Buy article online - an online subscription or single-article purchase is required to access this article.
Download citation
Download citation
link to html
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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807021733/mg2022sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807021733/mg2022Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](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

Computing details top

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]·10H2OF(000) = 2520
Mr = 1333.16Dx = 2.916 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 3398 reflections
a = 23.553 (5) Åθ = 3.2–27.5°
b = 11.549 (2) ŵ = 3.84 mm1
c = 11.227 (2) ÅT = 298 K
β = 96.06 (3)°Block, colorless
V = 3037.0 (10) Å30.14 × 0.13 × 0.12 mm
Z = 4
Data collection top
Rigaku R-AXIS RAPID IP
diffractometer
3398 independent reflections
Radiation source: fine-focus sealed tube3082 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.045
Detector resolution: 0.1 pixels mm-1θmax = 27.5°, θmin = 3.2°
ω scansh = 3030
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
k = 1413
Tmin = 0.588, Tmax = 0.632l = 1314
14015 measured reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.037H-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 reflectionsΔρmax = 1.75 e Å3
198 parametersΔρmin = 0.89 e Å3
1 restraintExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction 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
xyzUiso*/Ueq
Na11.00000.9662 (3)0.25000.0329 (8)
Ba11.00001.34833 (5)0.25000.03697 (17)
Al10.75000.75000.00000.0127 (4)
Mo10.68087 (2)0.64987 (4)0.21880 (4)0.01786 (13)
Mo20.82196 (2)0.65332 (4)0.24945 (4)0.01757 (13)
Mo30.89199 (2)0.75668 (4)0.03117 (4)0.01799 (13)
O10.80998 (16)0.7003 (3)0.0888 (3)0.0152 (7)
H10.80850.63470.12340.018*
O20.74858 (16)0.8830 (3)0.0989 (3)0.0152 (7)
H20.73970.94380.06250.018*
O30.69050 (16)0.6967 (3)0.1138 (3)0.0145 (7)
H30.68660.62750.13900.017*
O40.63246 (17)0.6160 (3)0.0727 (4)0.0211 (8)
O50.6829 (2)0.5136 (4)0.2771 (4)0.0334 (11)
O60.6337 (2)0.7256 (5)0.2950 (5)0.0387 (12)
O70.75046 (18)0.7129 (4)0.3002 (4)0.0212 (8)
O80.8208 (2)0.5166 (4)0.3063 (4)0.0291 (10)
O90.8659 (2)0.7318 (4)0.3498 (4)0.0297 (10)
O100.87202 (17)0.6260 (4)0.1263 (4)0.0222 (9)
O110.9360 (2)0.8310 (4)0.1342 (5)0.0352 (11)
O120.9360 (2)0.6859 (4)0.0567 (4)0.0330 (11)
O1W0.9655 (2)1.1348 (4)0.1305 (5)0.0362 (11)
H40.93471.11710.15940.043*
H50.96101.10980.05900.043*
O2W1.0293 (2)1.5533 (5)0.1446 (5)0.0477 (14)
H61.04891.60940.17610.057*
H71.04511.57570.08400.057*
O3W1.0854 (2)1.4145 (4)0.4297 (5)0.0425 (13)
H81.11381.38120.46860.051*
H91.10081.47460.40350.051*
O4W1.0631 (2)0.9301 (4)0.1059 (4)0.0313 (10)
H101.09120.88570.12710.038*
H111.08540.98790.10530.038*
O5W0.2619 (3)0.8988 (4)0.0431 (5)0.060 (2)
H120.27360.84670.09330.072*
H130.26750.87800.02740.072*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Na10.036 (2)0.029 (2)0.033 (2)0.0000.0042 (16)0.000
Ba10.0672 (4)0.0237 (3)0.0226 (3)0.0000.0167 (3)0.000
Al10.0147 (11)0.0110 (11)0.0128 (10)0.0000 (8)0.0035 (8)0.0006 (8)
Mo10.0216 (3)0.0166 (3)0.0166 (2)0.00318 (18)0.00774 (17)0.00191 (17)
Mo20.0207 (3)0.0155 (2)0.0161 (2)0.00083 (18)0.00007 (17)0.00394 (17)
Mo30.0129 (2)0.0190 (3)0.0224 (2)0.00064 (18)0.00339 (17)0.00123 (18)
O10.0180 (19)0.0101 (18)0.0186 (19)0.0006 (14)0.0072 (14)0.0036 (14)
O20.0182 (19)0.0124 (18)0.0156 (18)0.0016 (14)0.0040 (14)0.0001 (14)
O30.0167 (19)0.0115 (18)0.0158 (18)0.0017 (14)0.0033 (14)0.0014 (14)
O40.017 (2)0.018 (2)0.028 (2)0.0062 (15)0.0019 (16)0.0003 (16)
O50.044 (3)0.027 (2)0.028 (2)0.010 (2)0.000 (2)0.0108 (19)
O60.040 (3)0.047 (3)0.033 (3)0.006 (2)0.022 (2)0.007 (2)
O70.027 (2)0.021 (2)0.0159 (19)0.0004 (17)0.0054 (16)0.0005 (15)
O80.035 (3)0.020 (2)0.032 (2)0.0015 (18)0.0014 (19)0.0091 (18)
O90.031 (2)0.030 (2)0.026 (2)0.0054 (19)0.0074 (18)0.0031 (18)
O100.018 (2)0.019 (2)0.029 (2)0.0041 (16)0.0038 (16)0.0078 (16)
O110.024 (2)0.036 (3)0.044 (3)0.008 (2)0.003 (2)0.000 (2)
O120.026 (2)0.034 (3)0.041 (3)0.007 (2)0.013 (2)0.005 (2)
O1W0.033 (3)0.041 (3)0.035 (3)0.002 (2)0.001 (2)0.004 (2)
O2W0.051 (4)0.041 (3)0.053 (3)0.014 (3)0.012 (3)0.005 (3)
O3W0.037 (3)0.027 (3)0.064 (4)0.003 (2)0.007 (3)0.006 (2)
O4W0.027 (2)0.027 (2)0.040 (3)0.0066 (19)0.0018 (19)0.0047 (19)
O5W0.141 (7)0.016 (3)0.025 (3)0.001 (3)0.018 (3)0.0021 (19)
Geometric parameters (Å, º) top
Na1—O112.447 (5)Mo1—O51.704 (4)
Na1—O11i2.447 (5)Mo1—O61.713 (5)
Na1—O1Wi2.453 (6)Mo1—O71.933 (4)
Na1—O1W2.453 (6)Mo2—O2iv2.280 (4)
Na1—O4Wi2.347 (5)Mo2—O3iv2.305 (4)
Na1—O4W2.347 (5)Mo2—O71.959 (4)
Ba1—O12ii2.798 (5)Mo2—O81.705 (4)
Ba1—O12iii2.798 (5)Mo2—O91.708 (4)
Ba1—O1W2.883 (5)Mo2—O101.936 (4)
Ba1—O1Wi2.883 (5)Mo3—O12.328 (4)
Ba1—O2Wi2.766 (5)Mo3—O3iv2.303 (4)
Ba1—O2W2.766 (5)Mo3—O4iv1.927 (4)
Ba1—O3Wi2.801 (6)Mo3—O101.935 (4)
Ba1—O3W2.801 (6)Mo3—O111.702 (5)
Al1—O11.902 (4)Mo3—O121.712 (5)
Al1—O1iv1.902 (4)O1—Mo1iv2.289 (4)
Al1—O21.894 (4)O2—Mo1iv2.278 (4)
Al1—O2iv1.894 (4)O2—Mo2iv2.280 (4)
Al1—O31.896 (4)O3—Mo3iv2.303 (4)
Al1—O3iv1.896 (4)O3—Mo2iv2.305 (4)
Mo1—O1iv2.289 (4)O4—Mo3iv1.927 (4)
Mo1—O2iv2.278 (4)O12—Ba1iii2.798 (5)
Mo1—O41.936 (4)
O4Wi—Na1—O4W159.5 (3)O5—Mo1—O7100.3 (2)
O4Wi—Na1—O1181.55 (18)O6—Mo1—O797.7 (2)
O4W—Na1—O1185.39 (18)O5—Mo1—O497.4 (2)
O4Wi—Na1—O11i85.39 (18)O6—Mo1—O499.9 (2)
O4W—Na1—O11i81.55 (18)O7—Mo1—O4150.57 (17)
O11—Na1—O11i100.7 (3)O5—Mo1—O2iv94.6 (2)
O4Wi—Na1—O1Wi87.80 (18)O6—Mo1—O2iv158.8 (2)
O4W—Na1—O1Wi108.72 (18)O7—Mo1—O2iv72.97 (15)
O11—Na1—O1Wi161.22 (19)O4—Mo1—O2iv82.35 (16)
O11i—Na1—O1Wi93.80 (17)O5—Mo1—O1iv160.58 (19)
O4Wi—Na1—O1W108.72 (18)O6—Mo1—O1iv92.4 (2)
O4W—Na1—O1W87.80 (18)O7—Mo1—O1iv83.37 (16)
O11—Na1—O1W93.80 (17)O4—Mo1—O1iv72.50 (15)
O11i—Na1—O1W161.22 (19)O2iv—Mo1—O1iv68.02 (13)
O1Wi—Na1—O1W75.0 (3)O8—Mo2—O9106.1 (2)
O2Wi—Ba1—O2W62.3 (2)O8—Mo2—O1098.7 (2)
O2Wi—Ba1—O12ii67.05 (16)O9—Mo2—O10100.7 (2)
O2W—Ba1—O12ii129.19 (16)O8—Mo2—O799.7 (2)
O2Wi—Ba1—O12iii129.19 (16)O9—Mo2—O795.8 (2)
O2W—Ba1—O12iii67.05 (16)O10—Mo2—O7150.75 (17)
O12ii—Ba1—O12iii163.7 (2)O8—Mo2—O2iv93.87 (19)
O2Wi—Ba1—O3Wi83.22 (16)O9—Mo2—O2iv158.48 (18)
O2W—Ba1—O3Wi69.57 (16)O10—Mo2—O2iv83.78 (16)
O12ii—Ba1—O3Wi101.08 (15)O7—Mo2—O2iv72.47 (15)
O12iii—Ba1—O3Wi83.40 (15)O8—Mo2—O3iv159.64 (18)
O2Wi—Ba1—O3W69.57 (16)O9—Mo2—O3iv93.65 (18)
O2W—Ba1—O3W83.22 (16)O10—Mo2—O3iv72.24 (15)
O12ii—Ba1—O3W83.40 (15)O7—Mo2—O3iv82.82 (15)
O12iii—Ba1—O3W101.08 (15)O2iv—Mo2—O3iv67.44 (13)
O3Wi—Ba1—O3W148.3 (2)O11—Mo3—O12105.7 (2)
O2Wi—Ba1—O1W149.35 (16)O11—Mo3—O4iv98.5 (2)
O2W—Ba1—O1W127.13 (16)O12—Mo3—O4iv100.1 (2)
O12ii—Ba1—O1W95.25 (14)O11—Mo3—O10100.6 (2)
O12iii—Ba1—O1W70.53 (15)O12—Mo3—O1098.2 (2)
O3Wi—Ba1—O1W75.68 (15)O4iv—Mo3—O10148.72 (17)
O3W—Ba1—O1W135.59 (14)O11—Mo3—O3iv95.0 (2)
O2Wi—Ba1—O1Wi127.13 (16)O12—Mo3—O3iv158.60 (19)
O2W—Ba1—O1Wi149.35 (16)O4iv—Mo3—O3iv81.63 (15)
O12ii—Ba1—O1Wi70.53 (15)O10—Mo3—O3iv72.28 (15)
O12iii—Ba1—O1Wi95.25 (14)O11—Mo3—O1160.56 (19)
O3Wi—Ba1—O1Wi135.59 (14)O12—Mo3—O192.75 (19)
O3W—Ba1—O1Wi75.68 (15)O4iv—Mo3—O171.74 (15)
O1W—Ba1—O1Wi62.4 (2)O10—Mo3—O182.29 (16)
O2—Al1—O2iv180.0 (2)O3iv—Mo3—O167.35 (13)
O2—Al1—O384.38 (16)Al1—O1—Mo1iv103.35 (16)
O2iv—Al1—O395.62 (16)Al1—O1—Mo3103.22 (16)
O2—Al1—O3iv95.62 (16)Mo1iv—O1—Mo391.67 (13)
O2iv—Al1—O3iv84.38 (16)Al1—O2—Mo1iv104.04 (16)
O3—Al1—O3iv180.000 (1)Al1—O2—Mo2iv104.59 (17)
O2—Al1—O1iv95.42 (16)Mo1iv—O2—Mo2iv92.94 (14)
O2iv—Al1—O1iv84.58 (16)Al1—O3—Mo3iv104.35 (16)
O3—Al1—O1iv85.08 (16)Al1—O3—Mo2iv103.58 (16)
O3iv—Al1—O1iv94.92 (16)Mo3iv—O3—Mo2iv92.10 (13)
O2—Al1—O184.58 (16)Mo3iv—O4—Mo1118.1 (2)
O2iv—Al1—O195.42 (16)Mo1—O7—Mo2116.2 (2)
O3—Al1—O194.92 (16)Mo3—O10—Mo2118.0 (2)
O3iv—Al1—O185.08 (16)Mo3—O11—Na1168.5 (3)
O1iv—Al1—O1180.000 (2)Mo3—O12—Ba1iii157.4 (3)
O5—Mo1—O6105.9 (3)Na1—O1W—Ba1111.33 (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···AD—HH···AD···AD—H···A
O1—H1···O8v0.851.952.790 (6)169
O2—H2···O5Wvi0.851.832.615 (6)153
O3—H3···O5v0.851.882.718 (6)169
O1W—H4···O6vii0.852.142.769 (7)130
O1W—H5···O4Wiii0.851.932.772 (7)169
O2W—H6···O9viii0.852.503.211 (7)142
O2W—H7···O3Wix0.852.062.895 (8)165
O3W—H8···O9x0.852.433.114 (7)139
O3W—H9···O10viii0.851.902.738 (7)167
O4W—H10···O9i0.852.052.848 (7)157
O4W—H11···O4xi0.851.912.747 (6)170
O5W—H12···O7xii0.852.072.810 (7)145
O5W—H13···O7xiii0.852.203.003 (6)157
Symmetry codes: (i) x+2, y, z+1/2; (iii) x+2, y+2, z; (v) x, y+1, z1/2; (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, z1/2; (x) x+2, y+2, z+1; (xi) x+1/2, y+1/2, z; (xii) x+1, y, z+1/2; (xiii) x1/2, y+3/2, z1/2.
 

Subscribe to Acta Crystallographica Section E: Crystallographic Communications

The full text of this article is available to subscribers to the journal.

If you have already registered and are using a computer listed in your registration details, please email support@iucr.org for assistance.

Buy online

You may purchase this article in PDF and/or HTML formats. For purchasers in the European Community who do not have a VAT number, VAT will be added at the local rate. Payments to the IUCr are handled by WorldPay, who will accept payment by credit card in several currencies. To purchase the article, please complete the form below (fields marked * are required), and then click on `Continue'.
E-mail address* 
Repeat e-mail address* 
(for error checking) 

Format*   PDF (US $40)
   HTML (US $40)
   PDF+HTML (US $50)
In order for VAT to be shown for your country javascript needs to be enabled.

VAT number 
(non-UK EC countries only) 
Country* 
 

Terms and conditions of use
Contact us

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds