Structure of KNbOB₂O₅ – a commensurately modulated structure

Members of the AMOB₂O₅ (A = K, Rb, Cs, Tl; M = Nb, Ta) family of compounds can be described as modulated structures with a single superspace group and very similar modulation functions. Single-crystal X-ray diffraction data (Mo Kα radiation) are used to solve and refine the structure of KNbOB₂O₅ in these terms for the first time. The average structure is solved and refined in the space group Pmn2₁. Subsequently, the atomic modulation functions are determined using JANA2000 and superspace-group symmetry Pmn2₁(0,0.375,0)s. The commensurately modulated structure is finally refined as a superstructure in the space group Pbn2₁ using SHELXS97 converging to R₁ = 0.024.

Computing details

Program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997b).

Figures

(c:_shelx_knbobo_knb-t00)

Crystal data

B8K4Nb4O24	Dx = 3.178 Mg m^−3
Mr = 3994.08	Mo Kα radiation, λ = 0.71069 Å
Orthorhombic, Pbn21	Cell parameters from 928 reflections
a = 7.3056 (11) Å	θ = 1.3–26.5°
b = 31.1632 (18) Å	µ = 3.06 mm^−1
c = 9.1659 (15) Å	T = 293 K
V = 2086.8 (5) Å^3	Block, colourless
Z = 4	0.23 × 0.23 × 0.18 mm
F(000) = 1888

Data collection

Three-circle goniometer diffractometer	4272 independent reflections
Radiation source: fine-focus sealed tube	3768 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.021
ω scans	θmax = 26.5°, θmin = 1.3°
Absorption correction: multi-scan ?	h = −9→6
Tmin = ?, Tmax = ?	k = −39→36
12617 measured reflections	l = −11→11

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0365P)^2] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.024	(Δ/σ)max = 0.189
wR(F^2) = 0.065	Δρmax = 0.40 e Å^−3
S = 0.97	Δρmin = −0.57 e Å^−3
4272 reflections	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
362 parameters	Extinction coefficient: 0.00051 (5)
1 restraint	Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.02 (4)

Special details

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
K-1	0.00601 (11)	0.06419 (4)	0.06652 (12)	0.0273 (3)
K-2	0.00937 (12)	0.18992 (4)	0.06582 (12)	0.0286 (3)
K-3	0.00190 (12)	0.31374 (4)	0.05438 (12)	0.0277 (3)
K-4	−0.00881 (11)	0.43877 (4)	0.05738 (12)	0.0252 (2)
Nb-1	0.03785 (4)	0.099635 (8)	0.66158 (4)	0.00733 (9)
Nb-2	−0.01804 (3)	0.225821 (9)	0.66236 (4)	0.00782 (9)
Nb-3	−0.01097 (3)	0.350713 (9)	0.66542 (4)	0.00744 (9)
Nb-4	0.01162 (3)	0.474595 (9)	0.66392 (4)	0.00744 (9)
B-1	0.3809 (5)	0.12755 (12)	0.8633 (4)	0.0137 (8)
B-2	0.3057 (5)	0.24716 (13)	0.8885 (5)	0.0140 (8)
B-3	0.3340 (5)	0.36772 (12)	0.8646 (4)	0.0130 (8)
B-4	0.3417 (5)	0.50490 (13)	0.8734 (4)	0.0141 (9)
B-5	0.2889 (5)	0.61869 (13)	0.8870 (5)	0.0145 (8)
B-6	0.3612 (5)	0.74498 (13)	0.8616 (4)	0.0140 (9)
B-7	0.3306 (5)	0.87847 (13)	0.8841 (5)	0.0136 (8)
B-8	0.3268 (5)	0.99105 (12)	0.8767 (5)	0.0140 (9)
O1-1	0.2063 (3)	0.11303 (9)	0.4914 (3)	0.0150 (6)
O1-2	0.1874 (4)	0.24127 (9)	0.5296 (3)	0.0180 (7)
O1-3	0.1425 (3)	0.34980 (8)	0.4868 (3)	0.0163 (6)
O1-4	0.1986 (4)	0.49345 (10)	0.5115 (3)	0.0154 (6)
O1-5	0.1597 (5)	0.60295 (10)	0.5163 (3)	0.0200 (8)
O1-6	0.1760 (3)	0.73273 (9)	0.4844 (3)	0.0191 (6)
O1-7	0.2137 (3)	0.86917 (9)	0.5288 (3)	0.0136 (6)
O1-8	0.1571 (4)	0.97204 (9)	0.4976 (3)	0.0159 (7)
O2-1	0.2416 (4)	0.11112 (10)	0.7887 (3)	0.0265 (7)
O2-2	0.1416 (4)	0.23778 (9)	0.8274 (3)	0.0196 (7)
O2-3	0.2081 (3)	0.34490 (8)	0.7879 (3)	0.0146 (6)
O2-4	0.1841 (4)	0.49283 (9)	0.8121 (3)	0.0199 (7)
O2-5	0.1347 (4)	0.60389 (10)	0.8224 (3)	0.0192 (7)
O2-6	0.2348 (3)	0.72312 (8)	0.7864 (3)	0.0168 (6)
O2-7	0.1661 (4)	0.86849 (8)	0.8275 (3)	0.0145 (6)
O2-8	0.1913 (4)	0.97104 (8)	0.8025 (3)	0.0144 (7)
O3-1	0.0652 (3)	0.04323 (6)	0.6590 (5)	0.0222 (5)
O3-2	0.0119 (3)	0.16999 (8)	0.6553 (5)	0.0311 (7)
O3-3	−0.0693 (3)	0.29562 (6)	0.6704 (4)	0.0188 (5)
O3-4	0.0709 (3)	0.41939 (6)	0.6655 (4)	0.0153 (4)
O4-1	0.5534 (3)	0.11972 (9)	0.8035 (3)	0.0191 (6)
O4-2	0.4612 (3)	0.24331 (10)	0.8032 (3)	0.0191 (6)
O4-3	0.5117 (3)	0.36810 (10)	0.8053 (3)	0.0193 (6)
O4-4	0.5045 (3)	0.49294 (10)	0.8057 (3)	0.0198 (7)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
K-1	0.0285 (5)	0.0271 (5)	0.0264 (6)	0.0059 (4)	−0.0041 (4)	0.0049 (5)
K-2	0.0312 (5)	0.0287 (6)	0.0259 (6)	−0.0071 (4)	0.0003 (4)	0.0069 (5)
K-3	0.0266 (5)	0.0299 (6)	0.0265 (7)	0.0007 (3)	0.0005 (4)	0.0063 (5)
K-4	0.0228 (5)	0.0267 (5)	0.0259 (6)	0.0031 (3)	−0.0016 (4)	0.0037 (4)
Nb-1	0.00728 (14)	0.00781 (15)	0.00691 (17)	0.00022 (9)	−0.0005 (4)	−0.00004 (17)
Nb-2	0.00839 (13)	0.00783 (16)	0.00724 (17)	0.00034 (8)	−0.0001 (2)	0.00023 (17)
Nb-3	0.00790 (13)	0.00731 (15)	0.00712 (19)	0.00016 (8)	0.0007 (3)	0.00016 (16)
Nb-4	0.00756 (13)	0.00765 (16)	0.00710 (17)	−0.00011 (8)	0.0006 (3)	0.00010 (17)
B-1	0.011 (2)	0.013 (2)	0.017 (2)	0.0020 (15)	−0.0005 (15)	0.0036 (16)
B-2	0.010 (2)	0.019 (2)	0.012 (2)	0.0011 (16)	−0.0046 (15)	0.0019 (17)
B-3	0.0081 (18)	0.017 (2)	0.014 (2)	−0.0002 (14)	−0.0003 (14)	0.0025 (16)
B-4	0.015 (2)	0.016 (2)	0.011 (2)	0.0017 (15)	0.0019 (15)	0.0013 (16)
B-5	0.0094 (19)	0.014 (2)	0.020 (2)	0.0011 (15)	−0.0027 (17)	−0.0026 (18)
B-6	0.011 (2)	0.020 (2)	0.011 (2)	0.0039 (15)	−0.0012 (14)	0.0002 (16)
B-7	0.013 (2)	0.012 (2)	0.016 (2)	0.0038 (15)	−0.0001 (16)	0.0019 (17)
B-8	0.0103 (19)	0.013 (2)	0.019 (2)	−0.0001 (14)	−0.0027 (16)	0.0001 (17)
O1-1	0.0081 (14)	0.0252 (15)	0.0118 (14)	0.0010 (10)	0.0006 (10)	0.0047 (11)
O1-2	0.0130 (14)	0.0296 (18)	0.0113 (15)	0.0009 (11)	0.0013 (11)	0.0018 (12)
O1-3	0.0135 (14)	0.0237 (15)	0.0116 (14)	0.0059 (11)	0.0031 (11)	0.0029 (11)
O1-4	0.0114 (15)	0.0208 (17)	0.0140 (15)	−0.0025 (13)	−0.0017 (12)	0.0029 (12)
O1-5	0.0105 (15)	0.038 (2)	0.0114 (14)	0.0073 (12)	0.0034 (12)	0.0099 (13)
O1-6	0.0152 (14)	0.0290 (16)	0.0132 (14)	0.0098 (11)	0.0025 (11)	0.0031 (12)
O1-7	0.0085 (13)	0.0195 (15)	0.0127 (13)	0.0004 (10)	−0.0016 (11)	0.0022 (11)
O1-8	0.0120 (15)	0.0201 (16)	0.0156 (14)	0.0034 (11)	0.0033 (11)	0.0060 (12)
O2-1	0.0167 (16)	0.0433 (18)	0.0194 (15)	−0.0046 (13)	−0.0061 (13)	−0.0073 (14)
O2-2	0.0135 (15)	0.0312 (16)	0.0140 (14)	−0.0036 (11)	−0.0007 (12)	0.0014 (12)
O2-3	0.0129 (13)	0.0133 (13)	0.0177 (14)	0.0003 (10)	−0.0017 (10)	−0.0024 (11)
O2-4	0.0153 (16)	0.0256 (19)	0.0186 (16)	−0.0009 (13)	−0.0073 (13)	−0.0068 (13)
O2-5	0.0161 (17)	0.0301 (18)	0.0116 (15)	−0.0070 (12)	−0.0047 (12)	0.0022 (12)
O2-6	0.0108 (13)	0.0227 (14)	0.0169 (14)	0.0044 (11)	−0.0036 (11)	−0.0011 (12)
O2-7	0.0113 (13)	0.0204 (15)	0.0117 (13)	0.0002 (10)	−0.0024 (11)	−0.0035 (11)
O2-8	0.0129 (15)	0.0160 (15)	0.0142 (14)	−0.0006 (10)	−0.0029 (11)	0.0021 (11)
O3-1	0.0257 (12)	0.0123 (11)	0.0285 (14)	−0.0009 (8)	0.000 (2)	−0.0005 (18)
O3-2	0.0474 (16)	0.0106 (13)	0.0353 (19)	0.0048 (9)	0.008 (2)	−0.0005 (18)
O3-3	0.0214 (11)	0.0107 (10)	0.0243 (14)	0.0001 (8)	0.0004 (19)	−0.0017 (17)
O3-4	0.0156 (11)	0.0095 (10)	0.0207 (12)	0.0012 (8)	0.0021 (18)	0.0014 (17)
O4-1	0.0116 (12)	0.0354 (17)	0.0105 (14)	0.0012 (11)	−0.0012 (11)	−0.0082 (12)
O4-2	0.0149 (13)	0.0331 (18)	0.0095 (15)	0.0004 (11)	−0.0007 (10)	−0.0031 (12)
O4-3	0.0160 (13)	0.0324 (18)	0.0095 (15)	−0.0023 (10)	0.0025 (10)	−0.0073 (12)
O4-4	0.0165 (14)	0.0301 (18)	0.0128 (16)	0.0036 (10)	−0.0006 (10)	−0.0075 (12)

Geometric parameters (Å, º)

K-1—O2-5^i	2.756 (3)	B-2—O4-2	1.384 (5)
K-1—O4-4^ii	2.825 (3)	B-2—K-2^viii	3.242 (4)
K-1—O1-4^ii	2.853 (3)	B-2—K-3^viii	3.398 (4)
K-1—O1-8^iii	2.859 (3)	B-3—O1-1^vii	1.340 (5)
K-1—O1-7^iii	2.999 (3)	B-3—O2-3	1.359 (5)
K-1—O4-3^ii	3.043 (3)	B-3—O4-3	1.407 (4)
K-1—B-5^i	3.199 (4)	B-3—K-3^viii	3.426 (4)
K-1—O3-4^ii	3.262 (2)	B-3—K-2^vii	3.470 (4)
K-1—O2-8^iii	3.342 (3)	B-4—O2-4	1.335 (5)
K-1—O2-1^iv	3.404 (3)	B-4—O1-8^xi	1.346 (5)
K-1—B-8^iii	3.572 (4)	B-4—O4-4	1.392 (4)
K-1—Nb-4^ii	3.8311 (10)	B-4—K-4^xii	3.559 (4)
K-2—O2-2^iv	2.817 (3)	B-5—O2-5	1.354 (5)
K-2—O4-3^ii	2.848 (3)	B-5—O1-7^xi	1.354 (5)
K-2—O1-7^iii	2.859 (3)	B-5—O4-1^xiii	1.383 (5)
K-2—O1-3^ii	2.920 (3)	B-5—K-1^xiv	3.199 (4)
K-2—O4-2^ii	3.018 (3)	B-5—K-2^xiv	3.516 (4)
K-2—O2-3^ii	3.096 (3)	B-6—O2-6	1.339 (5)
K-2—O1-2^ii	3.101 (3)	B-6—O1-6^xi	1.350 (5)
K-2—B-2^iv	3.242 (4)	B-6—O4-2^xiii	1.404 (5)
K-2—O2-6^i	3.288 (3)	B-6—K-3^xii	3.512 (4)
K-2—O3-3^v	3.385 (3)	B-6—K-2^xii	3.555 (4)
K-2—B-3^ii	3.470 (4)	B-7—O1-5^xi	1.345 (5)
K-2—B-5^i	3.516 (4)	B-7—O2-7	1.345 (5)
K-3—O1-2^ii	2.853 (3)	B-7—O4-3^xiii	1.398 (5)
K-3—O1-6^iii	2.859 (3)	B-7—K-4^xiv	3.403 (4)
K-3—O4-2^ii	2.904 (3)	B-7—K-3^xiv	3.522 (4)
K-3—O2-7^i	2.957 (3)	B-8—O1-4^xi	1.339 (5)
K-3—O2-3^iv	3.029 (3)	B-8—O2-8	1.353 (5)
K-3—O2-6^iii	3.106 (3)	B-8—O4-4^xiii	1.395 (5)
K-3—O4-1^ii	3.111 (3)	B-8—K-4^xiv	3.285 (4)
K-3—O1-1^ii	3.176 (3)	B-8—K-1^xii	3.572 (4)
K-3—O2-2^iv	3.313 (3)	O1-1—B-3^ii	1.340 (5)
K-3—B-2^iv	3.398 (4)	O1-1—K-4^vii	2.803 (3)
K-3—B-3^iv	3.426 (4)	O1-1—K-3^vii	3.176 (3)
K-3—B-1^ii	3.478 (4)	O1-2—B-2^ii	1.344 (5)
K-4—O1-5^iii	2.774 (3)	O1-2—K-3^vii	2.853 (3)
K-4—O1-1^ii	2.803 (3)	O1-2—K-2^vii	3.101 (3)
K-4—O2-8^i	2.871 (3)	O1-3—B-1^ii	1.345 (5)
K-4—O4-1^ii	2.919 (3)	O1-3—K-2^vii	2.920 (3)
K-4—O1-4^iii	3.034 (3)	O1-4—B-8^xv	1.339 (5)
K-4—O4-4^iii	3.117 (3)	O1-4—K-1^vii	2.853 (3)
K-4—O2-4^iv	3.143 (3)	O1-4—K-4^xii	3.034 (3)
K-4—O2-7^i	3.249 (3)	O1-5—B-7^xv	1.345 (5)
K-4—O2-1^ii	3.275 (3)	O1-5—Nb-1^x	1.967 (3)
K-4—B-8^i	3.285 (4)	O1-5—K-4^xii	2.774 (3)
K-4—B-7^i	3.403 (4)	O1-6—B-6^xv	1.350 (5)
K-4—O3-1^ii	3.418 (3)	O1-6—Nb-2^x	2.010 (3)
Nb-1—O3-1	1.769 (2)	O1-6—K-3^xii	2.859 (3)
Nb-1—O2-1	1.924 (3)	O1-7—B-5^xv	1.354 (5)
Nb-1—O2-5^vi	1.944 (3)	O1-7—Nb-3^x	2.023 (3)
Nb-1—O1-5^vi	1.967 (3)	O1-7—K-2^xii	2.859 (3)
Nb-1—O1-1	2.031 (3)	O1-7—K-1^xii	2.999 (3)
Nb-1—O3-2	2.201 (2)	O1-8—B-4^xv	1.346 (5)
Nb-1—K-4^vii	3.7660 (10)	O1-8—Nb-4^x	1.962 (3)
Nb-1—K-1^viii	3.8795 (13)	O1-8—K-1^xii	2.859 (3)
Nb-1—K-4^ix	4.1572 (10)	O2-1—K-4^vii	3.275 (3)
Nb-2—O3-2	1.755 (2)	O2-1—K-1^viii	3.404 (3)
Nb-2—O2-2	1.946 (3)	O2-2—K-2^viii	2.817 (3)
Nb-2—O2-6^vi	1.951 (3)	O2-2—K-3^viii	3.313 (3)
Nb-2—O1-2	1.991 (3)	O2-3—K-3^viii	3.029 (3)
Nb-2—O1-6^vi	2.010 (3)	O2-3—K-2^vii	3.096 (3)
Nb-2—O3-3	2.208 (2)	O2-4—K-4^viii	3.143 (3)
Nb-2—K-2^viii	3.8687 (13)	O2-5—Nb-1^x	1.944 (3)
Nb-2—K-3^ix	3.8723 (11)	O2-5—K-1^xiv	2.756 (3)
Nb-2—K-3^vii	4.0887 (11)	O2-6—Nb-2^x	1.951 (3)
Nb-3—O3-3	1.770 (2)	O2-6—K-3^xii	3.106 (3)
Nb-3—O2-7^vi	1.949 (3)	O2-6—K-2^xiv	3.288 (3)
Nb-3—O2-3	1.963 (3)	O2-7—Nb-3^x	1.949 (3)
Nb-3—O1-3	1.984 (3)	O2-7—K-3^xiv	2.957 (3)
Nb-3—O1-7^vi	2.023 (3)	O2-7—K-4^xiv	3.249 (3)
Nb-3—O3-4	2.2223 (19)	O2-8—Nb-4^x	1.955 (3)
Nb-3—K-3^viii	3.7480 (13)	O2-8—K-4^xiv	2.871 (3)
Nb-3—K-2^ix	3.9617 (11)	O2-8—K-1^xii	3.342 (3)
Nb-3—K-2^vii	3.9831 (11)	O3-1—Nb-4^vi	2.212 (2)
Nb-4—O3-4	1.7740 (19)	O3-1—K-4^vii	3.418 (3)
Nb-4—O2-4	1.938 (3)	O3-3—K-2^ix	3.385 (3)
Nb-4—O2-8^vi	1.955 (3)	O3-4—K-1^vii	3.262 (2)
Nb-4—O1-8^vi	1.962 (3)	O4-1—B-5^xvi	1.383 (5)
Nb-4—O1-4	2.041 (3)	O4-1—K-4^vii	2.919 (3)
Nb-4—O3-1^x	2.212 (2)	O4-1—K-3^vii	3.111 (3)
Nb-4—K-4^viii	3.7782 (13)	O4-2—B-6^xvi	1.404 (5)
Nb-4—K-1^vii	3.8311 (10)	O4-2—K-3^vii	2.904 (3)
Nb-4—K-1^ix	4.0692 (11)	O4-2—K-2^vii	3.018 (3)
B-1—O2-1	1.329 (5)	O4-3—B-7^xvi	1.398 (5)
B-1—O1-3^vii	1.345 (5)	O4-3—K-2^vii	2.848 (3)
B-1—O4-1	1.396 (4)	O4-3—K-1^vii	3.043 (3)
B-1—K-3^vii	3.478 (4)	O4-4—B-8^xvi	1.395 (5)
B-2—O1-2^vii	1.344 (5)	O4-4—K-1^vii	2.825 (3)
B-2—O2-2	1.355 (5)	O4-4—K-4^xii	3.117 (3)
O2-5^i—K-1—O4-4^ii	154.54 (9)	O1-1—Nb-1—K-4^ix	116.50 (8)
O2-5^i—K-1—O1-4^ii	114.91 (10)	O3-2—Nb-1—K-4^ix	101.58 (7)
O4-4^ii—K-1—O1-4^ii	76.16 (8)	K-4^vii—Nb-1—K-4^ix	134.40 (3)
O2-5^i—K-1—O1-8^iii	70.44 (9)	K-1^viii—Nb-1—K-4^ix	94.71 (2)
O4-4^ii—K-1—O1-8^iii	84.17 (8)	O3-2—Nb-2—O2-2	98.27 (16)
O1-4^ii—K-1—O1-8^iii	112.75 (9)	O3-2—Nb-2—O2-6^vi	94.58 (13)
O2-5^i—K-1—O1-7^iii	47.92 (7)	O2-2—Nb-2—O2-6^vi	92.41 (12)
O4-4^ii—K-1—O1-7^iii	120.44 (8)	O3-2—Nb-2—O1-2	97.07 (14)
O1-4^ii—K-1—O1-7^iii	162.63 (9)	O2-2—Nb-2—O1-2	88.67 (12)
O1-8^iii—K-1—O1-7^iii	67.23 (8)	O2-6^vi—Nb-2—O1-2	168.02 (11)
O2-5^i—K-1—O4-3^ii	104.89 (9)	O3-2—Nb-2—O1-6^vi	98.50 (16)
O4-4^ii—K-1—O4-3^ii	82.98 (8)	O2-2—Nb-2—O1-6^vi	162.65 (12)
O1-4^ii—K-1—O4-3^ii	126.58 (8)	O2-6^vi—Nb-2—O1-6^vi	90.65 (11)
O1-8^iii—K-1—O4-3^ii	113.27 (8)	O1-2—Nb-2—O1-6^vi	84.89 (12)
O1-7^iii—K-1—O4-3^ii	64.70 (7)	O3-2—Nb-2—O3-3	177.39 (9)
O2-5^i—K-1—B-5^i	24.88 (9)	O2-2—Nb-2—O3-3	83.53 (12)
O4-4^ii—K-1—B-5^i	135.67 (9)	O2-6^vi—Nb-2—O3-3	83.43 (10)
O1-4^ii—K-1—B-5^i	138.83 (10)	O1-2—Nb-2—O3-3	84.84 (12)
O1-8^iii—K-1—B-5^i	59.69 (9)	O1-6^vi—Nb-2—O3-3	79.86 (12)
O1-7^iii—K-1—B-5^i	24.97 (9)	O3-2—Nb-2—K-2^viii	75.05 (15)
O4-3^ii—K-1—B-5^i	88.47 (9)	O2-2—Nb-2—K-2^viii	44.06 (9)
O2-5^i—K-1—O3-4^ii	120.59 (10)	O2-6^vi—Nb-2—K-2^viii	58.17 (8)
O4-4^ii—K-1—O3-4^ii	84.77 (8)	O1-2—Nb-2—K-2^viii	127.95 (8)
O1-4^ii—K-1—O3-4^ii	55.33 (7)	O1-6^vi—Nb-2—K-2^viii	146.78 (8)
O1-8^iii—K-1—O3-4^ii	165.57 (8)	O3-3—Nb-2—K-2^viii	105.18 (11)
O1-7^iii—K-1—O3-4^ii	126.75 (7)	O3-2—Nb-2—K-3^ix	77.81 (9)
O4-3^ii—K-1—O3-4^ii	74.42 (7)	O2-2—Nb-2—K-3^ix	143.78 (9)
B-5^i—K-1—O3-4^ii	134.27 (9)	O2-6^vi—Nb-2—K-3^ix	52.72 (8)
O2-5^i—K-1—O2-8^iii	114.61 (8)	O1-2—Nb-2—K-3^ix	127.51 (8)
O4-4^ii—K-1—O2-8^iii	43.29 (7)	O1-6^vi—Nb-2—K-3^ix	45.77 (8)
O1-4^ii—K-1—O2-8^iii	115.34 (8)	O3-3—Nb-2—K-3^ix	99.62 (6)
O1-8^iii—K-1—O2-8^iii	53.12 (6)	K-2^viii—Nb-2—K-3^ix	101.51 (2)
O1-7^iii—K-1—O2-8^iii	79.18 (7)	O3-2—Nb-2—K-3^vii	64.98 (8)
O4-3^ii—K-1—O2-8^iii	74.52 (7)	O2-2—Nb-2—K-3^vii	72.13 (9)
B-5^i—K-1—O2-8^iii	92.52 (9)	O2-6^vi—Nb-2—K-3^vii	151.22 (8)
O3-4^ii—K-1—O2-8^iii	121.56 (10)	O1-2—Nb-2—K-3^vii	39.63 (8)
O2-5^i—K-1—O2-1^iv	52.27 (9)	O1-6^vi—Nb-2—K-3^vii	111.43 (8)
O4-4^ii—K-1—O2-1^iv	149.89 (8)	O3-3—Nb-2—K-3^vii	117.48 (6)
O1-4^ii—K-1—O2-1^iv	75.87 (8)	K-2^viii—Nb-2—K-3^vii	95.53 (2)
O1-8^iii—K-1—O2-1^iv	117.07 (9)	K-3^ix—Nb-2—K-3^vii	133.16 (3)
O1-7^iii—K-1—O2-1^iv	88.64 (8)	O3-3—Nb-3—O2-7^vi	96.67 (14)
O4-3^ii—K-1—O2-1^iv	105.17 (8)	O3-3—Nb-3—O2-3	95.29 (12)
B-5^i—K-1—O2-1^iv	74.19 (9)	O2-7^vi—Nb-3—O2-3	93.69 (12)
O3-4^ii—K-1—O2-1^iv	70.22 (8)	O3-3—Nb-3—O1-3	98.23 (14)
O2-8^iii—K-1—O2-1^iv	166.69 (8)	O2-7^vi—Nb-3—O1-3	164.05 (11)
O2-5^i—K-1—B-8^iii	136.54 (10)	O2-3—Nb-3—O1-3	90.58 (11)
O4-4^ii—K-1—B-8^iii	21.38 (8)	O3-3—Nb-3—O1-7^vi	96.62 (13)
O1-4^ii—K-1—B-8^iii	96.57 (9)	O2-7^vi—Nb-3—O1-7^vi	88.01 (11)
O1-8^iii—K-1—B-8^iii	70.04 (9)	O2-3—Nb-3—O1-7^vi	167.69 (10)
O1-7^iii—K-1—B-8^iii	99.47 (9)	O1-3—Nb-3—O1-7^vi	84.66 (11)
O4-3^ii—K-1—B-8^iii	75.29 (9)	O3-3—Nb-3—O3-4	177.77 (15)
B-5^i—K-1—B-8^iii	114.73 (9)	O2-7^vi—Nb-3—O3-4	83.25 (11)
O3-4^ii—K-1—B-8^iii	101.63 (10)	O2-3—Nb-3—O3-4	82.49 (10)
O2-8^iii—K-1—B-8^iii	22.25 (8)	O1-3—Nb-3—O3-4	82.07 (12)
O2-1^iv—K-1—B-8^iii	171.06 (8)	O1-7^vi—Nb-3—O3-4	85.61 (10)
O2-5^i—K-1—Nb-4^ii	132.37 (8)	O3-3—Nb-3—K-3^viii	71.55 (14)
O4-4^ii—K-1—Nb-4^ii	69.23 (5)	O2-7^vi—Nb-3—K-3^viii	51.46 (8)
O1-4^ii—K-1—Nb-4^ii	31.43 (6)	O2-3—Nb-3—K-3^viii	53.64 (8)
O1-8^iii—K-1—Nb-4^ii	138.34 (7)	O1-3—Nb-3—K-3^viii	140.02 (8)
O1-7^iii—K-1—Nb-4^ii	154.22 (6)	O1-7^vi—Nb-3—K-3^viii	133.99 (7)
O4-3^ii—K-1—Nb-4^ii	95.17 (5)	O3-4—Nb-3—K-3^viii	106.80 (10)
B-5^i—K-1—Nb-4^ii	155.08 (8)	O3-3—Nb-3—K-2^ix	58.29 (8)
O3-4^ii—K-1—Nb-4^ii	27.50 (3)	O2-7^vi—Nb-3—K-2^ix	74.45 (8)
O2-8^iii—K-1—Nb-4^ii	112.23 (6)	O2-3—Nb-3—K-2^ix	148.37 (7)
O2-1^iv—K-1—Nb-4^ii	81.08 (5)	O1-3—Nb-3—K-2^ix	108.93 (8)
B-8^iii—K-1—Nb-4^ii	89.98 (7)	O1-7^vi—Nb-3—K-2^ix	43.56 (8)
O2-2^iv—K-2—O4-3^ii	162.30 (9)	O3-4—Nb-3—K-2^ix	123.73 (6)
O2-2^iv—K-2—O1-7^iii	120.54 (9)	K-3^viii—Nb-3—K-2^ix	98.28 (2)
O4-3^ii—K-2—O1-7^iii	69.01 (8)	O3-3—Nb-3—K-2^vii	85.36 (8)
O2-2^iv—K-2—O1-3^ii	74.52 (9)	O2-7^vi—Nb-3—K-2^vii	143.14 (8)
O4-3^ii—K-2—O1-3^ii	88.23 (8)	O2-3—Nb-3—K-2^vii	49.60 (8)
O1-7^iii—K-2—O1-3^ii	110.83 (8)	O1-3—Nb-3—K-2^vii	44.49 (8)
O2-2^iv—K-2—O4-2^ii	99.78 (9)	O1-7^vi—Nb-3—K-2^vii	128.47 (7)
O4-3^ii—K-2—O4-2^ii	83.44 (8)	O3-4—Nb-3—K-2^vii	93.36 (6)
O1-7^iii—K-2—O4-2^ii	125.69 (8)	K-3^viii—Nb-3—K-2^vii	95.58 (2)
O1-3^ii—K-2—O4-2^ii	114.15 (7)	K-2^ix—Nb-3—K-2^vii	133.72 (3)
O2-2^iv—K-2—O2-3^ii	117.85 (8)	O3-4—Nb-4—O2-4	96.89 (14)
O4-3^ii—K-2—O2-3^ii	46.10 (7)	O3-4—Nb-4—O2-8^vi	97.17 (13)
O1-7^iii—K-2—O2-3^ii	110.86 (8)	O2-4—Nb-4—O2-8^vi	93.10 (13)
O1-3^ii—K-2—O2-3^ii	55.51 (6)	O3-4—Nb-4—O1-8^vi	96.91 (14)
O4-2^ii—K-2—O2-3^ii	73.75 (7)	O2-4—Nb-4—O1-8^vi	164.79 (12)
O2-2^iv—K-2—O1-2^ii	46.04 (7)	O2-8^vi—Nb-4—O1-8^vi	91.51 (11)
O4-3^ii—K-2—O1-2^ii	124.06 (8)	O3-4—Nb-4—O1-4	96.97 (14)
O1-7^iii—K-2—O1-2^ii	166.54 (10)	O2-4—Nb-4—O1-4	87.71 (9)
O1-3^ii—K-2—O1-2^ii	69.17 (8)	O2-8^vi—Nb-4—O1-4	165.63 (11)
O4-2^ii—K-2—O1-2^ii	63.23 (7)	O1-8^vi—Nb-4—O1-4	84.28 (12)
O2-3^ii—K-2—O1-2^ii	80.59 (7)	O3-4—Nb-4—O3-1^x	179.09 (17)
O2-2^iv—K-2—B-2^iv	24.58 (9)	O2-4—Nb-4—O3-1^x	84.01 (12)
O4-3^ii—K-2—B-2^iv	140.51 (9)	O2-8^vi—Nb-4—O3-1^x	82.87 (11)
O1-7^iii—K-2—B-2^iv	143.08 (10)	O1-8^vi—Nb-4—O3-1^x	82.19 (12)
O1-3^ii—K-2—B-2^iv	61.78 (9)	O1-4—Nb-4—O3-1^x	82.95 (12)
O4-2^ii—K-2—B-2^iv	86.25 (10)	O3-4—Nb-4—K-4^viii	73.46 (13)
O2-3^ii—K-2—B-2^iv	94.44 (9)	O2-4—Nb-4—K-4^viii	56.17 (9)
O1-2^ii—K-2—B-2^iv	24.34 (9)	O2-8^vi—Nb-4—K-4^viii	48.18 (9)
O2-2^iv—K-2—O2-6^i	54.21 (8)	O1-8^vi—Nb-4—K-4^viii	134.82 (8)
O4-3^ii—K-2—O2-6^i	140.43 (7)	O1-4—Nb-4—K-4^viii	139.91 (8)
O1-7^iii—K-2—O2-6^i	72.56 (7)	O3-1^x—Nb-4—K-4^viii	107.17 (11)
O1-3^ii—K-2—O2-6^i	114.37 (9)	O3-4—Nb-4—K-1^vii	58.09 (8)
O4-2^ii—K-2—O2-6^i	112.53 (8)	O2-4—Nb-4—K-1^vii	69.99 (9)
O2-3^ii—K-2—O2-6^i	169.82 (8)	O2-8^vi—Nb-4—K-1^vii	146.19 (8)
O1-2^ii—K-2—O2-6^i	94.97 (8)	O1-8^vi—Nb-4—K-1^vii	112.58 (9)
B-2^iv—K-2—O2-6^i	78.38 (9)	O1-4—Nb-4—K-1^vii	46.80 (8)
O2-2^iv—K-2—O3-3^v	118.36 (9)	O3-1^x—Nb-4—K-1^vii	122.26 (7)
O4-3^ii—K-2—O3-3^v	79.34 (8)	K-4^viii—Nb-4—K-1^vii	99.53 (2)
O1-7^iii—K-2—O3-3^v	53.25 (7)	O3-4—Nb-4—K-1^ix	86.59 (7)
O1-3^ii—K-2—O3-3^v	162.56 (7)	O2-4—Nb-4—K-1^ix	147.68 (9)
O4-2^ii—K-2—O3-3^v	76.80 (8)	O2-8^vi—Nb-4—K-1^ix	54.63 (9)
O2-3^ii—K-2—O3-3^v	119.60 (10)	O1-8^vi—Nb-4—K-1^ix	39.98 (9)
O1-2^ii—K-2—O3-3^v	128.08 (7)	O1-4—Nb-4—K-1^ix	123.89 (8)
B-2^iv—K-2—O3-3^v	134.66 (9)	O3-1^x—Nb-4—K-1^ix	92.70 (6)
O2-6^i—K-2—O3-3^v	70.33 (8)	K-4^viii—Nb-4—K-1^ix	94.87 (2)
O2-2^iv—K-2—B-3^ii	140.67 (9)	K-1^vii—Nb-4—K-1^ix	135.23 (3)
O4-3^ii—K-2—B-3^ii	23.17 (8)	O2-1—B-1—O1-3^vii	122.6 (3)
O1-7^iii—K-2—B-3^ii	90.54 (9)	O2-1—B-1—O4-1	115.0 (3)
O1-3^ii—K-2—B-3^ii	71.88 (9)	O1-3^vii—B-1—O4-1	122.5 (3)
O4-2^ii—K-2—B-3^ii	76.37 (9)	O2-1—B-1—K-3^vii	88.4 (2)
O2-3^ii—K-2—B-3^ii	22.99 (8)	O1-3^vii—B-1—K-3^vii	116.1 (2)
O1-2^ii—K-2—B-3^ii	101.94 (9)	O4-1—B-1—K-3^vii	63.26 (18)
B-2^iv—K-2—B-3^ii	117.41 (9)	O1-2^vii—B-2—O2-2	119.3 (4)
O2-6^i—K-2—B-3^ii	163.08 (8)	O1-2^vii—B-2—O4-2	122.4 (3)
O3-3^v—K-2—B-3^ii	99.13 (10)	O2-2—B-2—O4-2	118.3 (4)
O2-2^iv—K-2—B-5^i	100.67 (10)	O1-2^vii—B-2—K-2^viii	71.9 (2)
O4-3^ii—K-2—B-5^i	85.71 (9)	O2-2—B-2—K-2^viii	59.9 (2)
O1-7^iii—K-2—B-5^i	21.51 (8)	O4-2—B-2—K-2^viii	141.6 (3)
O1-3^ii—K-2—B-5^i	99.01 (9)	O1-2^vii—B-2—K-3^viii	55.2 (2)
O4-2^ii—K-2—B-5^i	144.62 (8)	O2-2—B-2—K-3^viii	74.9 (2)
O2-3^ii—K-2—B-5^i	119.91 (9)	O4-2—B-2—K-3^viii	147.3 (3)
O1-2^ii—K-2—B-5^i	146.04 (9)	K-2^viii—B-2—K-3^viii	71.05 (9)
B-2^iv—K-2—B-5^i	121.83 (11)	O1-1^vii—B-3—O2-3	122.3 (3)
O2-6^i—K-2—B-5^i	59.95 (8)	O1-1^vii—B-3—O4-3	122.2 (3)
O3-3^v—K-2—B-5^i	68.12 (8)	O2-3—B-3—O4-3	115.4 (3)
B-3^ii—K-2—B-5^i	104.22 (10)	O1-1^vii—B-3—K-3^viii	67.93 (19)
O1-2^ii—K-3—O1-6^iii	109.89 (9)	O2-3—B-3—K-3^viii	61.74 (19)
O1-2^ii—K-3—O4-2^ii	67.72 (8)	O4-3—B-3—K-3^viii	148.6 (2)
O1-6^iii—K-3—O4-2^ii	86.76 (8)	O1-1^vii—B-3—K-2^vii	171.3 (3)
O1-2^ii—K-3—O2-7^i	128.39 (9)	O2-3—B-3—K-2^vii	62.86 (19)
O1-6^iii—K-3—O2-7^i	77.80 (8)	O4-3—B-3—K-2^vii	52.79 (17)
O4-2^ii—K-3—O2-7^i	160.74 (8)	K-3^viii—B-3—K-2^vii	112.34 (11)
O1-2^ii—K-3—O2-3^iv	74.51 (7)	O2-4—B-4—O1-8^xi	120.8 (3)
O1-6^iii—K-3—O2-3^iv	113.29 (9)	O2-4—B-4—O4-4	118.3 (3)
O4-2^ii—K-3—O2-3^iv	141.56 (7)	O1-8^xi—B-4—O4-4	120.9 (3)
O2-7^i—K-3—O2-3^iv	56.94 (8)	O2-4—B-4—K-4^xii	93.5 (2)
O1-2^ii—K-3—O2-6^iii	109.39 (8)	O1-8^xi—B-4—K-4^xii	115.0 (2)
O1-6^iii—K-3—O2-6^iii	56.18 (7)	O4-4—B-4—K-4^xii	60.47 (19)
O4-2^ii—K-3—O2-6^iii	45.12 (7)	O2-5—B-5—O1-7^xi	120.2 (3)
O2-7^i—K-3—O2-6^iii	115.72 (7)	O2-5—B-5—O4-1^xiii	117.3 (3)
O2-3^iv—K-3—O2-6^iii	169.36 (8)	O1-7^xi—B-5—O4-1^xiii	122.5 (3)
O1-2^ii—K-3—O4-1^ii	124.21 (8)	O2-5—B-5—K-1^xiv	58.9 (2)
O1-6^iii—K-3—O4-1^ii	113.21 (8)	O1-7^xi—B-5—K-1^xiv	69.2 (2)
O4-2^ii—K-3—O4-1^ii	81.01 (8)	O4-1^xiii—B-5—K-1^xiv	149.1 (3)
O2-7^i—K-3—O4-1^ii	94.45 (8)	O2-5—B-5—K-2^xiv	84.4 (2)
O2-3^iv—K-3—O4-1^ii	116.28 (8)	O1-7^xi—B-5—K-2^xiv	50.74 (18)
O2-6^iii—K-3—O4-1^ii	70.27 (7)	O4-1^xiii—B-5—K-2^xiv	139.4 (3)
O1-2^ii—K-3—O1-1^ii	83.30 (7)	K-1^xiv—B-5—K-2^xiv	71.21 (8)
O1-6^iii—K-3—O1-1^ii	151.87 (9)	O2-6—B-6—O1-6^xi	123.5 (3)
O4-2^ii—K-3—O1-1^ii	121.37 (8)	O2-6—B-6—O4-2^xiii	115.0 (3)
O2-7^i—K-3—O1-1^ii	74.70 (8)	O1-6^xi—B-6—O4-2^xiii	121.5 (3)
O2-3^iv—K-3—O1-1^ii	44.70 (7)	O2-6—B-6—K-3^xii	61.57 (19)
O2-6^iii—K-3—O1-1^ii	144.28 (8)	O1-6^xi—B-6—K-3^xii	174.5 (3)
O4-1^ii—K-3—O1-1^ii	75.04 (7)	O4-2^xiii—B-6—K-3^xii	53.46 (18)
O1-2^ii—K-3—O2-2^iv	43.59 (7)	O2-6—B-6—K-2^xii	96.2 (2)
O1-6^iii—K-3—O2-2^iv	75.74 (8)	O1-6^xi—B-6—K-2^xii	113.8 (2)
O4-2^ii—K-3—O2-2^iv	91.56 (8)	O4-2^xiii—B-6—K-2^xii	56.58 (19)
O2-7^i—K-3—O2-2^iv	95.66 (9)	K-3^xii—B-6—K-2^xii	66.22 (8)
O2-3^iv—K-3—O2-2^iv	64.50 (8)	O1-5^xi—B-7—O2-7	119.6 (4)
O2-6^iii—K-3—O2-2^iv	111.06 (8)	O1-5^xi—B-7—O4-3^xiii	121.5 (4)
O4-1^ii—K-3—O2-2^iv	167.79 (8)	O2-7—B-7—O4-3^xiii	118.9 (3)
O1-1^ii—K-3—O2-2^iv	101.09 (7)	O1-5^xi—B-7—K-4^xiv	51.5 (2)
O1-2^ii—K-3—B-2^iv	22.76 (9)	O2-7—B-7—K-4^xiv	72.0 (2)
O1-6^iii—K-3—B-2^iv	97.71 (9)	O4-3^xiii—B-7—K-4^xiv	159.8 (3)
O4-2^ii—K-3—B-2^iv	85.24 (9)	O1-5^xi—B-7—K-3^xiv	83.3 (2)
O2-7^i—K-3—B-2^iv	107.99 (10)	O2-7—B-7—K-3^xiv	54.72 (19)
O2-3^iv—K-3—B-2^iv	60.66 (9)	O4-3^xiii—B-7—K-3^xiv	131.7 (3)
O2-6^iii—K-3—B-2^iv	119.41 (9)	K-4^xiv—B-7—K-3^xiv	68.47 (8)
O4-1^ii—K-3—B-2^iv	145.14 (9)	O1-4^xi—B-8—O2-8	121.9 (4)
O1-1^ii—K-3—B-2^iv	85.35 (9)	O1-4^xi—B-8—O4-4^xiii	122.5 (3)
O2-2^iv—K-3—B-2^iv	23.25 (8)	O2-8—B-8—O4-4^xiii	115.5 (3)
O1-2^ii—K-3—B-3^iv	72.02 (9)	O1-4^xi—B-8—K-4^xiv	67.4 (2)
O1-6^iii—K-3—B-3^iv	136.40 (10)	O2-8—B-8—K-4^xiv	60.50 (19)
O4-2^ii—K-3—B-3^iv	129.31 (9)	O4-4^xiii—B-8—K-4^xiv	151.7 (3)
O2-7^i—K-3—B-3^iv	69.74 (9)	O1-4^xi—B-8—K-1^xii	163.5 (3)
O2-3^iv—K-3—B-3^iv	23.27 (8)	O2-8—B-8—K-1^xii	69.3 (2)
O2-6^iii—K-3—B-3^iv	166.86 (9)	O4-4^xiii—B-8—K-1^xii	47.56 (18)
O4-1^ii—K-3—B-3^iv	97.90 (9)	K-4^xiv—B-8—K-1^xii	114.92 (11)
O1-1^ii—K-3—B-3^iv	23.02 (8)	B-3^ii—O1-1—Nb-1	128.7 (2)
O2-2^iv—K-3—B-3^iv	79.27 (9)	B-3^ii—O1-1—K-4^vii	128.2 (2)
B-2^iv—K-3—B-3^iv	67.05 (10)	Nb-1—O1-1—K-4^vii	101.16 (11)
O1-2^ii—K-3—B-1^ii	100.66 (9)	B-3^ii—O1-1—K-3^vii	89.1 (2)
O1-6^iii—K-3—B-1^ii	130.85 (9)	Nb-1—O1-1—K-3^vii	114.51 (11)
O4-2^ii—K-3—B-1^ii	70.12 (9)	K-4^vii—O1-1—K-3^vii	81.10 (7)
O2-7^i—K-3—B-1^ii	111.79 (9)	B-2^ii—O1-2—Nb-2	132.9 (3)
O2-3^iv—K-3—B-1^ii	111.43 (9)	B-2^ii—O1-2—K-3^vii	102.0 (2)
O2-6^iii—K-3—B-1^ii	77.99 (9)	Nb-2—O1-2—K-3^vii	113.94 (12)
O4-1^ii—K-3—B-1^ii	23.62 (8)	B-2^ii—O1-2—K-2^vii	83.7 (2)
O1-1^ii—K-3—B-1^ii	66.73 (8)	Nb-2—O1-2—K-2^vii	129.81 (12)
O2-2^iv—K-3—B-1^ii	144.23 (9)	K-3^vii—O1-2—K-2^vii	80.72 (7)
B-2^iv—K-3—B-1^ii	121.66 (10)	B-1^ii—O1-3—Nb-3	128.0 (2)
B-3^iv—K-3—B-1^ii	88.89 (9)	B-1^ii—O1-3—K-2^vii	122.8 (2)
O1-5^iii—K-4—O1-1^ii	112.89 (10)	Nb-3—O1-3—K-2^vii	107.07 (11)
O1-5^iii—K-4—O2-8^i	69.42 (9)	B-8^xv—O1-4—Nb-4	130.0 (3)
O1-1^ii—K-4—O2-8^i	113.08 (9)	B-8^xv—O1-4—K-1^vii	119.7 (2)
O1-5^iii—K-4—O4-1^ii	73.42 (8)	Nb-4—O1-4—K-1^vii	101.77 (11)
O1-1^ii—K-4—O4-1^ii	83.99 (8)	B-8^xv—O1-4—K-4^xii	88.5 (2)
O2-8^i—K-4—O4-1^ii	142.72 (8)	Nb-4—O1-4—K-4^xii	125.26 (12)
O1-5^iii—K-4—O1-4^iii	72.09 (9)	K-1^vii—O1-4—K-4^xii	83.17 (7)
O1-1^ii—K-4—O1-4^iii	157.88 (10)	B-7^xv—O1-5—Nb-1^x	132.2 (3)
O2-8^i—K-4—O1-4^iii	46.88 (7)	B-7^xv—O1-5—K-4^xii	106.2 (2)
O4-1^ii—K-4—O1-4^iii	117.59 (8)	Nb-1^x—O1-5—K-4^xii	121.62 (13)
O1-5^iii—K-4—O4-4^iii	116.50 (8)	B-6^xv—O1-6—Nb-2^x	128.0 (2)
O1-1^ii—K-4—O4-4^iii	121.75 (8)	B-6^xv—O1-6—K-3^xii	128.0 (2)
O2-8^i—K-4—O4-4^iii	111.68 (8)	Nb-2^x—O1-6—K-3^xii	103.99 (11)
O4-1^ii—K-4—O4-4^iii	82.27 (8)	B-5^xv—O1-7—Nb-3^x	131.5 (2)
O1-4^iii—K-4—O4-4^iii	69.39 (8)	B-5^xv—O1-7—K-2^xii	107.7 (2)
O1-5^iii—K-4—O2-4^iv	123.07 (9)	Nb-3^x—O1-7—K-2^xii	107.25 (11)
O1-1^ii—K-4—O2-4^iv	78.51 (8)	B-5^xv—O1-7—K-1^xii	85.8 (2)
O2-8^i—K-4—O2-4^iv	55.85 (9)	Nb-3^x—O1-7—K-1^xii	130.31 (12)
O4-1^ii—K-4—O2-4^iv	159.67 (8)	K-2^xii—O1-7—K-1^xii	83.93 (7)
O1-4^iii—K-4—O2-4^iv	81.00 (9)	B-4^xv—O1-8—Nb-4^x	129.7 (3)
O4-4^iii—K-4—O2-4^iv	98.18 (8)	B-4^xv—O1-8—K-1^xii	113.1 (2)
O1-5^iii—K-4—O2-7^i	44.54 (7)	Nb-4^x—O1-8—K-1^xii	113.85 (12)
O1-1^ii—K-4—O2-7^i	75.56 (8)	B-1—O2-1—Nb-1	167.4 (3)
O2-8^i—K-4—O2-7^i	62.89 (8)	B-1—O2-1—K-4^vii	93.4 (2)
O4-1^ii—K-4—O2-7^i	92.33 (8)	Nb-1—O2-1—K-4^vii	88.90 (10)
O1-4^iii—K-4—O2-7^i	97.48 (8)	B-1—O2-1—K-1^viii	99.6 (2)
O4-4^iii—K-4—O2-7^i	160.84 (7)	Nb-1—O2-1—K-1^viii	88.97 (10)
O2-4^iv—K-4—O2-7^i	93.22 (8)	K-4^vii—O2-1—K-1^viii	125.58 (10)
O1-5^iii—K-4—O2-1^ii	112.69 (9)	B-2—O2-2—Nb-2	153.2 (3)
O1-1^ii—K-4—O2-1^ii	52.86 (7)	B-2—O2-2—K-2^viii	95.6 (2)
O2-8^i—K-4—O2-1^ii	165.86 (10)	Nb-2—O2-2—K-2^viii	107.22 (12)
O4-1^ii—K-4—O2-1^ii	43.09 (7)	B-2—O2-2—K-3^viii	81.9 (2)
O1-4^iii—K-4—O2-1^ii	147.17 (9)	Nb-2—O2-2—K-3^viii	116.12 (12)
O4-4^iii—K-4—O2-1^ii	80.38 (8)	K-2^viii—O2-2—K-3^viii	77.60 (8)
O2-4^iv—K-4—O2-1^ii	116.75 (7)	B-3—O2-3—Nb-3	143.1 (2)
O2-7^i—K-4—O2-1^ii	108.10 (8)	B-3—O2-3—K-3^viii	95.0 (2)
O1-5^iii—K-4—B-8^i	63.05 (9)	Nb-3—O2-3—K-3^viii	94.90 (9)
O1-1^ii—K-4—B-8^i	137.25 (10)	B-3—O2-3—K-2^vii	94.2 (2)
O2-8^i—K-4—B-8^i	24.22 (9)	Nb-3—O2-3—K-2^vii	101.53 (11)
O4-1^ii—K-4—B-8^i	128.35 (9)	K-3^viii—O2-3—K-2^vii	138.54 (9)
O1-4^iii—K-4—B-8^i	24.05 (8)	B-4—O2-4—Nb-4	159.7 (3)
O4-4^iii—K-4—B-8^i	92.95 (9)	B-4—O2-4—K-4^viii	103.7 (2)
O2-4^iv—K-4—B-8^i	71.98 (9)	Nb-4—O2-4—K-4^viii	93.01 (11)
O2-7^i—K-4—B-8^i	75.95 (9)	B-5—O2-5—Nb-1^x	153.4 (3)
O2-1^ii—K-4—B-8^i	169.54 (10)	B-5—O2-5—K-1^xiv	96.2 (2)
O1-5^iii—K-4—B-7^i	22.31 (9)	Nb-1^x—O2-5—K-1^xiv	110.08 (13)
O1-1^ii—K-4—B-7^i	97.23 (10)	B-6—O2-6—Nb-2^x	146.9 (2)
O2-8^i—K-4—B-7^i	59.53 (9)	B-6—O2-6—K-3^xii	96.2 (2)
O4-1^ii—K-4—B-7^i	86.48 (9)	Nb-2^x—O2-6—K-3^xii	97.30 (11)
O1-4^iii—K-4—B-7^i	80.39 (9)	B-6—O2-6—K-2^xiv	97.7 (2)
O4-4^iii—K-4—B-7^i	137.67 (9)	Nb-2^x—O2-6—K-2^xiv	91.55 (9)
O2-4^iv—K-4—B-7^i	105.79 (9)	K-3^xii—O2-6—K-2^xiv	139.26 (8)
O2-7^i—K-4—B-7^i	23.18 (8)	B-7—O2-7—Nb-3^x	151.5 (3)
O2-1^ii—K-4—B-7^i	116.86 (9)	B-7—O2-7—K-3^xiv	103.5 (2)
B-8^i—K-4—B-7^i	63.27 (10)	Nb-3^x—O2-7—K-3^xiv	97.50 (10)
O1-5^iii—K-4—O3-1^ii	160.30 (9)	B-7—O2-7—K-4^xiv	84.8 (2)
O1-1^ii—K-4—O3-1^ii	53.55 (7)	Nb-3^x—O2-7—K-4^xiv	118.69 (11)
O2-8^i—K-4—O3-1^ii	127.18 (10)	K-3^xiv—O2-7—K-4^xiv	77.65 (7)
O4-1^ii—K-4—O3-1^ii	89.87 (8)	B-8—O2-8—Nb-4^x	148.7 (2)
O1-4^iii—K-4—O3-1^ii	126.26 (7)	B-8—O2-8—K-4^xiv	95.3 (2)
O4-4^iii—K-4—O3-1^ii	70.09 (7)	Nb-4^x—O2-8—K-4^xiv	101.33 (12)
O2-4^iv—K-4—O3-1^ii	71.44 (8)	B-8—O2-8—K-1^xii	88.5 (2)
O2-7^i—K-4—O3-1^ii	128.51 (8)	Nb-4^x—O2-8—K-1^xii	96.87 (11)
O2-1^ii—K-4—O3-1^ii	48.42 (7)	K-4^xiv—O2-8—K-1^xii	136.96 (9)
B-8^i—K-4—O3-1^ii	136.58 (9)	Nb-1—O3-1—Nb-4^vi	158.73 (13)
B-7^i—K-4—O3-1^ii	150.78 (9)	Nb-1—O3-1—K-4^vii	87.00 (8)
O3-1—Nb-1—O2-1	96.07 (14)	Nb-4^vi—O3-1—K-4^vii	113.88 (9)
O3-1—Nb-1—O2-5^vi	98.69 (15)	Nb-2—O3-2—Nb-1	175.8 (2)
O2-1—Nb-1—O2-5^vi	91.70 (14)	Nb-3—O3-3—Nb-2	156.05 (13)
O3-1—Nb-1—O1-5^vi	97.23 (15)	Nb-3—O3-3—K-2^ix	95.30 (9)
O2-1—Nb-1—O1-5^vi	165.51 (14)	Nb-2—O3-3—K-2^ix	106.43 (8)
O2-5^vi—Nb-1—O1-5^vi	91.95 (10)	Nb-4—O3-4—Nb-3	150.25 (11)
O3-1—Nb-1—O1-1	97.22 (15)	Nb-4—O3-4—K-1^vii	94.42 (9)
O2-1—Nb-1—O1-1	87.60 (11)	Nb-3—O3-4—K-1^vii	113.95 (8)
O2-5^vi—Nb-1—O1-1	164.06 (12)	B-5^xvi—O4-1—B-1	122.6 (3)
O1-5^vi—Nb-1—O1-1	85.06 (12)	B-5^xvi—O4-1—K-4^vii	120.4 (2)
O3-1—Nb-1—O3-2	177.26 (19)	B-1—O4-1—K-4^vii	108.2 (2)
O2-1—Nb-1—O3-2	84.09 (13)	B-5^xvi—O4-1—K-3^vii	122.0 (2)
O2-5^vi—Nb-1—O3-2	84.04 (13)	B-1—O4-1—K-3^vii	93.1 (2)
O1-5^vi—Nb-1—O3-2	82.35 (13)	K-4^vii—O4-1—K-3^vii	80.47 (7)
O1-1—Nb-1—O3-2	80.05 (12)	B-2—O4-2—B-6^xvi	122.7 (3)
O3-1—Nb-1—K-4^vii	65.02 (8)	B-2—O4-2—K-3^vii	124.9 (2)
O2-1—Nb-1—K-4^vii	60.39 (9)	B-6^xvi—O4-2—K-3^vii	103.7 (2)
O2-5^vi—Nb-1—K-4^vii	143.74 (9)	B-2—O4-2—K-2^vii	113.9 (2)
O1-5^vi—Nb-1—K-4^vii	121.04 (10)	B-6^xvi—O4-2—K-2^vii	100.6 (2)
O1-1—Nb-1—K-4^vii	46.90 (8)	K-3^vii—O4-2—K-2^vii	81.34 (8)
O3-2—Nb-1—K-4^vii	112.86 (7)	B-7^xvi—O4-3—B-3	124.3 (3)
O3-1—Nb-1—K-1^viii	74.74 (14)	B-7^xvi—O4-3—K-2^vii	126.1 (2)
O2-1—Nb-1—K-1^viii	61.31 (10)	B-3—O4-3—K-2^vii	104.0 (2)
O2-5^vi—Nb-1—K-1^viii	41.85 (9)	B-7^xvi—O4-3—K-1^vii	104.3 (2)
O1-5^vi—Nb-1—K-1^viii	128.22 (9)	B-3—O4-3—K-1^vii	104.1 (2)
O1-1—Nb-1—K-1^viii	146.10 (7)	K-2^vii—O4-3—K-1^vii	83.30 (8)
O3-2—Nb-1—K-1^viii	107.66 (12)	B-8^xvi—O4-4—B-4	123.9 (3)
K-4^vii—Nb-1—K-1^viii	101.94 (2)	B-8^xvi—O4-4—K-1^vii	111.1 (2)
O3-1—Nb-1—K-4^ix	79.39 (8)	B-4—O4-4—K-1^vii	119.4 (2)
O2-1—Nb-1—K-4^ix	155.79 (10)	B-8^xvi—O4-4—K-4^xii	113.4 (2)
O2-5^vi—Nb-1—K-4^ix	65.86 (10)	B-4—O4-4—K-4^xii	96.7 (2)
O1-5^vi—Nb-1—K-4^ix	34.63 (9)	K-1^vii—O4-4—K-4^xii	82.12 (8)

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