A pseudo-merohedrally twinned rare-earth sulfate: K₆[Ce(HSO₄)₂(SO₄)₄]·H₂O, a novel structure type

A novel structure type of an acidic rare-earth sulfate, hexa­potassium cerium dihydrogensulfate tetra­sulfate monohydrate, is reported. The crystal is twinned, mimicking tetra­gonal symmetry. The Ce^IV atom is nine-coordinate, connecting to one corner-sharing and four edge-sharing sulfate groups. One of the potassium ions is disordered over two general positions. The compound is unique as it contains rare-earth monomers, [Ce(HSO₄)(SO₄)₄]^5-. The structure is composed of these monomers, water mol­ecules, discrete hydrogensulfate ions and potassium ions held together by ionic inter­actions. There are two types of alternating layers in the structure, with compositions [K₄Ce(HSO₄)(SO₄)₄]^- and [K₂(HSO₄)(H₂O)]⁺.

Computing details

Data collection: SMART (Siemens, 1995); cell refinement: SAINT (Siemens, 1995); data reduction: SAINT and SADABS (Sheldrick, 2002); program(s) used to solve structure: SHELXTL (Bruker, 2003); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2001); software used to prepare material for publication: SHELXTL.

hexapotassium cerium dihydrogensulfate tethrasulfate monohydrate

Crystal data

K6[Ce(HSO4)2(SO4)4]·H2O	F(000) = 1880
Mr = 969.10	Dx = 2.564 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 8192 reflections
a = 11.2377 (2) Å	θ = 1.0–32.8°
b = 19.8722 (4) Å	µ = 3.41 mm^−1
c = 11.2430 (2) Å	T = 295 K
β = 90.142 (1)°	Plate, light yellow
V = 2510.75 (8) Å^3	0.36 × 0.36 × 0.07 mm
Z = 4

Data collection

Bruker SMART CCD area-detector diffractometer	8933 independent reflections
Radiation source: fine-focus sealed tube	7743 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.041
φ and ω scans	θmax = 32.8°, θmin = 1.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 2002)	h = −17→17
Tmin = 0.373, Tmax = 0.796	k = −30→29
43581 measured reflections	l = −17→16

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.033	H-atom parameters not defined
wR(F^2) = 0.089	w = 1/[σ^2(Fo^2) + (0.0464P)^2 + 3.996P] where P = (Fo^2 + 2Fc^2)/3
S = 1.01	(Δ/σ)max < 0.001
8933 reflections	Δρmax = 1.68 e Å^−3
353 parameters	Δρmin = −0.74 e Å^−3
0 restraints

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	Occ. (<1)
Ce	0.75014 (9)	0.064031 (8)	0.232910 (19)	0.01618 (5)
K1	0.93502 (14)	0.07506 (8)	0.80057 (14)	0.0326 (3)
K2	0.57187 (14)	0.07894 (7)	0.67944 (13)	0.0299 (3)
K3	0.81131 (15)	0.41926 (7)	0.56166 (12)	0.0300 (3)
K4	1.19505 (16)	0.07933 (8)	0.43179 (14)	0.0341 (3)
K5	1.10531 (16)	0.25484 (7)	0.95974 (14)	0.0403 (3)
K6A	1.0276 (2)	0.25264 (12)	0.5850 (2)	0.0318 (5)	0.50
K6B	0.9724 (2)	0.24450 (14)	0.3688 (3)	0.0344 (6)	0.50
S1	0.75229 (18)	−0.12899 (4)	0.24366 (8)	0.02206 (15)
O11	0.8637 (5)	−0.1487 (3)	0.2884 (7)	0.092 (2)
O12	0.6607 (6)	−0.1391 (3)	0.3361 (5)	0.080 (2)
O13	0.7227 (5)	−0.1684 (2)	0.1392 (3)	0.0499 (11)
O14	0.7528 (7)	−0.05769 (14)	0.2100 (4)	0.0455 (10)
S2	0.64239 (13)	0.08980 (7)	−0.01228 (11)	0.0188 (2)
O21	0.5310 (4)	0.1225 (2)	−0.0412 (4)	0.0296 (8)
O22	0.7216 (4)	0.1355 (2)	0.0598 (3)	0.0227 (7)
O23	0.7034 (5)	0.0642 (2)	−0.1173 (4)	0.0330 (11)
O24	0.6220 (4)	0.03094 (18)	0.0741 (3)	0.0235 (8)
S3	0.99851 (15)	0.09101 (7)	0.13175 (11)	0.0200 (2)
O31	1.0280 (4)	0.1243 (2)	0.0203 (4)	0.0337 (10)
O32	0.9224 (4)	0.1371 (2)	0.2097 (3)	0.0240 (8)
O33	1.1022 (5)	0.0677 (3)	0.1975 (5)	0.0335 (11)
O34	0.9142 (4)	0.03368 (18)	0.1126 (3)	0.0229 (8)
S4	0.85770 (13)	0.08670 (7)	0.47858 (10)	0.0200 (2)
O41	0.9720 (4)	0.1178 (2)	0.5009 (4)	0.0312 (9)
O42	0.8707 (4)	0.02686 (17)	0.3928 (3)	0.0233 (8)
O43	0.7753 (4)	0.1326 (2)	0.4111 (3)	0.0221 (7)
O44	0.8008 (5)	0.0622 (2)	0.5874 (4)	0.0328 (11)
S5	0.50690 (14)	0.08712 (7)	0.34547 (11)	0.0187 (2)
O51	0.4881 (4)	0.1196 (2)	0.4588 (4)	0.0322 (9)
O52	0.5740 (4)	0.1341 (2)	0.2624 (3)	0.0206 (7)
O53	0.5918 (4)	0.02902 (18)	0.3561 (3)	0.0232 (8)
O54	0.3960 (4)	0.0637 (2)	0.2915 (4)	0.0279 (10)
S6	0.7556 (2)	0.24696 (16)	0.73797 (14)	0.0455 (3)
O61	0.7299 (6)	0.2921 (3)	0.8446 (6)	0.0501 (14)
O62	0.8553 (8)	0.2033 (4)	0.7716 (8)	0.081 (2)
O63	0.6455 (6)	0.2103 (3)	0.7063 (5)	0.0493 (14)
O64	0.7880 (6)	0.2899 (3)	0.6354 (6)	0.0564 (16)
O1	0.8654 (4)	0.2533 (2)	1.0285 (4)	0.0387 (11)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ce	0.01854 (9)	0.01464 (7)	0.01537 (8)	0.00082 (13)	0.0010 (2)	−0.00053 (6)
K1	0.0305 (7)	0.0239 (6)	0.0433 (7)	0.0017 (5)	−0.0091 (6)	−0.0002 (5)
K2	0.0344 (7)	0.0229 (6)	0.0325 (6)	−0.0028 (5)	−0.0087 (5)	0.0012 (4)
K3	0.0379 (8)	0.0221 (6)	0.0300 (6)	−0.0020 (5)	0.0070 (5)	0.0010 (5)
K4	0.0368 (8)	0.0264 (6)	0.0391 (7)	0.0001 (5)	0.0120 (6)	0.0029 (5)
K5	0.0468 (8)	0.0306 (6)	0.0436 (7)	0.0074 (6)	0.0119 (6)	0.0017 (5)
K6A	0.0349 (12)	0.0230 (10)	0.0374 (12)	0.0001 (9)	−0.0074 (9)	0.0082 (9)
K6B	0.0310 (12)	0.0173 (10)	0.0548 (16)	−0.0031 (9)	0.0018 (11)	−0.0090 (9)
S1	0.0262 (5)	0.0173 (3)	0.0227 (6)	0.0013 (7)	0.0020 (6)	0.0027 (3)
O11	0.058 (4)	0.078 (4)	0.139 (6)	−0.007 (3)	−0.061 (4)	0.052 (4)
O12	0.107 (5)	0.057 (3)	0.075 (3)	0.026 (3)	0.069 (3)	0.023 (3)
O13	0.077 (3)	0.0351 (19)	0.037 (2)	−0.008 (2)	−0.002 (2)	−0.0121 (16)
O14	0.079 (3)	0.0179 (13)	0.039 (2)	−0.004 (3)	0.009 (3)	0.0005 (13)
S2	0.0198 (6)	0.0198 (5)	0.0168 (5)	0.0015 (4)	−0.0009 (4)	0.0009 (4)
O21	0.0232 (18)	0.0283 (19)	0.037 (2)	0.0029 (15)	−0.0047 (16)	−0.0002 (16)
O22	0.0235 (18)	0.0219 (17)	0.0225 (16)	−0.0052 (14)	−0.0022 (14)	0.0003 (13)
O23	0.039 (3)	0.042 (2)	0.0181 (18)	0.0114 (19)	−0.0004 (18)	−0.0019 (15)
O24	0.030 (2)	0.0186 (16)	0.0215 (17)	−0.0032 (14)	−0.0021 (15)	−0.0035 (12)
S3	0.0189 (6)	0.0214 (6)	0.0197 (5)	0.0019 (4)	0.0027 (4)	−0.0005 (4)
O31	0.040 (2)	0.035 (2)	0.0265 (19)	−0.0045 (17)	0.0098 (17)	0.0028 (15)
O32	0.0243 (18)	0.0212 (17)	0.0264 (17)	0.0011 (14)	0.0020 (14)	−0.0048 (13)
O33	0.022 (2)	0.044 (2)	0.035 (2)	0.0062 (17)	−0.0032 (17)	0.0002 (18)
O34	0.0213 (17)	0.0198 (16)	0.0276 (18)	0.0018 (13)	0.0026 (14)	−0.0030 (13)
S4	0.0206 (6)	0.0221 (5)	0.0173 (5)	−0.0002 (4)	−0.0020 (4)	0.0015 (4)
O41	0.0222 (18)	0.030 (2)	0.042 (2)	−0.0084 (15)	−0.0072 (17)	−0.0034 (17)
O42	0.0310 (19)	0.0166 (15)	0.0221 (17)	0.0020 (14)	−0.0012 (15)	−0.0067 (12)
O43	0.0226 (18)	0.0225 (17)	0.0211 (16)	0.0040 (14)	−0.0026 (14)	−0.0024 (13)
O44	0.040 (3)	0.037 (2)	0.021 (2)	−0.0038 (19)	0.0039 (19)	0.0061 (15)
S5	0.0182 (5)	0.0184 (5)	0.0194 (5)	−0.0011 (4)	0.0025 (4)	−0.0019 (4)
O51	0.039 (2)	0.037 (2)	0.0200 (16)	−0.0001 (17)	0.0090 (16)	−0.0020 (15)
O52	0.0214 (17)	0.0197 (16)	0.0206 (15)	0.0004 (14)	0.0024 (13)	0.0031 (12)
O53	0.0235 (18)	0.0202 (16)	0.0259 (18)	−0.0019 (13)	0.0027 (14)	0.0086 (13)
O54	0.0151 (19)	0.033 (2)	0.036 (2)	−0.0017 (14)	−0.0027 (16)	−0.0002 (17)
S6	0.0548 (9)	0.0240 (6)	0.0575 (10)	−0.0001 (6)	−0.0097 (10)	0.0007 (7)
O61	0.060 (3)	0.041 (3)	0.050 (3)	0.009 (2)	−0.004 (3)	−0.016 (2)
O62	0.075 (5)	0.053 (4)	0.116 (6)	0.037 (3)	−0.005 (4)	0.009 (4)
O63	0.061 (3)	0.040 (3)	0.047 (3)	−0.023 (2)	0.009 (2)	−0.006 (2)
O64	0.068 (4)	0.046 (3)	0.055 (3)	−0.024 (3)	0.002 (3)	0.016 (2)
O1	0.049 (3)	0.0155 (17)	0.051 (2)	−0.0143 (18)	−0.0041 (19)	0.0096 (15)

Geometric parameters (Å, º)

Ce—O53	2.363 (4)	K6B—O21^vi	2.905 (5)
Ce—O42	2.367 (4)	K6B—O41	2.922 (6)
Ce—O34	2.367 (4)	K6B—O61^viii	2.997 (7)
Ce—O24	2.384 (4)	K6B—O43	3.175 (5)
Ce—O22	2.430 (4)	K6B—S6^viii	3.513 (3)
Ce—O14	2.433 (3)	K6B—S4	3.609 (3)
Ce—O32	2.435 (4)	K6B—S1^vii	3.779 (3)
Ce—O43	2.439 (4)	S1—O11	1.404 (5)
Ce—O52	2.443 (4)	S1—O13	1.450 (4)
Ce—S4	3.0457 (12)	S1—O14	1.466 (3)
Ce—S5	3.0498 (13)	S1—O12	1.478 (5)
Ce—S2	3.0514 (12)	S1—K3^x	3.6334 (17)
K1—O62	2.721 (7)	S1—K1^ii	3.708 (2)
K1—O23^i	2.772 (5)	S1—K5^ii	3.7502 (18)
K1—O44	2.840 (5)	S1—K6B^x	3.779 (3)
K1—O31^i	2.853 (5)	O11—K6A^ii	2.788 (6)
K1—O33^ii	2.868 (5)	O11—K1^ii	2.876 (7)
K1—O11^ii	2.876 (7)	O12—K2^iii	2.880 (7)
K1—O34^ii	2.913 (4)	O12—K4^ii	3.290 (8)
K1—S3^ii	3.468 (2)	O13—K6B^x	2.795 (5)
K1—S1^ii	3.708 (2)	O13—K5^ii	2.817 (5)
K1—S4	3.7281 (19)	O13—K3^x	2.877 (4)
K1—K4^ii	4.284 (2)	O14—K3^x	3.170 (5)
K1—K2	4.300 (2)	S2—O21	1.447 (4)
K2—O23^i	2.734 (5)	S2—O23	1.458 (5)
K2—O63	2.755 (5)	S2—O22	1.507 (4)
K2—O51	2.772 (5)	S2—O24	1.538 (4)
K2—O44	2.796 (6)	S2—K3^x	3.474 (2)
K2—O53^iii	2.853 (4)	S2—K6A^iv	3.560 (3)
K2—O54^iii	2.875 (5)	S2—K2^xi	3.5601 (19)
K2—O12^iii	2.880 (7)	O21—K3^iv	2.852 (5)
K2—O21^i	3.291 (4)	O21—K6A^iv	2.859 (5)
K2—S5^iii	3.4280 (19)	O21—K6B^iv	2.905 (5)
K2—S2^i	3.5601 (19)	O21—K2^xi	3.291 (4)
K2—K5^iv	4.142 (2)	O22—K6A^iv	3.127 (5)
K2—K6B^v	4.255 (3)	O23—K2^xi	2.734 (5)
K3—O64	2.714 (6)	O23—K1^xi	2.772 (5)
K3—O54^vi	2.773 (5)	O23—K3^x	2.952 (5)
K3—O24^vii	2.797 (4)	O24—K3^x	2.797 (4)
K3—O33^v	2.818 (5)	S3—O33	1.454 (5)
K3—O21^vi	2.852 (5)	S3—O31	1.456 (4)
K3—O13^vii	2.877 (4)	S3—O34	1.497 (4)
K3—O23^vii	2.952 (5)	S3—O32	1.531 (4)
K3—O14^vii	3.170 (5)	S3—K1^ii	3.468 (2)
K3—O31^v	3.331 (5)	S3—K3^viii	3.610 (2)
K3—S2^vii	3.474 (2)	O31—K5^xi	2.819 (5)
K3—S3^v	3.610 (2)	O31—K1^xi	2.853 (5)
K3—S1^vii	3.6334 (17)	O31—K3^viii	3.331 (5)
K4—O41	2.735 (4)	O33—K3^viii	2.818 (5)
K4—O61^viii	2.765 (6)	O33—K1^ii	2.868 (5)
K4—O54^ix	2.775 (5)	O34—K1^ii	2.913 (4)
K4—O44^ii	2.822 (5)	S4—O41	1.447 (4)
K4—O33	2.840 (5)	S4—O44	1.465 (5)
K4—O42^ii	2.982 (4)	S4—O43	1.503 (4)
K4—O12^ii	3.290 (8)	S4—O42	1.538 (4)
K4—O51^ix	3.402 (5)	S4—K4^ii	3.501 (2)
K4—S4^ii	3.501 (2)	O42—K4^ii	2.982 (4)
K4—S5^ix	3.642 (2)	O43—K5^iv	2.993 (4)
K4—K6B	4.186 (3)	O44—K4^ii	2.822 (5)
K4—K2^ii	4.282 (2)	S5—O51	1.444 (4)
K5—O1	2.807 (5)	S5—O54	1.461 (5)
K5—O13^ii	2.817 (5)	S5—O53	1.502 (4)
K5—O31^i	2.819 (5)	S5—O52	1.522 (4)
K5—O51^vi	2.821 (5)	S5—K2^iii	3.4281 (19)
K5—O63^vi	2.892 (6)	S5—K5^iv	3.568 (2)
K5—O64^vi	2.982 (7)	S5—K4^xii	3.642 (2)
K5—O43^vi	2.993 (4)	O51—K5^iv	2.821 (5)
K5—O52^vi	3.149 (4)	O51—K4^xii	3.402 (5)
K5—S6^vi	3.551 (2)	O52—K6A^iv	3.050 (5)
K5—S5^vi	3.568 (2)	O52—K5^iv	3.149 (4)
K5—S1^ii	3.7502 (18)	O53—K2^iii	2.853 (4)
K5—K2^vi	4.142 (2)	O54—K3^iv	2.773 (5)
K6A—K6B	2.512 (4)	O54—K4^xii	2.775 (5)
K6A—O11^ii	2.788 (6)	O54—K2^iii	2.875 (5)
K6A—O64	2.850 (8)	S6—O62	1.465 (7)
K6A—O21^vi	2.859 (5)	S6—O63	1.478 (6)
K6A—O41	2.908 (5)	S6—O64	1.481 (6)
K6A—O62	3.022 (9)	S6—O61	1.525 (6)
K6A—O52^vi	3.050 (5)	S6—K6B^v	3.513 (3)
K6A—O22^vi	3.126 (5)	S6—K5^iv	3.551 (2)
K6A—S6	3.513 (3)	O61—K4^v	2.765 (6)
K6A—S2^vi	3.560 (3)	O61—K6B^v	2.997 (7)
K6B—O13^vii	2.795 (5)	O63—K6B^v	2.819 (7)
K6B—O63^viii	2.819 (7)	O63—K5^iv	2.892 (6)
K6B—O32	2.840 (5)	O64—K5^iv	2.982 (7)
O53—Ce—O42	83.88 (14)	O13^ii—K5—K2^vi	141.73 (11)
O53—Ce—O34	148.07 (14)	O31^i—K5—K2^vi	124.12 (10)
O42—Ce—O34	84.81 (16)	O51^vi—K5—K2^vi	41.77 (9)
O53—Ce—O24	84.46 (16)	O63^vi—K5—K2^vi	41.54 (11)
O42—Ce—O24	145.75 (13)	O64^vi—K5—K2^vi	84.61 (11)
O34—Ce—O24	88.36 (14)	O43^vi—K5—K2^vi	64.65 (8)
O53—Ce—O22	122.92 (13)	O52^vi—K5—K2^vi	81.45 (8)
O42—Ce—O22	149.89 (13)	S6^vi—K5—K2^vi	61.73 (6)
O34—Ce—O22	78.04 (13)	S5^vi—K5—K2^vi	58.96 (3)
O24—Ce—O22	58.86 (13)	S1^ii—K5—K2^vi	159.22 (6)
O53—Ce—O14	77.21 (17)	O11^ii—K6A—O64	120.2 (2)
O42—Ce—O14	76.28 (17)	O11^ii—K6A—O21^vi	152.88 (18)
O34—Ce—O14	71.12 (17)	O64—K6A—O21^vi	83.50 (16)
O24—Ce—O14	69.76 (18)	O11^ii—K6A—O41	64.99 (18)
O22—Ce—O14	119.88 (14)	O64—K6A—O41	95.84 (16)
O53—Ce—O32	147.01 (13)	O21^vi—K6A—O41	129.86 (16)
O42—Ce—O32	79.26 (13)	O11^ii—K6A—O62	71.7 (2)
O34—Ce—O32	58.02 (13)	O64—K6A—O62	48.62 (13)
O24—Ce—O32	124.29 (12)	O21^vi—K6A—O62	129.45 (17)
O22—Ce—O32	70.67 (13)	O41—K6A—O62	77.85 (19)
O14—Ce—O32	124.9 (2)	O11^ii—K6A—O52^vi	97.99 (19)
O53—Ce—O43	76.65 (13)	O64—K6A—O52^vi	80.70 (16)
O42—Ce—O43	59.01 (12)	O21^vi—K6A—O52^vi	71.45 (12)
O34—Ce—O43	121.52 (13)	O41—K6A—O52^vi	158.17 (15)
O24—Ce—O43	146.96 (13)	O62—K6A—O52^vi	83.94 (19)
O22—Ce—O43	110.26 (16)	O11^ii—K6A—O22^vi	105.57 (16)
O14—Ce—O43	129.86 (14)	O64—K6A—O22^vi	119.50 (16)
O32—Ce—O43	70.36 (13)	O21^vi—K6A—O22^vi	47.77 (12)
O53—Ce—O52	58.45 (12)	O41—K6A—O22^vi	140.76 (15)
O42—Ce—O52	122.50 (12)	O62—K6A—O22^vi	137.9 (2)
O34—Ce—O52	148.74 (12)	O52^vi—K6A—O22^vi	54.33 (9)
O24—Ce—O52	76.75 (13)	O11^ii—K6A—S6	96.14 (18)
O22—Ce—O52	70.73 (13)	O64—K6A—S6	24.16 (13)
O14—Ce—O52	126.2 (2)	O21^vi—K6A—S6	106.47 (12)
O32—Ce—O52	108.61 (16)	O41—K6A—S6	86.74 (12)
O43—Ce—O52	70.29 (12)	O62—K6A—S6	24.46 (14)
O53—Ce—S4	79.03 (10)	O52^vi—K6A—S6	81.45 (11)
O42—Ce—S4	29.78 (9)	O22^vi—K6A—S6	132.46 (12)
O34—Ce—S4	104.36 (10)	O11^ii—K6A—S2^vi	130.53 (15)
O24—Ce—S4	163.30 (10)	O64—K6A—S2^vi	100.12 (13)
O22—Ce—S4	133.72 (10)	O21^vi—K6A—S2^vi	22.89 (9)
O14—Ce—S4	103.77 (13)	O41—K6A—S2^vi	141.99 (13)
O32—Ce—S4	72.24 (9)	O62—K6A—S2^vi	137.05 (17)
O43—Ce—S4	29.23 (10)	O52^vi—K6A—S2^vi	59.37 (8)
O52—Ce—S4	96.47 (9)	O22^vi—K6A—S2^vi	24.98 (8)
O53—Ce—S5	28.82 (9)	S6—K6A—S2^vi	119.68 (9)
O42—Ce—S5	104.10 (10)	O11^ii—K6A—K3	152.4 (2)
O34—Ce—S5	167.28 (10)	O64—K6A—K3	41.04 (12)
O24—Ce—S5	79.17 (10)	O21^vi—K6A—K3	43.82 (9)
O22—Ce—S5	97.34 (10)	O41—K6A—K3	126.43 (11)
O14—Ce—S5	101.81 (16)	O62—K6A—K3	85.74 (14)
O32—Ce—S5	131.94 (10)	O52^vi—K6A—K3	63.14 (9)
O43—Ce—S5	71.18 (9)	O22^vi—K6A—K3	80.45 (9)
O52—Ce—S5	29.64 (9)	S6—K6A—K3	62.78 (7)
S4—Ce—S5	87.45 (4)	S2^vi—K6A—K3	59.14 (5)
O53—Ce—S2	106.33 (10)	O11^ii—K6A—K4	54.41 (19)
O42—Ce—S2	164.53 (9)	O64—K6A—K4	134.76 (15)
O34—Ce—S2	80.46 (10)	O21^vi—K6A—K4	119.42 (12)
O24—Ce—S2	29.76 (9)	O41—K6A—K4	39.07 (9)
O22—Ce—S2	29.20 (9)	O62—K6A—K4	107.52 (15)
O14—Ce—S2	94.37 (13)	O52^vi—K6A—K4	141.32 (10)
O32—Ce—S2	96.72 (9)	O22^vi—K6A—K4	103.16 (10)
O43—Ce—S2	133.90 (10)	S6—K6A—K4	123.65 (9)
O52—Ce—S2	72.96 (9)	S2^vi—K6A—K4	115.04 (7)
S4—Ce—S2	161.83 (4)	K3—K6A—K4	151.67 (7)
S5—Ce—S2	89.75 (4)	O13^vii—K6B—O63^viii	108.93 (17)
O62—K1—O23^i	78.7 (2)	O13^vii—K6B—O32	106.91 (16)
O62—K1—O44	79.0 (2)	O63^viii—K6B—O32	88.10 (17)
O23^i—K1—O44	77.12 (15)	O13^vii—K6B—O21^vi	67.96 (14)
O62—K1—O31^i	84.4 (2)	O63^viii—K6B—O21^vi	77.27 (16)
O23^i—K1—O31^i	94.60 (14)	O32—K6B—O21^vi	161.32 (17)
O44—K1—O31^i	162.56 (16)	O13^vii—K6B—O41	123.19 (15)
O62—K1—O33^ii	151.6 (2)	O63^viii—K6B—O41	127.29 (16)
O23^i—K1—O33^ii	77.48 (14)	O32—K6B—O41	70.87 (13)
O44—K1—O33^ii	80.83 (14)	O21^vi—K6B—O41	127.41 (17)
O31^i—K1—O33^ii	112.71 (15)	O13^vii—K6B—O61^viii	154.83 (18)
O62—K1—O11^ii	75.0 (2)	O63^viii—K6B—O61^viii	49.48 (12)
O23^i—K1—O11^ii	153.55 (19)	O32—K6B—O61^viii	87.13 (16)
O44—K1—O11^ii	99.70 (17)	O21^vi—K6B—O61^viii	91.99 (16)
O31^i—K1—O11^ii	80.79 (18)	O41—K6B—O61^viii	80.80 (15)
O33^ii—K1—O11^ii	128.4 (2)	K6A—K6B—O43	94.06 (13)
O62—K1—O34^ii	157.8 (2)	O13^vii—K6B—O43	83.74 (13)
O23^i—K1—O34^ii	112.12 (13)	O63^viii—K6B—O43	143.40 (17)
O44—K1—O34^ii	121.57 (13)	O32—K6B—O43	55.32 (10)
O31^i—K1—O34^ii	75.70 (13)	O21^vi—K6B—O43	137.95 (14)
O33^ii—K1—O34^ii	49.34 (13)	O41—K6B—O43	47.05 (11)
O11^ii—K1—O34^ii	92.10 (15)	O61^viii—K6B—O43	121.18 (16)
O62—K1—S3^ii	171.26 (19)	K6A—K6B—S6^viii	100.40 (10)
O23^i—K1—S3^ii	93.14 (11)	O13^vii—K6B—S6^viii	131.91 (15)
O44—K1—S3^ii	102.33 (11)	O63^viii—K6B—S6^viii	23.94 (12)
O31^i—K1—S3^ii	93.35 (11)	O32—K6B—S6^viii	87.16 (11)
O33^ii—K1—S3^ii	24.25 (11)	O21^vi—K6B—S6^viii	84.11 (12)
O11^ii—K1—S3^ii	113.05 (14)	O41—K6B—S6^viii	104.90 (12)
O34^ii—K1—S3^ii	25.27 (8)	O61^viii—K6B—S6^viii	25.55 (12)
O62—K1—S1^ii	91.4 (2)	O43—K6B—S6^viii	136.83 (12)
O23^i—K1—S1^ii	163.31 (11)	O13^vii—K6B—S4	105.55 (12)
O44—K1—S1^ii	114.46 (12)	O63^viii—K6B—S4	138.25 (14)
O31^i—K1—S1^ii	70.85 (9)	O32—K6B—S4	59.48 (10)
O33^ii—K1—S1^ii	115.17 (11)	O21^vi—K6B—S4	138.79 (14)
O11^ii—K1—S1^ii	19.93 (10)	O41—K6B—S4	22.62 (8)
O34^ii—K1—S1^ii	73.06 (9)	O61^viii—K6B—S4	99.56 (13)
S3^ii—K1—S1^ii	95.78 (5)	O43—K6B—S4	24.55 (8)
O62—K1—S4	75.51 (19)	S6^viii—K6B—S4	120.65 (10)
O23^i—K1—S4	96.40 (10)	O13^vii—K6B—S1^vii	18.86 (8)
O44—K1—S4	20.62 (11)	O63^viii—K6B—S1^vii	91.87 (15)
O31^i—K1—S4	154.62 (11)	O32—K6B—S1^vii	99.09 (12)
O33^ii—K1—S4	92.01 (12)	O21^vi—K6B—S1^vii	70.23 (10)
O11^ii—K1—S4	79.18 (14)	O41—K6B—S1^vii	137.82 (12)
O34^ii—K1—S4	120.36 (9)	O61^viii—K6B—S1^vii	140.86 (15)
S3^ii—K1—S4	108.77 (5)	O43—K6B—S1^vii	92.88 (10)
S1^ii—K1—S4	94.04 (5)	S6^viii—K6B—S1^vii	115.65 (11)
O62—K1—K4^ii	119.1 (2)	S4—K6B—S1^vii	116.96 (8)
O23^i—K1—K4^ii	80.11 (11)	O13^vii—K6B—K4	163.64 (13)
O44—K1—K4^ii	40.67 (11)	O63^viii—K6B—K4	86.93 (12)
O31^i—K1—K4^ii	153.81 (11)	O32—K6B—K4	68.57 (10)
O33^ii—K1—K4^ii	41.12 (11)	O21^vi—K6B—K4	121.33 (12)
O11^ii—K1—K4^ii	114.83 (18)	O41—K6B—K4	40.58 (9)
O34^ii—K1—K4^ii	82.56 (8)	O61^viii—K6B—K4	41.27 (11)
S3^ii—K1—K4^ii	61.66 (3)	O43—K6B—K4	80.93 (10)
S1^ii—K1—K4^ii	116.56 (4)	S6^viii—K6B—K4	64.35 (7)
S4—K1—K4^ii	51.24 (4)	S4—K6B—K4	58.32 (5)
O62—K1—K2	68.5 (2)	S1^vii—K6B—K4	167.62 (8)
O23^i—K1—K2	38.35 (9)	O11—S1—O13	110.0 (4)
O44—K1—K2	39.89 (11)	O11—S1—O14	111.0 (4)
O31^i—K1—K2	127.82 (11)	O13—S1—O14	108.3 (3)
O33^ii—K1—K2	83.21 (11)	O11—S1—O12	109.4 (4)
O11^ii—K1—K2	128.86 (11)	O13—S1—O12	109.7 (3)
O34^ii—K1—K2	132.10 (9)	O14—S1—O12	108.4 (3)
S3^ii—K1—K2	106.88 (5)	O11—S1—K3^x	125.8 (3)
S1^ii—K1—K2	148.35 (5)	O13—S1—K3^x	48.16 (17)
S4—K1—K2	58.17 (4)	O14—S1—K3^x	60.15 (18)
K4^ii—K1—K2	59.84 (4)	O12—S1—K3^x	124.4 (3)
O23^i—K2—O63	81.27 (18)	O13—S1—K1^ii	105.2 (2)
O23^i—K2—O51	163.96 (16)	O14—S1—K1^ii	71.5 (3)
O63—K2—O51	85.60 (17)	O12—S1—K1^ii	142.7 (3)
O23^i—K2—O44	78.49 (15)	K3^x—S1—K1^ii	88.93 (5)
O63—K2—O44	82.90 (18)	O11—S1—K5^ii	69.5 (4)
O51—K2—O44	90.82 (14)	O14—S1—K5^ii	119.02 (19)
O23^i—K2—O53^iii	112.54 (14)	O12—S1—K5^ii	129.5 (2)
O63—K2—O53^iii	157.11 (18)	K3^x—S1—K5^ii	71.52 (4)
O51—K2—O53^iii	82.90 (13)	K1^ii—S1—K5^ii	72.85 (5)
O44—K2—O53^iii	116.90 (14)	O11—S1—K6B^x	121.9 (3)
O23^i—K2—O54^iii	74.46 (14)	O14—S1—K6B^x	124.0 (3)
O63—K2—O54^iii	152.11 (19)	O12—S1—K6B^x	71.3 (3)
O51—K2—O54^iii	115.54 (15)	K3^x—S1—K6B^x	74.31 (6)
O44—K2—O54^iii	79.02 (14)	K1^ii—S1—K6B^x	141.26 (6)
O53^iii—K2—O54^iii	49.87 (12)	K5^ii—S1—K6B^x	68.78 (5)
O23^i—K2—O12^iii	125.74 (17)	S1—O11—K6A^ii	141.1 (4)
O63—K2—O12^iii	83.4 (2)	S1—O11—K1^ii	115.8 (3)
O51—K2—O12^iii	61.19 (14)	K6A^ii—O11—K1^ii	102.2 (2)
O44—K2—O12^iii	149.66 (15)	S1—O12—K2^iii	122.3 (3)
O53^iii—K2—O12^iii	73.69 (16)	S1—O12—K4^ii	99.6 (4)
O54^iii—K2—O12^iii	122.01 (16)	K2^iii—O12—K4^ii	110.09 (17)
O23^i—K2—O21^i	46.14 (12)	S1—O13—K6B^x	122.6 (3)
O63—K2—O21^i	71.87 (14)	S1—O13—K5^ii	119.5 (3)
O51—K2—O21^i	136.84 (11)	K6B^x—O13—K5^ii	98.56 (13)
O44—K2—O21^i	121.02 (13)	S1—O13—K3^x	109.8 (2)
O53^iii—K2—O21^i	103.88 (11)	K6B^x—O13—K3^x	104.30 (16)
O54^iii—K2—O21^i	99.72 (13)	K5^ii—O13—K3^x	98.59 (13)
O12^iii—K2—O21^i	79.62 (15)	S1—O14—Ce	159.0 (2)
O23^i—K2—S5^iii	95.97 (12)	S1—O14—K3^x	96.19 (19)
O63—K2—S5^iii	176.97 (16)	Ce—O14—K3^x	104.05 (14)
O51—K2—S5^iii	96.92 (11)	O21—S2—O23	112.5 (3)
O44—K2—S5^iii	95.35 (11)	O21—S2—O22	111.1 (2)
O53^iii—K2—S5^iii	25.64 (8)	O23—S2—O22	111.6 (3)
O54^iii—K2—S5^iii	24.88 (9)	O21—S2—O24	110.7 (2)
O12^iii—K2—S5^iii	99.25 (14)	O23—S2—O24	108.5 (2)
O21^i—K2—S5^iii	107.13 (9)	O22—S2—O24	102.0 (2)
O23^i—K2—S2^i	22.21 (10)	O21—S2—Ce	128.29 (18)
O63—K2—S2^i	76.69 (13)	O23—S2—Ce	119.1 (2)
O51—K2—S2^i	158.13 (11)	O22—S2—Ce	51.89 (15)
O44—K2—S2^i	99.48 (10)	O24—S2—Ce	50.30 (15)
O53^iii—K2—S2^i	108.89 (9)	O21—S2—K3^x	122.15 (19)
O54^iii—K2—S2^i	85.51 (10)	O23—S2—K3^x	57.3 (2)
O12^iii—K2—S2^i	103.53 (13)	O22—S2—K3^x	125.85 (17)
O21^i—K2—S2^i	23.98 (7)	O24—S2—K3^x	51.78 (14)
S5^iii—K2—S2^i	101.22 (5)	Ce—S2—K3^x	85.49 (4)
O23^i—K2—K5^iv	122.29 (12)	O21—S2—K6A^iv	50.21 (18)
O63—K2—K5^iv	44.12 (13)	O23—S2—K6A^iv	136.6 (2)
O51—K2—K5^iv	42.68 (10)	O22—S2—K6A^iv	61.21 (17)
O44—K2—K5^iv	77.82 (10)	O24—S2—K6A^iv	114.86 (16)
O53^iii—K2—K5^iv	125.14 (9)	Ce—S2—K6A^iv	90.75 (5)
O54^iii—K2—K5^iv	147.36 (11)	K3^x—S2—K6A^iv	164.12 (7)
O12^iii—K2—K5^iv	73.51 (11)	O21—S2—K2^xi	67.54 (18)
O21^i—K2—K5^iv	111.86 (9)	O23—S2—K2^xi	45.1 (2)
S5^iii—K2—K5^iv	137.97 (5)	O22—S2—K2^xi	133.62 (16)
S2^i—K2—K5^iv	120.79 (5)	O24—S2—K2^xi	122.38 (15)
O23^i—K2—K6B^v	79.18 (11)	Ce—S2—K2^xi	162.99 (5)
O63—K2—K6B^v	40.80 (13)	K3^x—S2—K2^xi	79.54 (4)
O51—K2—K6B^v	96.81 (11)	K6A^iv—S2—K2^xi	105.82 (5)
O44—K2—K6B^v	121.75 (11)	S2—O21—K3^iv	121.8 (2)
O53^iii—K2—K6B^v	121.35 (10)	S2—O21—K6A^iv	106.9 (2)
O54^iii—K2—K6B^v	142.09 (12)	K3^iv—O21—K6A^iv	92.22 (14)
O12^iii—K2—K6B^v	56.53 (15)	S2—O21—K6B^iv	133.0 (3)
O21^i—K2—K6B^v	42.95 (9)	K3^iv—O21—K6B^iv	102.15 (14)
S5^iii—K2—K6B^v	140.05 (6)	K6A^iv—O21—K6B^iv	51.68 (11)
S2^i—K2—K6B^v	61.37 (5)	S2—O21—K2^xi	88.48 (19)
K5^iv—K2—K6B^v	70.44 (5)	K3^iv—O21—K2^xi	115.70 (13)
O64—K3—O54^vi	82.19 (18)	K6A^iv—O21—K2^xi	134.76 (16)
O64—K3—O24^vii	160.84 (18)	K6B^iv—O21—K2^xi	86.51 (13)
O54^vi—K3—O24^vii	108.65 (13)	S2—O22—Ce	98.91 (19)
O64—K3—O33^v	80.81 (19)	S2—O22—K6A^iv	93.81 (19)
O54^vi—K3—O33^v	76.60 (12)	Ce—O22—K6A^iv	115.69 (14)
O24^vii—K3—O33^v	116.59 (14)	S2—O23—K2^xi	112.6 (3)
O64—K3—O21^vi	86.13 (18)	S2—O23—K1^xi	133.3 (3)
O54^vi—K3—O21^vi	96.79 (13)	K2^xi—O23—K1^xi	102.67 (15)
O24^vii—K3—O21^vi	77.08 (13)	S2—O23—K3^x	98.2 (2)
O33^v—K3—O21^vi	166.03 (15)	K2^xi—O23—K3^x	104.55 (17)
O64—K3—O13^vii	69.73 (17)	K1^xi—O23—K3^x	101.52 (16)
O54^vi—K3—O13^vii	148.25 (13)	S2—O24—Ce	99.94 (19)
O24^vii—K3—O13^vii	95.02 (12)	S2—O24—K3^x	102.63 (18)
O33^v—K3—O13^vii	111.82 (16)	Ce—O24—K3^x	117.75 (16)
O21^vi—K3—O13^vii	67.60 (14)	O33—S3—O31	113.5 (3)
O64—K3—O23^vii	148.64 (19)	O33—S3—O34	109.7 (3)
O54^vi—K3—O23^vii	72.68 (12)	O31—S3—O34	111.6 (3)
O24^vii—K3—O23^vii	49.95 (12)	O33—S3—O32	110.3 (3)
O33^v—K3—O23^vii	75.41 (14)	O31—S3—O32	110.4 (3)
O21^vi—K3—O23^vii	114.76 (14)	O34—S3—O32	100.6 (2)
O13^vii—K3—O23^vii	138.57 (12)	O33—S3—Ce	119.0 (2)
O64—K3—O14^vii	114.18 (16)	O31—S3—Ce	127.5 (2)
O54^vi—K3—O14^vii	163.17 (14)	O34—S3—Ce	48.95 (15)
O24^vii—K3—O14^vii	54.55 (12)	O32—S3—Ce	51.79 (16)
O33^v—K3—O14^vii	108.7 (2)	O33—S3—K1^ii	54.1 (2)
O21^vi—K3—O14^vii	81.15 (16)	O31—S3—K1^ii	124.9 (2)
O13^vii—K3—O14^vii	45.71 (9)	O34—S3—K1^ii	56.18 (15)
O23^vii—K3—O14^vii	92.89 (11)	O32—S3—K1^ii	124.36 (17)
O64—K3—O31^v	72.76 (17)	Ce—S3—K1^ii	87.02 (5)
O54^vi—K3—O31^v	119.18 (12)	O33—S3—K3^viii	46.6 (2)
O24^vii—K3—O31^v	112.80 (13)	O31—S3—K3^viii	67.3 (2)
O33^v—K3—O31^v	45.68 (13)	O34—S3—K3^viii	122.82 (16)
O21^vi—K3—O31^v	134.08 (9)	O32—S3—K3^viii	134.78 (17)
O13^vii—K3—O31^v	66.92 (13)	Ce—S3—K3^viii	163.65 (5)
O23^vii—K3—O31^v	103.25 (14)	K1^ii—S3—K3^viii	77.57 (4)
O14^vii—K3—O31^v	71.84 (16)	S3—O31—K5^xi	134.2 (3)
O64—K3—S2^vii	170.95 (16)	S3—O31—K1^xi	120.4 (3)
O54^vi—K3—S2^vii	88.76 (10)	K5^xi—O31—K1^xi	102.64 (14)
O24^vii—K3—S2^vii	25.59 (8)	S3—O31—K3^viii	88.9 (2)
O33^v—K3—S2^vii	97.03 (11)	K5^xi—O31—K3^viii	88.73 (13)
O21^vi—K3—S2^vii	95.10 (10)	K1^xi—O31—K3^viii	112.29 (14)
O13^vii—K3—S2^vii	119.02 (9)	S3—O32—Ce	98.6 (2)
O23^vii—K3—S2^vii	24.56 (9)	S3—O32—K6B	134.5 (2)
O14^vii—K3—S2^vii	74.86 (7)	Ce—O32—K6B	122.48 (16)
O31^v—K3—S2^vii	112.02 (10)	S3—O33—K3^viii	111.3 (3)
O64—K3—S3^v	77.59 (15)	S3—O33—K4	137.5 (3)
O54^vi—K3—S3^v	97.79 (10)	K3^viii—O33—K4	100.97 (17)
O24^vii—K3—S3^v	115.23 (10)	S3—O33—K1^ii	101.7 (3)
O33^v—K3—S3^v	22.04 (11)	K3^viii—O33—K1^ii	102.54 (16)
O21^vi—K3—S3^v	156.39 (10)	K4—O33—K1^ii	97.28 (17)
O13^vii—K3—S3^v	90.55 (11)	S3—O34—Ce	102.56 (19)
O23^vii—K3—S3^v	87.35 (11)	S3—O34—K1^ii	98.55 (19)
O14^vii—K3—S3^v	89.97 (15)	Ce—O34—K1^ii	116.79 (15)
O31^v—K3—S3^v	23.78 (8)	O41—S4—O44	112.7 (3)
S2^vii—K3—S3^v	103.67 (6)	O41—S4—O43	111.9 (3)
O64—K3—S1^vii	91.14 (15)	O44—S4—O43	110.7 (3)
O54^vi—K3—S1^vii	168.29 (11)	O41—S4—O42	110.7 (2)
O24^vii—K3—S1^vii	75.30 (9)	O44—S4—O42	108.0 (3)
O33^v—K3—S1^vii	111.96 (13)	O43—S4—O42	102.3 (2)
O21^vi—K3—S1^vii	73.05 (9)	O41—S4—Ce	124.80 (19)
O13^vii—K3—S1^vii	22.06 (7)	O44—S4—Ce	122.4 (2)
O23^vii—K3—S1^vii	116.53 (10)	O43—S4—Ce	52.39 (15)
O14^vii—K3—S1^vii	23.66 (5)	O42—S4—Ce	49.86 (15)
O31^v—K3—S1^vii	67.29 (8)	O41—S4—K4^ii	120.26 (19)
S2^vii—K3—S1^vii	97.80 (4)	O44—S4—K4^ii	51.1 (2)
S3^v—K3—S1^vii	90.11 (5)	O43—S4—K4^ii	127.77 (18)
O41—K4—O61^viii	88.45 (17)	O42—S4—K4^ii	57.86 (15)
O41—K4—O54^ix	160.12 (16)	Ce—S4—K4^ii	93.13 (5)
O61^viii—K4—O54^ix	77.64 (17)	O41—S4—K6B	50.96 (19)
O41—K4—O44^ii	108.41 (16)	O44—S4—K6B	137.0 (2)
O61^viii—K4—O44^ii	153.09 (18)	O43—S4—K6B	61.34 (17)
O54^ix—K4—O44^ii	80.28 (15)	O42—S4—K6B	115.03 (16)
O41—K4—O33	87.22 (15)	Ce—S4—K6B	87.70 (6)
O61^viii—K4—O33	78.36 (18)	K4^ii—S4—K6B	168.00 (7)
O54^ix—K4—O33	76.19 (13)	O41—S4—K1	69.72 (18)
O44^ii—K4—O33	81.61 (14)	O43—S4—K1	132.01 (15)
O41—K4—O42^ii	77.37 (13)	O42—S4—K1	122.57 (15)
O61^viii—K4—O42^ii	157.51 (16)	Ce—S4—K1	164.25 (5)
O54^ix—K4—O42^ii	119.97 (13)	K4^ii—S4—K1	72.62 (4)
O44^ii—K4—O42^ii	49.40 (12)	K6B—S4—K1	107.65 (7)
O33—K4—O42^ii	117.68 (14)	S4—O41—K4	130.1 (2)
O41—K4—O12^ii	97.10 (14)	S4—O41—K6A	129.8 (3)
O61^viii—K4—O12^ii	82.96 (16)	K4—O41—K6A	98.85 (14)
O54^ix—K4—O12^ii	95.24 (15)	S4—O41—K6B	106.4 (2)
O44^ii—K4—O12^ii	114.37 (15)	K4—O41—K6B	95.39 (14)
O33—K4—O12^ii	160.72 (15)	K6A—O41—K6B	51.05 (10)
O42^ii—K4—O12^ii	81.59 (12)	S4—O42—Ce	100.35 (19)
O41—K4—O51^ix	142.79 (10)	S4—O42—K4^ii	96.24 (17)
O61^viii—K4—O51^ix	71.10 (16)	Ce—O42—K4^ii	125.51 (16)
O54^ix—K4—O51^ix	44.61 (13)	S4—O43—Ce	98.4 (2)
O44^ii—K4—O51^ix	103.03 (15)	S4—O43—K5^iv	138.9 (2)
O33—K4—O51^ix	117.07 (13)	Ce—O43—K5^iv	119.65 (14)
O42^ii—K4—O51^ix	110.43 (12)	S4—O43—K6B	94.11 (19)
O12^ii—K4—O51^ix	50.92 (12)	Ce—O43—K6B	110.36 (14)
O41—K4—S4^ii	91.49 (10)	K5^iv—O43—K6B	87.12 (12)
O61^viii—K4—S4^ii	175.72 (15)	S4—O44—K2	132.4 (3)
O54^ix—K4—S4^ii	101.33 (11)	S4—O44—K4^ii	105.0 (2)
O44^ii—K4—S4^ii	23.83 (10)	K2—O44—K4^ii	99.32 (17)
O33—K4—S4^ii	97.37 (11)	S4—O44—K1	116.3 (3)
O42^ii—K4—S4^ii	25.89 (7)	K2—O44—K1	99.45 (15)
O12^ii—K4—S4^ii	101.28 (10)	K4^ii—O44—K1	98.34 (16)
O51^ix—K4—S4^ii	111.14 (10)	O51—S5—O54	112.5 (3)
O41—K4—S5^ix	161.24 (11)	O51—S5—O53	111.6 (3)
O61^viii—K4—S5^ix	74.27 (14)	O54—S5—O53	109.2 (2)
O54^ix—K4—S5^ix	21.32 (10)	O51—S5—O52	109.9 (2)
O44^ii—K4—S5^ix	90.35 (13)	O54—S5—O52	111.4 (3)
O33—K4—S5^ix	96.19 (11)	O53—S5—O52	101.8 (2)
O42^ii—K4—S5^ix	116.51 (10)	O51—S5—Ce	124.52 (19)
O12^ii—K4—S5^ix	73.95 (11)	O54—S5—Ce	123.0 (2)
O51^ix—K4—S5^ix	23.34 (7)	O53—S5—Ce	49.29 (14)
S4^ii—K4—S5^ix	106.29 (6)	O52—S5—Ce	52.54 (15)
O41—K4—K6B	44.03 (10)	O51—S5—K2^iii	117.7 (2)
O61^viii—K4—K6B	45.63 (14)	O54—S5—K2^iii	55.88 (19)
O54^ix—K4—K6B	118.60 (12)	O53—S5—K2^iii	55.27 (16)
O44^ii—K4—K6B	141.14 (13)	O52—S5—K2^iii	131.96 (16)
O33—K4—K6B	71.88 (12)	Ce—S5—K2^iii	93.02 (5)
O42^ii—K4—K6B	121.17 (9)	O51—S5—K5^iv	48.30 (19)
O12^ii—K4—K6B	98.27 (11)	O54—S5—K5^iv	133.92 (19)
O51^ix—K4—K6B	114.11 (10)	O53—S5—K5^iv	116.86 (16)
S4^ii—K4—K6B	133.32 (6)	O52—S5—K5^iv	61.80 (15)
S5^ix—K4—K6B	119.78 (6)	Ce—S5—K5^iv	90.26 (4)
O41—K4—K2^ii	148.23 (10)	K2^iii—S5—K5^iv	163.05 (6)
O61^viii—K4—K2^ii	119.20 (14)	O51—S5—K4^xii	68.94 (19)
O54^ix—K4—K2^ii	41.61 (10)	O53—S5—K4^xii	123.87 (16)
O44^ii—K4—K2^ii	40.11 (12)	O52—S5—K4^xii	131.92 (17)
O33—K4—K2^ii	83.85 (11)	Ce—S5—K4^xii	165.51 (5)
O42^ii—K4—K2^ii	79.98 (8)	K2^iii—S5—K4^xii	74.48 (5)
O12^ii—K4—K2^ii	101.33 (11)	K5^iv—S5—K4^xii	103.83 (5)
O51^ix—K4—K2^ii	66.81 (9)	S5—O51—K2	127.5 (3)
S4^ii—K4—K2^ii	59.73 (3)	S5—O51—K5^iv	109.2 (2)
S5^ix—K4—K2^ii	50.48 (4)	K2—O51—K5^iv	95.55 (15)
K6B—K4—K2^ii	153.17 (7)	S5—O51—K4^xii	87.7 (2)
O1—K5—O13^ii	139.69 (15)	K2—O51—K4^xii	109.74 (13)
O1—K5—O31^i	68.05 (14)	K5^iv—O51—K4^xii	131.33 (17)
O13^ii—K5—O31^i	75.33 (14)	S5—O52—Ce	97.8 (2)
O1—K5—O51^vi	64.03 (13)	S5—O52—K6A^iv	140.3 (2)
O13^ii—K5—O51^vi	149.16 (13)	Ce—O52—K6A^iv	117.98 (14)
O31^i—K5—O51^vi	132.08 (14)	S5—O52—K5^iv	92.97 (16)
O1—K5—O63^vi	83.48 (17)	Ce—O52—K5^iv	113.94 (14)
O13^ii—K5—O63^vi	114.76 (15)	K6A^iv—O52—K5^iv	87.83 (12)
O31^i—K5—O63^vi	92.08 (16)	S5—O53—Ce	101.89 (18)
O51^vi—K5—O63^vi	82.17 (14)	S5—O53—K2^iii	99.09 (19)
O1—K5—O64^vi	118.33 (18)	Ce—O53—K2^iii	128.72 (16)
O13^ii—K5—O64^vi	66.89 (14)	S5—O54—K3^iv	129.7 (3)
O31^i—K5—O64^vi	77.16 (17)	S5—O54—K4^xii	115.0 (3)
O51^vi—K5—O64^vi	125.96 (15)	K3^iv—O54—K4^xii	103.77 (16)
O63^vi—K5—O64^vi	47.98 (11)	S5—O54—K2^iii	99.2 (2)
O1—K5—O43^vi	132.28 (14)	K3^iv—O54—K2^iii	105.62 (16)
O13^ii—K5—O43^vi	86.82 (13)	K4^xii—O54—K2^iii	98.53 (15)
O31^i—K5—O43^vi	158.27 (14)	O62—S6—O63	114.1 (6)
O51^vi—K5—O43^vi	68.70 (13)	O62—S6—O64	110.6 (5)
O63^vi—K5—O43^vi	84.13 (15)	O63—S6—O64	107.7 (4)
O64^vi—K5—O43^vi	84.54 (16)	O62—S6—O61	106.9 (4)
O1—K5—O52^vi	95.53 (13)	O63—S6—O61	108.6 (4)
O13^ii—K5—O52^vi	102.98 (12)	O64—S6—O61	108.7 (5)
O31^i—K5—O52^vi	141.35 (13)	O62—S6—K6A	58.7 (4)
O51^vi—K5—O52^vi	47.64 (11)	O63—S6—K6A	128.8 (3)
O63^vi—K5—O52^vi	121.64 (13)	O64—S6—K6A	52.0 (3)
O64^vi—K5—O52^vi	138.72 (17)	O61—S6—K6A	122.1 (3)
O43^vi—K5—O52^vi	54.39 (8)	O62—S6—K6B^v	127.8 (4)
O1—K5—S6^vi	102.25 (12)	O63—S6—K6B^v	50.7 (2)
O13^ii—K5—S6^vi	90.94 (11)	O64—S6—K6B^v	121.6 (3)
O31^i—K5—S6^vi	85.65 (11)	O61—S6—K6B^v	57.9 (3)
O51^vi—K5—S6^vi	103.50 (11)	K6A—S6—K6B^v	173.54 (11)
O63^vi—K5—S6^vi	23.82 (12)	O62—S6—K5^iv	125.7 (3)
O64^vi—K5—S6^vi	24.25 (12)	O63—S6—K5^iv	52.2 (2)
O43^vi—K5—S6^vi	82.30 (9)	O64—S6—K5^iv	55.8 (3)
O52^vi—K5—S6^vi	132.84 (10)	O61—S6—K5^iv	127.4 (3)
O1—K5—S5^vi	79.17 (10)	K6A—S6—K5^iv	88.95 (6)
O13^ii—K5—S5^vi	127.37 (10)	K6B^v—S6—K5^iv	86.57 (8)
O31^i—K5—S5^vi	143.25 (12)	S6—O61—K4^v	148.2 (4)
O51^vi—K5—S5^vi	22.47 (8)	S6—O61—K6B^v	96.5 (3)
O63^vi—K5—S5^vi	100.47 (11)	K4^v—O61—K6B^v	93.11 (18)
O64^vi—K5—S5^vi	135.51 (13)	S6—O62—K1	146.8 (5)
O43^vi—K5—S5^vi	58.26 (8)	S6—O62—K6A	96.9 (4)
O52^vi—K5—S5^vi	25.22 (7)	K1—O62—K6A	100.1 (2)
S6^vi—K5—S5^vi	118.18 (7)	S6—O63—K2	138.1 (4)
O1—K5—S1^ii	124.90 (12)	S6—O63—K6B^v	105.4 (3)
O13^ii—K5—S1^ii	19.66 (9)	K2—O63—K6B^v	99.52 (19)
O31^i—K5—S1^ii	70.50 (9)	S6—O63—K5^iv	104.0 (3)
O51^vi—K5—S1^ii	141.93 (10)	K2—O63—K5^iv	94.34 (17)
O63^vi—K5—S1^ii	132.72 (12)	K6B^v—O63—K5^iv	116.0 (3)
O64^vi—K5—S1^ii	84.89 (12)	S6—O64—K3	143.9 (4)
O43^vi—K5—S1^ii	96.51 (9)	S6—O64—K6A	103.9 (3)
O52^vi—K5—S1^ii	94.86 (8)	K3—O64—K6A	95.37 (19)
S6^vi—K5—S1^ii	109.13 (7)	S6—O64—K5^iv	100.0 (3)
S5^vi—K5—S1^ii	119.99 (5)	K3—O64—K5^iv	98.4 (2)
O1—K5—K2^vi	75.88 (11)	K6A—O64—K5^iv	116.1 (3)

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