Monolanthanum tripotassium tetra­hydrogen deca­molybdodicobaltate(III) trideca­hydrate

Lee, U.; Joo, H.-C.

doi:10.1107/S1600536810000929

inorganic compounds

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 66| Part 2| February 2010| Page i10

https://doi.org/10.1107/S1600536810000929

Open

access

Monolanthanum tripotassium tetrahydrogen decamolybdodicobaltate(III) tridecahydrate

Uk Lee ^a ^* and Hea-Chung Joo ^b

^aDepartment of Chemistry, Pukyong National University, 599-1 Daeyeon 3-dong, Nam-gu, Busan 608-737, Republic of Korea, and ^bDepartment of Chemistry, Dongeui University, San 24 Kaya-dong Busanjin-gu, Busan 614-714, Republic of Korea
^*Correspondence e-mail: uklee@pknu.ac.kr

(Received 30 December 2009; accepted 7 January 2010; online 23 January 2010)

The title compound, K₃La[H₄Mo₁₀Co₂O₃₈].13H₂O, is an optically active chiral polyoxometalate (POM) which contains an anion with ideal point symmetry D2 (222). The crystals containing one of the enantiomer pairs in the POM were resolved at pH 2.5. The factor that governs the formation of the compound is the pH condition of the mother liquor. The racemate salt, K₆[H₄Mo₁₀Co₂O₃₈]·7H₂O, is obtained at pH 6.5 [Nolan et al. (1998 ). Aust. J. Chem. 51. 825–834]. Two non-acidic H atoms in the POM form intramolecular hydrogen bonds and the remaining two H atoms form hydrogen bonds with two water molecules. The POMs are connected by three K⁺ ions. The La³⁺ ion is coordinated by three O atoms of the POM and six water molecues with distances in the range 2.516 (5)–2.589 (5) Å.

Related literature

For the crystal structures of [H₄Mo₁₀Co₂O₃₈]⁶⁻, see: Evans & Showell (1969 ); Nolan et al. (1998). For the optical resolution, see: Ama et al. (1970 ). For a review of chirality in POM chemistry, see: Hasenknopf et al. (2008 ). For bond-valence sum calculations, see: Brown & Altermatt (1985 ); Brese & O'Keeffe (1991 ).

Experimental

Crystal data

K₃La[H₄Mo₁₀Co₂O₃₈]·13H₂O
M_r = 2179.71
Monoclinic, P 2₁
a = 10.4487 (6) Å
b = 18.598 (1) Å
c = 12.3179 (8) Å
β = 112.957 (4)°
V = 2204.1 (2) Å³
Z = 2
Mo Kα radiation
μ = 4.83 mm⁻¹
T = 298 K
0.28 × 0.24 × 0.20 mm

Data collection

Stoe STADI-4 diffractometer
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 1996 ) T_min = 0.349, T_max = 0.527
10417 measured reflections
10104 independent reflections
9949 reflections with I > 2σ(I)
R_int = 0.016
3 standard reflections every 60 min intensity decay: 2.3%

Refinement

R[F² > 2σ(F²)] = 0.025
wR(F²) = 0.069
S = 1.10
10104 reflections
630 parameters
22 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 1.37 e Å⁻³
Δρ_min = −1.27 e Å⁻³
Absolute structure: Flack (1983 )
Flack parameter: 0.001 (10)

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O7C—H7⋯O30T	0.79 (4)	2.16 (5)	2.891 (6)	152 (8)
O8C—H8⋯O9W	0.85 (4)	2.26 (6)	2.972 (10)	141 (7)
O9C—H9⋯O8Wⁱ	0.82 (4)	2.21 (6)	2.935 (9)	147 (8)
O10C—H10⋯O21T	0.80 (4)	2.27 (6)	2.932 (6)	141 (8)
Symmetry code: (i) x-1, y, z-1.

Data collection: STADI-4 (Stoe & Cie, 1996); cell refinement: X-RED (Stoe & Cie, 1996); data reduction: X-RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 (Farrugia, 1997 ) and DIAMOND (Brandenburg, 1998 ); software used to prepare material for publication: SHELXL97.

Supporting information

Crystal structure: contains datablocks global, I. DOI: https://doi.org/10.1107/S1600536810000929/br2132sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536810000929/br2132Isup2.hkl

checkCIF report

Comment top

The ammonium salt of [H₄Mo₁₀Co₂O₃₈]^6- heteropolyoxometalte has been briefly reported as a typical chiral polyoxometalate (POM) (Evans et al. 1969) and the crystal strucure of potassium salt, K₆[H₄Mo₁₀Co₂O₃₈].7H₂O was reported in detail by P2₁/c space group (Nolan et al. 1998). The study of optical resolution of this POM was carrried out by using [Co(en)₃]³⁺ (Ama et al. 1970). One of the enantiomer pair salts was obtained as crystals. But the crystal structral study of this salt was not carried out. Recently, the micro review of chirality in POM chemistry has been reported (Hasenknopf et al. 2008). Somtimes, the lanthanide cation, having a very large oxide affinity and stability at low pH range, is useful in isolating POMs because the lanthanide forms a very stable salt with POMs.

The title compound was obtained as a lantahanide-alkali metal double salt in the monoclinic system in chiral space group P2₁. Here we report the enantimorphous structure of [H₄Mo₁₀Co₂O₃₈]^6- heteropolyoxometalate. The structure of the [H₄Mo₁₀Co₂O₃₈]^6- POM (Fig. 1) has been discussed in detail (Nolan et al., 1998). The O atoms are classified in the Fig. 1, viz., Ot (O16-O24, O29-O38; terminal Mo═O atom), Ob (O11-O14, O25-O28; O bridged µ₂-O atom), Oc (O7-O10; µ₃-O atom of a Co and two Mo atoms), Od (O1, O2, O5, O6; µ₄-O atom of a Co and three Mo atoms), and Oq (O3, O4; µ₄-O atom of two Co and two Mo atoms). Fig. 2 shows the two enantiomers.

The four protonated O atoms, Oc(H) in the POM, were identified (Nolan et al., 1998) by calculation of bond-valence sums (BVS; Brown & Altermatt, 1985; Brese & O'Keeffe, 1991). The positions of four non-acidic H atoms on Oc atoms were found on difference Fourier map in this report. These H atoms formed hydrogen bond intramoleculely and with water molecules (Table. 1). All the water molecules formed hydrogen bonds with O atoms in the polyanions, and there are also Ow–H···Ow hydrogen-bond interactions except zeolitic O13w molecule. K⁺ ions are coordinated by eight O atoms, viz. [K1(Ot)₇(Ow)]⁺, [K2(Ot)₃(Ow)₄]⁺, and [K3(Ot)₃(Ob)₂(Ow)₃]⁺ in the range 2.69 (1)-3.276 (6) Å. La³⁺ ion is coordinated by nine O atoms, viz. [La(Ot)₃(Ow)₆]³⁺ in the range 2.516 (5)-2.589 (5) Å.

Related literature top

For the crystal structures of [H₄Mo₁₀Co₂O₃₈]^6-, see: Evans & Showell (1969); Nolan et al. (1998). For the optical resolution, see: Ama et al. (1970). For a review of chirality in POM chemistry, see: Hasenknopf et al. (2008). For bond-valence sum calculations, see: Brown & Altermatt (1985); Brese & O'Keeffe (1991).

Experimental top

Crystals of the title compound were obtained from the aqueous solution of La(NO₃)₃.6H₂O and K₆[H₄Co₂Mo₁₀O₃₈].7H₂O (Nolan et al., 1998) at pH 2.5.

Structure description top

Computing details top

Data collection: STADI-4 (Stoe & Cie, 1996); cell refinement: X-RED (Stoe & Cie, 1996); data reduction: X-RED (Stoe & Cie, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 (Farrugia, 1997) and DIAMOND (Brandenburg, 1998); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top

	Fig. 1. The structure of the [H₄Mo₁₀Co₂O₃₈]^6- POM with the atom numbering scheme. Displacement ellipsoids are drawn at the 50% probability level. H atoms are presented as a small spheres of arbitrary radius.
	Fig. 2. The two enantiomers of the La[Mo₁₀Co₂O₃₈]^7- POM. The structure described here is (A).

Monolanthanum tripotassium tetrahydrogen decamolybdodicobaltate(III) tridecahydrate top

Crystal data top

LaK₃[H₄Mo₁₀Co₂O₃₈]·13H₂O	F(000) = 2052
M_r = 2179.71	D_x = 3.284 Mg m⁻³
Monoclinic, P2₁	Mo Kα radiation, λ = 0.71069 Å
Hall symbol: P 2yb	Cell parameters from 28 reflections
a = 10.4487 (6) Å	θ = 19.0–20.9°
b = 18.598 (1) Å	µ = 4.83 mm⁻¹
c = 12.3179 (8) Å	T = 298 K
β = 112.957 (4)°	Polyhedron, blue
V = 2204.1 (2) Å³	0.28 × 0.24 × 0.20 mm
Z = 2

Data collection top

Stoe STADI-4 diffractometer	9949 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.016
Graphite monochromator	θ_max = 27.5°, θ_min = 1.8°
ω/2θ scans	h = −13→13
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 1996)	k = −24→24
T_min = 0.349, T_max = 0.527	l = −15→15
10417 measured reflections	3 standard reflections every 60 min
10104 independent reflections	intensity decay: 2.3%

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	H atoms treated by a mixture of independent and constrained refinement
R[F² > 2σ(F²)] = 0.025	w = 1/[σ²(F_o²) + (0.0432P)² + 5.9397P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.069	(Δ/σ)_max < 0.001
S = 1.10	Δρ_max = 1.37 e Å⁻³
10104 reflections	Δρ_min = −1.27 e Å⁻³
630 parameters	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
22 restraints	Extinction coefficient: 0.00255 (10)
Primary atom site location: structure-invariant direct methods	Absolute structure: Flack (1983)
Secondary atom site location: difference Fourier map	Absolute structure parameter: 0.001 (10)

Crystal data top

LaK₃[H₄Mo₁₀Co₂O₃₈]·13H₂O	V = 2204.1 (2) Å³
M_r = 2179.71	Z = 2
Monoclinic, P2₁	Mo Kα radiation
a = 10.4487 (6) Å	µ = 4.83 mm⁻¹
b = 18.598 (1) Å	T = 298 K
c = 12.3179 (8) Å	0.28 × 0.24 × 0.20 mm
β = 112.957 (4)°

Data collection top

Stoe STADI-4 diffractometer	9949 reflections with I > 2σ(I)
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 1996)	R_int = 0.016
T_min = 0.349, T_max = 0.527	3 standard reflections every 60 min
10417 measured reflections	intensity decay: 2.3%
10104 independent reflections

Refinement top

R[F² > 2σ(F²)] = 0.025	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.069	Δρ_max = 1.37 e Å⁻³
S = 1.10	Δρ_min = −1.27 e Å⁻³
10104 reflections	Absolute structure: Flack (1983)
630 parameters	Absolute structure parameter: 0.001 (10)
22 restraints

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 > 2sigma(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
La	0.44544 (3)	0.446924 (17)	0.14123 (3)	0.01703 (7)
Mo1	0.35787 (6)	0.30183 (3)	0.62418 (4)	0.02049 (11)
Mo2	0.09792 (5)	0.18531 (3)	0.54287 (4)	0.01769 (10)
Mo3	−0.02214 (5)	0.11683 (3)	0.27366 (4)	0.01671 (10)
Mo4	0.42999 (5)	0.23358 (2)	0.20358 (4)	0.01407 (9)
Mo5	0.51945 (5)	0.32853 (3)	0.44537 (4)	0.01653 (10)
Mo6	0.13311 (5)	0.32304 (2)	0.16909 (4)	0.01389 (9)
Mo7	0.05653 (5)	0.25070 (3)	−0.09176 (4)	0.01733 (10)
Mo8	0.06410 (5)	0.07332 (3)	−0.11493 (4)	0.01639 (10)
Mo9	0.18216 (5)	−0.02480 (3)	0.12967 (4)	0.01894 (10)
Mo10	0.30682 (5)	0.05651 (2)	0.38835 (4)	0.01552 (9)
Co1	0.25776 (8)	0.21760 (4)	0.36757 (6)	0.01310 (14)
Co2	0.16831 (8)	0.15142 (4)	0.14734 (6)	0.01251 (14)
K1	0.0300 (2)	−0.11545 (10)	0.3699 (2)	0.0461 (4)
K2	0.6309 (3)	0.28591 (13)	0.9870 (2)	0.0595 (6)
K3	0.6994 (3)	0.11419 (19)	0.4003 (3)	0.0811 (8)
O1D	0.1934 (4)	0.1345 (2)	0.4209 (3)	0.0144 (7)
O2D	0.3143 (4)	0.2948 (2)	0.2990 (3)	0.0152 (8)
O3Q	0.3316 (4)	0.1562 (2)	0.2853 (4)	0.0165 (8)
O4Q	0.0974 (4)	0.2140 (2)	0.2295 (3)	0.0148 (7)
O5D	0.1119 (4)	0.0722 (2)	0.2175 (3)	0.0153 (7)
O6D	0.2314 (4)	0.2341 (2)	0.0927 (3)	0.0146 (7)
O7C	0.1753 (4)	0.2738 (2)	0.4538 (3)	0.0154 (7)
H7	0.130 (7)	0.305 (4)	0.412 (6)	0.023*
O8C	0.4303 (4)	0.2347 (2)	0.5049 (3)	0.0168 (8)
H8	0.487 (7)	0.201 (3)	0.512 (7)	0.025*
O9C	0.0078 (4)	0.1540 (2)	−0.0016 (4)	0.0177 (8)
H9	−0.073 (5)	0.159 (5)	−0.007 (7)	0.027*
O10C	0.2394 (4)	0.0811 (2)	0.0682 (4)	0.0164 (8)
H10	0.312 (6)	0.091 (4)	0.066 (7)	0.025*
O11B	0.2833 (5)	0.2093 (3)	0.6447 (4)	0.0247 (9)
O12B	−0.0505 (4)	0.1808 (2)	0.3825 (4)	0.0202 (8)
O13B	0.5637 (4)	0.2485 (2)	0.3574 (4)	0.0177 (8)
O14B	0.4073 (5)	0.3666 (2)	0.5211 (4)	0.0217 (8)
O15T	0.5119 (5)	0.2980 (3)	0.7427 (4)	0.0347 (11)
O16T	0.2563 (6)	0.3602 (3)	0.6628 (5)	0.0337 (11)
O17T	0.0054 (6)	0.2421 (3)	0.5929 (4)	0.0316 (11)
O18T	0.0785 (6)	0.1022 (3)	0.5926 (5)	0.0320 (11)
O19T	−0.0674 (6)	0.0388 (3)	0.3207 (5)	0.0333 (11)
O20T	−0.1582 (5)	0.1366 (3)	0.1435 (4)	0.0292 (10)
O21T	0.4985 (5)	0.1640 (3)	0.1549 (4)	0.0256 (9)
O22T	0.4651 (4)	0.3102 (2)	0.1398 (4)	0.0202 (8)
O23T	0.5226 (5)	0.3973 (2)	0.3514 (4)	0.0246 (9)
O24T	0.6782 (5)	0.3278 (3)	0.5558 (4)	0.0291 (10)
O25B	−0.0026 (4)	0.3003 (2)	0.0225 (4)	0.0191 (8)
O26B	0.1374 (4)	0.1659 (2)	−0.1320 (4)	0.0205 (8)
O27B	0.0277 (4)	0.0062 (2)	−0.0117 (4)	0.0203 (8)
O28B	0.3425 (5)	0.0027 (2)	0.2733 (4)	0.0215 (9)
O29T	0.2215 (4)	0.3920 (2)	0.1336 (4)	0.0223 (9)
O30T	0.0460 (5)	0.3621 (2)	0.2463 (4)	0.0228 (9)
O31T	0.1538 (5)	0.3148 (2)	−0.1229 (4)	0.0260 (9)
O32T	−0.1007 (5)	0.2530 (3)	−0.2044 (4)	0.0298 (10)
O33T	−0.0996 (5)	0.0761 (3)	−0.2239 (4)	0.0278 (10)
O34T	0.1615 (5)	0.0218 (3)	−0.1690 (4)	0.0258 (9)
O35T	0.2728 (6)	−0.0787 (3)	0.0729 (5)	0.0336 (11)
O36T	0.0954 (6)	−0.0806 (3)	0.1858 (5)	0.0334 (11)
O37T	0.4685 (5)	0.0749 (3)	0.4933 (4)	0.0279 (10)
O38T	0.2395 (5)	−0.0078 (3)	0.4493 (4)	0.0264 (9)
O1W	0.3980 (6)	0.3956 (3)	−0.0655 (4)	0.0354 (12)
H1A	0.429 (11)	0.419 (5)	−0.117 (8)	0.053*
H1B	0.327 (9)	0.373 (5)	−0.060 (9)	0.053*
O2W	0.5027 (5)	0.5444 (3)	0.0224 (4)	0.0336 (11)
H2A	0.5342	0.5939	0.0474	0.050*
H2B	0.4543	0.5348	−0.0603	0.050*
O3W	0.6426 (6)	0.5253 (3)	0.2868 (5)	0.0436 (14)
H3A	0.7189	0.4949	0.3327	0.065*
H3B	0.6734	0.5593	0.2435	0.065*
O4W	0.2314 (5)	0.5129 (3)	0.0086 (5)	0.0403 (13)
H4A	0.2581	0.5535	−0.0260	0.060*
H4B	0.1804	0.5293	0.0540	0.060*
O5W	0.6810 (5)	0.3994 (3)	0.1512 (5)	0.0337 (11)
H5A	0.7359	0.3822	0.2301	0.051*
H5B	0.7321	0.4376	0.1325	0.051*
O6W	0.3676 (6)	0.5322 (4)	0.2677 (5)	0.0470 (16)
H6A	0.4185	0.5505	0.3236	0.071*
H6B	0.2906	0.5318	0.2551	0.071*
O7W	0.0072 (8)	−0.0501 (4)	0.5720 (7)	0.067 (2)
H7A	0.0214	−0.0456	0.6523	0.101*
H7B	0.0600	−0.0188	0.5680	0.101*
O8W	0.7068 (8)	0.1744 (5)	0.8755 (8)	0.069 (2)
H8A	0.7537	0.1937	0.8288	0.104*
H8B	0.6251	0.1489	0.8255	0.104*
O9W	0.7144 (9)	0.1721 (4)	0.6059 (9)	0.115 (5)
H9A	0.7267	0.2218	0.6169	0.172*
H9B	0.7625	0.1503	0.6639	0.172*
O10W	0.7381 (9)	−0.0065 (4)	0.5288 (12)	0.110 (5)
H10A	0.8166	−0.0032	0.5439	0.165*
H10B	0.7127	0.0026	0.5759	0.165*
O11W	0.4099 (6)	0.1777 (3)	0.8878 (5)	0.0381 (12)
H11A	0.3306	0.1915	0.9041	0.057*
H11C	0.3838	0.1748	0.8041	0.057*
O12W	0.5854 (7)	−0.0010 (4)	0.2258 (6)	0.0480 (15)
H12A	0.515 (7)	−0.010 (7)	0.246 (10)	0.072*
H12B	0.650 (8)	−0.027 (6)	0.290 (8)	0.072*
O13W	0.8073 (8)	0.3096 (4)	0.3319 (9)	0.077 (3)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
La	0.01867 (15)	0.01501 (14)	0.01674 (15)	−0.00193 (12)	0.00619 (11)	0.00159 (11)
Mo1	0.0262 (3)	0.0214 (2)	0.0125 (2)	−0.00452 (19)	0.00618 (19)	−0.00344 (18)
Mo2	0.0230 (2)	0.0174 (2)	0.0143 (2)	−0.00067 (18)	0.00903 (18)	0.00012 (17)
Mo3	0.0166 (2)	0.0177 (2)	0.0167 (2)	−0.00258 (17)	0.00736 (18)	−0.00267 (17)
Mo4	0.0144 (2)	0.0130 (2)	0.0148 (2)	−0.00060 (16)	0.00567 (16)	0.00003 (16)
Mo5	0.0182 (2)	0.0155 (2)	0.0132 (2)	−0.00354 (17)	0.00326 (17)	0.00012 (17)
Mo6	0.0151 (2)	0.0118 (2)	0.0142 (2)	0.00074 (16)	0.00515 (16)	0.00089 (16)
Mo7	0.0207 (2)	0.0162 (2)	0.0136 (2)	0.00059 (17)	0.00507 (17)	0.00143 (17)
Mo8	0.0162 (2)	0.0170 (2)	0.0149 (2)	0.00093 (17)	0.00489 (17)	−0.00296 (17)
Mo9	0.0241 (2)	0.0126 (2)	0.0193 (2)	−0.00084 (18)	0.00764 (19)	−0.00130 (17)
Mo10	0.0178 (2)	0.0132 (2)	0.0144 (2)	0.00079 (17)	0.00502 (16)	0.00198 (16)
Co1	0.0160 (3)	0.0119 (3)	0.0106 (3)	−0.0016 (3)	0.0043 (3)	−0.0003 (2)
Co2	0.0148 (3)	0.0104 (3)	0.0115 (3)	−0.0005 (2)	0.0043 (3)	−0.0003 (2)
K1	0.0452 (10)	0.0339 (9)	0.0664 (12)	−0.0074 (7)	0.0297 (9)	0.0064 (8)
K2	0.0837 (16)	0.0500 (12)	0.0427 (11)	−0.0020 (11)	0.0224 (11)	−0.0147 (9)
K3	0.0781 (18)	0.0793 (19)	0.087 (2)	0.0011 (15)	0.0335 (16)	−0.0015 (16)
O1D	0.022 (2)	0.0108 (17)	0.0138 (17)	−0.0020 (14)	0.0103 (15)	−0.0014 (14)
O2D	0.0138 (18)	0.0146 (18)	0.0137 (18)	−0.0019 (14)	0.0015 (15)	0.0010 (14)
O3Q	0.021 (2)	0.0143 (18)	0.0153 (18)	0.0000 (15)	0.0076 (16)	0.0013 (14)
O4Q	0.0154 (18)	0.0138 (18)	0.0129 (17)	−0.0014 (14)	0.0033 (14)	0.0004 (14)
O5D	0.0175 (18)	0.0121 (18)	0.0160 (18)	−0.0011 (14)	0.0063 (15)	0.0002 (14)
O6D	0.0160 (17)	0.0128 (17)	0.0127 (17)	−0.0025 (15)	0.0031 (14)	0.0015 (14)
O7C	0.021 (2)	0.0117 (17)	0.0128 (18)	−0.0010 (15)	0.0053 (15)	−0.0004 (14)
O8C	0.0208 (19)	0.0126 (18)	0.0155 (18)	0.0023 (15)	0.0053 (15)	0.0035 (14)
O9C	0.0156 (18)	0.019 (2)	0.0180 (19)	−0.0010 (16)	0.0059 (16)	−0.0024 (15)
O10C	0.0157 (18)	0.0152 (18)	0.0175 (19)	−0.0008 (15)	0.0056 (15)	−0.0008 (15)
O11B	0.027 (2)	0.027 (2)	0.019 (2)	−0.0025 (18)	0.0072 (18)	0.0035 (17)
O12B	0.021 (2)	0.021 (2)	0.019 (2)	0.0033 (16)	0.0083 (16)	−0.0012 (16)
O13B	0.0154 (18)	0.018 (2)	0.0174 (19)	−0.0010 (15)	0.0043 (15)	−0.0003 (15)
O14B	0.033 (2)	0.0134 (18)	0.022 (2)	−0.0033 (17)	0.0131 (18)	−0.0028 (16)
O15T	0.036 (3)	0.043 (3)	0.020 (2)	−0.010 (2)	0.006 (2)	−0.006 (2)
O16T	0.042 (3)	0.033 (3)	0.031 (2)	−0.001 (2)	0.020 (2)	−0.006 (2)
O17T	0.043 (3)	0.029 (3)	0.029 (2)	0.005 (2)	0.020 (2)	−0.005 (2)
O18T	0.041 (3)	0.027 (2)	0.031 (2)	−0.005 (2)	0.017 (2)	0.004 (2)
O19T	0.040 (3)	0.025 (2)	0.041 (3)	−0.004 (2)	0.022 (2)	0.001 (2)
O20T	0.019 (2)	0.039 (3)	0.026 (2)	0.0009 (18)	0.0043 (18)	−0.005 (2)
O21T	0.029 (2)	0.021 (2)	0.029 (2)	−0.0005 (18)	0.0133 (19)	−0.0043 (17)
O22T	0.022 (2)	0.020 (2)	0.021 (2)	−0.0010 (16)	0.0103 (17)	0.0050 (16)
O23T	0.028 (2)	0.021 (2)	0.021 (2)	−0.0080 (18)	0.0054 (18)	−0.0030 (17)
O24T	0.027 (2)	0.026 (2)	0.027 (2)	−0.0026 (19)	0.0034 (19)	0.0036 (19)
O25B	0.0191 (19)	0.0190 (19)	0.0174 (19)	0.0049 (16)	0.0052 (16)	0.0001 (16)
O26B	0.023 (2)	0.022 (2)	0.019 (2)	0.0008 (17)	0.0111 (17)	0.0024 (16)
O27B	0.020 (2)	0.020 (2)	0.020 (2)	−0.0043 (16)	0.0071 (16)	−0.0037 (16)
O28B	0.022 (2)	0.018 (2)	0.021 (2)	0.0026 (16)	0.0056 (17)	0.0000 (16)
O29T	0.020 (2)	0.020 (2)	0.024 (2)	0.0011 (16)	0.0055 (17)	0.0069 (17)
O30T	0.029 (2)	0.018 (2)	0.023 (2)	0.0017 (17)	0.0121 (18)	−0.0042 (17)
O31T	0.031 (2)	0.020 (2)	0.030 (2)	−0.0030 (18)	0.0149 (19)	0.0047 (18)
O32T	0.030 (2)	0.030 (2)	0.021 (2)	0.005 (2)	0.0013 (18)	0.0008 (19)
O33T	0.025 (2)	0.030 (2)	0.025 (2)	0.0004 (19)	0.0060 (18)	−0.0020 (19)
O34T	0.033 (2)	0.023 (2)	0.025 (2)	0.0072 (19)	0.0155 (19)	−0.0044 (18)
O35T	0.043 (3)	0.027 (2)	0.031 (3)	0.009 (2)	0.016 (2)	−0.005 (2)
O36T	0.043 (3)	0.022 (2)	0.033 (3)	−0.007 (2)	0.013 (2)	0.000 (2)
O37T	0.026 (2)	0.030 (2)	0.022 (2)	0.0021 (19)	0.0039 (18)	0.0057 (18)
O38T	0.033 (2)	0.020 (2)	0.028 (2)	0.0039 (18)	0.014 (2)	0.0063 (18)
O1W	0.049 (3)	0.036 (3)	0.020 (2)	−0.013 (2)	0.012 (2)	−0.003 (2)
O2W	0.033 (3)	0.035 (3)	0.029 (2)	−0.011 (2)	0.008 (2)	0.006 (2)
O3W	0.042 (3)	0.053 (4)	0.034 (3)	−0.025 (3)	0.014 (2)	−0.016 (3)
O4W	0.024 (2)	0.046 (3)	0.047 (3)	0.006 (2)	0.010 (2)	0.027 (3)
O5W	0.030 (2)	0.033 (3)	0.042 (3)	−0.008 (2)	0.017 (2)	0.003 (2)
O6W	0.028 (3)	0.061 (4)	0.042 (3)	0.008 (3)	0.003 (2)	−0.025 (3)
O7W	0.080 (5)	0.054 (4)	0.056 (4)	−0.028 (4)	0.013 (4)	0.006 (4)
O8W	0.062 (5)	0.072 (5)	0.089 (6)	0.009 (4)	0.045 (4)	0.015 (5)
O9W	0.086 (6)	0.044 (4)	0.118 (8)	−0.021 (4)	−0.064 (6)	0.034 (5)
O10W	0.055 (5)	0.031 (4)	0.231 (14)	−0.005 (3)	0.040 (7)	−0.025 (6)
O11W	0.040 (3)	0.046 (3)	0.033 (3)	0.009 (2)	0.019 (2)	0.012 (2)
O12W	0.038 (3)	0.052 (4)	0.054 (4)	−0.001 (3)	0.018 (3)	−0.015 (3)
O13W	0.050 (4)	0.061 (5)	0.128 (7)	0.027 (4)	0.045 (5)	0.050 (5)

Geometric parameters (Å, º) top

Mo1—Mo5	3.2938 (7)	Mo6—O30T	1.714 (4)
Mo1—Mo2	3.3098 (7)	Mo6—O29T	1.734 (4)
Mo1—Co1	3.3106 (9)	Mo6—O25B	1.858 (4)
Mo2—Co1	3.2599 (9)	Mo6—O2D	2.014 (4)
Mo2—Mo3	3.3086 (7)	Mo6—O4Q	2.240 (4)
Mo3—Co2	3.0348 (9)	Mo6—O6D	2.330 (4)
Mo3—Co1	3.2809 (9)	Mo7—O32T	1.688 (5)
Mo3—Mo10	3.3586 (7)	Mo7—O31T	1.705 (4)
Mo3—Mo9	4.1946 (7)	Mo7—O26B	1.943 (4)
Mo4—O21T	1.697 (5)	Mo7—O25B	1.973 (4)
Mo4—O22T	1.734 (4)	Mo7—O9C	2.273 (4)
Mo4—O13B	1.885 (4)	Mo7—O6D	2.314 (4)
Mo4—O6D	1.991 (4)	Mo8—O34T	1.710 (4)
Mo4—O3Q	2.224 (4)	Mo8—O33T	1.714 (5)
Mo4—O2D	2.290 (4)	Mo8—O27B	1.922 (4)
Mo4—Co2	2.9687 (9)	Mo8—O26B	1.928 (4)
Mo4—Co1	3.2004 (9)	Mo8—O9C	2.278 (4)
Mo4—Mo6	3.3975 (7)	Mo8—O10C	2.290 (4)
Mo5—Co1	3.2569 (9)	Mo9—O36T	1.693 (5)
Mo5—Mo6	4.1438 (7)	Mo9—O35T	1.705 (5)
Mo5—Co2	5.2232 (9)	Mo9—O27B	1.944 (4)
Mo6—Co1	3.0057 (8)	Mo9—O28B	1.972 (4)
Mo6—Co2	3.2359 (9)	Mo9—O10C	2.271 (4)
Mo6—Mo7	3.2816 (7)	Mo9—O5D	2.363 (4)
Mo7—Co2	3.2810 (9)	Mo10—O38T	1.704 (5)
Mo8—Co2	3.3148 (8)	Mo10—O37T	1.714 (5)
Mo8—Mo9	3.3213 (7)	Mo10—O28B	1.887 (4)
Mo9—Co2	3.2915 (9)	Mo10—O1D	2.009 (4)
Mo9—Mo10	3.3014 (7)	Mo10—O5D	2.306 (4)
Mo10—Co1	3.0334 (9)	Mo10—O3Q	2.318 (4)
Mo10—Co2	3.2667 (9)	Co1—O4Q	1.866 (4)
Co1—Co2	2.7874 (10)	Co1—O2D	1.874 (4)
La—O4W	2.516 (5)	Co1—O3Q	1.880 (4)
La—O29T	2.521 (4)	Co1—O1D	1.902 (4)
La—O2W	2.543 (5)	Co1—O7C	1.918 (4)
La—O22T	2.552 (4)	Co1—O8C	1.958 (4)
La—O23T	2.564 (5)	Co2—O4Q	1.874 (4)
La—O6W	2.567 (5)	Co2—O3Q	1.883 (4)
La—O5W	2.572 (5)	Co2—O6D	1.897 (4)
La—O1W	2.579 (5)	Co2—O5D	1.913 (4)
La—O3W	2.589 (5)	Co2—O10C	1.944 (4)
Mo1—O15T	1.702 (5)	Co2—O9C	1.944 (4)
Mo1—O16T	1.711 (5)	K1—O36T	2.690 (6)
Mo1—O11B	1.946 (5)	K1—O17Tⁱ	2.739 (5)
Mo1—O14B	1.960 (4)	K1—O38T	2.843 (5)
Mo1—O8C	2.271 (4)	K1—O7W	2.863 (9)
Mo1—O7C	2.279 (4)	K1—O16Tⁱ	2.894 (6)
Mo2—O17T	1.701 (5)	K1—O24Tⁱⁱ	3.011 (5)
Mo2—O18T	1.704 (5)	K1—O19T	3.025 (6)
Mo2—O11B	1.905 (5)	K1—O31Tⁱⁱⁱ	3.174 (5)
Mo2—O12B	1.981 (4)	K2—O8W	2.770 (9)
Mo2—O7C	2.293 (4)	K2—O15T	2.781 (5)
Mo2—O1D	2.306 (4)	K2—O5W^iv	2.827 (6)
Mo3—O19T	1.697 (5)	K2—O35T^v	2.912 (5)
Mo3—O20T	1.717 (5)	K2—O11W	2.945 (7)
Mo3—O12B	1.900 (4)	K2—O1W^iv	3.046 (7)
Mo3—O5D	1.971 (4)	K2—O22T^iv	3.048 (5)
Mo3—O1D	2.299 (4)	K3—O10W	2.685 (12)
Mo3—O4Q	2.378 (4)	K3—O9W	2.700 (13)
Mo5—O24T	1.686 (5)	K3—O13B	2.819 (5)
Mo5—O23T	1.734 (5)	K3—O12W	2.939 (7)
Mo5—O14B	1.898 (4)	K3—O12B^vi	2.977 (5)
Mo5—O13B	1.998 (4)	K3—O21T	3.075 (6)
Mo5—O8C	2.232 (4)	K3—O37T	3.134 (6)
Mo5—O2D	2.286 (4)	K3—O19T^vi	3.276 (6)

Co2—Mo3—Mo9	51.149 (17)	O34T—Mo8—O26B	97.8 (2)
Co1—Mo3—Mo9	88.689 (18)	O33T—Mo8—O26B	101.8 (2)
Mo2—Mo3—Mo9	127.515 (17)	O27B—Mo8—O26B	147.24 (18)
Mo10—Mo3—Mo9	50.358 (13)	O34T—Mo8—O9C	160.5 (2)
Co2—Mo4—Mo6	60.658 (18)	O33T—Mo8—O9C	92.4 (2)
Co1—Mo4—Mo6	54.102 (17)	O27B—Mo8—O9C	81.79 (17)
Co1—Mo5—Mo6	46.018 (15)	O26B—Mo8—O9C	71.78 (17)
Mo1—Mo5—Mo6	87.491 (16)	O34T—Mo8—O10C	92.88 (19)
Co1—Mo6—Mo7	113.07 (2)	O33T—Mo8—O10C	160.05 (19)
Co2—Mo6—Mo7	60.447 (17)	O27B—Mo8—O10C	71.20 (16)
Co1—Mo6—Mo5	51.231 (17)	O26B—Mo8—O10C	81.51 (16)
Co2—Mo6—Mo5	89.230 (18)	O9C—Mo8—O10C	69.71 (15)
Mo7—Mo6—Mo5	126.989 (17)	O36T—Mo9—O35T	106.2 (3)
Mo4—Mo6—Mo5	50.202 (12)	O36T—Mo9—O27B	99.1 (2)
Co2—Mo8—Mo9	59.471 (17)	O35T—Mo9—O27B	101.9 (2)
Co2—Mo9—Mo8	60.167 (17)	O36T—Mo9—O28B	101.3 (2)
Mo10—Mo9—Mo8	119.405 (19)	O35T—Mo9—O28B	96.2 (2)
Co2—Mo9—Mo3	45.892 (16)	O27B—Mo9—O28B	147.68 (18)
Mo10—Mo9—Mo3	51.573 (13)	O36T—Mo9—O10C	156.9 (2)
Mo8—Mo9—Mo3	88.185 (16)	O35T—Mo9—O10C	96.4 (2)
Co1—Mo10—Mo3	61.518 (18)	O27B—Mo9—O10C	71.25 (16)
Co2—Mo10—Mo3	54.502 (17)	O28B—Mo9—O10C	80.34 (17)
Mo9—Mo10—Mo3	78.068 (16)	O36T—Mo9—O5D	88.2 (2)
Mo6—Co1—Mo10	135.92 (3)	O35T—Mo9—O5D	163.3 (2)
Co2—Co1—Mo5	119.37 (3)	O27B—Mo9—O5D	83.44 (16)
Mo6—Co1—Mo5	82.75 (2)	O28B—Mo9—O5D	72.42 (16)
Mo10—Co1—Mo5	120.40 (3)	O10C—Mo9—O5D	70.10 (14)
Mo4—Co1—Mo5	60.838 (18)	O38T—Mo10—O37T	105.2 (2)
Co2—Co1—Mo2	119.96 (3)	O38T—Mo10—O28B	101.3 (2)
Mo6—Co1—Mo2	119.18 (3)	O37T—Mo10—O28B	104.3 (2)
Mo10—Co1—Mo2	82.85 (2)	O38T—Mo10—O1D	92.40 (19)
Mo4—Co1—Mo2	174.10 (3)	O37T—Mo10—O1D	101.0 (2)
Mo5—Co1—Mo2	120.67 (2)	O28B—Mo10—O1D	146.84 (17)
Co1—Co2—Mo3	68.45 (2)	O38T—Mo10—O5D	97.01 (19)
Mo4—Co2—Mo3	135.88 (3)	O37T—Mo10—O5D	157.32 (19)
Co1—Co2—Mo6	59.31 (2)	O28B—Mo10—O5D	75.21 (16)
Mo4—Co2—Mo6	66.238 (19)	O1D—Mo10—O5D	73.20 (15)
Mo3—Co2—Mo6	92.76 (2)	O38T—Mo10—O3Q	163.06 (19)
Co1—Co2—Mo10	59.51 (2)	O37T—Mo10—O3Q	88.05 (19)
Mo4—Co2—Mo10	91.42 (2)	O28B—Mo10—O3Q	85.20 (17)
Mo3—Co2—Mo10	64.292 (19)	O1D—Mo10—O3Q	74.46 (15)
Mo6—Co2—Mo10	118.82 (2)	O5D—Mo10—O3Q	69.28 (14)
Co1—Co2—Mo7	119.47 (3)	O4Q—Co1—O2D	86.85 (17)
Mo4—Co2—Mo7	83.84 (2)	O4Q—Co1—O3Q	84.16 (17)
Mo3—Co2—Mo7	120.30 (3)	O2D—Co1—O3Q	87.36 (18)
Mo6—Co2—Mo7	60.465 (17)	O4Q—Co1—O1D	88.47 (18)
Mo10—Co2—Mo7	175.05 (3)	O2D—Co1—O1D	173.81 (17)
O4W—La—O29T	66.17 (15)	O3Q—Co1—O1D	88.13 (17)
O4W—La—O2W	68.13 (17)	O4Q—Co1—O7C	94.97 (18)
O29T—La—O2W	133.65 (15)	O2D—Co1—O7C	96.95 (17)
O4W—La—O22T	122.37 (17)	O3Q—Co1—O7C	175.56 (18)
O29T—La—O22T	70.86 (14)	O1D—Co1—O7C	87.49 (17)
O2W—La—O22T	131.96 (16)	O4Q—Co1—O8C	171.94 (17)
O4W—La—O23T	132.93 (17)	O2D—Co1—O8C	85.36 (16)
O29T—La—O23T	79.26 (14)	O3Q—Co1—O8C	97.53 (18)
O2W—La—O23T	141.80 (15)	O1D—Co1—O8C	99.44 (17)
O22T—La—O23T	69.73 (14)	O7C—Co1—O8C	83.94 (17)
O4W—La—O6W	71.4 (2)	O4Q—Co2—O3Q	83.85 (17)
O29T—La—O6W	76.34 (18)	O4Q—Co2—O6D	87.29 (17)
O2W—La—O6W	96.3 (2)	O3Q—Co2—O6D	87.93 (17)
O22T—La—O6W	131.68 (19)	O4Q—Co2—O5D	88.76 (17)
O23T—La—O6W	70.06 (18)	O3Q—Co2—O5D	87.67 (17)
O4W—La—O5W	142.23 (18)	O6D—Co2—O5D	174.38 (17)
O29T—La—O5W	136.00 (15)	O4Q—Co2—O10C	176.06 (18)
O2W—La—O5W	80.62 (17)	O3Q—Co2—O10C	95.49 (18)
O22T—La—O5W	65.16 (15)	O6D—Co2—O10C	96.57 (17)
O23T—La—O5W	84.83 (16)	O5D—Co2—O10C	87.33 (17)
O6W—La—O5W	134.97 (17)	O4Q—Co2—O9C	96.70 (17)
O4W—La—O1W	76.1 (2)	O3Q—Co2—O9C	174.21 (19)
O29T—La—O1W	89.71 (17)	O6D—Co2—O9C	86.34 (17)
O2W—La—O1W	72.13 (18)	O5D—Co2—O9C	98.10 (18)
O22T—La—O1W	67.04 (16)	O10C—Co2—O9C	84.35 (17)
O23T—La—O1W	136.64 (16)	O36T—K1—O38T	72.89 (15)
O6W—La—O1W	147.46 (19)	O36T—K1—O7W	139.94 (19)
O5W—La—O1W	74.47 (19)	O38T—K1—O7W	73.50 (18)
O4W—La—O3W	116.2 (2)	O36T—K1—O19T	77.21 (16)
O29T—La—O3W	136.91 (17)	O38T—K1—O19T	63.57 (14)
O2W—La—O3W	72.26 (18)	O7W—K1—O19T	68.66 (19)
O22T—La—O3W	121.42 (18)	O8W—K2—O15T	67.5 (2)
O23T—La—O3W	69.62 (17)	O8W—K2—O11W	67.2 (2)
O6W—La—O3W	65.58 (19)	O15T—K2—O11W	70.08 (16)
O5W—La—O3W	70.87 (19)	O10W—K3—O9W	80.8 (3)
O1W—La—O3W	133.36 (18)	O10W—K3—O13B	143.2 (3)
O15T—Mo1—O16T	105.6 (3)	O9W—K3—O13B	70.32 (19)
O15T—Mo1—O11B	98.3 (2)	O10W—K3—O12W	75.3 (3)
O16T—Mo1—O11B	101.7 (2)	O9W—K3—O12W	146.7 (3)
O15T—Mo1—O14B	100.4 (2)	O13B—K3—O12W	118.57 (19)
O16T—Mo1—O14B	98.0 (2)	O10W—K3—O21T	136.0 (3)
O11B—Mo1—O14B	148.00 (18)	O9W—K3—O21T	124.7 (2)
O15T—Mo1—O8C	95.2 (2)	O13B—K3—O21T	56.49 (13)
O16T—Mo1—O8C	158.2 (2)	O12W—K3—O21T	64.78 (18)
O11B—Mo1—O8C	81.34 (18)	O10W—K3—O37T	63.2 (2)
O14B—Mo1—O8C	71.38 (16)	O9W—K3—O37T	61.4 (2)
O15T—Mo1—O7C	162.4 (2)	O13B—K3—O37T	82.69 (15)
O16T—Mo1—O7C	90.8 (2)	O12W—K3—O37T	86.96 (18)
O11B—Mo1—O7C	71.57 (17)	Co1—O1D—Mo10	101.68 (17)
O14B—Mo1—O7C	83.18 (16)	Co1—O1D—Mo3	102.32 (17)
O8C—Mo1—O7C	69.45 (14)	Mo10—O1D—Mo3	102.24 (16)
O17T—Mo2—O18T	105.6 (3)	Co1—O1D—Mo2	101.13 (16)
O17T—Mo2—O11B	101.0 (2)	Mo10—O1D—Mo2	149.8 (2)
O18T—Mo2—O11B	102.1 (2)	Mo3—O1D—Mo2	91.87 (14)
O17T—Mo2—O12B	93.1 (2)	Co1—O2D—Mo6	101.18 (17)
O18T—Mo2—O12B	99.4 (2)	Co1—O2D—Mo5	102.60 (16)
O11B—Mo2—O12B	149.98 (18)	Mo6—O2D—Mo5	148.9 (2)
O17T—Mo2—O7C	94.8 (2)	Co1—O2D—Mo4	99.97 (17)
O18T—Mo2—O7C	159.6 (2)	Mo6—O2D—Mo4	104.06 (16)
O11B—Mo2—O7C	71.90 (17)	Mo5—O2D—Mo4	91.22 (14)
O12B—Mo2—O7C	80.67 (16)	Co1—O3Q—Co2	95.60 (18)
O17T—Mo2—O1D	160.4 (2)	Co1—O3Q—Mo4	102.17 (18)
O18T—Mo2—O1D	90.3 (2)	Co2—O3Q—Mo4	92.20 (16)
O11B—Mo2—O1D	86.44 (18)	Co1—O3Q—Mo10	91.93 (16)
O12B—Mo2—O1D	72.67 (16)	Co2—O3Q—Mo10	101.58 (18)
O7C—Mo2—O1D	70.10 (14)	Mo4—O3Q—Mo10	159.3 (2)
O19T—Mo3—O20T	105.2 (3)	Co1—O4Q—Co2	96.37 (18)
O19T—Mo3—O12B	98.9 (2)	Co1—O4Q—Mo6	93.67 (16)
O20T—Mo3—O12B	103.0 (2)	Co2—O4Q—Mo6	103.37 (18)
O19T—Mo3—O5D	95.2 (2)	Co1—O4Q—Mo3	100.57 (17)
O20T—Mo3—O5D	101.8 (2)	Co2—O4Q—Mo3	90.27 (15)
O12B—Mo3—O5D	147.02 (18)	Mo6—O4Q—Mo3	159.10 (19)
O19T—Mo3—O1D	99.8 (2)	Co2—O5D—Mo3	102.77 (18)
O20T—Mo3—O1D	154.9 (2)	Co2—O5D—Mo10	101.07 (17)
O12B—Mo3—O1D	74.24 (16)	Mo3—O5D—Mo10	103.20 (17)
O5D—Mo3—O1D	74.05 (15)	Co2—O5D—Mo9	100.13 (17)
O19T—Mo3—O4Q	165.8 (2)	Mo3—O5D—Mo9	150.7 (2)
O20T—Mo3—O4Q	86.6 (2)	Mo10—O5D—Mo9	89.97 (14)
O12B—Mo3—O4Q	85.74 (16)	Co2—O6D—Mo4	99.54 (17)
O5D—Mo3—O4Q	74.38 (15)	Co2—O6D—Mo7	101.89 (16)
O1D—Mo3—O4Q	68.36 (13)	Mo4—O6D—Mo7	152.5 (2)
O21T—Mo4—O22T	105.9 (2)	Co2—O6D—Mo6	99.41 (17)
O21T—Mo4—O13B	102.6 (2)	Mo4—O6D—Mo6	103.42 (16)
O22T—Mo4—O13B	97.43 (19)	Mo7—O6D—Mo6	89.92 (14)
O21T—Mo4—O6D	103.4 (2)	Co1—O7C—Mo1	103.82 (18)
O22T—Mo4—O6D	91.90 (18)	Co1—O7C—Mo2	101.06 (17)
O13B—Mo4—O6D	148.71 (17)	Mo1—O7C—Mo2	92.75 (14)
O21T—Mo4—O3Q	90.01 (19)	Co1—O7C—H7	109 (6)
O22T—Mo4—O3Q	162.41 (17)	Mo1—O7C—H7	120 (6)
O13B—Mo4—O3Q	86.14 (16)	Mo2—O7C—H7	126 (6)
O6D—Mo4—O3Q	76.79 (15)	Co1—O8C—Mo5	101.83 (17)
O21T—Mo4—O2D	160.03 (19)	Co1—O8C—Mo1	102.79 (18)
O22T—Mo4—O2D	94.07 (17)	Mo5—O8C—Mo1	94.00 (15)
O13B—Mo4—O2D	75.14 (16)	Co1—O8C—H8	110 (6)
O6D—Mo4—O2D	74.45 (15)	Mo5—O8C—H8	105 (6)
O3Q—Mo4—O2D	70.10 (15)	Mo1—O8C—H8	137 (6)
O24T—Mo5—O23T	106.0 (2)	Co2—O9C—Mo7	101.86 (18)
O24T—Mo5—O14B	102.0 (2)	Co2—O9C—Mo8	103.17 (18)
O23T—Mo5—O14B	103.2 (2)	Mo7—O9C—Mo8	93.49 (16)
O24T—Mo5—O13B	94.0 (2)	Co2—O9C—H9	124 (6)
O23T—Mo5—O13B	96.80 (19)	Mo7—O9C—H9	107 (6)
O14B—Mo5—O13B	149.63 (17)	Mo8—O9C—H9	121 (6)
O24T—Mo5—O8C	97.73 (19)	Co2—O10C—Mo9	102.40 (18)
O23T—Mo5—O8C	156.16 (18)	Co2—O10C—Mo8	102.77 (17)
O14B—Mo5—O8C	73.36 (16)	Mo9—O10C—Mo8	93.47 (15)
O13B—Mo5—O8C	79.06 (16)	Co2—O10C—H10	114 (6)
O24T—Mo5—O2D	163.6 (2)	Mo9—O10C—H10	127 (6)
O23T—Mo5—O2D	86.08 (18)	Mo8—O10C—H10	113 (6)
O14B—Mo5—O2D	85.50 (17)	Mo2—O11B—Mo1	118.5 (2)
O13B—Mo5—O2D	73.24 (15)	Mo3—O12B—Mo2	117.0 (2)
O8C—Mo5—O2D	70.21 (14)	Mo4—O13B—Mo5	114.7 (2)
O32T—Mo7—O31T	105.8 (2)	Mo5—O14B—Mo1	117.2 (2)
O32T—Mo7—O26B	101.1 (2)	Mo6—O25B—Mo7	117.8 (2)
O31T—Mo7—O26B	98.9 (2)	Mo8—O26B—Mo7	117.8 (2)
O32T—Mo7—O25B	95.7 (2)	Mo8—O27B—Mo9	118.4 (2)
O31T—Mo7—O25B	102.3 (2)	Mo10—O28B—Mo9	117.6 (2)
O26B—Mo7—O25B	148.24 (17)	H1A—O1W—H1B	144 (10)
O32T—Mo7—O9C	95.2 (2)	H2A—O2W—H2B	118.6
O31T—Mo7—O9C	158.44 (19)	H3A—O3W—H3B	109.5
O26B—Mo7—O9C	71.65 (17)	H4A—O4W—H4B	109.5
O25B—Mo7—O9C	80.17 (17)	H5A—O5W—H5B	108.4
O32T—Mo7—O6D	162.4 (2)	H6A—O6W—H6B	119.8
O31T—Mo7—O6D	90.14 (19)	H7A—O7W—H7B	99.6
O26B—Mo7—O6D	83.51 (17)	H8A—O8W—H8B	109.5
O25B—Mo7—O6D	73.08 (16)	H9A—O9W—H9B	111.5
O9C—Mo7—O6D	69.90 (14)	H10A—O10W—H10B	117.6
O34T—Mo8—O33T	106.0 (2)	H11A—O11W—H11C	109.5
O34T—Mo8—O27B	101.2 (2)	H12A—O12W—H12B	94 (6)
O33T—Mo8—O27B	98.2 (2)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O7C—H7···O30T	0.79 (4)	2.16 (5)	2.891 (6)	152 (8)
O8C—H8···O9W	0.85 (4)	2.26 (6)	2.972 (10)	141 (7)
O9C—H9···O8W^vii	0.82 (4)	2.21 (6)	2.935 (9)	147 (8)
O10C—H10···O21T	0.80 (4)	2.27 (6)	2.932 (6)	141 (8)
O1W—H1A···O12W^viii	0.92 (7)	1.97 (9)	2.809 (8)	151 (9)
O1W—H1B···O31T	0.87 (8)	1.99 (8)	2.803 (7)	154 (10)
O2W—H2A···O11W^v	0.99	1.75	2.724 (8)	171
O2W—H2B···O12W^viii	0.96	2.03	2.951 (9)	161
O3W—H3A···O38T^v	0.96	2.55	3.055 (8)	113
O3W—H3B···O34T^viii	0.96	2.35	2.936 (7)	119
O4W—H4A···O20T^ix	0.96	2.10	2.876 (7)	137
O4W—H4B···O27B^ix	0.96	2.07	2.725 (7)	124
O5W—H5A···O13W	0.97	1.79	2.682 (9)	151
O5W—H5B···O34T^viii	0.97	1.87	2.768 (7)	153
O6W—H6A···O37T^v	0.77	2.15	2.880 (7)	161
O6W—H6B···O33T^ix	0.76	2.05	2.761 (7)	156
O7W—H7A···O30Tⁱ	0.94	2.38	2.991 (8)	122
O7W—H7B···O18T	0.82	2.27	2.915 (9)	136
O8W—H8A···O32T^x	0.96	2.05	2.950 (9)	156
O8W—H8B···O6Wⁱⁱ	0.96	2.47	3.105 (12)	123
O9W—H9A···O24T	0.94	2.10	2.955 (9)	151
O9W—H9A···O32T^x	0.94	2.31	2.817 (10)	113
O9W—H9B···O33T^x	0.80	2.08	2.861 (9)	163
O10W—H10A···O7W^vi	0.77	2.08	2.771 (12)	150
O11W—H11A···O26B^iv	0.96	1.95	2.770 (7)	142
O11W—H11C···O11B	0.96	1.94	2.824 (7)	152
O12W—H12A···O28B	0.88 (5)	1.97 (5)	2.819 (8)	161 (11)
O12W—H12B···O16Tⁱⁱ	0.94 (5)	2.30 (9)	3.083 (9)	140 (10)

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

Experimental details

Crystal data
Chemical formula	LaK₃[H₄Mo₁₀Co₂O₃₈]·13H₂O
M_r	2179.71
Crystal system, space group	Monoclinic, P2₁
Temperature (K)	298
a, b, c (Å)	10.4487 (6), 18.598 (1), 12.3179 (8)
β (°)	112.957 (4)
V (Å³)	2204.1 (2)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	4.83
Crystal size (mm)	0.28 × 0.24 × 0.20

Data collection
Diffractometer	Stoe STADI-4
Absorption correction	Numerical (X-SHAPE; Stoe & Cie, 1996)
T_min, T_max	0.349, 0.527
No. of measured, independent and observed [I > 2σ(I)] reflections	10417, 10104, 9949
R_int	0.016
(sin θ/λ)_max (Å⁻¹)	0.650

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.025, 0.069, 1.10
No. of reflections	10104
No. of parameters	630
No. of restraints	22
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	1.37, −1.27
Absolute structure	Flack (1983)
Absolute structure parameter	0.001 (10)

Computer programs: STADI-4 (Stoe & Cie, 1996), X-RED (Stoe & Cie, 1996), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEP-3 (Farrugia, 1997) and DIAMOND (Brandenburg, 1998).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O7C—H7···O30T	0.79 (4)	2.16 (5)	2.891 (6)	152 (8)
O8C—H8···O9W	0.85 (4)	2.26 (6)	2.972 (10)	141 (7)
O9C—H9···O8Wⁱ	0.82 (4)	2.21 (6)	2.935 (9)	147 (8)
O10C—H10···O21T	0.80 (4)	2.27 (6)	2.932 (6)	141 (8)

Symmetry code: (i) x−1, y, z−1.

Acknowledgements

This work was supported by the Pukyong National University Research Abroad Fund in 2006 (grant No. PS-2006-013).

References

Ama, T., Hidaka, J. & Shimura, Y. (1970). Bull. Chem. Soc. Jpn, 43, 2654. CrossRef Web of Science Google Scholar
Brandenburg, K. (1998). DIAMOND. Crystal Impact GbR, Bonn, Germany. Google Scholar
Brese, N. E. & O'Keeffe, M. (1991). Acta Cryst. B47, 192–197. CrossRef CAS Web of Science IUCr Journals Google Scholar
Brown, I. D. & Altermatt, D. (1985). Acta Cryst. B41, 244–247. CrossRef CAS Web of Science IUCr Journals Google Scholar
Evans, H. T. Jr & Showell, J. S. (1969). J. Am. Chem. Soc. 91. 6881–6882. Google Scholar
Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. CrossRef IUCr Journals Google Scholar
Flack, H. D. (1983). Acta Cryst. A39, 876–881. CrossRef CAS Web of Science IUCr Journals Google Scholar
Hasenknopf, B., Micone, K., Lacôte, E., Thorimbert, S., Malacria, M. & Thouvenot, R. (2008). Eur. J. Inorg. Chem. pp. 5001–5013. Web of Science CrossRef Google Scholar
Nolan, A. L., Allen, C. C., Burns, R. C., Craig, D. C. & Lawrance, G. A. (1998). Aust. J. Chem. 51. 825–834. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Stoe & Cie (1996). STADI-4, X-RED and X-SHAPE. Stoe & Cie Gmbh, Darmstadt, Germany. Google Scholar

This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 66| Part 2| February 2010| Page i10

https://doi.org/10.1107/S1600536810000929

Open

access

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Plain Text

Format		BIBTeX
		EndNote
		RefMan
		Refer
		Medline
		CIF
		SGML
		Plain Text

Search IUCr Journals		doi		Advanced search
Author		volume	page

inorganic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Monolanthanum tripotassium tetra­hydrogen deca­molybdodicobaltate(III) trideca­hydrate

Related literature

Experimental

Crystal data

Data collection

Refinement

Supporting information

Acknowledgements

References

inorganic compounds

Monolanthanum tripotassium tetrahydrogen decamolybdodicobaltate(III) tridecahydrate