Rb1ⁱ	16.3 (3)	O7—B5—O8—B4^x	−179.4 (2)
O5—B3—O4—Rb1ⁱ	136.02 (16)	O9—B5—O8—B4^x	3.0 (4)
O3—B3—O4—Rb1ⁱ	−104.4 (2)	Rb1ⁱⁱ—B5—O8—B4^x	96.7 (4)
Rb1—B3—O4—Rb1ⁱ	79.14 (15)	O7—B5—O8—Rb1ⁱ	−1.6 (4)
O6—B4—O5—B3	18.6 (4)	O9—B5—O8—Rb1ⁱ	−179.15 (17)
O8^ix—B4—O5—B3	−159.9 (2)	Rb1ⁱⁱ—B5—O8—Rb1ⁱ	−85.5 (4)
Na1—B4—O5—B3	−19.5 (3)	O7—B5—O9—B2^xi	−177.7 (2)
Rb1ⁱⁱⁱ—B4—O5—B3	−163.3 (3)	O8—B5—O9—B2^xi	−0.1 (4)
Rb1ⁱⁱ—B4—O5—B3	53.5 (3)	Rb1ⁱⁱ—B5—O9—B2^xi	−144.7 (2)
O6—B4—O5—Rb1	−91.7 (3)	O7—B5—O9—Rb1ⁱⁱ	−33.1 (2)
O8^ix—B4—O5—Rb1	89.8 (3)	O8—B5—O9—Rb1ⁱⁱ	144.5 (2)
Na1—B4—O5—Rb1	−129.89 (11)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1···O2^xii	0.82	2.11	2.869 (3)	155
O10—H10B···O1^iv	0.84	2.16	2.916 (3)	151

Symmetry codes: (iv) −x, −y+1, −z+2; (xii) −x−1, −y, −z+2.

Acknowledgements

This work was supported by the National Natural Science Foundation of China (No. 21975224).

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