[Al(H(2)O)(6)][Cr(OH)(6)Mo(6)O(18)]·10H(2)O.

The title compound, [Al(H(2)O)(6)][Cr(OH)(6)Mo(6)O(18)]·10H(2)O, hexa-aqua-aluminium hexa-hydroxidoocta-deca-oxido-molybdo-chromate(III) deca-hydrate, crystallizes isotypically with its gallium analogue [Ga(H(2)O)(6)][Cr(OH)(6)Mo(6)O(18)].10H(2)O. In the structure of the title compound, both the [Al(H(2)O)(6)](3+) cation and the Anderson-type [Cr(OH)(6)Mo(6)O(18)](3-) anion lie on centres of inversion. The anion is composed of seven edge-sharing octa-hedra, six of which are MoO(6) octa-hedra that are arranged hexa-gonally around the central Cr(OH)(6) octa-hedron. The anions are linked to each other by O-H⋯O hydrogen bonds into infinite chains along [100]. These chains are further connected with the [Al(H(2)O)(6)](3+) cations through O-H⋯O hydrogen bonds into sheets parallel to (01). O-H⋯O hydrogen bonds involving all the lattice water mol-ecules finally link the sheets into a three-dimensional network.

Related literature

For background literature on polyoxometalates, see: An et al. (2005 ▶); Shivaiah et al. (2003 ▶). The isotypic gallium analogue was reported by Kaziev et al. (2002 ▶).

Experimental

Crystal data

[Al(H2O)6][Cr(OH)6Mo6O18]·10H2O

M = 1332.92

Triclinic,

a = 6.809 (5) Å

b = 11.267 (7) Å

c = 11.596 (9) Å

α = 101.26 (3)°

β = 97.02 (3)°

γ = 101.81 (3)°

V = 841.7 (10) Å3

Z = 1

Mo Kα radiation

μ = 2.63 mm−1

T = 290 K

0.12 × 0.12 × 0.11 mm

Data collection

Rigaku R-AXIS RAPID diffractometer

Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T min = 0.745, T max = 0.770

8257 measured reflections

3801 independent reflections

3346 reflections with I > 2σ(I)

R int = 0.037

Refinement

R[F 2 > 2σ(F 2)] = 0.033

wR(F 2) = 0.093

S = 1.10

3801 reflections

217 parameters

24 restraints

H-atom parameters constrained

Δρmax = 0.89 e Å−3

Δρmin = −0.86 e Å−3

Data collection: RAPID-AUTO (Rigaku, 1998 ▶); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: PLATON (Spek, 2009 ▶); software used to prepare material for publication: SHELXL97.

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810053936/wm2434sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810053936/wm2434Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Al(H2O)6][Cr(OH)6Mo6O18]·10H2O	Z = 1
Mr = 1332.92	F(000) = 647
Triclinic, P1	Dx = 2.630 Mg m−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 6.809 (5) Å	Cell parameters from 7543 reflections
b = 11.267 (7) Å	θ = 3.2–27.1°
c = 11.596 (9) Å	µ = 2.63 mm−1
α = 101.26 (3)°	T = 290 K
β = 97.02 (3)°	Block, colorless
γ = 101.81 (3)°	0.12 × 0.12 × 0.11 mm
V = 841.7 (10) Å3

Rigaku R-AXIS RAPID diffractometer	3801 independent reflections
Radiation source: fine-focus sealed tube	3346 reflections with I > 2σ(I)
graphite	Rint = 0.037
ω scans	θmax = 27.5°, θmin = 3.2°
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	h = −7→8
Tmin = 0.745, Tmax = 0.770	k = −14→14
8257 measured reflections	l = −15→15

Refinement on F2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.033	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.093	H-atom parameters constrained
S = 1.10	w = 1/[σ2(Fo2) + (0.0331P)2 + 2.719P] where P = (Fo2 + 2Fc2)/3
3801 reflections	(Δ/σ)max = 0.009
217 parameters	Δρmax = 0.89 e Å−3
24 restraints	Δρmin = −0.86 e Å−3

Experimental. (See detailed section in the paper)

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.

	x	y	z	Uiso*/Ueq
Al1	0.0000	0.5000	0.5000	0.0162 (4)
Cr1	0.0000	0.0000	0.0000	0.01424 (19)
Mo1	0.37029 (5)	0.16663 (3)	−0.10502 (3)	0.01629 (11)
Mo2	0.33617 (6)	0.24360 (3)	0.17992 (3)	0.01870 (11)
Mo3	−0.02648 (6)	0.07285 (3)	0.29050 (3)	0.01802 (11)
OH1	0.2099 (4)	−0.0332 (3)	−0.0983 (3)	0.0156 (6)
H1	0.2955	−0.0782	−0.0941	0.023*
OB1	0.1450 (5)	0.1055 (3)	−0.2357 (3)	0.0203 (6)
OT1	0.5602 (5)	0.1125 (3)	−0.1683 (3)	0.0251 (7)
OT2	0.4158 (5)	0.3199 (3)	−0.1095 (3)	0.0287 (8)
OH2	0.1174 (4)	0.1756 (3)	0.0024 (3)	0.0159 (6)
H2	0.0530	0.2258	−0.0217	0.024*
OB2	0.4843 (5)	0.1784 (3)	0.0594 (3)	0.0209 (6)
OT3	0.3656 (6)	0.3945 (3)	0.1671 (3)	0.0321 (8)
OT4	0.5053 (6)	0.2483 (4)	0.3027 (3)	0.0365 (9)
OB3	0.0878 (5)	0.2295 (3)	0.2494 (3)	0.0202 (6)
OH3	0.1830 (5)	0.0372 (3)	0.1527 (3)	0.0166 (6)
H3	0.2705	−0.0068	0.1480	0.025*
OT5	0.1586 (6)	0.0662 (3)	0.3999 (3)	0.0315 (8)
OT6	−0.2117 (6)	0.1163 (4)	0.3617 (3)	0.0334 (8)
OW1	0.1050 (5)	0.3690 (3)	0.5388 (3)	0.0242 (7)
H4	0.2073	0.3992	0.5942	0.036*
H5	0.0411	0.3152	0.5715	0.036*
OW2	0.0105 (5)	0.5686 (3)	0.6627 (3)	0.0234 (7)
H6	−0.0143	0.6394	0.6869	0.035*
H7	0.0689	0.5534	0.7255	0.035*
OW3	0.2655 (5)	0.5935 (3)	0.5085 (3)	0.0254 (7)
H8	0.3070	0.6445	0.5758	0.038*
H9	0.3240	0.6029	0.4491	0.038*
OW4	0.9017 (6)	0.2342 (3)	0.6599 (4)	0.0379 (9)
H10	0.9862	0.2141	0.7084	0.057*
H11	0.8043	0.2487	0.6955	0.057*
OW5	0.0885 (6)	0.6667 (3)	0.0685 (4)	0.0361 (9)
H12	0.1879	0.7302	0.0967	0.054*
H13	0.1180	0.6225	0.0079	0.054*
OW6	0.1882 (6)	0.5186 (4)	0.8662 (4)	0.0378 (9)
H14	0.1337	0.4753	0.9112	0.057*
H15	0.3078	0.5567	0.9018	0.057*
OW7	0.4894 (4)	0.3814 (3)	0.6484 (3)	0.0359 (9)
H16	0.5251	0.4239	0.7199	0.054*
H17	0.4701	0.3052	0.6506	0.054*
OW8	0.4860 (4)	0.1318 (3)	0.5850 (3)	0.0407 (9)
H18	0.4573	0.0970	0.6416	0.061*
H19	0.5475	0.0869	0.5416	0.061*

	U11	U22	U33	U12	U13	U23
Al1	0.0168 (9)	0.0139 (8)	0.0166 (9)	0.0037 (6)	0.0007 (7)	0.0011 (7)
Cr1	0.0137 (5)	0.0128 (4)	0.0148 (4)	0.0034 (3)	0.0000 (4)	0.0008 (3)
Mo1	0.01433 (19)	0.01556 (18)	0.0194 (2)	0.00386 (13)	0.00296 (14)	0.00448 (14)
Mo2	0.0168 (2)	0.01554 (18)	0.0188 (2)	0.00120 (13)	−0.00073 (14)	−0.00287 (14)
Mo3	0.0201 (2)	0.01879 (19)	0.01451 (19)	0.00612 (14)	0.00132 (14)	0.00159 (14)
OH1	0.0144 (14)	0.0151 (13)	0.0187 (15)	0.0084 (11)	0.0020 (12)	0.0026 (11)
OB1	0.0223 (16)	0.0205 (14)	0.0188 (16)	0.0051 (12)	0.0015 (13)	0.0073 (12)
OT1	0.0228 (17)	0.0310 (17)	0.0256 (18)	0.0124 (13)	0.0065 (14)	0.0086 (14)
OT2	0.0266 (19)	0.0228 (16)	0.037 (2)	0.0030 (13)	0.0062 (15)	0.0107 (15)
OH2	0.0146 (14)	0.0126 (13)	0.0205 (15)	0.0038 (11)	0.0020 (12)	0.0040 (11)
OB2	0.0183 (16)	0.0221 (15)	0.0199 (16)	0.0041 (12)	0.0001 (13)	0.0017 (12)
OT3	0.036 (2)	0.0178 (15)	0.038 (2)	0.0020 (14)	0.0096 (17)	−0.0011 (14)
OT4	0.030 (2)	0.043 (2)	0.0262 (19)	0.0073 (16)	−0.0073 (16)	−0.0069 (16)
OB3	0.0233 (17)	0.0163 (14)	0.0188 (15)	0.0053 (12)	0.0018 (13)	−0.0007 (12)
OH3	0.0175 (15)	0.0166 (13)	0.0149 (14)	0.0069 (11)	−0.0005 (12)	0.0005 (11)
OT5	0.030 (2)	0.0379 (19)	0.0242 (18)	0.0091 (15)	−0.0051 (15)	0.0070 (15)
OT6	0.036 (2)	0.038 (2)	0.032 (2)	0.0184 (16)	0.0136 (17)	0.0051 (16)
OW1	0.0248 (18)	0.0189 (14)	0.0286 (18)	0.0078 (13)	−0.0001 (14)	0.0047 (13)
OW2	0.0310 (19)	0.0222 (15)	0.0169 (15)	0.0106 (13)	0.0017 (13)	0.0008 (12)
OW3	0.0215 (17)	0.0267 (16)	0.0216 (16)	−0.0024 (13)	0.0032 (13)	−0.0013 (13)
OW4	0.034 (2)	0.0346 (19)	0.050 (2)	0.0118 (16)	−0.0007 (18)	0.0218 (18)
OW5	0.035 (2)	0.0285 (18)	0.044 (2)	0.0106 (15)	0.0019 (18)	0.0068 (16)
OW6	0.036 (2)	0.044 (2)	0.039 (2)	0.0160 (17)	0.0056 (18)	0.0174 (18)
OW7	0.030 (2)	0.048 (2)	0.030 (2)	0.0101 (17)	0.0063 (16)	0.0080 (17)
OW8	0.036 (2)	0.048 (2)	0.035 (2)	0.0049 (18)	−0.0012 (18)	0.0113 (18)

Al1—OW1i	1.872 (3)	Mo3—OB1ii	1.951 (3)
Al1—OW1	1.872 (3)	Mo3—OB3	1.951 (3)
Al1—OW3i	1.877 (3)	Mo3—OH3	2.300 (3)
Al1—OW3	1.877 (3)	Mo3—OH1ii	2.330 (3)
Al1—OW2	1.881 (3)	OH1—Mo3ii	2.330 (3)
Al1—OW2i	1.881 (3)	OH1—H1	0.8500
Cr1—OH3ii	1.954 (3)	OB1—Mo3ii	1.951 (3)
Cr1—OH3	1.954 (3)	OH2—H2	0.8499
Cr1—OH2	1.970 (3)	OH3—H3	0.8501
Cr1—OH2ii	1.970 (3)	OW1—H4	0.8500
Cr1—OH1ii	1.983 (3)	OW1—H5	0.8500
Cr1—OH1	1.983 (3)	OW2—H6	0.8501
Mo1—OT2	1.703 (3)	OW2—H7	0.8499
Mo1—OT1	1.721 (3)	OW3—H8	0.8500
Mo1—OB1	1.927 (3)	OW3—H9	0.8500
Mo1—OB2	1.937 (4)	OW4—H10	0.8500
Mo1—OH2	2.252 (3)	OW4—H11	0.8500
Mo1—OH1	2.314 (3)	OW5—H12	0.8559
Mo2—OT4	1.703 (4)	OW5—H13	0.8496
Mo2—OT3	1.709 (4)	OW6—H14	0.8500
Mo2—OB2	1.939 (3)	OW6—H15	0.8500
Mo2—OB3	1.951 (3)	OW7—H16	0.8509
Mo2—OH2	2.283 (3)	OW7—H17	0.8480
Mo2—OH3	2.288 (3)	OW8—H18	0.8499
Mo3—OT6	1.691 (4)	OW8—H19	0.8500
Mo3—OT5	1.699 (4)
OW1i—Al1—OW1	180.000 (1)	OT4—Mo2—OH3	94.98 (16)
OW1i—Al1—OW3i	89.98 (16)	OT3—Mo2—OH3	158.26 (16)
OW1—Al1—OW3i	90.02 (16)	OB2—Mo2—OH3	82.20 (13)
OW1i—Al1—OW3	90.02 (16)	OB3—Mo2—OH3	71.27 (12)
OW1—Al1—OW3	89.98 (16)	OH2—Mo2—OH3	69.73 (11)
OW3i—Al1—OW3	180.0 (2)	OT6—Mo3—OT5	105.4 (2)
OW1i—Al1—OW2	89.59 (15)	OT6—Mo3—OB1ii	99.75 (17)
OW1—Al1—OW2	90.41 (15)	OT5—Mo3—OB1ii	97.91 (16)
OW3i—Al1—OW2	90.13 (15)	OT6—Mo3—OB3	99.14 (17)
OW3—Al1—OW2	89.87 (15)	OT5—Mo3—OB3	102.04 (17)
OW1i—Al1—OW2i	90.41 (15)	OB1ii—Mo3—OB3	147.66 (13)
OW1—Al1—OW2i	89.59 (15)	OT6—Mo3—OH3	163.68 (15)
OW3i—Al1—OW2i	89.87 (15)	OT5—Mo3—OH3	89.62 (16)
OW3—Al1—OW2i	90.13 (15)	OB1ii—Mo3—OH3	84.03 (12)
OW2—Al1—OW2i	180.000 (1)	OB3—Mo3—OH3	71.00 (12)
OH3ii—Cr1—OH3	180.00 (18)	OT6—Mo3—OH1ii	95.90 (16)
OH3ii—Cr1—OH2	96.53 (13)	OT5—Mo3—OH1ii	157.46 (14)
OH3—Cr1—OH2	83.47 (13)	OB1ii—Mo3—OH1ii	70.90 (12)
OH3ii—Cr1—OH2ii	83.47 (13)	OB3—Mo3—OH1ii	81.26 (13)
OH3—Cr1—OH2ii	96.53 (13)	OH3—Mo3—OH1ii	70.18 (12)
OH2—Cr1—OH2ii	180.00 (18)	Cr1—OH1—Mo1	101.22 (12)
OH3ii—Cr1—OH1ii	94.97 (14)	Cr1—OH1—Mo3ii	101.37 (13)
OH3—Cr1—OH1ii	85.03 (14)	Mo1—OH1—Mo3ii	92.79 (11)
OH2—Cr1—OH1ii	95.90 (12)	Cr1—OH1—H1	131.8
OH2ii—Cr1—OH1ii	84.10 (12)	Mo1—OH1—H1	110.7
OH3ii—Cr1—OH1	85.03 (14)	Mo3ii—OH1—H1	111.9
OH3—Cr1—OH1	94.97 (14)	Mo1—OB1—Mo3ii	120.22 (16)
OH2—Cr1—OH1	84.10 (12)	Cr1—OH2—Mo1	103.79 (12)
OH2ii—Cr1—OH1	95.90 (12)	Cr1—OH2—Mo2	103.22 (13)
OH1ii—Cr1—OH1	180.00 (15)	Mo1—OH2—Mo2	93.30 (12)
OT2—Mo1—OT1	104.94 (17)	Cr1—OH2—H2	125.8
OT2—Mo1—OB1	97.87 (16)	Mo1—OH2—H2	106.7
OT1—Mo1—OB1	101.08 (16)	Mo2—OH2—H2	118.4
OT2—Mo1—OB2	100.85 (16)	Mo1—OB2—Mo2	116.61 (16)
OT1—Mo1—OB2	96.87 (16)	Mo2—OB3—Mo3	118.42 (15)
OB1—Mo1—OB2	149.69 (14)	Cr1—OH3—Mo2	103.55 (13)
OT2—Mo1—OH2	94.45 (14)	Cr1—OH3—Mo3	103.34 (14)
OT1—Mo1—OH2	159.55 (14)	Mo2—OH3—Mo3	93.88 (11)
OB1—Mo1—OH2	82.26 (14)	Cr1—OH3—H3	110.0
OB2—Mo1—OH2	72.74 (13)	Mo2—OH3—H3	110.7
OT2—Mo1—OH1	162.67 (14)	Mo3—OH3—H3	131.6
OT1—Mo1—OH1	90.85 (14)	Al1—OW1—H4	108.5
OB1—Mo1—OH1	71.64 (12)	Al1—OW1—H5	122.9
OB2—Mo1—OH1	83.95 (13)	H4—OW1—H5	97.7
OH2—Mo1—OH1	70.89 (11)	Al1—OW2—H6	122.0
OT4—Mo2—OT3	105.5 (2)	Al1—OW2—H7	131.7
OT4—Mo2—OB2	98.10 (17)	H6—OW2—H7	103.9
OT3—Mo2—OB2	101.59 (16)	Al1—OW3—H8	111.0
OT4—Mo2—OB3	99.29 (18)	Al1—OW3—H9	125.4
OT3—Mo2—OB3	97.85 (16)	H8—OW3—H9	120.8
OB2—Mo2—OB3	149.30 (13)	H10—OW4—H11	107.7
OT4—Mo2—OH2	162.45 (15)	H12—OW5—H13	108.5
OT3—Mo2—OH2	90.88 (16)	H14—OW6—H15	107.7
OB2—Mo2—OH2	72.01 (13)	H16—OW7—H17	107.5
OB3—Mo2—OH2	84.24 (13)	H18—OW8—H19	107.7

D—H···A	D—H	H···A	D···A	D—H···A
OH3—H3···OT1iii	0.85	1.85	2.681 (4)	167.
OH1—H1···OB2iii	0.85	2.10	2.944 (4)	172.
OH2—H2···OW5iv	0.85	1.82	2.665 (5)	178.
OW3—H8···OT4v	0.85	1.83	2.628 (5)	156.
OW3—H9···OW7v	0.85	1.81	2.632 (5)	163.
OW1—H4···OW7	0.85	2.01	2.730 (5)	142.
OW1—H5···OW4vi	0.85	1.74	2.577 (5)	167.
OW2—H6···OB3i	0.85	1.72	2.559 (4)	171.
OW2—H7···OW6	0.85	1.88	2.728 (5)	178.
OW4—H10···OB1vii	0.85	1.94	2.737 (5)	156.
OW5—H12···OT1viii	0.86	2.15	3.002 (6)	179.
OW5—H13···OW6ix	0.85	1.99	2.842 (6)	180.
OW6—H14···OW5i	0.85	2.04	2.800 (6)	149.
OW6—H15···OT3v	0.85	2.45	3.091 (6)	133.
OW7—H16···OT3v	0.85	2.13	2.878 (5)	146.
OW7—H17···OW8	0.85	1.98	2.759 (5)	152.
OW8—H18···OT1x	0.85	2.19	2.902 (5)	141.
OW8—H18···OT6xi	0.85	2.62	3.241 (5)	131.
OW8—H19···OW8xii	0.85	2.56	3.283 (6)	144.

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
OH3—H3⋯OT1i	0.85	1.85	2.681 (4)	167
OH1—H1⋯OB2i	0.85	2.10	2.944 (4)	172
OH2—H2⋯OW5ii	0.85	1.82	2.665 (5)	178
OW3—H8⋯OT4iii	0.85	1.83	2.628 (5)	156
OW3—H9⋯OW7iii	0.85	1.81	2.632 (5)	163
OW1—H4⋯OW7	0.85	2.01	2.730 (5)	142
OW1—H5⋯OW4iv	0.85	1.74	2.577 (5)	167
OW2—H6⋯OB3v	0.85	1.72	2.559 (4)	171
OW2—H7⋯OW6	0.85	1.88	2.728 (5)	178
OW4—H10⋯OB1vi	0.85	1.94	2.737 (5)	156
OW5—H12⋯OT1vii	0.86	2.15	3.002 (6)	179
OW5—H13⋯OW6viii	0.85	1.99	2.842 (6)	180
OW6—H14⋯OW5v	0.85	2.04	2.800 (6)	149
OW6—H15⋯OT3iii	0.85	2.45	3.091 (6)	133
OW7—H16⋯OT3iii	0.85	2.13	2.878 (5)	146
OW7—H17⋯OW8	0.85	1.98	2.759 (5)	152
OW8—H18⋯OT1ix	0.85	2.19	2.902 (5)	141
OW8—H18⋯OT6x	0.85	2.62	3.241 (5)	131
OW8—H19⋯OW8xi	0.85	2.56	3.283 (6)	144

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) ; (vii) ; (viii) ; (ix) ; (x) ; (xi) .