Potassium zinc borate, KZnB3O6

Wu, Y.; Yao, J.-Y.; Zhang, J.-X.; Fu, P.-Z.; Wu, Y.-C.

doi:10.1107/S1600536810015175

Potassium zinc borate, KZnB₃O₆

Y. Wu, J.-Y. Yao, J.-X. Zhang, P.-Z. Fu and Y.-C. Wu

The title compound, KZnB₃O₆ contains a remarkable [B₆O₁₂]^6- group ( $\overline{1}$ symmetry) formed by two rings linked by edge-sharing BO₄ tetrahedra, a feature that has only been observed previously under high pressure conditions. These borate groups are connected through distorted ZnO₄ tetrahedra in edge-shared pairs ( $\overline{1}$ symmetry), forming a three-dimensional network whose cavities are filled by K⁺ cations.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536810015175/mg2092sup1.cif Contains datablocks I, global
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536810015175/mg2092Isup2.hkl Contains datablock I

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Key indicators

Single-crystal X-ray study
T = 93 K
Mean (O-B) = 0.003 Å
R factor = 0.020
wR factor = 0.050
Data-to-parameter ratio = 12.2

checkCIF/PLATON results

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Alert level C
PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.600          6
PLAT913_ALERT_3_C Missing # of Very Strong Reflections in FCF ....          1
PLAT912_ALERT_4_C Missing # of FCF Reflections Above STh/L=  0.600          7

Alert level G
PLAT154_ALERT_1_G The su's on the Cell Angles are Equal  (x 10000)       3000 Deg.

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   3 ALERT level C = Check and explain
   1 ALERT level G = General alerts; check

   1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   0 ALERT type 2 Indicator that the structure model may be wrong or deficient
   2 ALERT type 3 Indicator that the structure quality may be low
   1 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

Comment top

In efforts to identify new borates as optical materials or catalysts, investigations have been carried out in the K₂O–ZnO–B₂O₃ system, where only one quaternary compound so far, KZn₄B₃O₉, has been structurally characterized (Smith et al., 1992; Chen et al., 2005). Here, we report a new compound, KZnB₃O₆, with an unusual anion group. It is the first example of a borate prepared at ambient conditions that contains edge-sharing BO₄ tetrahedra, a feature that has only been previously found in high-pressure phases (Huppertz & von der Eltz, 2002; Huppertz, 2003; Huppertz & Emme, 2004; Emme & Huppertz, 2003, 2004, 2005; Knyrim et al., 2007).

The structure consists of BO₃ triangles, BO₄ tetrahedra, and ZnO₄ tetrahedra linked to form a three-dimensional framework whose cavities are filled with K⁺ cations in nine-coordinate environments (Fig. 1). The fundamental building block is a [B₆O₁₂]^6- anion in which two six-membered rings formed by borate polyhedra are connected through a shared edge between two BO₄ tetrahedra (Fig. 2). Within the resulting B₂O₂ ring, the transannular B–B distance [2.080 (5) Å] is similar to those in HP-NiB₂O₄ [2.088 (2) Å] and Dy₄B₆O₁₅ [2.072 (8) Å] (Knyrim et al., 2007; Huppertz & von der Eltz, 2002). The Raman spectrum of KZnB₃O₆ shows bands at 1319 and 1456 cm^-1, which lie in the range (about 1200 to 1450 cm^-1) expected for the Raman-active modes of edge-sharing BO₄ tetrahedra (Knyrim et al., 2007). Two distorted ZnO₄ tetrahedra also share a common edge, similar to the case of Zn₃B₂O₆ (Chen et al., 2005).

Related literature top

For an independent determination of the title compound, see: Chen et al. (2010). For related structures, see: Chen et al. (2005); Emme & Huppertz (2003, 2004, 2005); Huppertz (2003); Huppertz & Emme (2004); Huppertz & von der Eltz (2002); Knyrim et al. (2007); Smith et al. (1992).

Experimental top

A mixture of 7 mmol K₂CO₃, 10 mmol ZnO, and 43 mmol H₃BO₃ (all from Beijing Chemical Reagents Company) was heated to 1173 K in a platinum crucible. The transparent melt was cooled slowly from 1173 K to 1053 K at 1 K h^-1. Upon further cooling to room temperature, column-shaped colorless crystals were obtained.

Structure description top

Computing details top

Data collection: CrystalClear (Rigaku, 2008); cell refinement: CrystalClear (Rigaku, 2008); data reduction: CrystalClear (Rigaku, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ATOMS (Dowty, 1998); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top

	Fig. 1. KZnB₃O₆ viewed along b axis showing ZnO₄ tetrahedra (magenta) linked by BO₃ triangles and BO₄ tetrahedra, with K⁺ cations (blue) located within the three-dimensional framework.
	Fig. 2. [B₆O₁₂]^6- anion, with displacement ellipsoids drawn at the 50% probability level. [Symmetry code: (i) -x, -y, -z.]

potassium zinc triborate top

Crystal data top

KZnB₃O₆	Z = 2
M_r = 232.90	F(000) = 224
Triclinic, P1	D_x = 2.871 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 6.7139 (13) Å	Cell parameters from 1009 reflections
b = 6.9301 (14) Å	θ = 3.3–27.5°
c = 7.0632 (14) Å	µ = 5.29 mm⁻¹
α = 63.12 (3)°	T = 93 K
β = 72.02 (3)°	Prism, colorless
γ = 68.99 (3)°	0.50 × 0.30 × 0.20 mm
V = 269.37 (12) Å³

Data collection top

Rigaku Saturn 724+ diffractometer	1223 independent reflections
Radiation source: fine-focus sealed tube	1118 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.023
ω scans	θ_max = 27.5°, θ_min = 3.3°
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	h = −7→8
T_min = 0.480, T_max = 1.000	k = −8→9
2707 measured reflections	l = −9→8

Refinement top

Refinement on F²	0 restraints
Least-squares matrix: full	Primary atom site location: structure-invariant direct methods
R[F² > 2σ(F²)] = 0.020	Secondary atom site location: difference Fourier map
wR(F²) = 0.050	w = 1/[σ²(F_o²) + (0.030P)²] where P = (F_o² + 2F_c²)/3
S = 0.94	(Δ/σ)_max = 0.001
1223 reflections	Δρ_max = 0.38 e Å⁻³
100 parameters	Δρ_min = −0.58 e Å⁻³

Crystal data top

KZnB₃O₆	γ = 68.99 (3)°
M_r = 232.90	V = 269.37 (12) Å³
Triclinic, P1	Z = 2
a = 6.7139 (13) Å	Mo Kα radiation
b = 6.9301 (14) Å	µ = 5.29 mm⁻¹
c = 7.0632 (14) Å	T = 93 K
α = 63.12 (3)°	0.50 × 0.30 × 0.20 mm
β = 72.02 (3)°

Data collection top

Rigaku Saturn 724+ diffractometer	1223 independent reflections
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	1118 reflections with I > 2σ(I)
T_min = 0.480, T_max = 1.000	R_int = 0.023
2707 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.020	100 parameters
wR(F²) = 0.050	0 restraints
S = 0.94	Δρ_max = 0.38 e Å⁻³
1223 reflections	Δρ_min = −0.58 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. 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.

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

	x	y	z	U_iso*/U_eq
K	0.25708 (8)	0.29494 (8)	0.57923 (7)	0.00606 (12)
Zn	0.67490 (4)	0.35335 (4)	0.12712 (4)	0.00346 (9)
B1	0.0964 (4)	0.9933 (4)	0.0944 (4)	0.0048 (5)
B2	0.2441 (4)	0.8171 (4)	0.4350 (4)	0.0050 (5)
B3	0.2977 (4)	0.1817 (4)	0.1685 (4)	0.0052 (5)
O1	0.8584 (2)	0.0829 (3)	0.0849 (2)	0.0046 (3)
O2	0.3702 (3)	0.3605 (3)	0.1211 (2)	0.0054 (3)
O3	0.1393 (3)	0.8112 (3)	0.2984 (2)	0.0055 (3)
O4	0.7213 (3)	0.3533 (3)	0.3794 (2)	0.0065 (3)
O5	0.1989 (3)	0.1716 (3)	0.0323 (2)	0.0056 (3)
O6	0.3232 (3)	0.0056 (3)	0.3678 (2)	0.0058 (3)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
K	0.0064 (3)	0.0064 (2)	0.0060 (2)	−0.00214 (19)	−0.00063 (19)	−0.00281 (19)
Zn	0.00389 (15)	0.00353 (14)	0.00324 (14)	−0.00047 (10)	−0.00134 (10)	−0.00143 (10)
B1	0.0042 (12)	0.0045 (12)	0.0061 (11)	0.0002 (10)	−0.0021 (9)	−0.0027 (9)
B2	0.0038 (12)	0.0070 (12)	0.0047 (11)	−0.0002 (10)	−0.0002 (9)	−0.0041 (9)
B3	0.0027 (12)	0.0052 (12)	0.0061 (11)	0.0011 (10)	−0.0001 (9)	−0.0030 (9)
O1	0.0036 (8)	0.0068 (8)	0.0046 (7)	−0.0004 (6)	−0.0018 (6)	−0.0032 (6)
O2	0.0048 (8)	0.0056 (8)	0.0062 (7)	−0.0020 (6)	−0.0024 (6)	−0.0013 (6)
O3	0.0058 (8)	0.0053 (8)	0.0055 (7)	−0.0013 (6)	−0.0030 (6)	−0.0008 (6)
O4	0.0096 (9)	0.0056 (8)	0.0050 (7)	−0.0022 (7)	−0.0034 (6)	−0.0013 (6)
O5	0.0074 (8)	0.0052 (7)	0.0044 (7)	−0.0024 (6)	−0.0019 (6)	−0.0008 (6)
O6	0.0071 (8)	0.0059 (8)	0.0056 (7)	−0.0022 (7)	−0.0035 (6)	−0.0013 (6)

Geometric parameters (Å, º) top

K—O4ⁱ	2.6404 (16)	B1—B1^viii	2.080 (5)
K—O3ⁱⁱ	2.7890 (18)	B1—Kⁱⁱ	3.286 (3)
K—O1ⁱⁱⁱ	2.791 (2)	B1—K^ix	3.330 (3)
K—O6	2.8476 (17)	B2—O4ⁱ	1.326 (3)
K—O5^iv	2.8491 (17)	B2—O3	1.380 (3)
K—O6ⁱⁱⁱ	2.856 (2)	B2—O6^vi	1.412 (3)
K—O2	2.9418 (17)	B2—Kⁱ	3.135 (3)
K—O4	3.0888 (19)	B3—O2	1.357 (3)
K—B2ⁱ	3.135 (3)	B3—O5	1.363 (3)
K—O3	3.144 (2)	B3—O6	1.395 (3)
K—B3	3.244 (3)	O1—B1^v	1.492 (3)
K—B2	3.261 (3)	O1—B1^x	1.503 (3)
Zn—O4	1.9013 (15)	O1—Kⁱⁱⁱ	2.791 (2)
Zn—O1	1.9347 (17)	O2—Zn^v	1.9628 (18)
Zn—O2^v	1.9628 (18)	O3—Kⁱⁱ	2.7890 (18)
Zn—O2	2.0414 (16)	O4—B2ⁱ	1.326 (3)
Zn—Zn^v	2.9584 (14)	O4—Kⁱ	2.6404 (16)
B1—O3	1.450 (3)	O5—B1^xi	1.458 (3)
B1—O5^vi	1.458 (3)	O5—K^xii	2.8491 (17)
B1—O1^v	1.492 (3)	O6—B2^xi	1.412 (3)
B1—O1^vii	1.503 (3)	O6—Kⁱⁱⁱ	2.856 (2)

O4ⁱ—K—O3ⁱⁱ	119.60 (6)	O1—Zn—Kⁱⁱⁱ	41.67 (5)
O4ⁱ—K—O1ⁱⁱⁱ	125.80 (5)	O2^v—Zn—Kⁱⁱⁱ	153.56 (5)
O3ⁱⁱ—K—O1ⁱⁱⁱ	52.15 (6)	O2—Zn—Kⁱⁱⁱ	83.72 (6)
O4ⁱ—K—O6	156.86 (5)	Zn^v—Zn—Kⁱⁱⁱ	121.23 (3)
O3ⁱⁱ—K—O6	76.47 (5)	K—Zn—Kⁱⁱⁱ	75.71 (4)
O1ⁱⁱⁱ—K—O6	76.88 (5)	O4—Zn—Kⁱ	32.09 (5)
O4ⁱ—K—O5^iv	75.13 (5)	O1—Zn—Kⁱ	131.51 (5)
O3ⁱⁱ—K—O5^iv	81.16 (6)	O2^v—Zn—Kⁱ	85.63 (5)
O1ⁱⁱⁱ—K—O5^iv	51.22 (5)	O2—Zn—Kⁱ	118.91 (5)
O6—K—O5^iv	126.26 (5)	Zn^v—Zn—Kⁱ	106.44 (3)
O4ⁱ—K—O6ⁱⁱⁱ	103.77 (5)	K—Zn—Kⁱ	75.22 (3)
O3ⁱⁱ—K—O6ⁱⁱⁱ	127.90 (5)	Kⁱⁱⁱ—Zn—Kⁱ	120.74 (2)
O1ⁱⁱⁱ—K—O6ⁱⁱⁱ	79.99 (6)	O3—B1—O5^vi	113.83 (19)
O6—K—O6ⁱⁱⁱ	73.35 (6)	O3—B1—O1^v	113.47 (18)
O5^iv—K—O6ⁱⁱⁱ	83.76 (6)	O5^vi—B1—O1^v	111.49 (18)
O4ⁱ—K—O2	109.74 (5)	O3—B1—O1^vii	112.28 (18)
O3ⁱⁱ—K—O2	101.75 (6)	O5^vi—B1—O1^vii	111.87 (19)
O1ⁱⁱⁱ—K—O2	124.46 (5)	O1^v—B1—O1^vii	92.02 (17)
O6—K—O2	47.88 (5)	O3—B1—B1^viii	124.0 (2)
O5^iv—K—O2	171.41 (5)	O5^vi—B1—B1^viii	122.1 (2)
O6ⁱⁱⁱ—K—O2	88.14 (6)	O1^v—B1—B1^viii	46.22 (12)
O4ⁱ—K—O4	72.24 (6)	O1^vii—B1—B1^viii	45.79 (12)
O3ⁱⁱ—K—O4	167.20 (5)	O3—B1—Kⁱⁱ	57.50 (11)
O1ⁱⁱⁱ—K—O4	126.59 (6)	O5^vi—B1—Kⁱⁱ	150.31 (15)
O6—K—O4	90.79 (5)	O1^v—B1—Kⁱⁱ	97.21 (12)
O5^iv—K—O4	107.95 (5)	O1^vii—B1—Kⁱⁱ	57.78 (10)
O6ⁱⁱⁱ—K—O4	46.94 (5)	B1^viii—B1—Kⁱⁱ	72.83 (13)
O2—K—O4	67.96 (5)	O3—B1—K^ix	151.61 (16)
O4ⁱ—K—B2ⁱ	79.31 (7)	O5^vi—B1—K^ix	58.34 (11)
O3ⁱⁱ—K—B2ⁱ	154.09 (6)	O1^v—B1—K^ix	56.22 (10)
O1ⁱⁱⁱ—K—B2ⁱ	103.00 (7)	O1^vii—B1—K^ix	95.19 (13)
O6—K—B2ⁱ	91.80 (6)	B1^viii—B1—K^ix	70.52 (13)
O5^iv—K—B2ⁱ	87.75 (7)	Kⁱⁱ—B1—K^ix	143.35 (9)
O6ⁱⁱⁱ—K—B2ⁱ	26.75 (5)	O4ⁱ—B2—O3	121.2 (2)
O2—K—B2ⁱ	86.28 (7)	O4ⁱ—B2—O6^vi	120.5 (2)
O4—K—B2ⁱ	24.59 (6)	O3—B2—O6^vi	118.2 (2)
O4ⁱ—K—O3	47.12 (4)	O4ⁱ—B2—Kⁱ	75.76 (14)
O3ⁱⁱ—K—O3	102.99 (5)	O3—B2—Kⁱ	128.91 (16)
O1ⁱⁱⁱ—K—O3	150.43 (5)	O6^vi—B2—Kⁱ	65.55 (12)
O6—K—O3	116.19 (5)	O4ⁱ—B2—K	51.19 (11)
O5^iv—K—O3	116.19 (5)	O3—B2—K	72.85 (12)
O6ⁱⁱⁱ—K—O3	128.27 (5)	O6^vi—B2—K	158.31 (17)
O2—K—O3	71.27 (5)	Kⁱ—B2—K	92.88 (8)
O4—K—O3	81.38 (6)	O2—B3—O5	122.7 (2)
B2ⁱ—K—O3	102.92 (7)	O2—B3—O6	117.3 (2)
O4ⁱ—K—B3	133.81 (6)	O5—B3—O6	119.95 (19)
O3ⁱⁱ—K—B3	82.79 (6)	O2—B3—K	65.06 (11)
O1ⁱⁱⁱ—K—B3	100.12 (6)	O5—B3—K	149.00 (16)
O6—K—B3	25.42 (5)	O6—B3—K	61.19 (11)
O5^iv—K—B3	151.06 (6)	B1^v—O1—B1^x	87.98 (17)
O6ⁱⁱⁱ—K—B3	87.36 (6)	B1^v—O1—Zn	132.19 (14)
O2—K—B3	24.73 (5)	B1^x—O1—Zn	125.03 (13)
O4—K—B3	85.14 (6)	B1^v—O1—Kⁱⁱⁱ	97.40 (12)
B2ⁱ—K—B3	96.54 (7)	B1^x—O1—Kⁱⁱⁱ	95.11 (12)
O3—K—B3	90.81 (6)	Zn—O1—Kⁱⁱⁱ	110.89 (7)
O4ⁱ—K—B2	23.03 (5)	B3—O2—Zn^v	126.73 (15)
O3ⁱⁱ—K—B2	117.32 (7)	B3—O2—Zn	126.50 (16)
O1ⁱⁱⁱ—K—B2	145.28 (6)	Zn^v—O2—Zn	95.24 (7)
O6—K—B2	136.67 (6)	B3—O2—K	90.21 (13)
O5^iv—K—B2	97.00 (6)	Zn^v—O2—K	126.87 (7)
O6ⁱⁱⁱ—K—B2	113.85 (6)	Zn—O2—K	87.73 (6)
O2—K—B2	88.87 (6)	B2—O3—B1	123.45 (18)
O4—K—B2	71.34 (6)	B2—O3—Kⁱⁱ	124.93 (14)
B2ⁱ—K—B2	87.12 (8)	B1—O3—Kⁱⁱ	96.48 (13)
O3—K—B2	24.79 (5)	B2—O3—K	82.36 (13)
B3—K—B2	111.77 (7)	B1—O3—K	149.76 (13)
O4—Zn—O1	109.34 (7)	Kⁱⁱ—O3—K	77.01 (5)
O4—Zn—O2^v	117.70 (7)	B2ⁱ—O4—Zn	128.77 (15)
O1—Zn—O2^v	120.18 (7)	B2ⁱ—O4—Kⁱ	105.78 (13)
O4—Zn—O2	117.57 (7)	Zn—O4—Kⁱ	125.42 (8)
O1—Zn—O2	104.70 (7)	B2ⁱ—O4—K	79.65 (13)
O2^v—Zn—O2	84.76 (7)	Zn—O4—K	86.04 (6)
O4—Zn—Zn^v	128.89 (6)	Kⁱ—O4—K	107.76 (6)
O1—Zn—Zn^v	120.57 (5)	B3—O5—B1^xi	122.58 (18)
O2^v—Zn—Zn^v	43.41 (5)	B3—O5—K^xii	136.44 (13)
O2—Zn—Zn^v	41.35 (5)	B1^xi—O5—K^xii	95.84 (12)
O4—Zn—K	61.28 (5)	B3—O6—B2^xi	121.34 (18)
O1—Zn—K	117.35 (6)	B3—O6—K	93.39 (12)
O2^v—Zn—K	116.70 (6)	B2^xi—O6—K	130.47 (13)
O2—Zn—K	56.78 (5)	B3—O6—Kⁱⁱⁱ	118.51 (14)
Zn^v—Zn—K	85.42 (3)	B2^xi—O6—Kⁱⁱⁱ	87.70 (14)
O4—Zn—Kⁱⁱⁱ	88.71 (6)	K—O6—Kⁱⁱⁱ	106.65 (6)

O4ⁱ—K—Zn—O4	50.46 (9)	Kⁱⁱⁱ—Zn—O2—Zn^v	−156.16 (5)
O3ⁱⁱ—K—Zn—O4	−170.08 (8)	Kⁱ—Zn—O2—Zn^v	82.07 (6)
O1ⁱⁱⁱ—K—Zn—O4	−95.13 (8)	O4—Zn—O2—K	−8.22 (8)
O6—K—Zn—O4	−137.47 (7)	O1—Zn—O2—K	113.32 (6)
O5^iv—K—Zn—O4	−19.56 (8)	O2^v—Zn—O2—K	−126.83 (7)
O6ⁱⁱⁱ—K—Zn—O4	−53.81 (7)	Zn^v—Zn—O2—K	−126.83 (7)
O2—K—Zn—O4	171.69 (8)	Kⁱⁱⁱ—Zn—O2—K	77.02 (5)
B2ⁱ—K—Zn—O4	−23.73 (8)	Kⁱ—Zn—O2—K	−44.76 (6)
O3—K—Zn—O4	95.11 (7)	O4ⁱ—K—O2—B3	−168.31 (13)
B3—K—Zn—O4	−163.59 (8)	O3ⁱⁱ—K—O2—B3	−40.67 (14)
B2—K—Zn—O4	70.13 (8)	O1ⁱⁱⁱ—K—O2—B3	11.21 (15)
O4ⁱ—K—Zn—O1	148.61 (6)	O6—K—O2—B3	18.64 (13)
O3ⁱⁱ—K—Zn—O1	−71.93 (8)	O6ⁱⁱⁱ—K—O2—B3	87.72 (14)
O1ⁱⁱⁱ—K—Zn—O1	3.02 (9)	O4—K—O2—B3	131.35 (14)
O6—K—Zn—O1	−39.32 (6)	B2ⁱ—K—O2—B3	114.45 (14)
O5^iv—K—Zn—O1	78.59 (8)	O3—K—O2—B3	−140.57 (14)
O6ⁱⁱⁱ—K—Zn—O1	44.34 (6)	B2—K—O2—B3	−158.37 (14)
O2—K—Zn—O1	−90.16 (8)	O4ⁱ—K—O2—Zn^v	−29.68 (10)
O4—K—Zn—O1	98.15 (8)	O3ⁱⁱ—K—O2—Zn^v	97.96 (9)
B2ⁱ—K—Zn—O1	74.42 (8)	O1ⁱⁱⁱ—K—O2—Zn^v	149.85 (8)
O3—K—Zn—O1	−166.75 (6)	O6—K—O2—Zn^v	157.27 (11)
B3—K—Zn—O1	−65.44 (8)	O6ⁱⁱⁱ—K—O2—Zn^v	−133.65 (9)
B2—K—Zn—O1	168.27 (7)	O4—K—O2—Zn^v	−90.02 (9)
O4ⁱ—K—Zn—O2^v	−58.07 (6)	B2ⁱ—K—O2—Zn^v	−106.92 (10)
O3ⁱⁱ—K—Zn—O2^v	81.39 (8)	O3—K—O2—Zn^v	−1.94 (7)
O1ⁱⁱⁱ—K—Zn—O2^v	156.34 (7)	B3—K—O2—Zn^v	138.63 (18)
O6—K—Zn—O2^v	114.00 (6)	B2—K—O2—Zn^v	−19.73 (9)
O5^iv—K—Zn—O2^v	−128.09 (7)	O4ⁱ—K—O2—Zn	65.17 (7)
O6ⁱⁱⁱ—K—Zn—O2^v	−162.34 (6)	O3ⁱⁱ—K—O2—Zn	−167.19 (5)
O2—K—Zn—O2^v	63.16 (9)	O1ⁱⁱⁱ—K—O2—Zn	−115.30 (6)
O4—K—Zn—O2^v	−108.53 (8)	O6—K—O2—Zn	−107.88 (8)
B2ⁱ—K—Zn—O2^v	−132.26 (8)	O6ⁱⁱⁱ—K—O2—Zn	−38.80 (5)
O3—K—Zn—O2^v	−13.42 (6)	O4—K—O2—Zn	4.83 (5)
B3—K—Zn—O2^v	87.88 (8)	B2ⁱ—K—O2—Zn	−12.07 (6)
B2—K—Zn—O2^v	−38.41 (7)	O3—K—O2—Zn	92.91 (6)
O4ⁱ—K—Zn—O2	−121.23 (7)	B3—K—O2—Zn	−126.52 (15)
O3ⁱⁱ—K—Zn—O2	18.23 (7)	B2—K—O2—Zn	75.12 (7)
O1ⁱⁱⁱ—K—Zn—O2	93.19 (8)	O4ⁱ—B2—O3—B1	179.7 (2)
O6—K—Zn—O2	50.85 (7)	O6^vi—B2—O3—B1	−3.2 (3)
O5^iv—K—Zn—O2	168.75 (8)	Kⁱ—B2—O3—B1	−83.4 (3)
O6ⁱⁱⁱ—K—Zn—O2	134.50 (6)	K—B2—O3—B1	−162.96 (19)
O4—K—Zn—O2	−171.69 (8)	O4ⁱ—B2—O3—Kⁱⁱ	50.9 (3)
B2ⁱ—K—Zn—O2	164.58 (8)	O6^vi—B2—O3—Kⁱⁱ	−132.00 (17)
O3—K—Zn—O2	−76.58 (7)	Kⁱ—B2—O3—Kⁱⁱ	147.80 (11)
B3—K—Zn—O2	24.72 (8)	K—B2—O3—Kⁱⁱ	68.26 (12)
B2—K—Zn—O2	−101.56 (8)	O4ⁱ—B2—O3—K	−17.4 (2)
O4ⁱ—K—Zn—Zn^v	−89.18 (4)	O6^vi—B2—O3—K	159.7 (2)
O3ⁱⁱ—K—Zn—Zn^v	50.27 (6)	Kⁱ—B2—O3—K	79.54 (16)
O1ⁱⁱⁱ—K—Zn—Zn^v	125.23 (5)	O5^vi—B1—O3—B2	7.7 (3)
O6—K—Zn—Zn^v	82.89 (4)	O1^v—B1—O3—B2	136.6 (2)
O5^iv—K—Zn—Zn^v	−159.20 (5)	O1^vii—B1—O3—B2	−120.7 (2)
O6ⁱⁱⁱ—K—Zn—Zn^v	166.54 (4)	B1^viii—B1—O3—B2	−171.5 (2)
O2—K—Zn—Zn^v	32.04 (5)	Kⁱⁱ—B1—O3—B2	−140.0 (2)
O4—K—Zn—Zn^v	−139.64 (6)	K^ix—B1—O3—B2	74.7 (4)
B2ⁱ—K—Zn—Zn^v	−163.37 (6)	O5^vi—B1—O3—Kⁱⁱ	147.63 (16)
O3—K—Zn—Zn^v	−44.54 (4)	O1^v—B1—O3—Kⁱⁱ	−83.43 (18)
B3—K—Zn—Zn^v	56.77 (6)	O1^vii—B1—O3—Kⁱⁱ	19.24 (17)
B2—K—Zn—Zn^v	−69.52 (6)	B1^viii—B1—O3—Kⁱⁱ	−31.5 (3)
O4ⁱ—K—Zn—Kⁱⁱⁱ	146.95 (4)	K^ix—B1—O3—Kⁱⁱ	−145.3 (3)
O3ⁱⁱ—K—Zn—Kⁱⁱⁱ	−73.59 (6)	O5^vi—B1—O3—K	−137.1 (2)
O1ⁱⁱⁱ—K—Zn—Kⁱⁱⁱ	1.37 (4)	O1^v—B1—O3—K	−8.2 (4)
O6—K—Zn—Kⁱⁱⁱ	−40.97 (4)	O1^vii—B1—O3—K	94.5 (3)
O5^iv—K—Zn—Kⁱⁱⁱ	76.93 (6)	B1^viii—B1—O3—K	43.7 (4)
O6ⁱⁱⁱ—K—Zn—Kⁱⁱⁱ	42.68 (4)	Kⁱⁱ—B1—O3—K	75.3 (2)
O2—K—Zn—Kⁱⁱⁱ	−91.82 (6)	K^ix—B1—O3—K	−70.0 (4)
O4—K—Zn—Kⁱⁱⁱ	96.49 (6)	O4ⁱ—K—O3—B2	10.06 (12)
B2ⁱ—K—Zn—Kⁱⁱⁱ	72.76 (7)	O3ⁱⁱ—K—O3—B2	128.59 (13)
O3—K—Zn—Kⁱⁱⁱ	−168.40 (3)	O1ⁱⁱⁱ—K—O3—B2	98.98 (15)
B3—K—Zn—Kⁱⁱⁱ	−67.10 (6)	O6—K—O3—B2	−150.28 (12)
B2—K—Zn—Kⁱⁱⁱ	166.62 (5)	O5^iv—K—O3—B2	42.17 (13)
O4ⁱ—K—Zn—Kⁱ	19.17 (4)	O6ⁱⁱⁱ—K—O3—B2	−61.35 (14)
O3ⁱⁱ—K—Zn—Kⁱ	158.63 (6)	O2—K—O3—B2	−133.21 (13)
O1ⁱⁱⁱ—K—Zn—Kⁱ	−126.42 (5)	O4—K—O3—B2	−63.66 (13)
O6—K—Zn—Kⁱ	−168.76 (4)	B2ⁱ—K—O3—B2	−51.73 (16)
O5^iv—K—Zn—Kⁱ	−50.85 (5)	B3—K—O3—B2	−148.62 (13)
O6ⁱⁱⁱ—K—Zn—Kⁱ	−85.10 (4)	O4ⁱ—K—O3—B1	161.0 (3)
O2—K—Zn—Kⁱ	140.40 (6)	O3ⁱⁱ—K—O3—B1	−80.5 (3)
O4—K—Zn—Kⁱ	−31.29 (6)	O1ⁱⁱⁱ—K—O3—B1	−110.1 (3)
B2ⁱ—K—Zn—Kⁱ	−55.02 (6)	O6—K—O3—B1	0.7 (3)
O3—K—Zn—Kⁱ	63.81 (4)	O5^iv—K—O3—B1	−166.9 (3)
B3—K—Zn—Kⁱ	165.12 (6)	O6ⁱⁱⁱ—K—O3—B1	89.6 (3)
B2—K—Zn—Kⁱ	38.83 (5)	O2—K—O3—B1	17.7 (3)
O3ⁱⁱ—K—B2—O4ⁱ	101.89 (15)	O4—K—O3—B1	87.3 (3)
O1ⁱⁱⁱ—K—B2—O4ⁱ	39.7 (2)	B2ⁱ—K—O3—B1	99.2 (3)
O6—K—B2—O4ⁱ	−158.69 (12)	B3—K—O3—B1	2.3 (3)
O5^iv—K—B2—O4ⁱ	18.26 (15)	B2—K—O3—B1	150.9 (3)
O6ⁱⁱⁱ—K—B2—O4ⁱ	−67.98 (15)	O4ⁱ—K—O3—Kⁱⁱ	−118.53 (7)
O2—K—B2—O4ⁱ	−155.45 (14)	O3ⁱⁱ—K—O3—Kⁱⁱ	0.0
O4—K—B2—O4ⁱ	−88.37 (15)	O1ⁱⁱⁱ—K—O3—Kⁱⁱ	−29.61 (10)
B2ⁱ—K—B2—O4ⁱ	−69.11 (14)	O6—K—O3—Kⁱⁱ	81.13 (6)
O3—K—B2—O4ⁱ	160.9 (2)	O5^iv—K—O3—Kⁱⁱ	−86.42 (6)
B3—K—B2—O4ⁱ	−165.01 (14)	O6ⁱⁱⁱ—K—O3—Kⁱⁱ	170.06 (5)
O4ⁱ—K—B2—O3	−160.9 (2)	O2—K—O3—Kⁱⁱ	98.19 (5)
O3ⁱⁱ—K—B2—O3	−59.00 (14)	O4—K—O3—Kⁱⁱ	167.74 (5)
O1ⁱⁱⁱ—K—B2—O3	−121.16 (12)	B2ⁱ—K—O3—Kⁱⁱ	179.68 (6)
O6—K—B2—O3	40.42 (16)	B3—K—O3—Kⁱⁱ	82.79 (6)
O5^iv—K—B2—O3	−142.63 (12)	B2—K—O3—Kⁱⁱ	−128.59 (13)
O6ⁱⁱⁱ—K—B2—O3	131.12 (12)	O1—Zn—O4—B2ⁱ	−37.9 (2)
O2—K—B2—O3	43.66 (12)	O2^v—Zn—O4—B2ⁱ	−179.73 (18)
O4—K—B2—O3	110.73 (13)	O2—Zn—O4—B2ⁱ	81.2 (2)
B2ⁱ—K—B2—O3	129.99 (15)	Zn^v—Zn—O4—B2ⁱ	129.37 (18)
B3—K—B2—O3	34.10 (14)	K—Zn—O4—B2ⁱ	73.35 (19)
O4ⁱ—K—B2—O6^vi	74.8 (4)	Kⁱⁱⁱ—Zn—O4—B2ⁱ	−1.03 (19)
O3ⁱⁱ—K—B2—O6^vi	176.7 (4)	Kⁱ—Zn—O4—B2ⁱ	−177.6 (3)
O1ⁱⁱⁱ—K—B2—O6^vi	114.5 (4)	O1—Zn—O4—Kⁱ	139.70 (9)
O6—K—B2—O6^vi	−83.9 (4)	O2^v—Zn—O4—Kⁱ	−2.11 (12)
O5^iv—K—B2—O6^vi	93.0 (4)	O2—Zn—O4—Kⁱ	−101.18 (10)
O6ⁱⁱⁱ—K—B2—O6^vi	6.8 (4)	Zn^v—Zn—O4—Kⁱ	−53.01 (11)
O2—K—B2—O6^vi	−80.7 (4)	K—Zn—O4—Kⁱ	−109.03 (10)
O4—K—B2—O6^vi	−13.6 (4)	Kⁱⁱⁱ—Zn—O4—Kⁱ	176.59 (8)
B2ⁱ—K—B2—O6^vi	5.7 (4)	O1—Zn—O4—K	−111.28 (6)
O3—K—B2—O6^vi	−124.3 (5)	O2^v—Zn—O4—K	106.92 (7)
B3—K—B2—O6^vi	−90.2 (4)	O2—Zn—O4—K	7.84 (7)
O4ⁱ—K—B2—Kⁱ	69.11 (14)	Zn^v—Zn—O4—K	56.02 (6)
O3ⁱⁱ—K—B2—Kⁱ	171.01 (5)	Kⁱⁱⁱ—Zn—O4—K	−74.39 (5)
O1ⁱⁱⁱ—K—B2—Kⁱ	108.85 (10)	Kⁱ—Zn—O4—K	109.03 (10)
O6—K—B2—Kⁱ	−89.57 (9)	O4ⁱ—K—O4—B2ⁱ	103.40 (14)
O5^iv—K—B2—Kⁱ	87.38 (7)	O3ⁱⁱ—K—O4—B2ⁱ	−98.0 (2)
O6ⁱⁱⁱ—K—B2—Kⁱ	1.13 (7)	O1ⁱⁱⁱ—K—O4—B2ⁱ	−18.42 (14)
O2—K—B2—Kⁱ	−86.33 (7)	O6—K—O4—B2ⁱ	−92.60 (13)
O4—K—B2—Kⁱ	−19.26 (4)	O5^iv—K—O4—B2ⁱ	36.17 (14)
B2ⁱ—K—B2—Kⁱ	0.0	O6ⁱⁱⁱ—K—O4—B2ⁱ	−26.49 (12)
O3—K—B2—Kⁱ	−129.99 (15)	O2—K—O4—B2ⁱ	−135.79 (14)
B3—K—B2—Kⁱ	−95.89 (8)	O3—K—O4—B2ⁱ	151.02 (13)
O4ⁱ—K—B3—O2	15.32 (17)	B3—K—O4—B2ⁱ	−117.42 (14)
O3ⁱⁱ—K—B3—O2	139.97 (14)	B2—K—O4—B2ⁱ	127.65 (12)
O1ⁱⁱⁱ—K—B3—O2	−170.63 (12)	O4ⁱ—K—O4—Zn	−126.01 (9)
O6—K—B3—O2	−146.5 (2)	O3ⁱⁱ—K—O4—Zn	32.6 (2)
O5^iv—K—B3—O2	−163.33 (11)	O1ⁱⁱⁱ—K—O4—Zn	112.17 (6)
O6ⁱⁱⁱ—K—B3—O2	−91.29 (13)	O6—K—O4—Zn	37.99 (6)
O4—K—B3—O2	−44.29 (13)	O5^iv—K—O4—Zn	166.76 (5)
B2ⁱ—K—B3—O2	−66.12 (14)	O6ⁱⁱⁱ—K—O4—Zn	104.10 (8)
O3—K—B3—O2	36.98 (13)	O2—K—O4—Zn	−5.20 (5)
B2—K—B3—O2	23.39 (15)	B2ⁱ—K—O4—Zn	130.59 (15)
O4ⁱ—K—B3—O5	−97.2 (3)	O3—K—O4—Zn	−78.39 (6)
O3ⁱⁱ—K—B3—O5	27.5 (3)	B3—K—O4—Zn	13.17 (6)
O1ⁱⁱⁱ—K—B3—O5	76.9 (3)	B2—K—O4—Zn	−101.76 (8)
O6—K—B3—O5	101.0 (3)	O4ⁱ—K—O4—Kⁱ	0.0
O5^iv—K—B3—O5	84.2 (3)	O3ⁱⁱ—K—O4—Kⁱ	158.64 (19)
O6ⁱⁱⁱ—K—B3—O5	156.2 (3)	O1ⁱⁱⁱ—K—O4—Kⁱ	−121.82 (6)
O2—K—B3—O5	−112.5 (4)	O6—K—O4—Kⁱ	164.00 (6)
O4—K—B3—O5	−156.8 (3)	O5^iv—K—O4—Kⁱ	−67.23 (7)
B2ⁱ—K—B3—O5	−178.6 (3)	O6ⁱⁱⁱ—K—O4—Kⁱ	−129.90 (8)
O3—K—B3—O5	−75.5 (3)	O2—K—O4—Kⁱ	120.81 (7)
B2—K—B3—O5	−89.1 (3)	B2ⁱ—K—O4—Kⁱ	−103.40 (14)
O4ⁱ—K—B3—O6	161.80 (11)	O3—K—O4—Kⁱ	47.62 (5)
O3ⁱⁱ—K—B3—O6	−73.54 (13)	B3—K—O4—Kⁱ	139.18 (7)
O1ⁱⁱⁱ—K—B3—O6	−24.14 (13)	B2—K—O4—Kⁱ	24.25 (6)
O5^iv—K—B3—O6	−16.8 (2)	O2—B3—O5—B1^xi	−171.9 (2)
O6ⁱⁱⁱ—K—B3—O6	55.19 (13)	O6—B3—O5—B1^xi	6.6 (3)
O2—K—B3—O6	146.5 (2)	K—B3—O5—B1^xi	−76.4 (4)
O4—K—B3—O6	102.19 (13)	O2—B3—O5—K^xii	40.2 (3)
B2ⁱ—K—B3—O6	80.36 (14)	O6—B3—O5—K^xii	−141.28 (16)
O3—K—B3—O6	−176.54 (12)	K—B3—O5—K^xii	135.7 (2)
B2—K—B3—O6	169.87 (12)	O2—B3—O6—B2^xi	177.2 (2)
O4—Zn—O1—B1^v	−173.34 (17)	O5—B3—O6—B2^xi	−1.4 (3)
O2^v—Zn—O1—B1^v	−32.6 (2)	K—B3—O6—B2^xi	142.9 (2)
O2—Zn—O1—B1^v	59.85 (19)	O2—B3—O6—K	34.3 (2)
Zn^v—Zn—O1—B1^v	18.13 (19)	O5—B3—O6—K	−144.30 (19)
K—Zn—O1—B1^v	119.73 (17)	O2—B3—O6—Kⁱⁱⁱ	−76.7 (2)
Kⁱⁱⁱ—Zn—O1—B1^v	122.1 (2)	O5—B3—O6—Kⁱⁱⁱ	104.7 (2)
Kⁱ—Zn—O1—B1^v	−146.02 (16)	K—B3—O6—Kⁱⁱⁱ	−111.02 (10)
O4—Zn—O1—B1^x	−48.07 (17)	O4ⁱ—K—O6—B3	−35.0 (2)
O2^v—Zn—O1—B1^x	92.65 (16)	O3ⁱⁱ—K—O6—B3	101.87 (13)
O2—Zn—O1—B1^x	−174.87 (15)	O1ⁱⁱⁱ—K—O6—B3	155.58 (13)
Zn^v—Zn—O1—B1^x	143.40 (14)	O5^iv—K—O6—B3	169.98 (12)
K—Zn—O1—B1^x	−115.00 (15)	O6ⁱⁱⁱ—K—O6—B3	−121.12 (14)
Kⁱⁱⁱ—Zn—O1—B1^x	−112.59 (17)	O2—K—O6—B3	−18.14 (12)
Kⁱ—Zn—O1—B1^x	−20.75 (18)	O4—K—O6—B3	−76.92 (13)
O4—Zn—O1—Kⁱⁱⁱ	64.52 (8)	B2ⁱ—K—O6—B3	−101.49 (14)
O2^v—Zn—O1—Kⁱⁱⁱ	−154.77 (6)	O3—K—O6—B3	3.86 (14)
O2—Zn—O1—Kⁱⁱⁱ	−62.29 (8)	B2—K—O6—B3	−13.77 (16)
Zn^v—Zn—O1—Kⁱⁱⁱ	−104.01 (6)	O4ⁱ—K—O6—B2^xi	−172.34 (18)
K—Zn—O1—Kⁱⁱⁱ	−2.41 (8)	O3ⁱⁱ—K—O6—B2^xi	−35.48 (19)
Kⁱ—Zn—O1—Kⁱⁱⁱ	91.84 (7)	O1ⁱⁱⁱ—K—O6—B2^xi	18.23 (19)
O5—B3—O2—Zn^v	6.8 (3)	O5^iv—K—O6—B2^xi	32.6 (2)
O6—B3—O2—Zn^v	−171.72 (14)	O6ⁱⁱⁱ—K—O6—B2^xi	101.5 (2)
K—B3—O2—Zn^v	−138.72 (16)	O2—K—O6—B2^xi	−155.5 (2)
O5—B3—O2—Zn	−127.1 (2)	O4—K—O6—B2^xi	145.74 (19)
O6—B3—O2—Zn	54.3 (3)	B2ⁱ—K—O6—B2^xi	121.17 (17)
K—B3—O2—Zn	87.33 (13)	O3—K—O6—B2^xi	−133.48 (18)
O5—B3—O2—K	145.6 (2)	B3—K—O6—B2^xi	−137.3 (3)
O6—B3—O2—K	−33.0 (2)	B2—K—O6—B2^xi	−151.1 (2)
O4—Zn—O2—B3	−96.81 (18)	O4ⁱ—K—O6—Kⁱⁱⁱ	86.13 (14)
O1—Zn—O2—B3	24.73 (18)	O3ⁱⁱ—K—O6—Kⁱⁱⁱ	−137.01 (6)
O2^v—Zn—O2—B3	144.6 (2)	O1ⁱⁱⁱ—K—O6—Kⁱⁱⁱ	−83.30 (6)
Zn^v—Zn—O2—B3	144.6 (2)	O5^iv—K—O6—Kⁱⁱⁱ	−68.90 (8)
K—Zn—O2—B3	−88.59 (17)	O6ⁱⁱⁱ—K—O6—Kⁱⁱⁱ	0.0
Kⁱⁱⁱ—Zn—O2—B3	−11.57 (16)	O2—K—O6—Kⁱⁱⁱ	102.98 (8)
Kⁱ—Zn—O2—B3	−133.34 (16)	O4—K—O6—Kⁱⁱⁱ	44.20 (5)
O4—Zn—O2—Zn^v	118.60 (7)	B2ⁱ—K—O6—Kⁱⁱⁱ	19.63 (6)
O1—Zn—O2—Zn^v	−119.85 (7)	O3—K—O6—Kⁱⁱⁱ	124.98 (6)
O2^v—Zn—O2—Zn^v	0.0	B3—K—O6—Kⁱⁱⁱ	121.12 (14)
K—Zn—O2—Zn^v	126.83 (7)	B2—K—O6—Kⁱⁱⁱ	107.35 (9)

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

Experimental details

Crystal data
Chemical formula	KZnB₃O₆
M_r	232.90
Crystal system, space group	Triclinic, P1
Temperature (K)	93
a, b, c (Å)	6.7139 (13), 6.9301 (14), 7.0632 (14)
α, β, γ (°)	63.12 (3), 72.02 (3), 68.99 (3)
V (Å³)	269.37 (12)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	5.29
Crystal size (mm)	0.50 × 0.30 × 0.20

Data collection
Diffractometer	Rigaku Saturn 724+
Absorption correction	Multi-scan (ABSCOR; Higashi, 1995)
T_min, T_max	0.480, 1.000
No. of measured, independent and observed [I > 2σ(I)] reflections	2707, 1223, 1118
R_int	0.023
(sin θ/λ)_max (Å⁻¹)	0.649

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.020, 0.050, 0.94
No. of reflections	1223
No. of parameters	100
Δρ_max, Δρ_min (e Å⁻³)	0.38, −0.58

Computer programs: CrystalClear (Rigaku, 2008), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ATOMS (Dowty, 1998).

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Format		BIBTeX
		EndNote
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		Medline
		CIF
		SGML
		Text
		Plain Text

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