Potassium deca­borate monohydrate

Gao, Y.-H.

doi:10.1107/S1600536811039109

inorganic compounds

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ISSN: 2056-9890

Volume 67| Part 10| October 2011| Page i57

https://doi.org/10.1107/S1600536811039109

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Potassium decaborate monohydrate

Yi-Hong Gao ^a ^*

^aCollege of Chemistry & Chemical Engineering, Xianyang Nomal University, Xianyang 712000, People's Republic of China
^*Correspondence e-mail: shanxiab@163.com

(Received 9 September 2011; accepted 23 September 2011; online 30 September 2011)

In the crystal structure of the title compound, K₂[B₁₀O₁₄(OH)₄]·H₂O, the polyborate [B₁₀O₁₄(OH)₄]²⁻ anions are linked together through their common O atoms, forming a helical chain-like structure. Adjacent chains are further connected into a three-dimensional structure by O—H⋯O hydrogen bonds. The water molecules and potassium cations are located between these chains. Further O—H⋯O hydrogen bonds occur between the anions and the water molecules

Related literature

For phases previously obtained in the K₂O—B₂O₃—H₂O system, see: Marezio (1969 ); Marezio et al. (1963 ); Dewey et al. (1975 ); Salentine (1987 ); Touboul et al. (2003 ); Zhang et al. (2005 ); Wang et al. (2006 ); Li et al. (2007 ). For a closely related structure, (NH₄)₂[B₁₀O₁₄(OH)₄]·H₂O, see: Li et al. (2003 ). For the non-linear optical properties of alkali metal borates, see: Mori et al. (1995 ).

Experimental

Crystal data

K₂[B₁₀O₁₄(OH)₄]·H₂O
M_r = 496.35
Triclinic, $[P \overline 1]$
a = 7.5612 (7) Å
b = 9.2236 (10) Å
c = 11.7298 (13) Å
α = 99.038 (6)°
β = 106.595 (6)°
γ = 91.314 (6)°
V = 772.26 (14) Å³
Z = 2
Mo Kα radiation
μ = 0.72 mm⁻¹
T = 100 K
0.16 × 0.08 × 0.05 mm

Data collection

Bruker APEXII diffractometer
Absorption correction: numerical (SADABS, Sheldrick, 2008a ) T_min = 0.895, T_max = 0.962
11219 measured reflections
3148 independent reflections
2141 reflections with I > 2σ(I)
R_int = 0.055

Refinement

R[F² > 2σ(F²)] = 0.045
wR(F²) = 0.113
S = 1.00
3148 reflections
298 parameters
5 restraints
All H-atom parameters refined
Δρ_max = 0.42 e Å⁻³
Δρ_min = −0.46 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1⋯O11ⁱ	0.88 (2)	1.76 (2)	2.599 (3)	159 (3)
O9—H9⋯O18ⁱⁱ	0.87 (2)	1.98 (2)	2.797 (3)	157 (3)
O11—H11⋯O19ⁱⁱⁱ	0.92 (2)	1.65 (2)	2.553 (3)	167 (3)
O18—H18⋯O5^iv	0.89 (2)	2.10 (2)	2.940 (3)	157 (3)
O18—H18⋯O12^iv	0.89 (2)	2.66 (3)	3.193 (3)	119 (3)
O19—H19A⋯O6^v	0.90 (2)	1.79 (3)	2.678 (3)	169 (3)
O19—H19B⋯O16^vi	0.91 (2)	1.79 (3)	2.696 (3)	173 (3)
Symmetry codes: (i) x-1, y-1, z; (ii) x-1, y, z; (iii) x+1, y+1, z; (iv) -x+2, -y+1, -z+2; (v) -x, -y, -z+1; (vi) -x+1, -y, -z+1.

Data collection: APEX2 (Bruker, 2009 ); cell refinement: SAINT (Bruker, 2009); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008b ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008b); molecular graphics: SHELXTL (Sheldrick, 2008b); software used to prepare material for publication: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536811039109/ru2014sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536811039109/ru2014Isup2.hkl

checkCIF report

Comment top

Boron can form many compounds because of the complexity of the structures involved. In the past several decades, much interest has focused on studies of alkali metals borates because some of these compounds show interesting physical properties, such as nonlinear optical behavior for CsLiB₆O₁₀ (Mori et al., 1995). So far, several phases had been obtained in the K₂O—B₂O₃—H₂O system (Marezio et al., 1963; Marezio, 1969; Dewey et al., 1975; Salentine,1987; Touboul et al., 2003; Zhang et al., 2005; Wang et al., 2006; Li et al., 2007). In this paper, we describe the synthesis and the crystal structure of a new potassium borate of K₂[B₁₀O₁₄(OH)₄]^.H₂O.

Single crystal diffraction has revealed that the title compound crystallizes in the triclinic space group P-1. It is composed of two K₊ cation and polyborate anion [B₁₀O₁₄(OH)₄]_2- (Fig.1), which is closely related to the reported compound of (NH₄)₂[B₁₀O₁₄(OH)₄]^.H₂O (Li et al., 2003).

The [B₁₀O₁₄(OH)₄]_2- anion could be considered as two [B₅O₇(OH)₂]_- cluster linked by the common oxygen atom (O3). Each of the [B₅O₇(OH)₂]_- cluster consists of two six-membered rings linked by a common BO₄ tetrahedron. Each six-membered ring consists of one BO₃ triangle, one BO₂(OH) triangle and a common BO₄ tetrahedron. The [B₁₀O₁₄(OH)₄]_2- units are linked together through common oxygen atoms (O17) to neighboring units, forming a 1-D helical chainlike structure (Fig. 2). Adjacent chains are further connected into a three-dimensional structure by O—H···O hydrogen bonds interactions (Fig.3). Water molecules and potassium ions are located among these chains. In addition, there exist O—H···O hydrogen bonds between the oxygen atoms in polyborate anions and Water molecules (Table 1).

Related literature top

For phases previously obtained in the K₂O—B₂O₃—H₂O system, see: Marezio (1969); Marezio et al. (1963); Dewey et al. (1975); Salentine (1987); Touboul et al. (2003); Zhang et al. (2005); Wang et al. (2006); Li et al. (2007). For a closely related structure, (NH₄)₂[B₁₀O₁₄(OH)₄].H₂O, see: Li et al. (2003). For the non-linear optical properties of alkali metal borates, see: Mori et al. (1995).

Experimental top

All reagents used in the synthesis were of analytic grade and were used without further purification. A mixture of K₂TeO₄ (0.216 g) and H₃BO₃ (0.992 g) was sealed in a teflon-lined bomb and heated at 473 K for 5 days and then cooled to room temperature. The resulting colorless and transparent crystals were recovered by washed with deionized water and dried at room temperature.

Structure description top

For phases previously obtained in the K₂O—B₂O₃—H₂O system, see: Marezio (1969); Marezio et al. (1963); Dewey et al. (1975); Salentine (1987); Touboul et al. (2003); Zhang et al. (2005); Wang et al. (2006); Li et al. (2007). For a closely related structure, (NH₄)₂[B₁₀O₁₄(OH)₄].H₂O, see: Li et al. (2003). For the non-linear optical properties of alkali metal borates, see: Mori et al. (1995).

Computing details top

Data collection: APEX2 (Bruker, 2009); cell refinement: SAINT (Bruker, 2009); data reduction: SAINT (Bruker, 2009); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008b); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008b); molecular graphics: SHELXTL (Sheldrick, 2008b); software used to prepare material for publication: SHELXTL (Sheldrick, 2008b).

Figures top

	Fig. 1. The asymmetric unit structure of title compound. Displacement ellipsoids are drawn at the 30% probability level.
	Fig. 2. The one-dimensional chain structure constructed by [B₁₀O₁₄(OH)₄]_2- units. B, O and H atoms are shown as yellow, red and green, respectively.
	Fig. 3. Packing View along the c axis of title compound, showing three-dimensional structure constructed by O—H···O hydrogen bonds, where all potassium cations are omitted for clarity. B, O and H atoms are shown as yellow, red and green, respectively.

(I) top

Crystal data top

H₆B₁₀K₂O₁₉	Z = 2
M_r = 496.35	F(000) = 492
Triclinic, P1	D_x = 2.135 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.5612 (7) Å	Cell parameters from 1883 reflections
b = 9.2236 (10) Å	θ = 2.6–23.1°
c = 11.7298 (13) Å	µ = 0.72 mm⁻¹
α = 99.038 (6)°	T = 100 K
β = 106.595 (6)°	Rod, colorless
γ = 91.314 (6)°	0.16 × 0.08 × 0.05 mm
V = 772.26 (14) Å³

Data collection top

Bruker APEXII diffractometer	3148 independent reflections
Radiation source: fine-focus sealed tube	2141 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.055
Detector resolution: 83.33 pixels mm^-1	θ_max = 26.5°, θ_min = 1.8°
combination of ω and φ–scans	h = −9→7
Absorption correction: numerical (SADABS, Sheldrick, 2008a)	k = −11→11
T_min = 0.895, T_max = 0.962	l = −13→14
11219 measured reflections

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.045	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.113	All H-atom parameters refined
S = 1.00	w = 1/[σ²(F_o²) + (0.0546P)²] where P = (F_o² + 2F_c²)/3
3148 reflections	(Δ/σ)_max = 0.002
298 parameters	Δρ_max = 0.42 e Å⁻³
5 restraints	Δρ_min = −0.46 e Å⁻³

Crystal data top

H₆B₁₀K₂O₁₉	γ = 91.314 (6)°
M_r = 496.35	V = 772.26 (14) Å³
Triclinic, P1	Z = 2
a = 7.5612 (7) Å	Mo Kα radiation
b = 9.2236 (10) Å	µ = 0.72 mm⁻¹
c = 11.7298 (13) Å	T = 100 K
α = 99.038 (6)°	0.16 × 0.08 × 0.05 mm
β = 106.595 (6)°

Data collection top

Bruker APEXII diffractometer	3148 independent reflections
Absorption correction: numerical (SADABS, Sheldrick, 2008a)	2141 reflections with I > 2σ(I)
T_min = 0.895, T_max = 0.962	R_int = 0.055
11219 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.045	5 restraints
wR(F²) = 0.113	All H-atom parameters refined
S = 1.00	Δρ_max = 0.42 e Å⁻³
3148 reflections	Δρ_min = −0.46 e Å⁻³
298 parameters

Special details top

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

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Hydroxyl and water H atoms were identified from a difference Fourier map and were included in with refined positional parameters. The thermal parameters of these H atoms were tied to that of the oxygen to which they are bonded. Mild O—H distances restraints were applied. All of the H atoms form good H-bonds to nearby O atoms.

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

	x	y	z	U_iso*/U_eq
K1	0.02003 (11)	−0.04398 (8)	0.24158 (6)	0.0193 (2)
K2	0.57020 (11)	0.25524 (8)	0.28774 (7)	0.0228 (2)
O1	0.1964 (3)	−0.0442 (2)	0.46853 (19)	0.0157 (5)
H1	0.132 (4)	−0.108 (3)	0.492 (3)	0.019*
O2	0.4077 (3)	0.1569 (2)	0.51318 (18)	0.0135 (5)
O3	0.6155 (3)	0.3561 (2)	0.54323 (18)	0.0133 (5)
O4	0.3447 (3)	0.0566 (2)	0.67480 (18)	0.0137 (5)
O5	0.5940 (3)	0.2474 (2)	0.71450 (18)	0.0129 (5)
O6	0.4224 (3)	0.2380 (2)	0.85610 (18)	0.0135 (5)
O7	0.6184 (3)	0.1485 (2)	1.02546 (18)	0.0133 (5)
O8	0.6280 (3)	0.0473 (2)	0.82680 (18)	0.0137 (5)
O9	0.4452 (3)	0.3433 (2)	1.06130 (19)	0.0158 (5)
H9	0.372 (4)	0.410 (3)	1.037 (3)	0.019*
O10	0.8021 (3)	0.5425 (2)	0.51410 (18)	0.0142 (5)
O11	0.9851 (3)	0.7373 (2)	0.48289 (19)	0.0162 (5)
H11	0.948 (4)	0.698 (3)	0.4022 (17)	0.019*
O12	0.7542 (3)	0.5525 (2)	0.70700 (18)	0.0134 (5)
O13	0.9867 (3)	0.7205 (2)	0.67953 (18)	0.0148 (5)
O14	0.8285 (3)	0.7940 (2)	0.82488 (18)	0.0129 (5)
O15	0.9989 (3)	0.7625 (2)	1.02361 (18)	0.0131 (5)
O16	1.0478 (3)	0.6058 (2)	0.85501 (19)	0.0144 (5)
O17	0.7994 (3)	0.9505 (2)	1.00052 (18)	0.0122 (5)
O18	1.2111 (3)	0.5743 (2)	1.04997 (19)	0.0149 (5)
H18	1.247 (4)	0.615 (3)	1.1280 (17)	0.018*
O19	−0.0980 (4)	−0.3366 (3)	0.2539 (2)	0.0208 (6)
H19A	−0.213 (4)	−0.315 (4)	0.214 (3)	0.025*
H19B	−0.079 (5)	−0.424 (3)	0.213 (3)	0.025*
B1	0.3158 (5)	0.0559 (4)	0.5553 (3)	0.0130 (8)
B2	0.5436 (5)	0.2550 (4)	0.5960 (3)	0.0114 (8)
B3	0.4978 (5)	0.1472 (4)	0.7673 (3)	0.0133 (8)
B4	0.4912 (5)	0.2461 (4)	0.9766 (3)	0.0130 (8)
B5	0.6787 (5)	0.0482 (4)	0.9462 (3)	0.0126 (8)
B6	0.7263 (5)	0.4844 (4)	0.5928 (3)	0.0144 (8)
B7	0.9241 (5)	0.6669 (4)	0.5601 (3)	0.0145 (8)
B8	0.9041 (5)	0.6680 (4)	0.7659 (3)	0.0125 (8)
B9	0.8708 (5)	0.8327 (4)	0.9451 (3)	0.0139 (8)
B10	1.0838 (5)	0.6471 (4)	0.9752 (3)	0.0131 (8)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
K1	0.0252 (5)	0.0164 (4)	0.0155 (4)	−0.0002 (3)	0.0045 (3)	0.0032 (3)
K2	0.0245 (5)	0.0231 (4)	0.0189 (4)	0.0053 (3)	0.0034 (3)	0.0028 (3)
O1	0.0177 (14)	0.0115 (12)	0.0170 (12)	−0.0047 (10)	0.0038 (10)	0.0028 (9)
O2	0.0161 (13)	0.0119 (12)	0.0119 (11)	−0.0017 (10)	0.0038 (10)	0.0015 (9)
O3	0.0137 (13)	0.0117 (12)	0.0138 (11)	−0.0025 (10)	0.0036 (10)	0.0017 (9)
O4	0.0138 (13)	0.0139 (12)	0.0123 (12)	−0.0025 (10)	0.0025 (10)	0.0020 (9)
O5	0.0150 (13)	0.0118 (12)	0.0123 (11)	−0.0014 (10)	0.0044 (10)	0.0029 (9)
O6	0.0152 (13)	0.0134 (12)	0.0129 (12)	0.0023 (10)	0.0050 (10)	0.0031 (9)
O7	0.0124 (13)	0.0140 (12)	0.0136 (12)	0.0031 (10)	0.0040 (10)	0.0015 (9)
O8	0.0143 (13)	0.0132 (12)	0.0132 (12)	0.0028 (10)	0.0038 (10)	0.0016 (9)
O9	0.0181 (14)	0.0137 (12)	0.0169 (12)	0.0052 (10)	0.0065 (10)	0.0030 (10)
O10	0.0174 (14)	0.0122 (12)	0.0134 (12)	−0.0025 (10)	0.0065 (10)	0.0000 (9)
O11	0.0186 (14)	0.0148 (12)	0.0155 (12)	−0.0012 (10)	0.0061 (11)	0.0016 (10)
O12	0.0131 (13)	0.0116 (12)	0.0150 (12)	−0.0032 (9)	0.0045 (10)	0.0010 (9)
O13	0.0171 (14)	0.0125 (12)	0.0150 (12)	−0.0008 (10)	0.0048 (10)	0.0031 (9)
O14	0.0136 (13)	0.0116 (12)	0.0132 (12)	0.0015 (9)	0.0039 (10)	0.0014 (9)
O15	0.0136 (13)	0.0108 (12)	0.0141 (12)	0.0041 (10)	0.0028 (10)	0.0015 (9)
O16	0.0141 (13)	0.0128 (12)	0.0146 (12)	0.0021 (10)	0.0019 (10)	0.0017 (9)
O17	0.0135 (13)	0.0101 (11)	0.0126 (11)	0.0015 (9)	0.0037 (9)	0.0010 (9)
O18	0.0161 (14)	0.0143 (12)	0.0128 (12)	0.0027 (10)	0.0023 (10)	0.0013 (10)
O19	0.0255 (16)	0.0176 (13)	0.0182 (13)	0.0077 (12)	0.0048 (11)	0.0015 (10)
B1	0.012 (2)	0.0091 (18)	0.020 (2)	0.0032 (16)	0.0077 (17)	0.0047 (15)
B2	0.008 (2)	0.0087 (18)	0.018 (2)	0.0039 (15)	0.0052 (16)	−0.0012 (15)
B3	0.012 (2)	0.014 (2)	0.014 (2)	0.0037 (16)	0.0050 (16)	0.0009 (15)
B4	0.012 (2)	0.0109 (19)	0.017 (2)	−0.0034 (16)	0.0061 (16)	0.0010 (15)
B5	0.011 (2)	0.0112 (19)	0.016 (2)	−0.0019 (16)	0.0053 (16)	0.0002 (15)
B6	0.012 (2)	0.0109 (19)	0.020 (2)	0.0038 (16)	0.0038 (17)	0.0052 (16)
B7	0.010 (2)	0.0108 (19)	0.023 (2)	0.0028 (15)	0.0047 (17)	0.0036 (16)
B8	0.011 (2)	0.0099 (19)	0.016 (2)	−0.0008 (15)	0.0042 (16)	0.0014 (15)
B9	0.012 (2)	0.0108 (19)	0.020 (2)	−0.0033 (15)	0.0054 (16)	0.0030 (16)
B10	0.012 (2)	0.0094 (19)	0.017 (2)	−0.0020 (16)	0.0031 (16)	0.0034 (15)

Geometric parameters (Å, º) top

K1—O1	2.615 (2)	O8—B5	1.341 (4)
K1—O17ⁱ	2.835 (2)	O8—B3	1.469 (4)
K1—O15ⁱ	2.841 (2)	O8—K1ⁱⁱⁱ	2.990 (2)
K1—O19	2.861 (3)	O8—K2ⁱⁱⁱ	3.052 (2)
K1—O14ⁱⁱ	2.862 (2)	O9—B4	1.358 (4)
K1—O13ⁱⁱ	2.988 (2)	O9—K2^viii	2.808 (2)
K1—O8ⁱⁱⁱ	2.990 (2)	O9—H9	0.865 (18)
K1—O4^iv	3.185 (2)	O10—B6	1.383 (4)
K1—B9ⁱ	3.335 (4)	O10—B7	1.390 (4)
K1—B9ⁱⁱ	3.402 (4)	O11—B7	1.366 (4)
K1—B8ⁱⁱ	3.521 (4)	O11—H11	0.918 (18)
K1—B5ⁱⁱⁱ	3.589 (4)	O12—B6	1.342 (4)
K1—H1	2.97 (3)	O12—B8	1.472 (4)
K1—H19A	2.95 (4)	O12—K2ⁱⁱ	3.069 (2)
K2—O9^v	2.808 (2)	O13—B7	1.350 (4)
K2—O3	2.913 (2)	O13—B8	1.468 (4)
K2—O14ⁱⁱ	2.918 (2)	O13—K1ⁱⁱ	2.988 (2)
K2—O4ⁱⁱⁱ	3.033 (2)	O13—K2^vi	3.260 (2)
K2—O8ⁱⁱⁱ	3.052 (2)	O14—B9	1.340 (4)
K2—O12ⁱⁱ	3.069 (2)	O14—B8	1.469 (4)
K2—O7^v	3.205 (2)	O14—K1ⁱⁱ	2.862 (2)
K2—O13^vi	3.260 (2)	O14—K2ⁱⁱ	2.918 (2)
K2—B4^v	3.513 (4)	O15—B9	1.383 (4)
K2—B8ⁱⁱ	3.568 (4)	O15—B10	1.385 (4)
K2—K1^vii	4.5268 (12)	O15—K1^ix	2.840 (2)
O1—B1	1.358 (4)	O16—B10	1.347 (4)
O1—H1	0.881 (18)	O16—B8	1.473 (4)
O2—B1	1.380 (4)	O17—B9	1.379 (4)
O2—B2	1.389 (4)	O17—B5^x	1.392 (4)
O3—B6	1.378 (4)	O17—K1^ix	2.835 (2)
O3—B2	1.378 (4)	O18—B10	1.370 (4)
O4—B1	1.355 (4)	O18—H18	0.892 (18)
O4—B3	1.473 (4)	O19—H19A	0.90 (2)
O4—K2ⁱⁱⁱ	3.033 (2)	O19—H19B	0.91 (2)
O4—K1^iv	3.185 (2)	B4—K2^viii	3.513 (4)
O5—B2	1.346 (4)	B5—O17^xi	1.392 (4)
O5—B3	1.474 (4)	B5—K1ⁱⁱⁱ	3.589 (4)
O6—B4	1.349 (4)	B8—K1ⁱⁱ	3.521 (4)
O6—B3	1.483 (4)	B8—K2ⁱⁱ	3.567 (4)
O7—B5	1.386 (4)	B9—K1^ix	3.335 (4)
O7—B4	1.396 (4)	B9—K1ⁱⁱ	3.402 (4)
O7—K2^viii	3.205 (2)

O1—K1—O17ⁱ	174.90 (7)	B4^v—K2—B8ⁱⁱ	85.73 (9)
O1—K1—O15ⁱ	133.58 (7)	O9^v—K2—K1^vii	102.67 (5)
O17ⁱ—K1—O15ⁱ	48.29 (6)	O3—K2—K1^vii	110.21 (5)
O1—K1—O19	82.07 (7)	O14ⁱⁱ—K2—K1^vii	128.57 (5)
O17ⁱ—K1—O19	95.19 (7)	O4ⁱⁱⁱ—K2—K1^vii	44.62 (4)
O15ⁱ—K1—O19	69.42 (7)	O8ⁱⁱⁱ—K2—K1^vii	74.44 (4)
O1—K1—O14ⁱⁱ	106.78 (7)	O12ⁱⁱ—K2—K1^vii	174.44 (5)
O17ⁱ—K1—O14ⁱⁱ	76.92 (6)	O7^v—K2—K1^vii	59.57 (4)
O15ⁱ—K1—O14ⁱⁱ	95.24 (6)	O13^vi—K2—K1^vii	41.24 (4)
O19—K1—O14ⁱⁱ	163.93 (7)	B4^v—K2—K1^vii	82.73 (7)
O1—K1—O13ⁱⁱ	84.58 (7)	B8ⁱⁱ—K2—K1^vii	151.92 (6)
O17ⁱ—K1—O13ⁱⁱ	95.68 (6)	O9^v—K2—K1	95.28 (5)
O15ⁱ—K1—O13ⁱⁱ	137.05 (6)	O3—K2—K1	92.11 (5)
O19—K1—O13ⁱⁱ	148.03 (7)	O14ⁱⁱ—K2—K1	33.68 (4)
O14ⁱⁱ—K1—O13ⁱⁱ	47.83 (6)	O4ⁱⁱⁱ—K2—K1	68.36 (5)
O1—K1—O8ⁱⁱⁱ	92.13 (7)	O8ⁱⁱⁱ—K2—K1	37.13 (4)
O17ⁱ—K1—O8ⁱⁱⁱ	92.85 (6)	O12ⁱⁱ—K2—K1	69.44 (4)
O15ⁱ—K1—O8ⁱⁱⁱ	65.98 (6)	O7^v—K2—K1	98.32 (4)
O19—K1—O8ⁱⁱⁱ	109.80 (7)	O13^vi—K2—K1	148.91 (4)
O14ⁱⁱ—K1—O8ⁱⁱⁱ	57.44 (6)	B4^v—K2—K1	94.67 (6)
O13ⁱⁱ—K1—O8ⁱⁱⁱ	99.57 (6)	B8ⁱⁱ—K2—K1	47.09 (6)
O1—K1—O4^iv	85.11 (7)	K1^vii—K2—K1	108.49 (2)
O17ⁱ—K1—O4^iv	89.86 (6)	B1—O1—K1	133.0 (2)
O15ⁱ—K1—O4^iv	114.24 (6)	B1—O1—H1	118 (2)
O19—K1—O4^iv	67.25 (6)	K1—O1—H1	105 (2)
O14ⁱⁱ—K1—O4^iv	125.91 (6)	B1—O2—B2	118.7 (3)
O13ⁱⁱ—K1—O4^iv	82.81 (6)	B6—O3—B2	131.3 (3)
O8ⁱⁱⁱ—K1—O4^iv	176.19 (6)	B6—O3—K2	114.9 (2)
O1—K1—B9ⁱ	157.71 (9)	B2—O3—K2	113.08 (18)
O17ⁱ—K1—B9ⁱ	24.12 (8)	B1—O4—B3	122.0 (3)
O15ⁱ—K1—B9ⁱ	24.22 (8)	B1—O4—K2ⁱⁱⁱ	105.55 (18)
O19—K1—B9ⁱ	82.81 (8)	B3—O4—K2ⁱⁱⁱ	103.33 (17)
O14ⁱⁱ—K1—B9ⁱ	84.64 (8)	B1—O4—K1^iv	115.2 (2)
O13ⁱⁱ—K1—B9ⁱ	116.44 (8)	B3—O4—K1^iv	111.89 (18)
O8ⁱⁱⁱ—K1—B9ⁱ	77.75 (8)	K2ⁱⁱⁱ—O4—K1^iv	93.40 (6)
O4^iv—K1—B9ⁱ	103.92 (8)	B2—O5—B3	123.1 (3)
O1—K1—B9ⁱⁱ	127.37 (8)	B4—O6—B3	123.6 (3)
O17ⁱ—K1—B9ⁱⁱ	56.94 (8)	B5—O7—B4	117.8 (3)
O15ⁱ—K1—B9ⁱⁱ	73.78 (8)	B5—O7—K2^viii	150.4 (2)
O19—K1—B9ⁱⁱ	143.12 (8)	B4—O7—K2^viii	90.76 (18)
O14ⁱⁱ—K1—B9ⁱⁱ	22.67 (7)	B5—O8—B3	123.5 (3)
O13ⁱⁱ—K1—B9ⁱⁱ	65.68 (8)	B5—O8—K1ⁱⁱⁱ	105.5 (2)
O8ⁱⁱⁱ—K1—B9ⁱⁱ	54.80 (8)	B3—O8—K1ⁱⁱⁱ	113.16 (19)
O4^iv—K1—B9ⁱⁱ	129.01 (8)	B5—O8—K2ⁱⁱⁱ	105.48 (19)
B9ⁱ—K1—B9ⁱⁱ	62.00 (11)	B3—O8—K2ⁱⁱⁱ	102.58 (18)
O1—K1—B8ⁱⁱ	98.97 (8)	K1ⁱⁱⁱ—O8—K2ⁱⁱⁱ	104.84 (6)
O17ⁱ—K1—B8ⁱⁱ	83.04 (7)	B4—O9—K2^viii	110.0 (2)
O15ⁱ—K1—B8ⁱⁱ	115.06 (8)	B4—O9—H9	118 (2)
O19—K1—B8ⁱⁱ	170.63 (8)	K2^viii—O9—H9	131 (2)
O14ⁱⁱ—K1—B8ⁱⁱ	23.88 (7)	B6—O10—B7	117.7 (3)
O13ⁱⁱ—K1—B8ⁱⁱ	24.34 (7)	B7—O11—H11	118 (2)
O8ⁱⁱⁱ—K1—B8ⁱⁱ	79.52 (8)	B6—O12—B8	122.0 (3)
O4^iv—K1—B8ⁱⁱ	103.49 (7)	B6—O12—K2ⁱⁱ	107.8 (2)
B9ⁱ—K1—B8ⁱⁱ	98.62 (9)	B8—O12—K2ⁱⁱ	97.29 (18)
B9ⁱⁱ—K1—B8ⁱⁱ	41.76 (8)	B7—O13—B8	121.6 (3)
O1—K1—B5ⁱⁱⁱ	113.22 (8)	B7—O13—K1ⁱⁱ	117.81 (19)
O17ⁱ—K1—B5ⁱⁱⁱ	71.76 (7)	B8—O13—K1ⁱⁱ	98.63 (17)
O15ⁱ—K1—B5ⁱⁱⁱ	51.42 (7)	B7—O13—K2^vi	99.5 (2)
O19—K1—B5ⁱⁱⁱ	111.08 (8)	B8—O13—K2^vi	124.05 (19)
O14ⁱⁱ—K1—B5ⁱⁱⁱ	53.30 (7)	K1ⁱⁱ—O13—K2^vi	92.77 (6)
O13ⁱⁱ—K1—B5ⁱⁱⁱ	100.87 (7)	B9—O14—B8	123.0 (3)
O8ⁱⁱⁱ—K1—B5ⁱⁱⁱ	21.09 (7)	B9—O14—K1ⁱⁱ	101.92 (19)
O4^iv—K1—B5ⁱⁱⁱ	161.47 (7)	B8—O14—K1ⁱⁱ	104.07 (18)
B9ⁱ—K1—B5ⁱⁱⁱ	58.07 (9)	B9—O14—K2ⁱⁱ	111.8 (2)
B9ⁱⁱ—K1—B5ⁱⁱⁱ	41.61 (9)	B8—O14—K2ⁱⁱ	103.88 (18)
B8ⁱⁱ—K1—B5ⁱⁱⁱ	77.18 (8)	K1ⁱⁱ—O14—K2ⁱⁱ	111.90 (7)
O1—K1—H1	16.6 (4)	B9—O15—B10	118.2 (3)
O17ⁱ—K1—H1	158.9 (5)	B9—O15—K1^ix	98.35 (19)
O15ⁱ—K1—H1	128.2 (6)	B10—O15—K1^ix	142.67 (19)
O19—K1—H1	67.4 (5)	B10—O16—B8	123.4 (3)
O14ⁱⁱ—K1—H1	122.9 (5)	B9—O17—B5^x	127.9 (3)
O13ⁱⁱ—K1—H1	94.0 (6)	B9—O17—K1^ix	98.70 (19)
O8ⁱⁱⁱ—K1—H1	104.0 (6)	B5^x—O17—K1^ix	132.52 (19)
O4^iv—K1—H1	72.8 (6)	B10—O18—H18	116 (2)
B9ⁱ—K1—H1	149.0 (5)	K1—O19—H19A	87 (2)
B9ⁱⁱ—K1—H1	143.9 (5)	K1—O19—H19B	129 (2)
B8ⁱⁱ—K1—H1	112.2 (5)	H19A—O19—H19B	106 (3)
B5ⁱⁱⁱ—K1—H1	124.6 (6)	O4—B1—O1	122.8 (3)
O1—K1—H19A	94.6 (6)	O4—B1—O2	122.0 (3)
O17ⁱ—K1—H19A	81.8 (6)	O1—B1—O2	115.2 (3)
O15ⁱ—K1—H19A	68.3 (7)	O5—B2—O3	125.8 (3)
O19—K1—H19A	17.8 (5)	O5—B2—O2	121.4 (3)
O14ⁱⁱ—K1—H19A	158.6 (6)	O3—B2—O2	112.9 (3)
O13ⁱⁱ—K1—H19A	138.3 (6)	O8—B3—O4	107.8 (3)
O8ⁱⁱⁱ—K1—H19A	122.1 (6)	O8—B3—O5	109.8 (3)
O4^iv—K1—H19A	55.7 (6)	O4—B3—O5	111.9 (3)
B9ⁱ—K1—H19A	74.9 (6)	O8—B3—O6	110.3 (3)
B9ⁱⁱ—K1—H19A	136.6 (6)	O4—B3—O6	109.0 (3)
B8ⁱⁱ—K1—H19A	154.1 (5)	O5—B3—O6	108.0 (3)
B5ⁱⁱⁱ—K1—H19A	117.3 (7)	O6—B4—O9	125.4 (3)
H1—K1—H19A	78.5 (7)	O6—B4—O7	121.1 (3)
O9^v—K2—O3	141.92 (7)	O9—B4—O7	113.5 (3)
O9^v—K2—O14ⁱⁱ	65.70 (6)	O6—B4—K2^viii	167.7 (2)
O3—K2—O14ⁱⁱ	105.21 (6)	O9—B4—K2^viii	48.70 (16)
O9^v—K2—O4ⁱⁱⁱ	124.58 (6)	O7—B4—K2^viii	65.83 (16)
O3—K2—O4ⁱⁱⁱ	92.81 (6)	O8—B5—O7	122.7 (3)
O14ⁱⁱ—K2—O4ⁱⁱⁱ	98.79 (6)	O8—B5—O17^xi	122.6 (3)
O9^v—K2—O8ⁱⁱⁱ	88.70 (6)	O7—B5—O17^xi	114.7 (3)
O3—K2—O8ⁱⁱⁱ	117.87 (6)	O8—B5—K1ⁱⁱⁱ	53.38 (16)
O14ⁱⁱ—K2—O8ⁱⁱⁱ	56.20 (6)	O7—B5—K1ⁱⁱⁱ	138.7 (2)
O4ⁱⁱⁱ—K2—O8ⁱⁱⁱ	45.99 (6)	O17^xi—B5—K1ⁱⁱⁱ	83.00 (19)
O9^v—K2—O12ⁱⁱ	72.67 (6)	O12—B6—O3	123.4 (3)
O3—K2—O12ⁱⁱ	75.21 (6)	O12—B6—O10	121.7 (3)
O14ⁱⁱ—K2—O12ⁱⁱ	47.02 (6)	O3—B6—O10	114.8 (3)
O4ⁱⁱⁱ—K2—O12ⁱⁱ	135.50 (6)	O13—B7—O11	118.4 (3)
O8ⁱⁱⁱ—K2—O12ⁱⁱ	102.11 (6)	O13—B7—O10	122.2 (3)
O9^v—K2—O7^v	44.43 (6)	O11—B7—O10	119.4 (3)
O3—K2—O7^v	167.31 (6)	O13—B8—O14	107.9 (3)
O14ⁱⁱ—K2—O7^v	87.46 (6)	O13—B8—O12	112.3 (3)
O4ⁱⁱⁱ—K2—O7^v	84.39 (6)	O14—B8—O12	108.8 (3)
O8ⁱⁱⁱ—K2—O7^v	68.47 (6)	O13—B8—O16	109.0 (3)
O12ⁱⁱ—K2—O7^v	115.24 (6)	O14—B8—O16	111.0 (3)
O9^v—K2—O13^vi	98.63 (7)	O12—B8—O16	107.9 (3)
O3—K2—O13^vi	93.83 (6)	O13—B8—K1ⁱⁱ	57.03 (15)
O14ⁱⁱ—K2—O13^vi	160.94 (6)	O14—B8—K1ⁱⁱ	52.05 (14)
O4ⁱⁱⁱ—K2—O13^vi	80.88 (6)	O12—B8—K1ⁱⁱ	136.1 (2)
O8ⁱⁱⁱ—K2—O13^vi	115.44 (6)	O16—B8—K1ⁱⁱ	115.82 (19)
O12ⁱⁱ—K2—O13^vi	141.42 (6)	O13—B8—K2ⁱⁱ	112.4 (2)
O7^v—K2—O13^vi	73.52 (6)	O14—B8—K2ⁱⁱ	52.56 (15)
O9^v—K2—B4^v	21.30 (7)	O12—B8—K2ⁱⁱ	58.56 (15)
O3—K2—B4^v	162.61 (8)	O16—B8—K2ⁱⁱ	138.4 (2)
O14ⁱⁱ—K2—B4^v	72.97 (8)	K1ⁱⁱ—B8—K2ⁱⁱ	85.00 (8)
O4ⁱⁱⁱ—K2—B4^v	104.57 (7)	O14—B9—O17	123.1 (3)
O8ⁱⁱⁱ—K2—B4^v	76.05 (7)	O14—B9—O15	122.4 (3)
O12ⁱⁱ—K2—B4^v	92.23 (8)	O17—B9—O15	114.4 (3)
O7^v—K2—B4^v	23.41 (7)	O14—B9—K1^ix	172.8 (2)
O13^vi—K2—B4^v	88.60 (8)	O17—B9—K1^ix	57.17 (16)
O9^v—K2—B8ⁱⁱ	71.35 (8)	O15—B9—K1^ix	57.43 (16)
O3—K2—B8ⁱⁱ	87.22 (7)	O14—B9—K1ⁱⁱ	55.40 (16)
O14ⁱⁱ—K2—B8ⁱⁱ	23.57 (7)	O17—B9—K1ⁱⁱ	90.79 (19)
O4ⁱⁱⁱ—K2—B8ⁱⁱ	115.36 (8)	O15—B9—K1ⁱⁱ	123.9 (2)
O8ⁱⁱⁱ—K2—B8ⁱⁱ	77.97 (7)	K1^ix—B9—K1ⁱⁱ	118.00 (11)
O12ⁱⁱ—K2—B8ⁱⁱ	24.15 (7)	O16—B10—O18	118.4 (3)
O7^v—K2—B8ⁱⁱ	105.18 (7)	O16—B10—O15	121.5 (3)
O13^vi—K2—B8ⁱⁱ	163.68 (7)	O18—B10—O15	120.0 (3)

O1—K1—K2—O9^v	−171.23 (7)	B8ⁱⁱ—K2—O3—B2	75.7 (2)
O17ⁱ—K1—K2—O9^v	6.68 (7)	K1^vii—K2—O3—B2	−81.7 (2)
O15ⁱ—K1—K2—O9^v	56.06 (7)	K1—K2—O3—B2	28.9 (2)
O19—K1—K2—O9^v	126.23 (9)	B3—O4—B1—O1	168.5 (3)
O14ⁱⁱ—K1—K2—O9^v	−27.88 (9)	K2ⁱⁱⁱ—O4—B1—O1	51.4 (4)
O13ⁱⁱ—K1—K2—O9^v	−81.77 (7)	K1^iv—O4—B1—O1	−50.1 (4)
O8ⁱⁱⁱ—K1—K2—O9^v	80.80 (8)	B3—O4—B1—O2	−10.9 (5)
O4^iv—K1—K2—O9^v	−105.08 (9)	K2ⁱⁱⁱ—O4—B1—O2	−128.0 (3)
B9ⁱ—K1—K2—O9^v	31.46 (8)	K1^iv—O4—B1—O2	130.5 (3)
B9ⁱⁱ—K1—K2—O9^v	−1.60 (10)	K1—O1—B1—O4	157.5 (2)
B8ⁱⁱ—K1—K2—O9^v	−58.36 (9)	K1—O1—B1—O2	−23.0 (4)
B5ⁱⁱⁱ—K1—K2—O9^v	54.42 (9)	B2—O2—B1—O4	4.9 (5)
O1—K1—K2—O3	−28.62 (7)	B2—O2—B1—O1	−174.6 (3)
O17ⁱ—K1—K2—O3	149.28 (6)	B3—O5—B2—O3	173.0 (3)
O15ⁱ—K1—K2—O3	−161.33 (6)	B3—O5—B2—O2	−6.7 (5)
O19—K1—K2—O3	−91.17 (9)	B6—O3—B2—O5	−12.3 (6)
O14ⁱⁱ—K1—K2—O3	114.72 (9)	K2—O3—B2—O5	156.9 (3)
O13ⁱⁱ—K1—K2—O3	60.83 (6)	B6—O3—B2—O2	167.4 (3)
O8ⁱⁱⁱ—K1—K2—O3	−136.60 (8)	K2—O3—B2—O2	−23.3 (3)
O4^iv—K1—K2—O3	37.52 (9)	B1—O2—B2—O5	3.9 (4)
B9ⁱ—K1—K2—O3	174.06 (8)	B1—O2—B2—O3	−175.8 (3)
B9ⁱⁱ—K1—K2—O3	141.00 (10)	B5—O8—B3—O4	−123.3 (3)
B8ⁱⁱ—K1—K2—O3	84.24 (9)	K1ⁱⁱⁱ—O8—B3—O4	107.5 (2)
B5ⁱⁱⁱ—K1—K2—O3	−162.98 (9)	K2ⁱⁱⁱ—O8—B3—O4	−4.9 (3)
O1—K1—K2—O14ⁱⁱ	−143.35 (9)	B5—O8—B3—O5	114.5 (3)
O17ⁱ—K1—K2—O14ⁱⁱ	34.55 (9)	K1ⁱⁱⁱ—O8—B3—O5	−14.7 (3)
O15ⁱ—K1—K2—O14ⁱⁱ	83.94 (9)	K2ⁱⁱⁱ—O8—B3—O5	−127.1 (2)
O19—K1—K2—O14ⁱⁱ	154.10 (11)	B5—O8—B3—O6	−4.4 (4)
O13ⁱⁱ—K1—K2—O14ⁱⁱ	−53.89 (9)	K1ⁱⁱⁱ—O8—B3—O6	−133.6 (2)
O8ⁱⁱⁱ—K1—K2—O14ⁱⁱ	108.68 (10)	K2ⁱⁱⁱ—O8—B3—O6	114.0 (2)
O4^iv—K1—K2—O14ⁱⁱ	−77.20 (10)	B1—O4—B3—O8	−113.3 (3)
B9ⁱ—K1—K2—O14ⁱⁱ	59.34 (10)	K2ⁱⁱⁱ—O4—B3—O8	5.0 (3)
B9ⁱⁱ—K1—K2—O14ⁱⁱ	26.28 (11)	K1^iv—O4—B3—O8	104.2 (2)
B8ⁱⁱ—K1—K2—O14ⁱⁱ	−30.49 (10)	B1—O4—B3—O5	7.6 (4)
B5ⁱⁱⁱ—K1—K2—O14ⁱⁱ	82.30 (11)	K2ⁱⁱⁱ—O4—B3—O5	125.8 (2)
O1—K1—K2—O4ⁱⁱⁱ	63.57 (7)	K1^iv—O4—B3—O5	−134.9 (2)
O17ⁱ—K1—K2—O4ⁱⁱⁱ	−118.53 (6)	B1—O4—B3—O6	126.9 (3)
O15ⁱ—K1—K2—O4ⁱⁱⁱ	−69.14 (6)	K2ⁱⁱⁱ—O4—B3—O6	−114.8 (2)
O19—K1—K2—O4ⁱⁱⁱ	1.02 (9)	K1^iv—O4—B3—O6	−15.6 (3)
O14ⁱⁱ—K1—K2—O4ⁱⁱⁱ	−153.08 (9)	B2—O5—B3—O8	120.7 (3)
O13ⁱⁱ—K1—K2—O4ⁱⁱⁱ	153.02 (6)	B2—O5—B3—O4	1.0 (4)
O8ⁱⁱⁱ—K1—K2—O4ⁱⁱⁱ	−44.41 (8)	B2—O5—B3—O6	−118.9 (3)
O4^iv—K1—K2—O4ⁱⁱⁱ	129.71 (10)	B4—O6—B3—O8	11.5 (4)
B9ⁱ—K1—K2—O4ⁱⁱⁱ	−93.75 (8)	B4—O6—B3—O4	129.8 (3)
B9ⁱⁱ—K1—K2—O4ⁱⁱⁱ	−126.81 (10)	B4—O6—B3—O5	−108.5 (3)
B8ⁱⁱ—K1—K2—O4ⁱⁱⁱ	176.43 (9)	B3—O6—B4—O9	169.7 (3)
B5ⁱⁱⁱ—K1—K2—O4ⁱⁱⁱ	−70.79 (9)	B3—O6—B4—O7	−11.6 (5)
O1—K1—K2—O8ⁱⁱⁱ	107.97 (9)	B3—O6—B4—K2^viii	−132.9 (10)
O17ⁱ—K1—K2—O8ⁱⁱⁱ	−74.12 (8)	K2^viii—O9—B4—O6	166.1 (3)
O15ⁱ—K1—K2—O8ⁱⁱⁱ	−24.74 (8)	K2^viii—O9—B4—O7	−12.7 (3)
O19—K1—K2—O8ⁱⁱⁱ	45.42 (10)	B5—O7—B4—O6	3.3 (5)
O14ⁱⁱ—K1—K2—O8ⁱⁱⁱ	−108.68 (10)	K2^viii—O7—B4—O6	−168.5 (3)
O13ⁱⁱ—K1—K2—O8ⁱⁱⁱ	−162.57 (8)	B5—O7—B4—O9	−177.9 (3)
O4^iv—K1—K2—O8ⁱⁱⁱ	174.12 (10)	K2^viii—O7—B4—O9	10.4 (3)
B9ⁱ—K1—K2—O8ⁱⁱⁱ	−49.34 (9)	B5—O7—B4—K2^viii	171.7 (3)
B9ⁱⁱ—K1—K2—O8ⁱⁱⁱ	−82.40 (11)	B3—O8—B5—O7	−2.9 (5)
B8ⁱⁱ—K1—K2—O8ⁱⁱⁱ	−139.17 (10)	K1ⁱⁱⁱ—O8—B5—O7	129.4 (3)
B5ⁱⁱⁱ—K1—K2—O8ⁱⁱⁱ	−26.38 (10)	K2ⁱⁱⁱ—O8—B5—O7	−119.9 (3)
O1—K1—K2—O12ⁱⁱ	−101.97 (7)	B3—O8—B5—O17^xi	178.6 (3)
O17ⁱ—K1—K2—O12ⁱⁱ	75.94 (6)	K1ⁱⁱⁱ—O8—B5—O17^xi	−49.1 (4)
O15ⁱ—K1—K2—O12ⁱⁱ	125.32 (6)	K2ⁱⁱⁱ—O8—B5—O17^xi	61.6 (3)
O19—K1—K2—O12ⁱⁱ	−164.51 (9)	B3—O8—B5—K1ⁱⁱⁱ	−132.3 (3)
O14ⁱⁱ—K1—K2—O12ⁱⁱ	41.38 (8)	K2ⁱⁱⁱ—O8—B5—K1ⁱⁱⁱ	110.65 (13)
O13ⁱⁱ—K1—K2—O12ⁱⁱ	−12.51 (6)	B4—O7—B5—O8	3.9 (5)
O8ⁱⁱⁱ—K1—K2—O12ⁱⁱ	150.06 (8)	K2^viii—O7—B5—O8	166.9 (2)
O4^iv—K1—K2—O12ⁱⁱ	−35.82 (8)	B4—O7—B5—O17^xi	−177.5 (3)
B9ⁱ—K1—K2—O12ⁱⁱ	100.72 (8)	K2^viii—O7—B5—O17^xi	−14.5 (6)
B9ⁱⁱ—K1—K2—O12ⁱⁱ	67.66 (9)	B4—O7—B5—K1ⁱⁱⁱ	73.8 (4)
B8ⁱⁱ—K1—K2—O12ⁱⁱ	10.89 (9)	K2^viii—O7—B5—K1ⁱⁱⁱ	−123.2 (3)
B5ⁱⁱⁱ—K1—K2—O12ⁱⁱ	123.68 (9)	B8—O12—B6—O3	165.6 (3)
O1—K1—K2—O7^v	144.12 (7)	K2ⁱⁱ—O12—B6—O3	−83.5 (3)
O17ⁱ—K1—K2—O7^v	−37.98 (6)	B8—O12—B6—O10	−17.2 (5)
O15ⁱ—K1—K2—O7^v	11.41 (6)	K2ⁱⁱ—O12—B6—O10	93.8 (3)
O19—K1—K2—O7^v	81.57 (9)	B2—O3—B6—O12	−15.1 (6)
O14ⁱⁱ—K1—K2—O7^v	−72.53 (8)	K2—O3—B6—O12	175.8 (2)
O13ⁱⁱ—K1—K2—O7^v	−126.43 (6)	B2—O3—B6—O10	167.5 (3)
O8ⁱⁱⁱ—K1—K2—O7^v	36.14 (8)	K2—O3—B6—O10	−1.6 (4)
O4^iv—K1—K2—O7^v	−149.74 (8)	B7—O10—B6—O12	6.3 (5)
B9ⁱ—K1—K2—O7^v	−13.20 (8)	B7—O10—B6—O3	−176.2 (3)
B9ⁱⁱ—K1—K2—O7^v	−46.26 (9)	B8—O13—B7—O11	169.1 (3)
B8ⁱⁱ—K1—K2—O7^v	−103.02 (9)	K1ⁱⁱ—O13—B7—O11	47.5 (4)
B5ⁱⁱⁱ—K1—K2—O7^v	9.76 (9)	K2^vi—O13—B7—O11	−50.7 (3)
O1—K1—K2—O13^vi	72.35 (10)	B8—O13—B7—O10	−11.6 (5)
O17ⁱ—K1—K2—O13^vi	−109.75 (9)	K1ⁱⁱ—O13—B7—O10	−133.2 (3)
O15ⁱ—K1—K2—O13^vi	−60.36 (9)	K2^vi—O13—B7—O10	128.6 (3)
O19—K1—K2—O13^vi	9.80 (12)	B6—O10—B7—O13	8.2 (5)
O14ⁱⁱ—K1—K2—O13^vi	−144.30 (11)	B6—O10—B7—O11	−172.5 (3)
O13ⁱⁱ—K1—K2—O13^vi	161.81 (12)	B7—O13—B8—O14	−118.7 (3)
O8ⁱⁱⁱ—K1—K2—O13^vi	−35.62 (10)	K1ⁱⁱ—O13—B8—O14	11.6 (3)
O4^iv—K1—K2—O13^vi	138.49 (10)	K2^vi—O13—B8—O14	110.9 (2)
B9ⁱ—K1—K2—O13^vi	−84.97 (11)	B7—O13—B8—O12	1.2 (4)
B9ⁱⁱ—K1—K2—O13^vi	−118.03 (12)	K1ⁱⁱ—O13—B8—O12	131.5 (2)
B8ⁱⁱ—K1—K2—O13^vi	−174.79 (12)	K2^vi—O13—B8—O12	−129.2 (2)
B5ⁱⁱⁱ—K1—K2—O13^vi	−62.00 (11)	B7—O13—B8—O16	120.7 (3)
O1—K1—K2—B4^v	167.40 (8)	K1ⁱⁱ—O13—B8—O16	−109.0 (2)
O17ⁱ—K1—K2—B4^v	−14.70 (8)	K2^vi—O13—B8—O16	−9.7 (3)
O15ⁱ—K1—K2—B4^v	34.69 (8)	B7—O13—B8—K1ⁱⁱ	−130.3 (3)
O19—K1—K2—B4^v	104.85 (10)	K2^vi—O13—B8—K1ⁱⁱ	99.29 (16)
O14ⁱⁱ—K1—K2—B4^v	−49.25 (10)	B7—O13—B8—K2ⁱⁱ	−62.6 (3)
O13ⁱⁱ—K1—K2—B4^v	−103.14 (8)	K1ⁱⁱ—O13—B8—K2ⁱⁱ	67.70 (15)
O8ⁱⁱⁱ—K1—K2—B4^v	59.43 (9)	K2^vi—O13—B8—K2ⁱⁱ	166.99 (8)
O4^iv—K1—K2—B4^v	−126.46 (9)	B9—O14—B8—O13	−127.0 (3)
B9ⁱ—K1—K2—B4^v	10.08 (9)	K1ⁱⁱ—O14—B8—O13	−12.4 (3)
B9ⁱⁱ—K1—K2—B4^v	−22.97 (11)	K2ⁱⁱ—O14—B8—O13	104.9 (2)
B8ⁱⁱ—K1—K2—B4^v	−79.74 (10)	B9—O14—B8—O12	110.9 (3)
B5ⁱⁱⁱ—K1—K2—B4^v	33.05 (10)	K1ⁱⁱ—O14—B8—O12	−134.4 (2)
O1—K1—K2—B8ⁱⁱ	−112.86 (10)	K2ⁱⁱ—O14—B8—O12	−17.1 (3)
O17ⁱ—K1—K2—B8ⁱⁱ	65.04 (9)	B9—O14—B8—O16	−7.6 (4)
O15ⁱ—K1—K2—B8ⁱⁱ	114.43 (9)	K1ⁱⁱ—O14—B8—O16	107.0 (2)
O19—K1—K2—B8ⁱⁱ	−175.41 (11)	K2ⁱⁱ—O14—B8—O16	−135.7 (2)
O14ⁱⁱ—K1—K2—B8ⁱⁱ	30.49 (10)	B9—O14—B8—K1ⁱⁱ	−114.6 (3)
O13ⁱⁱ—K1—K2—B8ⁱⁱ	−23.40 (9)	K2ⁱⁱ—O14—B8—K1ⁱⁱ	117.26 (12)
O8ⁱⁱⁱ—K1—K2—B8ⁱⁱ	139.17 (10)	B9—O14—B8—K2ⁱⁱ	128.1 (3)
O4^iv—K1—K2—B8ⁱⁱ	−46.71 (11)	K1ⁱⁱ—O14—B8—K2ⁱⁱ	−117.26 (12)
B9ⁱ—K1—K2—B8ⁱⁱ	89.82 (11)	B6—O12—B8—O13	12.9 (4)
B9ⁱⁱ—K1—K2—B8ⁱⁱ	56.77 (11)	K2ⁱⁱ—O12—B8—O13	−103.4 (2)
B5ⁱⁱⁱ—K1—K2—B8ⁱⁱ	112.79 (11)	B6—O12—B8—O14	132.3 (3)
O1—K1—K2—K1^vii	83.51 (6)	K2ⁱⁱ—O12—B8—O14	15.9 (2)
O17ⁱ—K1—K2—K1^vii	−98.58 (5)	B6—O12—B8—O16	−107.2 (3)
O15ⁱ—K1—K2—K1^vii	−49.20 (5)	K2ⁱⁱ—O12—B8—O16	136.4 (2)
O19—K1—K2—K1^vii	20.96 (9)	B6—O12—B8—K1ⁱⁱ	77.9 (4)
O14ⁱⁱ—K1—K2—K1^vii	−133.14 (8)	K2ⁱⁱ—O12—B8—K1ⁱⁱ	−38.4 (3)
O13ⁱⁱ—K1—K2—K1^vii	172.97 (5)	B6—O12—B8—K2ⁱⁱ	116.4 (3)
O8ⁱⁱⁱ—K1—K2—K1^vii	−24.46 (7)	B10—O16—B8—O13	127.4 (3)
O4^iv—K1—K2—K1^vii	149.66 (7)	B10—O16—B8—O14	8.7 (4)
B9ⁱ—K1—K2—K1^vii	−73.80 (7)	B10—O16—B8—O12	−110.5 (3)
B9ⁱⁱ—K1—K2—K1^vii	−106.86 (9)	B10—O16—B8—K1ⁱⁱ	65.6 (3)
B8ⁱⁱ—K1—K2—K1^vii	−163.63 (8)	B10—O16—B8—K2ⁱⁱ	−48.0 (4)
B5ⁱⁱⁱ—K1—K2—K1^vii	−50.84 (8)	B8—O14—B9—O17	−179.7 (3)
O17ⁱ—K1—O1—B1	−125.6 (7)	K1ⁱⁱ—O14—B9—O17	64.6 (3)
O15ⁱ—K1—O1—B1	125.2 (3)	K2ⁱⁱ—O14—B9—O17	−55.1 (4)
O19—K1—O1—B1	176.7 (3)	B8—O14—B9—O15	4.2 (5)
O14ⁱⁱ—K1—O1—B1	10.5 (3)	K1ⁱⁱ—O14—B9—O15	−111.5 (3)
O13ⁱⁱ—K1—O1—B1	−32.4 (3)	K2ⁱⁱ—O14—B9—O15	128.9 (3)
O8ⁱⁱⁱ—K1—O1—B1	67.0 (3)	B8—O14—B9—K1^ix	90.4 (19)
O4^iv—K1—O1—B1	−115.6 (3)	K1ⁱⁱ—O14—B9—K1^ix	−25 (2)
B9ⁱ—K1—O1—B1	129.0 (3)	K2ⁱⁱ—O14—B9—K1^ix	−145.0 (19)
B9ⁱⁱ—K1—O1—B1	21.2 (3)	B8—O14—B9—K1ⁱⁱ	115.7 (3)
B8ⁱⁱ—K1—O1—B1	−12.7 (3)	K2ⁱⁱ—O14—B9—K1ⁱⁱ	−119.68 (15)
B5ⁱⁱⁱ—K1—O1—B1	67.1 (3)	B5^x—O17—B9—O14	−1.0 (5)
O9^v—K2—O3—B6	−58.7 (2)	K1^ix—O17—B9—O14	−171.4 (3)
O14ⁱⁱ—K2—O3—B6	−128.5 (2)	B5^x—O17—B9—O15	175.3 (3)
O4ⁱⁱⁱ—K2—O3—B6	131.6 (2)	K1^ix—O17—B9—O15	4.9 (3)
O8ⁱⁱⁱ—K2—O3—B6	172.0 (2)	B5^x—O17—B9—K1^ix	170.3 (3)
O12ⁱⁱ—K2—O3—B6	−91.9 (2)	B5^x—O17—B9—K1ⁱⁱ	47.0 (3)
O7^v—K2—O3—B6	54.7 (4)	K1^ix—O17—B9—K1ⁱⁱ	−123.35 (8)
O13^vi—K2—O3—B6	50.5 (2)	B10—O15—B9—O14	−0.8 (5)
B4^v—K2—O3—B6	−47.0 (4)	K1^ix—O15—B9—O14	171.4 (3)
B8ⁱⁱ—K2—O3—B6	−113.1 (2)	B10—O15—B9—O17	−177.1 (3)
K1^vii—K2—O3—B6	89.4 (2)	K1^ix—O15—B9—O17	−4.9 (3)
K1—K2—O3—B6	−160.0 (2)	B10—O15—B9—K1^ix	−172.2 (3)
O9^v—K2—O3—B2	130.2 (2)	B10—O15—B9—K1ⁱⁱ	−68.3 (3)
O14ⁱⁱ—K2—O3—B2	60.3 (2)	K1^ix—O15—B9—K1ⁱⁱ	103.98 (19)
O4ⁱⁱⁱ—K2—O3—B2	−39.5 (2)	B8—O16—B10—O18	175.3 (3)
O8ⁱⁱⁱ—K2—O3—B2	0.9 (2)	B8—O16—B10—O15	−6.3 (5)
O12ⁱⁱ—K2—O3—B2	97.0 (2)	B9—O15—B10—O16	1.8 (5)
O7^v—K2—O3—B2	−116.4 (3)	K1^ix—O15—B10—O16	−165.4 (2)
O13^vi—K2—O3—B2	−120.6 (2)	B9—O15—B10—O18	−179.8 (3)
B4^v—K2—O3—B2	141.9 (3)	K1^ix—O15—B10—O18	13.0 (5)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1···O11^xii	0.88 (2)	1.76 (2)	2.599 (3)	159 (3)
O9—H9···O18^xiii	0.87 (2)	1.98 (2)	2.797 (3)	157 (3)
O11—H11···O19^xiv	0.92 (2)	1.65 (2)	2.553 (3)	167 (3)
O18—H18···O5^xv	0.89 (2)	2.10 (2)	2.940 (3)	157 (3)
O18—H18···O12^xv	0.89 (2)	2.66 (3)	3.193 (3)	119 (3)
O19—H19A···O6^iv	0.90 (2)	1.79 (3)	2.678 (3)	169 (3)
O19—H19B···O16ⁱⁱⁱ	0.91 (2)	1.79 (3)	2.696 (3)	173 (3)

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

Experimental details

Crystal data
Chemical formula	H₆B₁₀K₂O₁₉
M_r	496.35
Crystal system, space group	Triclinic, P1
Temperature (K)	100
a, b, c (Å)	7.5612 (7), 9.2236 (10), 11.7298 (13)
α, β, γ (°)	99.038 (6), 106.595 (6), 91.314 (6)
V (Å³)	772.26 (14)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	0.72
Crystal size (mm)	0.16 × 0.08 × 0.05

Data collection
Diffractometer	Bruker APEXII
Absorption correction	Numerical (SADABS, Sheldrick, 2008a)
T_min, T_max	0.895, 0.962
No. of measured, independent and observed [I > 2σ(I)] reflections	11219, 3148, 2141
R_int	0.055
(sin θ/λ)_max (Å⁻¹)	0.628

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.045, 0.113, 1.00
No. of reflections	3148
No. of parameters	298
No. of restraints	5
H-atom treatment	All H-atom parameters refined
Δρ_max, Δρ_min (e Å⁻³)	0.42, −0.46

Computer programs: APEX2 (Bruker, 2009), SAINT (Bruker, 2009), SHELXS97 (Sheldrick, 2008b), SHELXL97 (Sheldrick, 2008b), SHELXTL (Sheldrick, 2008b).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1···O11ⁱ	0.881 (18)	1.76 (2)	2.599 (3)	159 (3)
O9—H9···O18ⁱⁱ	0.865 (18)	1.98 (2)	2.797 (3)	157 (3)
O11—H11···O19ⁱⁱⁱ	0.918 (18)	1.651 (19)	2.553 (3)	167 (3)
O18—H18···O5^iv	0.892 (18)	2.10 (2)	2.940 (3)	157 (3)
O18—H18···O12^iv	0.892 (18)	2.66 (3)	3.193 (3)	119 (3)
O19—H19A···O6^v	0.90 (2)	1.79 (3)	2.678 (3)	169 (3)
O19—H19B···O16^vi	0.91 (2)	1.79 (3)	2.696 (3)	173 (3)

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

Acknowledgements

This project was supported by the National Natural Science Foundation of China (No. 20871078).

References

Bruker (2009). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Dewey, C. F., Cook, W. R., Hodgson, R. T. & Wynne, J. J. (1975). Appl. Phys. Lett. 26, 714–716. CrossRef CAS Web of Science Google Scholar
Li, L.-Y., Li, G.-B., Xiong, M., Wang, Y.-X. & Lin, J.-H. (2003). Acta Cryst. C59, i115–i116. Web of Science CrossRef CAS IUCr Journals Google Scholar
Li, H. J., Liu, Z. H. & Sun, L. M. (2007). Chin. J. Chem. . 25, 1131–1134. Web of Science CSD CrossRef CAS Google Scholar
Marezio, M. (1969). Acta Cryst. B25, 1787–1795. CrossRef CAS IUCr Journals Web of Science Google Scholar
Marezio, M., Plettinger, H. A. & Zachariasen, W. H. (1963). Acta Cryst. 16, 975–980. CrossRef CAS IUCr Journals Web of Science Google Scholar
Mori, Y., Kuroda, I., Nakajima, S., Sasaki, T. & Nakai, S. (1995). Jpn J. Appl. Phys. 34, 296–298. CrossRef Web of Science Google Scholar
Salentine, C. G. (1987). Inorg. Chem. 26, 128–132. CrossRef CAS Web of Science Google Scholar
Sheldrick, G. M. (2008a). SADABS. University of Göttingen, Germany. Google Scholar
Sheldrick, G. M. (2008b). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Touboul, M., Penin, N. & Nowogrocki, G. (2003). Solid State Sci. 5, 1327–1342. Web of Science CrossRef CAS Google Scholar
Wang, G. M., Sun, Y. Q., Zheng, S. T. & Yang, G. Y. (2006). Z. Anorg. Allg. Chem. 632, 1586–1590. Web of Science CrossRef CAS Google Scholar
Zhang, H. X., Zhang, J., Zheng, S. T. & Yang, G. Y. (2005). Cryst. Growth Des. 5, 157–161. Web of Science CSD CrossRef CAS Google Scholar