H3[AlMo6(OH)6O18]·10H2O

Liu, Y.; Dou, J.-M.; Wang, D.-Q.; Zhang, X.-X.; Zhou, L.

doi:10.1107/S1600536806044321

H₃[AlMo₆(OH)₆O₁₈]·10H₂O

Y. Liu, J.-M. Dou, D.-Q. Wang, X.-X. Zhang and L. Zhou

The title compound, trihydrogen hexahydroxooctadecaoxoaluminiumhexamolybdate decahydrate, crystallizes from an aqueous solution of potassium molybdate and aluminium(III) chloride. The structure features [Al(OH)₆Mo₆O₁₈]^3- clusters consisting of six edge-sharing MoO₆ octahedra, which are arranged hexagonally around a central {Al(OH)₆} octahedron. The overall symmetry of the Al(OH)₆Mo₆O₁₈ unit is $\overline{1}$ .

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806044321/fi2011sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536806044321/fi2011Isup2.hkl Contains datablock I

checkCIF report

Key indicators

Single-crystal X-ray study
T = 298 K
Mean (l-O) = 0.004 Å
R factor = 0.042
wR factor = 0.132
Data-to-parameter ratio = 13.4

checkCIF/PLATON results

No syntax errors found



Datablock: I


Alert level A
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O13
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O14
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O15
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O16
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......        O17

Alert level B
PLAT430_ALERT_2_B Short Inter D...A Contact  O1     ..  O10     ..       2.71 Ang.
PLAT430_ALERT_2_B Short Inter D...A Contact  O2     ..  O9      ..       2.83 Ang.
PLAT430_ALERT_2_B Short Inter D...A Contact  O3     ..  O13     ..       2.72 Ang.
PLAT430_ALERT_2_B Short Inter D...A Contact  O4     ..  O14     ..       2.73 Ang.
PLAT430_ALERT_2_B Short Inter D...A Contact  O5     ..  O17     ..       2.61 Ang.
PLAT430_ALERT_2_B Short Inter D...A Contact  O6     ..  O17     ..       2.78 Ang.
PLAT430_ALERT_2_B Short Inter D...A Contact  O8     ..  O16     ..       2.83 Ang.
PLAT430_ALERT_2_B Short Inter D...A Contact  O12    ..  O13     ..       2.79 Ang.
PLAT430_ALERT_2_B Short Inter D...A Contact  O13    ..  O15     ..       2.79 Ang.
PLAT430_ALERT_2_B Short Inter D...A Contact  O14    ..  O16     ..       2.82 Ang.

Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT214_ALERT_2_C Atom O13     (Anion/Solvent) ADP max/min Ratio         4.70 prola
PLAT430_ALERT_2_C Short Inter D...A Contact  O12    ..  O14     ..       2.85 Ang.

Alert level G
FORMU01_ALERT_1_G  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and _chemical_formula_moiety. This is
            usually due to the moiety formula being in the wrong format.
            Atom count from _chemical_formula_sum:   Al1 Mo6 O34
            Atom count from _chemical_formula_moiety:H20 Al1 Mo6 O34

   5 ALERT level A = In general: serious problem
  10 ALERT level B = Potentially serious problem
   3 ALERT level C = Check and explain
   1 ALERT level G = General alerts; check

   2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
  17 ALERT type 2 Indicator that the structure model may be wrong or deficient
   0 ALERT type 3 Indicator that the structure quality may be low
   0 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SHELXTL (Bruker, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

trihydrogen hexahydroxooctadecaoxoaluminiumhexamolybdenum decahydrate top

Crystal data top

H₃[AlMo₆(OH)₆O₁₈]·10H₂O	F(000) = 1074.0
M_r = 1175.83	D_x = 2.659 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 2511 reflections
a = 11.311 (2) Å	θ = 1.8–25.0°
b = 10.928 (2) Å	µ = 2.70 mm⁻¹
c = 11.744 (2) Å	T = 298 K
β = 99.409 (2)°	Block, colourless
V = 1432.1 (4) Å³	0.30 × 0.30 × 0.30 mm
Z = 2

Data collection top

Bruker SMART CCD area-detector diffractometer	2041 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.052
Graphite monochromator	θ_max = 25.0°, θ_min = 1.8°
φ and ω scans	h = −13→12
7286 measured reflections	k = −13→8
2511 independent reflections	l = −13→13

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	H-atom parameters not refined
R[F² > 2σ(F²)] = 0.042	w = 1/[σ²(F_o²) + (0.0856P)² + 3.7922P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.132	(Δ/σ)_max < 0.001
S = 1.00	Δρ_max = 1.32 e Å⁻³
2511 reflections	Δρ_min = −0.92 e Å⁻³
188 parameters	Extinction correction: SHELXTL (Bruker, 1999), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.0024 (5)
Primary atom site location: structure-invariant direct methods

Special details top

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 (Å²) top

	x	y	z	U_iso*/U_eq
Mo1	0.16170 (6)	0.23381 (5)	0.42916 (5)	0.0223 (2)
Mo2	0.29763 (5)	−0.01586 (6)	0.54656 (5)	0.0238 (2)
Mo3	0.13552 (6)	−0.24590 (5)	0.62019 (5)	0.0214 (2)
Al1	0.0000	0.0000	0.5000	0.0147 (6)
O1	0.1200 (4)	−0.1101 (4)	0.4680 (3)	0.0173 (9)
O2	0.1299 (4)	0.0981 (4)	0.5725 (3)	0.0179 (9)
O3	0.2439 (4)	−0.1147 (4)	0.6654 (4)	0.0264 (11)
O4	0.2585 (4)	0.0906 (4)	0.4151 (4)	0.0277 (11)
O5	0.0068 (4)	0.1010 (4)	0.3686 (4)	0.0194 (10)
O6	0.0152 (4)	0.3070 (4)	0.4638 (4)	0.0248 (10)
O7	0.2572 (5)	0.3214 (5)	0.5220 (4)	0.0363 (13)
O8	0.3963 (5)	0.0709 (6)	0.6387 (4)	0.0402 (14)
O9	0.1606 (5)	0.2940 (5)	0.2947 (5)	0.0387 (13)
O10	0.1299 (5)	−0.3034 (5)	0.7537 (4)	0.0371 (13)
O11	0.3805 (5)	−0.1190 (5)	0.4861 (5)	0.0411 (14)
O12	0.2244 (5)	−0.3451 (5)	0.5585 (5)	0.0361 (13)
O13	0.3240 (4)	0.9610 (4)	0.8850 (3)	0.0245 (10)
O14	0.3461 (6)	0.0115 (5)	0.2248 (5)	0.0503 (17)
O15	0.5005 (7)	0.6433 (10)	0.5925 (9)	0.107 (3)
O16	0.5084 (9)	0.2974 (9)	0.7036 (10)	0.114 (4)
O17	0.0119 (10)	0.9554 (6)	0.8499 (5)	0.095 (4)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mo1	0.0253 (4)	0.0199 (4)	0.0216 (4)	−0.0040 (2)	0.0034 (3)	0.0034 (2)
Mo2	0.0185 (4)	0.0270 (4)	0.0254 (4)	0.0002 (2)	0.0021 (3)	0.0024 (2)
Mo3	0.0249 (4)	0.0189 (4)	0.0198 (4)	0.0038 (2)	0.0018 (3)	0.0039 (2)
Al1	0.0173 (14)	0.0140 (14)	0.0126 (12)	−0.0006 (10)	0.0016 (10)	0.0007 (10)
O1	0.020 (2)	0.015 (2)	0.017 (2)	0.0013 (18)	0.0049 (18)	0.0015 (17)
O2	0.020 (2)	0.015 (2)	0.018 (2)	−0.0039 (18)	0.0017 (18)	−0.0015 (17)
O3	0.028 (3)	0.025 (3)	0.025 (2)	0.002 (2)	−0.002 (2)	0.002 (2)
O4	0.027 (3)	0.028 (3)	0.030 (3)	−0.001 (2)	0.009 (2)	0.005 (2)
O5	0.023 (2)	0.018 (2)	0.017 (2)	−0.0023 (19)	0.0012 (18)	0.0001 (18)
O6	0.031 (3)	0.017 (2)	0.028 (2)	−0.001 (2)	0.007 (2)	0.000 (2)
O7	0.035 (3)	0.030 (3)	0.042 (3)	−0.015 (2)	−0.001 (2)	−0.001 (2)
O8	0.028 (3)	0.050 (4)	0.039 (3)	−0.013 (3)	−0.003 (2)	0.001 (3)
O9	0.042 (3)	0.038 (3)	0.037 (3)	−0.004 (3)	0.008 (3)	0.014 (3)
O10	0.043 (3)	0.039 (3)	0.028 (3)	0.001 (3)	0.000 (2)	0.011 (2)
O11	0.038 (3)	0.042 (3)	0.046 (3)	0.012 (3)	0.015 (3)	0.003 (3)
O12	0.035 (3)	0.031 (3)	0.042 (3)	0.010 (2)	0.005 (2)	−0.001 (2)
O13	0.025 (2)	0.044 (3)	0.0031 (17)	−0.009 (2)	−0.0012 (17)	−0.0049 (18)
O14	0.075 (5)	0.053 (4)	0.030 (3)	−0.022 (3)	0.031 (3)	−0.025 (3)
O15	0.055 (5)	0.132 (10)	0.129 (8)	0.008 (5)	0.002 (5)	0.024 (6)
O16	0.104 (7)	0.077 (6)	0.143 (9)	−0.021 (6)	−0.034 (6)	−0.027 (6)
O17	0.235 (12)	0.028 (4)	0.028 (3)	0.003 (5)	0.037 (5)	−0.001 (3)

Geometric parameters (Å, º) top

Mo1—O7	1.699 (5)	Mo3—O12	1.717 (5)
Mo1—O9	1.709 (5)	Mo3—O3	1.905 (5)
Mo1—O4	1.932 (5)	Mo3—O6ⁱ	1.943 (5)
Mo1—O6	1.942 (5)	Mo3—O5ⁱ	2.277 (5)
Mo1—O5	2.297 (4)	Mo3—O1	2.307 (4)
Mo1—O2	2.315 (4)	Al1—O1	1.897 (4)
Mo2—O11	1.694 (5)	Al1—O1ⁱ	1.897 (4)
Mo2—O8	1.709 (5)	Al1—O2ⁱ	1.904 (4)
Mo2—O4	1.927 (5)	Al1—O2	1.904 (4)
Mo2—O3	1.940 (5)	Al1—O5ⁱ	1.909 (4)
Mo2—O1	2.312 (4)	Al1—O5	1.909 (4)
Mo2—O2	2.331 (4)	O5—Mo3ⁱ	2.277 (5)
Mo3—O10	1.700 (5)	O6—Mo3ⁱ	1.943 (5)

O7—Mo1—O9	106.5 (3)	O10—Mo3—O5ⁱ	94.0 (2)
O7—Mo1—O4	101.6 (2)	O12—Mo3—O5ⁱ	158.7 (2)
O9—Mo1—O4	98.7 (2)	O3—Mo3—O5ⁱ	83.64 (19)
O7—Mo1—O6	96.2 (2)	O6ⁱ—Mo3—O5ⁱ	72.45 (18)
O9—Mo1—O6	99.1 (2)	O10—Mo3—O1	160.5 (2)
O4—Mo1—O6	150.1 (2)	O12—Mo3—O1	93.2 (2)
O7—Mo1—O5	158.0 (2)	O3—Mo3—O1	72.31 (17)
O9—Mo1—O5	93.9 (2)	O6ⁱ—Mo3—O1	83.03 (17)
O4—Mo1—O5	82.88 (19)	O5ⁱ—Mo3—O1	68.43 (15)
O6—Mo1—O5	72.02 (18)	O1—Al1—O1ⁱ	180.000 (1)
O7—Mo1—O2	93.0 (2)	O1—Al1—O2ⁱ	94.53 (19)
O9—Mo1—O2	160.1 (2)	O1ⁱ—Al1—O2ⁱ	85.47 (19)
O4—Mo1—O2	72.61 (17)	O1—Al1—O2	85.47 (19)
O6—Mo1—O2	82.68 (17)	O1ⁱ—Al1—O2	94.53 (19)
O5—Mo1—O2	67.61 (15)	O2ⁱ—Al1—O2	180.00 (18)
O11—Mo2—O8	106.6 (3)	O1—Al1—O5ⁱ	85.29 (18)
O11—Mo2—O4	97.8 (2)	O1ⁱ—Al1—O5ⁱ	94.71 (18)
O8—Mo2—O4	102.3 (2)	O2ⁱ—Al1—O5ⁱ	84.60 (18)
O11—Mo2—O3	101.0 (2)	O2—Al1—O5ⁱ	95.40 (18)
O8—Mo2—O3	95.9 (2)	O1—Al1—O5	94.71 (18)
O4—Mo2—O3	148.8 (2)	O1ⁱ—Al1—O5	85.29 (18)
O11—Mo2—O1	92.3 (2)	O2ⁱ—Al1—O5	95.40 (18)
O8—Mo2—O1	159.3 (2)	O2—Al1—O5	84.60 (18)
O4—Mo2—O1	83.02 (18)	O5ⁱ—Al1—O5	180.000 (1)
O3—Mo2—O1	71.63 (17)	Al1—O1—Mo3	102.77 (17)
O11—Mo2—O2	158.1 (2)	Al1—O1—Mo2	103.98 (19)
O8—Mo2—O2	94.7 (2)	Mo3—O1—Mo2	91.50 (15)
O4—Mo2—O2	72.35 (17)	Al1—O2—Mo1	103.63 (18)
O3—Mo2—O2	81.13 (17)	Al1—O2—Mo2	103.05 (18)
O1—Mo2—O2	67.49 (15)	Mo1—O2—Mo2	91.18 (15)
O10—Mo3—O12	105.6 (3)	Mo3—O3—Mo2	118.8 (2)
O10—Mo3—O3	98.1 (2)	Mo2—O4—Mo1	118.7 (2)
O12—Mo3—O3	101.5 (2)	Al1—O5—Mo3ⁱ	103.48 (18)
O10—Mo3—O6ⁱ	100.3 (2)	Al1—O5—Mo1	104.16 (18)
O12—Mo3—O6ⁱ	95.4 (2)	Mo3ⁱ—O5—Mo1	93.07 (17)
O3—Mo3—O6ⁱ	150.7 (2)	Mo1—O6—Mo3ⁱ	117.4 (2)

Symmetry code: (i) −x, −y, −z+1.

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