Tri­potassium hexa­hydrogen­hexa­molybdo­cobaltate(III) potassium nitrate tetra­hydrate, K₃[H₆CoMo₆O₂₄]·KNO₃·4H₂O

The title double salt was obtained from the reaction of Y(NO₃)₃ and K₆[H₄Co₂Mo₁₀O₃₈]·5H₂O at a pH of about 2.0. The [H₆CoMo₆O₂₄]^3- anion is a typical B-type Anderson-structure heteropolyanion, and has an inversion center, with Co-O bond lengths in the range 1.907 (4)-1.919 (4) Å and Mo-O bond lengths in the ranges 1.709 (5)-1.721 (5), 1.902 (5)-1.951 (5) and 2.274 (4)-2.312 (4) Å.

S1. Comment

Obtaining suitable crystals for the structure determination of some kinds of B-type Anderson-structure heteropolyanions, such as [H₆Xⁿ⁺Mo₆O₂₄]^(6-n)- (X: Co²⁺, Co³⁺, Ni²⁺, Fe³⁺) (Anderson, 1937), is difficult. The salts of these polyanions have a cleavage property like mica because of the repulsion of interanions by six undissociated H atoms bound to O atoms in XO₆. The bulky counter-cation acts as a separator between the interanions in the crystal packing. Single crystals of some compounds, such as (18-crown-6.K⁺)₂K[H₆CoMo₆O₂₄].12H₂O (Nagano et al., 1990) and [Ga(H₂O)₆]₃[H₆CoMo₆O₂₄].10H₂O (Panneerselvam et al., 1996), have been were obtained. The role of potassium nitrate in the crystallization of these crystals is important.

The present polyanion is close to having D_{3 d}(−3 m) symmetry. The definition of O atoms in the polyanion is the same as in the previous report (Panneerselvam et al., 1996); O_n is the a nitrate O atom. The Mo—O distances show a similar tendency to those found in (18-crown-6.K⁺)₂K[H₆CoMo₆O₂₄].12H₂O (Nagano et al., 1990), Na₃[H₆CoMo₆O₂₄]·8H₂O (Nolan et al., 1998) and [Ga(H₂O)₆]₃[H₆CoMo₆O₂₄].10H₂O (Panneerselvam et al., 1996). KNO₃ not only contributes to the charge balance but also packs the cavity made by the polyanion with K⁺ and O_w. N and O_n17 atoms are located on the twofold axis. Reasonable displacement parameters of O_w14 and O_w15 were obtained by reducing the occupancy to 0.5. The K1 and K2 ions are coordinated to O atoms as [K1(O_t)₄(O_b)(O_w)(O_n)]⁺ and [K2(O_t)₃(O_b)(O_w)(O_n)₃]⁺. The distances between K and O atoms are in the range 2.63 (2)–3.21 (8) Å.

S2. Experimental

The title compound was prepared by mixing hot aqueous solutions of K₆[H₄Co₂Mo₁₀O₃₈]·5H₂O(0.5 mM per 20 ml) and Y(NO₃)₃·6H₂O(0.5 mM per 20 ml), adjusting the pH to about 2.0 with 3.0 M HNO₃. The solution was concentrated to about 20 ml by heating it in a water bath. After a day, monoclinic pale-blue crystals and an unstable colorless by-product were obtained.

S3. Refinement

Rather low completness of 93.05% for θ_max = 27.45° is due to the omission of the off-center reflections. The highest peaks in the difference map are 1.29 Å from Ow15 and 0.91 Å from K2, and the largest hole is 0.79 Å from K2. H atoms were not included in the structure model.

Computing details

Data collection: STADI4 (Stoe & Cie, 1996); cell refinement: STADI4; data reduction: X-RED (Stoe & Cie, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997).

(I)

Crystal data

K3[H6CoMo6O24]·KNO3·4H2O	F(000) = 2496
Mr = 1315.09	Dx = 2.959 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71069 Å
a = 24.191 (3) Å	Cell parameters from 26 reflections
b = 10.9675 (16) Å	θ = 9.6–10.5°
c = 11.6115 (15) Å	µ = 3.69 mm^−1
β = 106.644 (9)°	T = 298 K
V = 2951.6 (7) Å^3	Monoclinic, pale blue
Z = 4	0.20 × 0.15 × 0.07 mm

Data collection

Stoe Stadi-4 diffractometer	2574 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.000
Graphite monochromator	θmax = 27.5°, θmin = 1.8°
ω–2θ scans	h = −31→30
Absorption correction: numerical (Stoe & Cie, 1996)	k = 0→14
Tmin = 0.463, Tmax = 0.650	l = 0→15
3148 measured reflections	3 standard reflections every 60 min
3148 independent reflections	intensity decay: 2.8%

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)] = 0.042	H-atom parameters not refined
wR(F^2) = 0.119	Calculated w = 1/[σ^2(Fo^2) + (0.053P)^2 + 53.7384P] where P = (Fo^2 + 2Fc^2)/3
S = 1.09	(Δ/σ)max = 0.001
3148 reflections	Δρmax = 1.88 e Å^−3
206 parameters	Δρmin = −1.60 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)
Co	0.2500	0.2500	0.5000	0.0119 (2)
Mo1	0.32555 (2)	0.01247 (5)	0.63528 (5)	0.01787 (15)
Mo2	0.18205 (2)	0.00614 (5)	0.55866 (5)	0.01793 (15)
Mo3	0.39278 (2)	0.25481 (6)	0.57370 (5)	0.01880 (15)
K1	0.40533 (10)	−0.2782 (2)	0.75229 (17)	0.0452 (5)
K2	0.44023 (9)	0.1058 (3)	0.93029 (17)	0.0581 (7)
OC1	0.30999 (18)	0.1476 (4)	0.4786 (4)	0.0151 (9)
OC2	0.25304 (18)	0.1449 (4)	0.6339 (4)	0.0160 (9)
OC3	0.18868 (18)	0.1454 (4)	0.4153 (4)	0.0161 (9)
OB4	0.37415 (19)	0.1513 (5)	0.6916 (4)	0.0201 (10)
OB5	0.2534 (2)	−0.0570 (4)	0.5358 (4)	0.0203 (9)
OB6	0.36687 (19)	0.3603 (5)	0.4337 (4)	0.0201 (10)
OT7	0.3702 (2)	−0.0784 (5)	0.5813 (5)	0.0278 (11)
OT8	0.3266 (2)	−0.0486 (5)	0.7725 (4)	0.0296 (12)
OT9	0.1861 (3)	−0.0576 (6)	0.6960 (5)	0.0347 (13)
OT10	0.1362 (2)	−0.0844 (5)	0.4535 (5)	0.0338 (13)
OT11	0.4396 (2)	0.3517 (6)	0.6691 (5)	0.0335 (13)
OT12	0.4333 (2)	0.1584 (6)	0.5137 (5)	0.0317 (12)
OW13	0.2329 (3)	0.2088 (5)	0.8370 (5)	0.0430 (16)
OW14	0.4997 (7)	−0.4083 (14)	0.833 (2)	0.093 (7)	0.50
OW15	0.4542 (7)	0.3450 (16)	0.9294 (14)	0.061 (4)	0.50
ON16	0.5130 (3)	0.0945 (8)	1.1686 (6)	0.063 (2)
ON17	0.5000	−0.0728 (10)	1.2500	0.048 (2)
N	0.5000	0.0402 (11)	1.2500	0.036 (2)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Co	0.0128 (5)	0.0144 (5)	0.0093 (5)	0.0000 (4)	0.0043 (4)	−0.0004 (4)
Mo1	0.0190 (3)	0.0195 (3)	0.0155 (3)	0.0034 (2)	0.0054 (2)	0.0041 (2)
Mo2	0.0204 (3)	0.0179 (3)	0.0171 (3)	−0.0030 (2)	0.0080 (2)	0.0015 (2)
Mo3	0.0138 (3)	0.0247 (3)	0.0180 (3)	−0.0001 (2)	0.00475 (19)	0.0010 (2)
K1	0.0624 (13)	0.0454 (12)	0.0324 (9)	−0.0124 (10)	0.0208 (9)	−0.0017 (8)
K2	0.0414 (11)	0.106 (2)	0.0264 (9)	0.0040 (12)	0.0092 (8)	−0.0060 (11)
OC1	0.017 (2)	0.016 (2)	0.0144 (19)	0.0035 (17)	0.0081 (16)	−0.0001 (16)
OC2	0.016 (2)	0.019 (3)	0.0130 (19)	0.0013 (17)	0.0050 (16)	0.0006 (16)
OC3	0.015 (2)	0.021 (3)	0.0120 (19)	−0.0020 (17)	0.0031 (16)	−0.0025 (16)
OB4	0.018 (2)	0.026 (3)	0.015 (2)	0.0011 (19)	0.0016 (17)	0.0006 (18)
OB5	0.026 (2)	0.016 (2)	0.019 (2)	0.001 (2)	0.0066 (18)	−0.0017 (18)
OB6	0.020 (2)	0.027 (3)	0.018 (2)	0.0028 (19)	0.0123 (17)	0.0039 (18)
OT7	0.028 (3)	0.022 (3)	0.035 (3)	0.006 (2)	0.011 (2)	0.004 (2)
OT8	0.033 (3)	0.033 (3)	0.023 (2)	0.002 (2)	0.008 (2)	0.013 (2)
OT9	0.043 (3)	0.039 (3)	0.029 (3)	0.005 (3)	0.020 (2)	0.014 (2)
OT10	0.031 (3)	0.034 (3)	0.038 (3)	−0.010 (2)	0.012 (2)	−0.010 (2)
OT11	0.022 (3)	0.045 (4)	0.028 (3)	−0.011 (2)	−0.001 (2)	0.002 (2)
OT12	0.028 (3)	0.040 (3)	0.031 (3)	0.008 (2)	0.015 (2)	0.004 (2)
OW13	0.084 (5)	0.024 (3)	0.027 (3)	−0.006 (3)	0.026 (3)	−0.003 (2)
OW14	0.047 (9)	0.036 (9)	0.20 (2)	0.018 (7)	0.043 (12)	−0.002 (11)
OW15	0.061 (9)	0.059 (10)	0.080 (10)	0.017 (8)	0.049 (8)	0.002 (8)
ON16	0.067 (5)	0.088 (6)	0.031 (3)	−0.034 (5)	0.011 (3)	0.010 (4)
ON17	0.037 (5)	0.053 (6)	0.054 (5)	0.000	0.011 (4)	0.000
N	0.027 (5)	0.053 (7)	0.025 (4)	0.000	0.005 (4)	0.000

Geometric parameters (Å, º)

Co—OC1	1.907 (4)	K1—OT7	2.915 (6)
Co—OC1^i	1.907 (4)	K1—OW14^vi	3.100 (19)
Co—OC3	1.910 (4)	K1—OT12^iii	3.197 (6)
Co—OC3^i	1.910 (4)	K1—OT8	3.205 (6)
Co—OC2	1.919 (4)	K1—OW13^vii	3.207 (8)
Co—OC2^i	1.919 (4)	K1—Mo3^iii	3.8387 (19)
Co—Mo1	3.3091 (7)	K1—K2^ii	4.480 (3)
Co—Mo2	3.3106 (7)	K2—OW15	2.645 (18)
Co—Mo3	3.3123 (7)	K2—OT7^iii	2.781 (6)
Mo1—OT7	1.715 (5)	K2—OB4	2.819 (5)
Mo1—OT8	1.721 (5)	K2—ON16	2.826 (7)
Mo1—OB4	1.921 (5)	K2—ON16^v	2.859 (10)
Mo1—OB5	1.951 (5)	K2—ON17^v	2.888 (2)
Mo1—OC2	2.274 (4)	K2—OT12^vi	2.996 (6)
Mo1—OC1	2.293 (4)	K2—OT12^iii	3.075 (7)
Mo1—Mo3	3.2994 (9)	K2—N^v	3.282 (6)
Mo1—Mo2	3.3282 (9)	K2—OT8	3.301 (6)
Mo1—K1	3.772 (2)	K2—K2^v	3.700 (5)
Mo1—K2	3.877 (2)	OC3—Mo3^i	2.290 (4)
Mo2—OT10	1.712 (5)	OB6—Mo2^i	1.902 (5)
Mo2—OT9	1.718 (5)	OB6—K1^ii	2.690 (5)
Mo2—OB6^i	1.902 (5)	OT7—K2^ii	2.781 (6)
Mo2—OB5	1.947 (5)	OT10—K1^iv	2.760 (6)
Mo2—OC2	2.274 (4)	OT12—K2^vi	2.996 (6)
Mo2—OC3	2.298 (4)	OT12—K2^ii	3.075 (7)
Mo2—Mo3^i	3.3045 (9)	OT12—K1^ii	3.197 (6)
Mo2—Mo3	5.7396 (10)	OW13—K1^viii	3.207 (8)
Mo3—OT11	1.709 (5)	OW14—K1^vi	3.100 (19)
Mo3—OT12	1.719 (5)	ON16—N	1.232 (9)
Mo3—OB4	1.929 (5)	ON16—K1^v	2.786 (8)
Mo3—OB6	1.947 (4)	ON16—K2^v	2.859 (10)
Mo3—OC3^i	2.290 (4)	N—ON17	1.239 (15)
Mo3—OC1	2.312 (4)	ON17—K2^iii	2.888 (2)
Mo3—K1^ii	3.8387 (19)	ON17—K2^v	2.888 (2)
K1—OW14	2.627 (16)	N—ON16^ix	1.232 (9)
K1—OB6^iii	2.690 (5)	N—K2^iii	3.282 (6)
K1—OT10^iv	2.760 (6)	N—K2^v	3.282 (6)
K1—ON16^v	2.786 (8)
OC1—Co—OC1^i	180.0	OW14—K1—OB6^iii	89.9 (5)
OC1—Co—OC3	94.97 (19)	OW14—K1—OT10^iv	94.4 (5)
OC1^i—Co—OC3	85.03 (19)	OB6^iii—K1—OT10^iv	111.92 (17)
OC1—Co—OC3^i	85.03 (19)	OW14—K1—ON16^v	79.3 (4)
OC1^i—Co—OC3^i	94.97 (19)	OB6^iii—K1—ON16^v	110.83 (18)
OC3—Co—OC3^i	180.0	OT10^iv—K1—ON16^v	136.7 (2)
OC1—Co—OC2	84.14 (18)	OW14—K1—OT7	134.9 (5)
OC1^i—Co—OC2	95.86 (18)	OB6^iii—K1—OT7	133.34 (17)
OC3—Co—OC2	84.28 (18)	OT10^iv—K1—OT7	81.83 (17)
OC3^i—Co—OC2	95.72 (18)	ON16^v—K1—OT7	73.8 (2)
OC1—Co—OC2^i	95.86 (18)	OW14—K1—OW14^vi	38.4 (9)
OC1^i—Co—OC2^i	84.14 (18)	OB6^iii—K1—OW14^vi	123.4 (4)
OC3—Co—OC2^i	95.72 (18)	OT10^iv—K1—OW14^vi	65.9 (4)
OC3^i—Co—OC2^i	84.28 (18)	ON16^v—K1—OW14^vi	85.3 (3)
OC2—Co—OC2^i	180.0	OT7—K1—OW14^vi	103.1 (4)
OC1—Co—Mo1	42.33 (12)	OW14—K1—OT12^iii	87.6 (5)
OC1^i—Co—Mo1	137.67 (12)	OB6^iii—K1—OT12^iii	54.60 (14)
OC3—Co—Mo1	90.76 (13)	OT10^iv—K1—OT12^iii	166.43 (17)
OC3^i—Co—Mo1	89.24 (13)	ON16^v—K1—OT12^iii	56.83 (18)
OC2—Co—Mo1	41.84 (13)	OT7—K1—OT12^iii	106.19 (17)
OC2^i—Co—Mo1	138.16 (13)	OW14^vi—K1—OT12^iii	121.2 (4)
OC1—Co—Mo2	89.56 (13)	OW14—K1—OT8	150.9 (5)
OC1^i—Co—Mo2	90.44 (13)	OB6^iii—K1—OT8	81.94 (15)
OC3—Co—Mo2	42.48 (13)	OT10^iv—K1—OT8	114.55 (17)
OC3^i—Co—Mo2	137.52 (13)	ON16^v—K1—OT8	77.8 (2)
OC2—Co—Mo2	41.80 (13)	OT7—K1—OT8	52.86 (14)
OC2^i—Co—Mo2	138.20 (13)	OW14^vi—K1—OT8	153.6 (3)
Mo1—Co—Mo2	60.368 (16)	OT12^iii—K1—OT8	64.94 (15)
OC1—Co—Mo3	42.85 (13)	OW14—K1—OW13^vii	144.1 (4)
OC1^i—Co—Mo3	137.15 (13)	OB6^iii—K1—OW13^vii	71.10 (14)
OC3—Co—Mo3	137.82 (13)	OT10^iv—K1—OW13^vii	66.92 (16)
OC3^i—Co—Mo3	42.18 (13)	ON16^v—K1—OW13^vii	135.6 (2)
OC2—Co—Mo3	90.29 (13)	OT7—K1—OW13^vii	74.93 (15)
OC2^i—Co—Mo3	89.71 (13)	OW14^vi—K1—OW13^vii	132.5 (4)
Mo1—Co—Mo3	59.775 (15)	OT12^iii—K1—OW13^vii	104.06 (15)
Mo2—Co—Mo3	120.140 (15)	OT8—K1—OW13^vii	58.18 (15)
OT7—Mo1—OT8	105.5 (3)	OW14—K1—Mo1	152.9 (4)
OT7—Mo1—OB4	101.3 (2)	OB6^iii—K1—Mo1	107.99 (12)
OT8—Mo1—OB4	98.5 (2)	OT10^iv—K1—Mo1	97.33 (14)
OT7—Mo1—OB5	96.2 (2)	ON16^v—K1—Mo1	75.47 (19)
OT8—Mo1—OB5	99.8 (2)	OT7—K1—Mo1	25.89 (10)
OB4—Mo1—OB5	150.2 (2)	OW14^vi—K1—Mo1	128.6 (4)
OT7—Mo1—OC2	159.1 (2)	OT12^iii—K1—Mo1	86.68 (12)
OT8—Mo1—OC2	93.6 (2)	OT8—K1—Mo1	27.03 (9)
OB4—Mo1—OC2	83.77 (18)	OW13^vii—K1—Mo1	62.80 (11)
OB5—Mo1—OC2	71.81 (18)	OW14—K1—Mo3^iii	89.5 (5)
OT7—Mo1—OC1	93.6 (2)	OB6^iii—K1—Mo3^iii	28.31 (10)
OT8—Mo1—OC1	160.3 (2)	OT10^iv—K1—Mo3^iii	140.14 (14)
OB4—Mo1—OC1	72.74 (17)	ON16^v—K1—Mo3^iii	82.96 (14)
OB5—Mo1—OC1	82.35 (18)	OT7—K1—Mo3^iii	121.56 (12)
OC2—Mo1—OC1	68.30 (15)	OW14^vi—K1—Mo3^iii	127.9 (4)
OT7—Mo1—Mo3	89.27 (18)	OT12^iii—K1—Mo3^iii	26.32 (10)
OT8—Mo1—Mo3	129.5 (2)	OT8—K1—Mo3^iii	70.28 (9)
OB4—Mo1—Mo3	31.08 (13)	OW13^vii—K1—Mo3^iii	87.25 (11)
OB5—Mo1—Mo3	126.81 (14)	Mo1—K1—Mo3^iii	96.84 (5)
OC2—Mo1—Mo3	84.88 (11)	OW14—K1—K2^ii	100.1 (5)
OC1—Mo1—Mo3	44.47 (11)	OB6^iii—K1—K2^ii	170.00 (13)
OT7—Mo1—Co	127.15 (17)	OT10^iv—K1—K2^ii	67.46 (13)
OT8—Mo1—Co	127.28 (19)	ON16^v—K1—K2^ii	71.62 (14)
OB4—Mo1—Co	74.84 (14)	OT7—K1—K2^ii	37.09 (11)
OB5—Mo1—Co	75.38 (14)	OW14^vi—K1—K2^ii	66.0 (4)
OC2—Mo1—Co	34.27 (11)	OT12^iii—K1—K2^ii	125.43 (12)
OC1—Mo1—Co	34.06 (10)	OT8—K1—K2^ii	89.28 (11)
Mo3—Mo1—Co	60.161 (16)	OW13^vii—K1—K2^ii	100.20 (11)
OT7—Mo1—Mo2	127.47 (18)	Mo1—K1—K2^ii	62.75 (5)
OT8—Mo1—Mo2	88.71 (18)	Mo3^iii—K1—K2^ii	150.40 (7)
OB4—Mo1—Mo2	126.69 (14)	OW15—K2—OT7^iii	102.2 (3)
OB5—Mo1—Mo2	31.34 (14)	OW15—K2—OB4	81.8 (4)
OC2—Mo1—Mo2	42.96 (11)	OT7^iii—K2—OB4	111.27 (16)
OC1—Mo1—Mo2	83.09 (11)	OW15—K2—ON16	90.2 (4)
Mo3—Mo1—Mo2	120.00 (2)	OT7^iii—K2—ON16	72.47 (19)
Co—Mo1—Mo2	59.839 (15)	OB4—K2—ON16	171.7 (2)
OT7—Mo1—K1	47.93 (17)	OW15—K2—ON16^v	134.0 (3)
OT8—Mo1—K1	57.8 (2)	OT7^iii—K2—ON16^v	123.5 (2)
OB4—Mo1—K1	110.31 (14)	OB4—K2—ON16^v	85.37 (18)
OB5—Mo1—K1	99.32 (15)	ON16—K2—ON16^v	98.8 (2)
OC2—Mo1—K1	148.93 (11)	OW15—K2—ON17^v	91.8 (4)
OC1—Mo1—K1	141.52 (11)	OT7^iii—K2—ON17^v	164.9 (3)
Mo3—Mo1—K1	121.71 (4)	OB4—K2—ON17^v	64.54 (12)
Co—Mo1—K1	172.88 (3)	ON16—K2—ON17^v	113.81 (18)
Mo2—Mo1—K1	117.74 (4)	ON16^v—K2—ON17^v	43.5 (3)
OT7—Mo1—K2	96.32 (18)	OW15—K2—OT12^vi	71.7 (3)
OT8—Mo1—K2	57.85 (19)	OT7^iii—K2—OT12^vi	130.72 (16)
OB4—Mo1—K2	43.64 (14)	OB4—K2—OT12^vi	115.82 (16)
OB5—Mo1—K2	156.71 (14)	ON16—K2—OT12^vi	58.99 (18)
OC2—Mo1—K2	101.12 (11)	ON16^v—K2—OT12^vi	74.81 (19)
OC1—Mo1—K2	116.34 (12)	ON17^v—K2—OT12^vi	59.28 (13)
Mo3—Mo1—K2	72.93 (5)	OW15—K2—OT12^iii	162.6 (4)
Co—Mo1—K2	111.69 (5)	OT7^iii—K2—OT12^iii	66.50 (16)
Mo2—Mo1—K2	132.00 (4)	OB4—K2—OT12^iii	114.19 (17)
K1—Mo1—K2	75.06 (6)	ON16—K2—OT12^iii	74.0 (2)
OT10—Mo2—OT9	106.2 (3)	ON16^v—K2—OT12^iii	57.71 (18)
OT10—Mo2—OB6^i	101.3 (2)	ON17^v—K2—OT12^iii	101.2 (3)
OT9—Mo2—OB6^i	98.1 (2)	OT12^vi—K2—OT12^iii	104.90 (15)
OT10—Mo2—OB5	96.6 (2)	OW15—K2—N^v	113.7 (3)
OT9—Mo2—OB5	99.5 (2)	OT7^iii—K2—N^v	143.9 (2)
OB6^i—Mo2—OB5	150.3 (2)	OB4—K2—N^v	71.86 (13)
OT10—Mo2—OC2	157.8 (2)	ON16—K2—N^v	109.8 (2)
OT9—Mo2—OC2	94.6 (2)	ON16^v—K2—N^v	21.8 (2)
OB6^i—Mo2—OC2	82.98 (18)	ON17^v—K2—N^v	22.0 (3)
OB5—Mo2—OC2	71.89 (18)	OT12^vi—K2—N^v	67.86 (14)
OT10—Mo2—OC3	92.0 (2)	OT12^iii—K2—N^v	79.3 (2)
OT9—Mo2—OC3	161.0 (2)	OW15—K2—OT8	126.4 (4)
OB6^i—Mo2—OC3	72.26 (17)	OT7^iii—K2—OT8	74.58 (15)
OB5—Mo2—OC3	83.63 (17)	OB4—K2—OT8	52.95 (14)
OC2—Mo2—OC3	68.38 (15)	ON16—K2—OT8	135.0 (2)
OT10—Mo2—Mo3^i	88.4 (2)	ON16^v—K2—OT8	75.21 (19)
OT9—Mo2—Mo3^i	129.2 (2)	ON17^v—K2—OT8	92.47 (16)
OB6^i—Mo2—Mo3^i	31.23 (13)	OT12^vi—K2—OT8	148.78 (17)
OB5—Mo2—Mo3^i	127.42 (14)	OT12^iii—K2—OT8	65.13 (15)
OC2—Mo2—Mo3^i	84.28 (11)	N^v—K2—OT8	81.04 (15)
OC3—Mo2—Mo3^i	43.82 (11)	OW15—K2—K2^v	122.6 (4)
OT10—Mo2—Co	125.5 (2)	OT7^iii—K2—K2^v	101.35 (15)
OT9—Mo2—Co	128.3 (2)	OB4—K2—K2^v	133.88 (15)
OB6^i—Mo2—Co	74.89 (14)	ON16—K2—K2^v	49.8 (2)
OB5—Mo2—Co	75.38 (14)	ON16^v—K2—K2^v	49.00 (15)
OC2—Mo2—Co	34.23 (10)	ON17^v—K2—K2^v	75.38 (15)
OC3—Mo2—Co	34.15 (10)	OT12^vi—K2—K2^v	53.42 (13)
Mo3^i—Mo2—Co	60.095 (16)	OT12^iii—K2—K2^v	51.48 (12)
OT10—Mo2—Mo1	127.98 (19)	N^v—K2—K2^v	62.68 (12)
OT9—Mo2—Mo1	89.0 (2)	OT8—K2—K2^v	110.05 (16)
OB6^i—Mo2—Mo1	125.93 (15)	OW15—K2—Mo1	108.6 (4)
OB5—Mo2—Mo1	31.41 (13)	OT7^iii—K2—Mo1	96.76 (12)
OC2—Mo2—Mo1	42.96 (11)	OB4—K2—Mo1	28.05 (10)
OC3—Mo2—Mo1	84.03 (11)	ON16—K2—Mo1	160.2 (2)
Mo3^i—Mo2—Mo1	119.88 (2)	ON16^v—K2—Mo1	72.98 (15)
Co—Mo2—Mo1	59.793 (14)	ON17^v—K2—Mo1	72.93 (7)
OT10—Mo2—Mo3	133.27 (19)	OT12^vi—K2—Mo1	132.09 (11)
OT9—Mo2—Mo3	110.5 (2)	OT12^iii—K2—Mo1	86.54 (12)
OB6^i—Mo2—Mo3	101.04 (14)	N^v—K2—Mo1	69.03 (5)
OB5—Mo2—Mo3	50.14 (14)	OT8—K2—Mo1	26.20 (9)
OC2—Mo2—Mo3	26.32 (11)	K2^v—K2—Mo1	119.51 (12)
OC3—Mo2—Mo3	57.37 (10)	Co—OC1—Mo1	103.61 (17)
Mo3^i—Mo2—Mo3	90.033 (18)	Co—OC1—Mo3	103.03 (19)
Co—Mo2—Mo3	29.938 (8)	Mo1—OC1—Mo3	91.53 (15)
Mo1—Mo2—Mo3	29.858 (13)	Co—OC2—Mo2	103.97 (18)
OT11—Mo3—OT12	107.3 (3)	Co—OC2—Mo1	103.89 (18)
OT11—Mo3—OB4	98.7 (2)	Mo2—OC2—Mo1	94.08 (17)
OT12—Mo3—OB4	101.6 (2)	Co—OC3—Mo3^i	103.76 (19)
OT11—Mo3—OB6	99.6 (2)	Co—OC3—Mo2	103.37 (17)
OT12—Mo3—OB6	96.4 (2)	Mo3^i—OC3—Mo2	92.15 (15)
OB4—Mo3—OB6	149.06 (19)	Mo1—OB4—Mo3	118.0 (2)
OT11—Mo3—OC3^i	95.0 (2)	Mo1—OB4—K2	108.3 (2)
OT12—Mo3—OC3^i	156.4 (2)	Mo3—OB4—K2	128.3 (2)
OB4—Mo3—OC3^i	82.07 (18)	Mo2—OB5—Mo1	117.3 (2)
OB6—Mo3—OC3^i	71.71 (17)	Mo2^i—OB6—Mo3	118.3 (2)
OT11—Mo3—OC1	161.5 (2)	Mo2^i—OB6—K1^ii	130.8 (2)
OT12—Mo3—OC1	90.6 (2)	Mo3—OB6—K1^ii	110.7 (2)
OB4—Mo3—OC1	72.15 (17)	Mo1—OT7—K2^ii	148.7 (3)
OB6—Mo3—OC1	82.85 (18)	Mo1—OT7—K1	106.2 (2)
OC3^i—Mo3—OC1	68.18 (15)	K2^ii—OT7—K1	103.70 (18)
OT11—Mo3—Mo1	129.53 (19)	Mo1—OT8—K1	95.2 (2)
OT12—Mo3—Mo1	88.0 (2)	Mo1—OT8—K2	95.9 (2)
OB4—Mo3—Mo1	30.93 (13)	K1—OT8—K2	91.50 (15)
OB6—Mo3—Mo1	126.78 (14)	Mo2—OT10—K1^iv	159.3 (3)
OC3^i—Mo3—Mo1	83.55 (11)	Mo3—OT12—K2^vi	134.1 (3)
OC1—Mo3—Mo1	44.00 (10)	Mo3—OT12—K2^ii	142.8 (3)
OT11—Mo3—Co	128.7 (2)	K2^vi—OT12—K2^ii	75.10 (15)
OT12—Mo3—Co	123.97 (19)	Mo3—OT12—K1^ii	98.1 (2)
OB4—Mo3—Co	74.68 (13)	K2^vi—OT12—K1^ii	102.14 (16)
OB6—Mo3—Co	74.41 (13)	K2^ii—OT12—K1^ii	95.97 (16)
OC3^i—Mo3—Co	34.07 (11)	K1—OW14—K1^vi	106.4 (6)
OC1—Mo3—Co	34.11 (10)	N—ON16—K1^v	114.2 (5)
Mo1—Mo3—Co	60.064 (14)	N—ON16—K2	123.2 (5)
OT11—Mo3—K1^ii	111.53 (19)	K1^v—ON16—K2	118.4 (3)
OT12—Mo3—K1^ii	55.54 (18)	N—ON16—K2^v	98.8 (7)
OB4—Mo3—K1^ii	146.01 (15)	K1^v—ON16—K2^v	111.3 (3)
OB6—Mo3—K1^ii	40.95 (14)	K2—ON16—K2^v	81.2 (2)
OC3^i—Mo3—K1^ii	109.35 (11)	N—ON17—K2^iii	97.2 (2)
OC1—Mo3—K1^ii	82.43 (11)	N—ON17—K2^v	97.2 (2)
Mo1—Mo3—K1^ii	116.46 (4)	K2^iii—ON17—K2^v	165.6 (5)
Co—Mo3—K1^ii	96.71 (4)	ON16^ix—N—ON16	122.1 (13)
OT11—Mo3—Mo2	137.11 (19)	ON16^ix—N—ON17	119.0 (7)
OT12—Mo3—Mo2	107.4 (2)	ON16—N—ON17	119.0 (7)
OB4—Mo3—Mo2	49.91 (13)	ON16^ix—N—K2^iii	59.4 (5)
OB6—Mo3—Mo2	100.73 (14)	ON16—N—K2^iii	168.9 (3)
OC3^i—Mo3—Mo2	57.17 (11)	ON17—N—K2^iii	60.80 (19)
OC1—Mo3—Mo2	26.32 (10)	ON16^ix—N—K2^v	168.9 (3)
Mo1—Mo3—Mo2	30.146 (12)	ON16—N—K2^v	59.4 (5)
Co—Mo3—Mo2	29.922 (9)	ON17—N—K2^v	60.80 (19)
K1^ii—Mo3—Mo2	108.60 (4)	K2^iii—N—K2^v	121.6 (4)

Symmetry codes: (i) −x+1/2, −y+1/2, −z+1; (ii) x, −y, z−1/2; (iii) x, −y, z+1/2; (iv) −x+1/2, −y−1/2, −z+1; (v) −x+1, −y, −z+2; (vi) −x+1, y, −z+3/2; (vii) −x+1/2, y−1/2, −z+3/2; (viii) −x+1/2, y+1/2, −z+3/2; (ix) −x+1, y, −z+5/2.