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The title compound, NaBa[AlMo6(OH)6O18]·10H2O, contains a B-type Anderson polyanion [AlMo6(OH)6O18]3- having an inversion center with approximate D3d symmetry. There are two uncoordinated water molecules per formula unit, the remaining eight being coordinated to the Na+ and Ba2+ cations, which link the polyanions to form the three-dimensional structure. Hydrogen-bonding interactions exist to stabilize the structure.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (l-O) = 0.004 Å
- R factor = 0.037
- wR factor = 0.087
- Data-to-parameter ratio = 17.2
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.65 Ratio
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2
H2 O
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 3
H2 O
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 4
H2 O
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 7
Ba
Alert level G
PLAT794_ALERT_5_G Check Predicted Bond Valency for Mo1 (6) 6.01
PLAT794_ALERT_5_G Check Predicted Bond Valency for Mo2 (6) 5.95
PLAT794_ALERT_5_G Check Predicted Bond Valency for Mo3 (6) 5.97
PLAT794_ALERT_5_G Check Predicted Bond Valency for Al1 (3) 2.83
PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 1
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
5 ALERT level C = Check and explain
5 ALERT level G = General alerts; check
0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
1 ALERT type 2 Indicator that the structure model may be wrong or deficient
1 ALERT type 3 Indicator that the structure quality may be low
4 ALERT type 4 Improvement, methodology, query or suggestion
4 ALERT type 5 Informative message, check
Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: RAPID-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: CrystalStructure (Rigaku/MSC, 2002); software used to prepare material for publication: CrystalStructure.
Sodium barium hexahydrogenhexamolybdoaluminate(II) decahydrate
top
Crystal data top
NaBa[AlMo6(OH)6O18]·10H2O | F(000) = 2520 |
Mr = 1333.16 | Dx = 2.916 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 3398 reflections |
a = 23.553 (5) Å | θ = 3.2–27.5° |
b = 11.549 (2) Å | µ = 3.84 mm−1 |
c = 11.227 (2) Å | T = 298 K |
β = 96.06 (3)° | Block, colorless |
V = 3037.0 (10) Å3 | 0.14 × 0.13 × 0.12 mm |
Z = 4 | |
Data collection top
Rigaku R-AXIS RAPID IP diffractometer | 3398 independent reflections |
Radiation source: fine-focus sealed tube | 3082 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.045 |
Detector resolution: 0.1 pixels mm-1 | θmax = 27.5°, θmin = 3.2° |
ω scans | h = −30→30 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −14→13 |
Tmin = 0.588, Tmax = 0.632 | l = −13→14 |
14015 measured reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.037 | H-atom parameters constrained |
wR(F2) = 0.087 | w = 1/[σ2(Fo2) + 58.3693P] where P = (Fo2 + 2Fc2)/3 |
S = 1.14 | (Δ/σ)max = 0.001 |
3398 reflections | Δρmax = 1.75 e Å−3 |
198 parameters | Δρmin = −0.89 e Å−3 |
1 restraint | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.00071 (5) |
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 | Uiso*/Ueq | |
Na1 | 1.0000 | 0.9662 (3) | 0.2500 | 0.0329 (8) | |
Ba1 | 1.0000 | 1.34833 (5) | 0.2500 | 0.03697 (17) | |
Al1 | 0.7500 | 0.7500 | 0.0000 | 0.0127 (4) | |
Mo1 | 0.68087 (2) | 0.64987 (4) | 0.21880 (4) | 0.01786 (13) | |
Mo2 | 0.82196 (2) | 0.65332 (4) | 0.24945 (4) | 0.01757 (13) | |
Mo3 | 0.89199 (2) | 0.75668 (4) | 0.03117 (4) | 0.01799 (13) | |
O1 | 0.80998 (16) | 0.7003 (3) | −0.0888 (3) | 0.0152 (7) | |
H1 | 0.8085 | 0.6347 | −0.1234 | 0.018* | |
O2 | 0.74858 (16) | 0.8830 (3) | −0.0989 (3) | 0.0152 (7) | |
H2 | 0.7397 | 0.9438 | −0.0625 | 0.018* | |
O3 | 0.69050 (16) | 0.6967 (3) | −0.1138 (3) | 0.0145 (7) | |
H3 | 0.6866 | 0.6275 | −0.1390 | 0.017* | |
O4 | 0.63246 (17) | 0.6160 (3) | 0.0727 (4) | 0.0211 (8) | |
O5 | 0.6829 (2) | 0.5136 (4) | 0.2771 (4) | 0.0334 (11) | |
O6 | 0.6337 (2) | 0.7256 (5) | 0.2950 (5) | 0.0387 (12) | |
O7 | 0.75046 (18) | 0.7129 (4) | 0.3002 (4) | 0.0212 (8) | |
O8 | 0.8208 (2) | 0.5166 (4) | 0.3063 (4) | 0.0291 (10) | |
O9 | 0.8659 (2) | 0.7318 (4) | 0.3498 (4) | 0.0297 (10) | |
O10 | 0.87202 (17) | 0.6260 (4) | 0.1263 (4) | 0.0222 (9) | |
O11 | 0.9360 (2) | 0.8310 (4) | 0.1342 (5) | 0.0352 (11) | |
O12 | 0.9360 (2) | 0.6859 (4) | −0.0567 (4) | 0.0330 (11) | |
O1W | 0.9655 (2) | 1.1348 (4) | 0.1305 (5) | 0.0362 (11) | |
H4 | 0.9347 | 1.1171 | 0.1594 | 0.043* | |
H5 | 0.9610 | 1.1098 | 0.0590 | 0.043* | |
O2W | 1.0293 (2) | 1.5533 (5) | 0.1446 (5) | 0.0477 (14) | |
H6 | 1.0489 | 1.6094 | 0.1761 | 0.057* | |
H7 | 1.0451 | 1.5757 | 0.0840 | 0.057* | |
O3W | 1.0854 (2) | 1.4145 (4) | 0.4297 (5) | 0.0425 (13) | |
H8 | 1.1138 | 1.3812 | 0.4686 | 0.051* | |
H9 | 1.1008 | 1.4746 | 0.4035 | 0.051* | |
O4W | 1.0631 (2) | 0.9301 (4) | 0.1059 (4) | 0.0313 (10) | |
H10 | 1.0912 | 0.8857 | 0.1271 | 0.038* | |
H11 | 1.0854 | 0.9879 | 0.1053 | 0.038* | |
O5W | 0.2619 (3) | 0.8988 (4) | 0.0431 (5) | 0.060 (2) | |
H12 | 0.2736 | 0.8467 | 0.0933 | 0.072* | |
H13 | 0.2675 | 0.8780 | −0.0274 | 0.072* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Na1 | 0.036 (2) | 0.029 (2) | 0.033 (2) | 0.000 | 0.0042 (16) | 0.000 |
Ba1 | 0.0672 (4) | 0.0237 (3) | 0.0226 (3) | 0.000 | 0.0167 (3) | 0.000 |
Al1 | 0.0147 (11) | 0.0110 (11) | 0.0128 (10) | 0.0000 (8) | 0.0035 (8) | 0.0006 (8) |
Mo1 | 0.0216 (3) | 0.0166 (3) | 0.0166 (2) | −0.00318 (18) | 0.00774 (17) | 0.00191 (17) |
Mo2 | 0.0207 (3) | 0.0155 (2) | 0.0161 (2) | −0.00083 (18) | 0.00007 (17) | 0.00394 (17) |
Mo3 | 0.0129 (2) | 0.0190 (3) | 0.0224 (2) | −0.00064 (18) | 0.00339 (17) | 0.00123 (18) |
O1 | 0.0180 (19) | 0.0101 (18) | 0.0186 (19) | −0.0006 (14) | 0.0072 (14) | −0.0036 (14) |
O2 | 0.0182 (19) | 0.0124 (18) | 0.0156 (18) | 0.0016 (14) | 0.0040 (14) | −0.0001 (14) |
O3 | 0.0167 (19) | 0.0115 (18) | 0.0158 (18) | −0.0017 (14) | 0.0033 (14) | −0.0014 (14) |
O4 | 0.017 (2) | 0.018 (2) | 0.028 (2) | −0.0062 (15) | 0.0019 (16) | 0.0003 (16) |
O5 | 0.044 (3) | 0.027 (2) | 0.028 (2) | −0.010 (2) | 0.000 (2) | 0.0108 (19) |
O6 | 0.040 (3) | 0.047 (3) | 0.033 (3) | −0.006 (2) | 0.022 (2) | −0.007 (2) |
O7 | 0.027 (2) | 0.021 (2) | 0.0159 (19) | 0.0004 (17) | 0.0054 (16) | −0.0005 (15) |
O8 | 0.035 (3) | 0.020 (2) | 0.032 (2) | 0.0015 (18) | 0.0014 (19) | 0.0091 (18) |
O9 | 0.031 (2) | 0.030 (2) | 0.026 (2) | −0.0054 (19) | −0.0074 (18) | 0.0031 (18) |
O10 | 0.018 (2) | 0.019 (2) | 0.029 (2) | 0.0041 (16) | 0.0038 (16) | 0.0078 (16) |
O11 | 0.024 (2) | 0.036 (3) | 0.044 (3) | −0.008 (2) | −0.003 (2) | 0.000 (2) |
O12 | 0.026 (2) | 0.034 (3) | 0.041 (3) | 0.007 (2) | 0.013 (2) | 0.005 (2) |
O1W | 0.033 (3) | 0.041 (3) | 0.035 (3) | 0.002 (2) | 0.001 (2) | −0.004 (2) |
O2W | 0.051 (4) | 0.041 (3) | 0.053 (3) | −0.014 (3) | 0.012 (3) | 0.005 (3) |
O3W | 0.037 (3) | 0.027 (3) | 0.064 (4) | 0.003 (2) | 0.007 (3) | 0.006 (2) |
O4W | 0.027 (2) | 0.027 (2) | 0.040 (3) | −0.0066 (19) | 0.0018 (19) | 0.0047 (19) |
O5W | 0.141 (7) | 0.016 (3) | 0.025 (3) | 0.001 (3) | 0.018 (3) | −0.0021 (19) |
Geometric parameters (Å, º) top
Na1—O11 | 2.447 (5) | Mo1—O5 | 1.704 (4) |
Na1—O11i | 2.447 (5) | Mo1—O6 | 1.713 (5) |
Na1—O1Wi | 2.453 (6) | Mo1—O7 | 1.933 (4) |
Na1—O1W | 2.453 (6) | Mo2—O2iv | 2.280 (4) |
Na1—O4Wi | 2.347 (5) | Mo2—O3iv | 2.305 (4) |
Na1—O4W | 2.347 (5) | Mo2—O7 | 1.959 (4) |
Ba1—O12ii | 2.798 (5) | Mo2—O8 | 1.705 (4) |
Ba1—O12iii | 2.798 (5) | Mo2—O9 | 1.708 (4) |
Ba1—O1W | 2.883 (5) | Mo2—O10 | 1.936 (4) |
Ba1—O1Wi | 2.883 (5) | Mo3—O1 | 2.328 (4) |
Ba1—O2Wi | 2.766 (5) | Mo3—O3iv | 2.303 (4) |
Ba1—O2W | 2.766 (5) | Mo3—O4iv | 1.927 (4) |
Ba1—O3Wi | 2.801 (6) | Mo3—O10 | 1.935 (4) |
Ba1—O3W | 2.801 (6) | Mo3—O11 | 1.702 (5) |
Al1—O1 | 1.902 (4) | Mo3—O12 | 1.712 (5) |
Al1—O1iv | 1.902 (4) | O1—Mo1iv | 2.289 (4) |
Al1—O2 | 1.894 (4) | O2—Mo1iv | 2.278 (4) |
Al1—O2iv | 1.894 (4) | O2—Mo2iv | 2.280 (4) |
Al1—O3 | 1.896 (4) | O3—Mo3iv | 2.303 (4) |
Al1—O3iv | 1.896 (4) | O3—Mo2iv | 2.305 (4) |
Mo1—O1iv | 2.289 (4) | O4—Mo3iv | 1.927 (4) |
Mo1—O2iv | 2.278 (4) | O12—Ba1iii | 2.798 (5) |
Mo1—O4 | 1.936 (4) | | |
| | | |
O4Wi—Na1—O4W | 159.5 (3) | O5—Mo1—O7 | 100.3 (2) |
O4Wi—Na1—O11 | 81.55 (18) | O6—Mo1—O7 | 97.7 (2) |
O4W—Na1—O11 | 85.39 (18) | O5—Mo1—O4 | 97.4 (2) |
O4Wi—Na1—O11i | 85.39 (18) | O6—Mo1—O4 | 99.9 (2) |
O4W—Na1—O11i | 81.55 (18) | O7—Mo1—O4 | 150.57 (17) |
O11—Na1—O11i | 100.7 (3) | O5—Mo1—O2iv | 94.6 (2) |
O4Wi—Na1—O1Wi | 87.80 (18) | O6—Mo1—O2iv | 158.8 (2) |
O4W—Na1—O1Wi | 108.72 (18) | O7—Mo1—O2iv | 72.97 (15) |
O11—Na1—O1Wi | 161.22 (19) | O4—Mo1—O2iv | 82.35 (16) |
O11i—Na1—O1Wi | 93.80 (17) | O5—Mo1—O1iv | 160.58 (19) |
O4Wi—Na1—O1W | 108.72 (18) | O6—Mo1—O1iv | 92.4 (2) |
O4W—Na1—O1W | 87.80 (18) | O7—Mo1—O1iv | 83.37 (16) |
O11—Na1—O1W | 93.80 (17) | O4—Mo1—O1iv | 72.50 (15) |
O11i—Na1—O1W | 161.22 (19) | O2iv—Mo1—O1iv | 68.02 (13) |
O1Wi—Na1—O1W | 75.0 (3) | O8—Mo2—O9 | 106.1 (2) |
O2Wi—Ba1—O2W | 62.3 (2) | O8—Mo2—O10 | 98.7 (2) |
O2Wi—Ba1—O12ii | 67.05 (16) | O9—Mo2—O10 | 100.7 (2) |
O2W—Ba1—O12ii | 129.19 (16) | O8—Mo2—O7 | 99.7 (2) |
O2Wi—Ba1—O12iii | 129.19 (16) | O9—Mo2—O7 | 95.8 (2) |
O2W—Ba1—O12iii | 67.05 (16) | O10—Mo2—O7 | 150.75 (17) |
O12ii—Ba1—O12iii | 163.7 (2) | O8—Mo2—O2iv | 93.87 (19) |
O2Wi—Ba1—O3Wi | 83.22 (16) | O9—Mo2—O2iv | 158.48 (18) |
O2W—Ba1—O3Wi | 69.57 (16) | O10—Mo2—O2iv | 83.78 (16) |
O12ii—Ba1—O3Wi | 101.08 (15) | O7—Mo2—O2iv | 72.47 (15) |
O12iii—Ba1—O3Wi | 83.40 (15) | O8—Mo2—O3iv | 159.64 (18) |
O2Wi—Ba1—O3W | 69.57 (16) | O9—Mo2—O3iv | 93.65 (18) |
O2W—Ba1—O3W | 83.22 (16) | O10—Mo2—O3iv | 72.24 (15) |
O12ii—Ba1—O3W | 83.40 (15) | O7—Mo2—O3iv | 82.82 (15) |
O12iii—Ba1—O3W | 101.08 (15) | O2iv—Mo2—O3iv | 67.44 (13) |
O3Wi—Ba1—O3W | 148.3 (2) | O11—Mo3—O12 | 105.7 (2) |
O2Wi—Ba1—O1W | 149.35 (16) | O11—Mo3—O4iv | 98.5 (2) |
O2W—Ba1—O1W | 127.13 (16) | O12—Mo3—O4iv | 100.1 (2) |
O12ii—Ba1—O1W | 95.25 (14) | O11—Mo3—O10 | 100.6 (2) |
O12iii—Ba1—O1W | 70.53 (15) | O12—Mo3—O10 | 98.2 (2) |
O3Wi—Ba1—O1W | 75.68 (15) | O4iv—Mo3—O10 | 148.72 (17) |
O3W—Ba1—O1W | 135.59 (14) | O11—Mo3—O3iv | 95.0 (2) |
O2Wi—Ba1—O1Wi | 127.13 (16) | O12—Mo3—O3iv | 158.60 (19) |
O2W—Ba1—O1Wi | 149.35 (16) | O4iv—Mo3—O3iv | 81.63 (15) |
O12ii—Ba1—O1Wi | 70.53 (15) | O10—Mo3—O3iv | 72.28 (15) |
O12iii—Ba1—O1Wi | 95.25 (14) | O11—Mo3—O1 | 160.56 (19) |
O3Wi—Ba1—O1Wi | 135.59 (14) | O12—Mo3—O1 | 92.75 (19) |
O3W—Ba1—O1Wi | 75.68 (15) | O4iv—Mo3—O1 | 71.74 (15) |
O1W—Ba1—O1Wi | 62.4 (2) | O10—Mo3—O1 | 82.29 (16) |
O2—Al1—O2iv | 180.0 (2) | O3iv—Mo3—O1 | 67.35 (13) |
O2—Al1—O3 | 84.38 (16) | Al1—O1—Mo1iv | 103.35 (16) |
O2iv—Al1—O3 | 95.62 (16) | Al1—O1—Mo3 | 103.22 (16) |
O2—Al1—O3iv | 95.62 (16) | Mo1iv—O1—Mo3 | 91.67 (13) |
O2iv—Al1—O3iv | 84.38 (16) | Al1—O2—Mo1iv | 104.04 (16) |
O3—Al1—O3iv | 180.000 (1) | Al1—O2—Mo2iv | 104.59 (17) |
O2—Al1—O1iv | 95.42 (16) | Mo1iv—O2—Mo2iv | 92.94 (14) |
O2iv—Al1—O1iv | 84.58 (16) | Al1—O3—Mo3iv | 104.35 (16) |
O3—Al1—O1iv | 85.08 (16) | Al1—O3—Mo2iv | 103.58 (16) |
O3iv—Al1—O1iv | 94.92 (16) | Mo3iv—O3—Mo2iv | 92.10 (13) |
O2—Al1—O1 | 84.58 (16) | Mo3iv—O4—Mo1 | 118.1 (2) |
O2iv—Al1—O1 | 95.42 (16) | Mo1—O7—Mo2 | 116.2 (2) |
O3—Al1—O1 | 94.92 (16) | Mo3—O10—Mo2 | 118.0 (2) |
O3iv—Al1—O1 | 85.08 (16) | Mo3—O11—Na1 | 168.5 (3) |
O1iv—Al1—O1 | 180.000 (2) | Mo3—O12—Ba1iii | 157.4 (3) |
O5—Mo1—O6 | 105.9 (3) | Na1—O1W—Ba1 | 111.33 (19) |
Symmetry codes: (i) −x+2, y, −z+1/2; (ii) x, −y+2, z+1/2; (iii) −x+2, −y+2, −z; (iv) −x+3/2, −y+3/2, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1···O8v | 0.85 | 1.95 | 2.790 (6) | 169 |
O2—H2···O5Wvi | 0.85 | 1.83 | 2.615 (6) | 153 |
O3—H3···O5v | 0.85 | 1.88 | 2.718 (6) | 169 |
O1W—H4···O6vii | 0.85 | 2.14 | 2.769 (7) | 130 |
O1W—H5···O4Wiii | 0.85 | 1.93 | 2.772 (7) | 169 |
O2W—H6···O9viii | 0.85 | 2.50 | 3.211 (7) | 142 |
O2W—H7···O3Wix | 0.85 | 2.06 | 2.895 (8) | 165 |
O3W—H8···O9x | 0.85 | 2.43 | 3.114 (7) | 139 |
O3W—H9···O10viii | 0.85 | 1.90 | 2.738 (7) | 167 |
O4W—H10···O9i | 0.85 | 2.05 | 2.848 (7) | 157 |
O4W—H11···O4xi | 0.85 | 1.91 | 2.747 (6) | 170 |
O5W—H12···O7xii | 0.85 | 2.07 | 2.810 (7) | 145 |
O5W—H13···O7xiii | 0.85 | 2.20 | 3.003 (6) | 157 |
Symmetry codes: (i) −x+2, y, −z+1/2; (iii) −x+2, −y+2, −z; (v) x, −y+1, z−1/2; (vi) −x+1, −y+2, −z; (vii) −x+3/2, y+1/2, −z+1/2; (viii) −x+2, y+1, −z+1/2; (ix) x, −y+3, z−1/2; (x) −x+2, −y+2, −z+1; (xi) x+1/2, y+1/2, z; (xii) −x+1, y, −z+1/2; (xiii) x−1/2, −y+3/2, z−1/2. |
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