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The crystal structure of the novel polyoxometalate supramolecular compound bis­[ennea­aqua­lanthanum(III)] octacosaoxodecavanadate(V) octahydrate is reported. The V10 cluster, with a 6- charge, plays a host role and [La(H2O)9]3+acts as a guest. The oxidation number of La is three and the oxidation number of V is five. There are four water mol­ecules in the asymmetric unit, disordered over five sites. The corresponding site-occupation factors are 1.0, 0.54. 0.67, 0.85 and 0.94. Extensive intermolecular hydrogen-bonding interactions generate a three-dimensional supramolecular network structure. The polyoxovanadate anion has crystallographic inversion symmetry.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802019700/bt6186sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802019700/bt6186Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](La-O) = 0.005 Å
  • Disorder in solvent or counterion
  • R factor = 0.039
  • wR factor = 0.124
  • Data-to-parameter ratio = 12.4

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Red Alert Alert Level A:
ABSMU_01 Alert A The ratio of given/expected absorption coefficient lies outside the range 0.90 <> 1.10 Calculated value of mu = 7.885 Value of mu given = 3.942 DENSD_01 Alert A The ratio of the submitted crystal density and that calculated from the formula is outside the range 0.90 <> 1.10 Crystal density given = 2.501 Calculated crystal density = 5.002
Yellow Alert Alert Level C:
PLAT_302 Alert C Anion/Solvent Disorder ....................... 60.00 Perc. General Notes
FORMU_01 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: H104 La4 O108 V20 Atom count from _chemical_formula_moiety:H52 La2 O54 V10 FORMU_01 There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:H104 La4 O108 V20 Atom count from the _atom_site data: H52 La2 O54 V10 CELLZ_01 From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_sum H104 La4 O108 V20 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff H 208.00 104.00 104.00 La 8.00 4.00 4.00 O 216.00 108.00 108.00 V 40.00 20.00 20.00 Difference between formula and atom_site contents detected. ALERT: Large difference may be due to a symmetry error - see SYMMG tests CHEMW_03 From the CIF: _cell_formula_units_Z 2 From the CIF: _chemical_formula_weight 3407.27 TEST: Calculate formula weight from _atom_site_* atom mass num sum H 1.01 52.00 52.42 O 16.00 54.00 863.95 V 50.94 10.00 509.42 La 138.91 2.00 277.81 Calculated formula weight 1703.59 ALERT: The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.90 <> 1.10
2 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check

Comment top

Since the idea of supramolecular chemistry was brought forward by Lehn (1988), polyacid supramolecular chemistry has fast developed due to the fact that polyacid supramolecular compounds possess the ability to store electrons. Polyacids belong to a kind of ligand which can form a supramolecule with organic or inorganic ions, and possess electricity, magnetic and non-linear optical properties. In order to investigate the relativity between the macroproperty and microproperty of polyacid supramolecular compounds, the novel title compound was synthesized.

The crystal data of the title compound shows that V cluster plays a main role with with a 6- charge and La(H2O)9 with a 3+ charge plays a guest role in the polyacid supramolecular compound. The oxidation number of La is three and the oxidation number of V is five. All the coordination polyhedrons of V are distorted octahedrons. The O atoms as bridging ligands coordinate to V with four types: (i) end coordinated (O18, O19, O20 and O22), with V—O distances in the range 1.604 (5)–1.620 (4) Å; (ii) bridged coordination (O10, O11, O12, O13, O14, O15 and O21), with V—O distances in the range 1.677 (4)–2.037 (4) Å; (iii) tribridged coordination (O16 and O17), with V—O distances in the range 1.927 (4)–1.935 (4) Å; and (iv) hexbridged coordination (O23), with V—O distances in the range 2.098 (4)–2.308 (4) Å. The V—V distances are in the range 3.0563 (16)–3.1093 (16) Å, the O—V—O bond angles are in the range 74.09 (15)–174.9 (2)°, and the V—O—V bond angles are in the range 82.95 (14)–171.0 (2)°. The La(H2O)9 cations are arranged as pillars (see Fig. 3) along the a axis, with La—O distances in the range 2.414 (5)–2.540 (5) Å. There are 35 hydrogen bonds formed (Table 2) in a molecule of the polyacid supramolecular compound, with O···O distance in the range 2.58 (2)–3.606 (7) Å, which form a three-dimensional network.

Experimental top

The title compound was prepared as follows. NaV10O28.12H2O (1 mmol), La(NO3)3 (2 mmol) and distilled water (100 ml) were mixed to form an aqueous solution with stirring and the pH was adjusted to 4.0. The mixture was stirred for 4 h and placed in an ice-box at 277 K for a few weeks. Red crystals suitable for diffraction studies were obtained.

Refinement top

The positions of all H atoms were fixed geometrically; O—H = 0.82–0.96 Å. The site-occupation factors of the five water O atoms were refined, constraining them to 4.

Computing details top

Data collection: CAD-4 Operations Manual (Enraf-Nonius, 1977); cell refinement: CAD-4 SDP/VAX (Enraf-Nonius, 1989); data reduction: TEXSAN (Molecular Structure Corporation, 1989); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXL97.

Figures top
[Figure 1] Fig. 1. View of the title compound (30% probability ellipsoids) without the molecules of crystal water.
[Figure 2] Fig. 2. A view of the packing in the crystal of the title compond.
[Figure 3] Fig. 3. The La(H2O)9 cations arranged as pillars along the a axis.
bis(enneaaqualanthanum) vanadium octacosaoxide octahydrate top
Crystal data top
[La(H2O)9]2[V10O28]·8H2OF(000) = 1656
Mr = 1703.64Dx = 2.501 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 25 reflections
a = 9.818 (2) Åθ = 15.1–15.9°
b = 11.935 (2) ŵ = 3.94 mm1
c = 19.514 (4) ÅT = 293 K
β = 98.42 (3)°Block, red
V = 2262.0 (8) Å30.30 × 0.20 × 0.20 mm
Z = 2
Data collection top
Enraf-nonius CAD-4
diffractometer
3460 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.034
Graphite monochromatorθmax = 25.0°, θmin = 2.0°
ω/2θ scansh = 1111
Absorption correction: ψ scan
(North et al., 1968)
k = 014
Tmin = 0.403, Tmax = 0.456l = 023
4226 measured reflections5 standard reflections every 300 reflections
3979 independent reflections intensity decay: 0.001%
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.039Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.124H-atom parameters constrained
S = 1.07 w = 1/[σ2(Fo2) + (0.067P)2 + 0.7084P]
where P = (Fo2 + 2Fc2)/3
3979 reflections(Δ/σ)max < 0.001
322 parametersΔρmax = 0.79 e Å3
1 restraintΔρmin = 0.79 e Å3
Crystal data top
[La(H2O)9]2[V10O28]·8H2OV = 2262.0 (8) Å3
Mr = 1703.64Z = 2
Monoclinic, P21/cMo Kα radiation
a = 9.818 (2) ŵ = 3.94 mm1
b = 11.935 (2) ÅT = 293 K
c = 19.514 (4) Å0.30 × 0.20 × 0.20 mm
β = 98.42 (3)°
Data collection top
Enraf-nonius CAD-4
diffractometer
3460 reflections with I > 2σ(I)
Absorption correction: ψ scan
(North et al., 1968)
Rint = 0.034
Tmin = 0.403, Tmax = 0.4565 standard reflections every 300 reflections
4226 measured reflections intensity decay: 0.001%
3979 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0391 restraint
wR(F2) = 0.124H-atom parameters constrained
S = 1.07Δρmax = 0.79 e Å3
3979 reflectionsΔρmin = 0.79 e Å3
322 parameters
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*/UeqOcc. (<1)
O1W0.5178 (5)0.5362 (4)0.6431 (3)0.0390 (12)
H1WB0.60430.54620.65260.08 (3)*
H1WA0.49730.51600.60110.08 (4)*
O2W0.4188 (15)0.2303 (14)0.6324 (7)0.081 (4)0.54
H2WA0.35440.22080.59870.08 (7)*0.54
H2WB0.44220.29890.63490.08 (8)*0.54
O3W0.3216 (8)0.0736 (7)0.5484 (4)0.0390 (18)0.67
H3WA0.33390.08620.50680.08 (6)*0.67
H3WB0.24260.09710.55460.08 (6)*0.67
O4W0.2164 (7)0.9638 (6)0.6884 (4)0.0500 (16)0.85
H4WA0.20560.89480.67830.075*0.85
H4WB0.16900.98050.72010.060*0.85
O5W0.6931 (7)0.2731 (5)0.7205 (3)0.0576 (17)0.94
H5WA0.78030.26740.72620.08 (4)*0.94
H5WB0.66380.28660.67810.08 (4)*0.94
La10.66859 (3)0.89783 (3)0.665970 (16)0.01592 (14)
O10.4940 (5)1.0022 (5)0.7138 (3)0.0445 (13)
H1B0.51931.01330.75510.067*
H1A0.40990.96000.70800.067*
O20.8725 (5)0.7939 (5)0.7194 (3)0.0452 (13)
H2A0.95380.83620.71480.068*
H2B0.87610.72280.69670.068*
O30.8081 (5)1.0632 (4)0.7076 (3)0.0389 (12)
H3B0.90001.05440.69720.058*
H3A0.81061.06910.75680.058*
O40.6115 (5)1.0593 (4)0.5853 (3)0.0373 (11)
H4A0.61911.12510.60200.045*
H4B0.54821.05060.55100.045*
O50.4448 (5)0.8726 (4)0.5884 (3)0.0420 (13)
H5A0.40100.94410.57960.063*
H5B0.46160.84000.54550.063*
O60.8550 (5)0.9273 (4)0.5902 (3)0.0388 (12)
H6B0.88020.99050.57640.058*
H6A0.88810.86420.58080.058*
O70.6835 (5)0.7407 (4)0.5879 (3)0.0360 (11)
H7B0.61750.71590.55880.054*
H7A0.76490.71470.59440.054*
O80.5430 (6)0.7422 (4)0.7079 (3)0.0478 (14)
H8B0.46710.72210.67330.072*
H8A0.50880.76440.74950.072*
O90.6969 (6)0.8929 (4)0.7969 (3)0.0417 (13)
H9A0.74800.94390.81270.062*
H9B0.73660.82260.81330.062*
V10.29404 (10)0.85710 (9)0.97797 (5)0.0233 (3)
V20.14616 (10)1.06478 (8)1.02313 (5)0.0196 (2)
V30.09330 (11)0.82825 (9)1.08500 (5)0.0219 (3)
V40.02089 (11)0.73544 (9)0.93521 (6)0.0251 (3)
V50.06799 (11)0.96833 (9)0.87162 (5)0.0227 (3)
O100.2080 (4)0.7287 (4)0.9422 (2)0.0260 (9)
O110.2494 (4)0.9315 (4)0.8926 (2)0.0260 (9)
O120.3050 (4)1.0141 (3)1.0193 (2)0.0242 (9)
O130.2683 (4)0.8157 (3)1.0685 (2)0.0241 (9)
O140.0254 (4)0.7104 (4)1.0300 (2)0.0259 (9)
O150.0083 (4)0.8269 (4)0.8548 (2)0.0261 (10)
O160.1006 (4)1.1095 (3)0.9276 (2)0.0208 (9)
O170.1206 (4)0.9900 (3)1.1083 (2)0.0199 (8)
O180.0967 (5)0.7778 (4)1.1623 (2)0.0325 (11)
O190.0293 (5)0.6153 (4)0.9032 (3)0.0388 (12)
O200.0570 (5)1.0199 (4)0.7947 (2)0.0321 (11)
O210.1663 (4)1.1937 (4)1.0572 (2)0.0254 (9)
O220.4543 (5)0.8292 (4)0.9797 (2)0.0328 (11)
O230.0694 (4)1.0880 (3)1.0195 (2)0.0219 (9)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
O1W0.038 (3)0.045 (3)0.034 (3)0.002 (2)0.004 (2)0.005 (2)
O2W0.086 (10)0.050 (13)0.066 (9)0.041 (9)0.010 (8)0.014 (8)
O3W0.038 (4)0.045 (4)0.034 (4)0.002 (4)0.004 (3)0.005 (3)
O4W0.050 (4)0.050 (4)0.050 (4)0.000 (3)0.007 (3)0.000 (3)
O5W0.070 (5)0.049 (4)0.052 (4)0.001 (3)0.006 (3)0.016 (3)
La10.0187 (2)0.0127 (2)0.0159 (2)0.00020 (11)0.00115 (14)0.00258 (12)
O10.041 (3)0.055 (3)0.038 (3)0.008 (3)0.006 (2)0.013 (2)
O20.042 (3)0.055 (3)0.036 (3)0.015 (3)0.002 (2)0.008 (3)
O30.040 (3)0.034 (3)0.040 (3)0.001 (2)0.003 (2)0.008 (2)
O40.039 (3)0.032 (3)0.040 (3)0.001 (2)0.004 (2)0.010 (2)
O50.040 (3)0.031 (3)0.051 (3)0.000 (2)0.010 (2)0.009 (2)
O60.040 (3)0.022 (2)0.058 (3)0.004 (2)0.018 (3)0.001 (2)
O70.029 (2)0.037 (3)0.040 (3)0.002 (2)0.000 (2)0.016 (2)
O80.063 (4)0.041 (3)0.042 (3)0.018 (3)0.017 (3)0.007 (2)
O90.048 (3)0.047 (3)0.028 (3)0.001 (2)0.001 (2)0.009 (2)
V10.0229 (5)0.0218 (6)0.0244 (6)0.0021 (4)0.0014 (4)0.0013 (4)
V20.0213 (5)0.0178 (5)0.0186 (5)0.0016 (4)0.0001 (4)0.0018 (4)
V30.0264 (5)0.0186 (5)0.0201 (5)0.0017 (4)0.0019 (4)0.0045 (4)
V40.0276 (6)0.0183 (5)0.0285 (6)0.0004 (4)0.0010 (4)0.0031 (4)
V50.0259 (6)0.0234 (6)0.0183 (5)0.0020 (4)0.0015 (4)0.0013 (4)
O100.028 (2)0.023 (2)0.025 (2)0.0028 (18)0.0004 (18)0.0023 (18)
O110.027 (2)0.025 (2)0.026 (2)0.0022 (19)0.0045 (18)0.0029 (19)
O120.023 (2)0.023 (2)0.025 (2)0.0026 (18)0.0016 (17)0.0025 (18)
O130.025 (2)0.021 (2)0.025 (2)0.0027 (18)0.0011 (18)0.0032 (18)
O140.030 (2)0.020 (2)0.028 (2)0.0009 (18)0.0030 (18)0.0033 (18)
O150.028 (2)0.028 (2)0.021 (2)0.0004 (19)0.0000 (18)0.0037 (18)
O160.025 (2)0.018 (2)0.018 (2)0.0015 (16)0.0005 (17)0.0008 (16)
O170.022 (2)0.020 (2)0.0168 (19)0.0007 (17)0.0009 (16)0.0018 (16)
O180.039 (3)0.031 (2)0.027 (2)0.001 (2)0.004 (2)0.010 (2)
O190.039 (3)0.026 (3)0.049 (3)0.001 (2)0.001 (2)0.003 (2)
O200.035 (3)0.037 (3)0.025 (2)0.001 (2)0.0037 (19)0.003 (2)
O210.026 (2)0.023 (2)0.025 (2)0.0007 (18)0.0006 (18)0.0036 (18)
O220.028 (2)0.037 (3)0.033 (3)0.002 (2)0.0004 (19)0.003 (2)
O230.023 (2)0.024 (2)0.019 (2)0.0014 (17)0.0008 (17)0.0001 (17)
Geometric parameters (Å, º) top
O1W—H1WB0.8502V1—V43.0563 (16)
O1W—H1WA0.8499V1—V23.0664 (15)
O2W—H2WA0.8500V1—V33.0936 (17)
O2W—H2WB0.8501V1—V53.1058 (17)
O3W—H3WA0.8501V2—O211.677 (4)
O3W—H3WB0.8502V2—O121.685 (4)
O4W—H4WA0.8500V2—O161.927 (4)
O4W—H4WB0.8501V2—O171.935 (4)
O5W—H5WA0.8500V2—O23i2.098 (4)
O5W—H5WB0.8500V2—O232.126 (4)
La1—O12.414 (5)V2—V4i3.0703 (15)
La1—O72.433 (4)V3—O181.620 (4)
La1—O82.437 (5)V3—O131.799 (4)
La1—O22.454 (5)V3—O141.835 (4)
La1—O32.470 (5)V3—O171.992 (4)
La1—O52.497 (5)V3—O16i2.025 (4)
La1—O42.500 (5)V3—O23i2.253 (4)
La1—O92.529 (5)V3—V5i3.0840 (15)
La1—O62.540 (5)V3—V43.1093 (16)
O1—H1B0.8200V4—O191.612 (5)
O1—H1A0.9596V4—O101.824 (4)
O2—H2A0.9600V4—O141.867 (4)
O2—H2B0.9604V4—O151.900 (4)
O3—H3B0.9600V4—O21i2.048 (4)
O3—H3A0.9598V4—O23i2.307 (4)
O4—H4A0.8500V4—V2i3.0703 (15)
O4—H4B0.8500V4—V53.1061 (16)
O5—H5A0.9601V5—O201.610 (4)
O5—H5B0.9600V5—O151.801 (5)
O6—H6B0.8501V5—O111.823 (4)
O6—H6A0.8501V5—O162.008 (4)
O7—H7B0.8501V5—O17i2.010 (4)
O7—H7A0.8499V5—O23i2.226 (4)
O8—H8B0.9602V5—V3i3.0840 (15)
O8—H8A0.9598O16—V3i2.025 (4)
O9—H9A0.8200O17—V5i2.010 (4)
O9—H9B0.9600O21—V4i2.048 (4)
V1—O221.604 (5)O23—V2i2.098 (4)
V1—O101.837 (4)O23—V5i2.226 (4)
V1—O111.882 (4)O23—V3i2.253 (4)
V1—O131.888 (4)O23—V4i2.307 (4)
V1—O122.037 (4)O23—V1i2.308 (4)
V1—O23i2.308 (4)
H1WB—O1W—H1WA109.8O13—V3—O1496.10 (19)
H2WA—O2W—H2WB109.7O18—V3—O1799.4 (2)
H3WA—O3W—H3WB109.7O13—V3—O1791.21 (18)
H4WA—O4W—H4WB109.5O14—V3—O17154.38 (18)
H5WA—O5W—H5WB109.5O18—V3—O16i98.1 (2)
O1—La1—O7138.63 (17)O13—V3—O16i156.05 (18)
O1—La1—O880.83 (18)O14—V3—O16i87.47 (18)
O7—La1—O872.70 (17)O17—V3—O16i76.39 (16)
O1—La1—O2132.66 (17)O18—V3—O23i173.3 (2)
O7—La1—O275.92 (17)O13—V3—O23i81.41 (17)
O8—La1—O283.9 (2)O14—V3—O23i80.19 (17)
O1—La1—O381.46 (18)O17—V3—O23i76.67 (15)
O7—La1—O3137.73 (17)O16i—V3—O23i75.86 (16)
O8—La1—O3141.44 (18)O18—V3—V5i88.74 (17)
O2—La1—O383.42 (18)O13—V3—V5i131.02 (14)
O1—La1—O571.63 (18)O14—V3—V5i127.39 (14)
O7—La1—O569.87 (17)O17—V3—V5i39.81 (12)
O8—La1—O570.61 (19)O16i—V3—V5i39.92 (11)
O2—La1—O5141.94 (18)O23i—V3—V5i84.83 (11)
O3—La1—O5133.77 (17)O18—V3—V1137.90 (17)
O1—La1—O474.87 (18)O13—V3—V133.86 (13)
O7—La1—O4103.21 (18)O14—V3—V184.43 (14)
O8—La1—O4136.18 (18)O17—V3—V188.20 (12)
O2—La1—O4138.69 (18)O16i—V3—V1123.89 (12)
O3—La1—O469.73 (17)O23i—V3—V148.04 (11)
O5—La1—O467.35 (17)V5i—V3—V1120.08 (4)
O1—La1—O966.50 (17)O18—V3—V4135.54 (18)
O7—La1—O9127.31 (17)O13—V3—V484.00 (14)
O8—La1—O968.22 (18)O14—V3—V433.21 (13)
O2—La1—O966.21 (17)O17—V3—V4124.35 (12)
O3—La1—O973.33 (17)O16i—V3—V486.26 (12)
O5—La1—O9124.48 (18)O23i—V3—V447.75 (11)
O4—La1—O9129.45 (17)V5i—V3—V4118.85 (4)
O1—La1—O6140.02 (17)V1—V3—V459.04 (4)
O7—La1—O668.16 (16)O19—V4—O10103.7 (2)
O8—La1—O6138.11 (17)O19—V4—O14101.7 (2)
O2—La1—O672.84 (17)O10—V4—O1492.34 (19)
O3—La1—O670.66 (17)O19—V4—O15102.2 (2)
O5—La1—O6107.99 (18)O10—V4—O1591.74 (19)
O4—La1—O668.95 (16)O14—V4—O15154.02 (19)
O9—La1—O6127.52 (18)O19—V4—O21i99.7 (2)
La1—O1—H1B109.5O10—V4—O21i156.57 (19)
La1—O1—H1A109.3O14—V4—O21i83.47 (18)
H1B—O1—H1A109.4O15—V4—O21i82.64 (18)
La1—O2—H2A109.4O19—V4—O23i174.2 (2)
La1—O2—H2B109.5O10—V4—O23i82.08 (17)
H2A—O2—H2B109.5O14—V4—O23i78.10 (17)
La1—O3—H3B109.7O15—V4—O23i77.08 (17)
La1—O3—H3A108.6O21i—V4—O23i74.50 (16)
H3B—O3—H3A109.5O19—V4—V1137.26 (19)
La1—O4—H4A118.1O10—V4—V133.55 (14)
La1—O4—H4B118.1O14—V4—V185.01 (14)
H4A—O4—H4B115.4O15—V4—V184.32 (13)
La1—O5—H5A109.5O21i—V4—V1123.03 (13)
La1—O5—H5B109.3O23i—V4—V148.53 (11)
H5A—O5—H5B109.5O19—V4—V2i130.44 (19)
La1—O6—H6B125.2O10—V4—V2i125.85 (14)
La1—O6—H6A109.5O14—V4—V2i78.38 (14)
H6B—O6—H6A125.4O15—V4—V2i78.46 (14)
La1—O7—H7B125.3O21i—V4—V2i30.74 (12)
La1—O7—H7A109.4O23i—V4—V2i43.77 (11)
H7B—O7—H7A125.4V1—V4—V2i92.30 (4)
La1—O8—H8B109.4O19—V4—V5134.1 (2)
La1—O8—H8A109.3O10—V4—V582.08 (14)
H8B—O8—H8A109.5O14—V4—V5123.76 (14)
La1—O9—H9A109.5O15—V4—V531.98 (13)
La1—O9—H9B109.8O21i—V4—V581.20 (13)
H9A—O9—H9B109.0O23i—V4—V545.67 (11)
O22—V1—O10103.3 (2)V1—V4—V560.52 (4)
O22—V1—O11102.5 (2)V2i—V4—V561.79 (4)
O10—V1—O1191.3 (2)O19—V4—V3134.1 (2)
O22—V1—O13101.0 (2)O10—V4—V381.72 (14)
O10—V1—O1391.16 (19)O14—V4—V332.56 (13)
O11—V1—O13155.05 (19)O15—V4—V3123.36 (14)
O22—V1—O12100.8 (2)O21i—V4—V382.48 (12)
O10—V1—O12155.85 (19)O23i—V4—V346.28 (11)
O11—V1—O1284.79 (18)V1—V4—V360.22 (4)
O13—V1—O1282.88 (18)V2i—V4—V362.09 (4)
O22—V1—O23i174.9 (2)V5—V4—V391.71 (4)
O10—V1—O23i81.79 (17)O20—V5—O15102.3 (2)
O11—V1—O23i77.63 (17)O20—V5—O11103.3 (2)
O13—V1—O23i78.17 (16)O15—V5—O1195.5 (2)
O12—V1—O23i74.09 (15)O20—V5—O1699.8 (2)
O22—V1—V4136.58 (18)O15—V5—O16155.10 (19)
O10—V1—V433.27 (14)O11—V5—O1690.46 (19)
O11—V1—V484.33 (14)O20—V5—O17i98.6 (2)
O13—V1—V484.19 (13)O15—V5—O17i89.02 (18)
O12—V1—V4122.60 (13)O11—V5—O17i156.06 (19)
O23i—V1—V448.52 (10)O16—V5—O17i76.36 (17)
O22—V1—V2131.74 (18)O20—V5—O23i174.0 (2)
O10—V1—V2124.94 (14)O15—V5—O23i81.21 (17)
O11—V1—V279.33 (14)O11—V5—O23i81.00 (18)
O13—V1—V278.94 (13)O16—V5—O23i75.87 (16)
O12—V1—V230.95 (12)O17i—V5—O23i76.47 (16)
O23i—V1—V243.15 (10)O20—V5—V3i89.32 (17)
V4—V1—V291.66 (4)O15—V5—V3i128.41 (14)
O22—V1—V3133.04 (18)O11—V5—V3i130.76 (15)
O10—V1—V381.99 (14)O16—V5—V3i40.31 (12)
O11—V1—V3124.17 (14)O17i—V5—V3i39.39 (12)
O13—V1—V332.07 (12)O23i—V5—V3i84.70 (11)
O12—V1—V380.61 (13)O20—V5—V1136.84 (17)
O23i—V1—V346.54 (11)O15—V5—V184.42 (14)
V4—V1—V360.74 (4)O11—V5—V133.65 (14)
V2—V1—V361.36 (3)O16—V5—V187.34 (12)
O22—V1—V5134.90 (18)O17i—V5—V1124.32 (12)
O10—V1—V581.90 (14)O23i—V5—V147.87 (11)
O11—V1—V532.44 (13)V3i—V5—V1119.90 (4)
O13—V1—V5123.83 (13)O20—V5—V4136.08 (18)
O12—V1—V582.12 (12)O15—V5—V433.97 (14)
O23i—V1—V545.67 (11)O11—V5—V483.81 (14)
V4—V1—V560.53 (4)O16—V5—V4123.67 (12)
V2—V1—V561.60 (3)O17i—V5—V487.03 (12)
V3—V1—V592.01 (4)O23i—V5—V447.85 (11)
O21—V2—O12106.9 (2)V3i—V5—V4118.84 (5)
O21—V2—O1697.28 (19)V1—V5—V458.95 (3)
O12—V2—O1698.2 (2)V4—O10—V1113.2 (2)
O21—V2—O1796.04 (19)V5—O11—V1113.9 (2)
O12—V2—O1796.29 (19)V2—O12—V1110.6 (2)
O16—V2—O17156.54 (18)V3—O13—V1114.1 (2)
O21—V2—O23i165.88 (19)V3—O14—V4114.2 (2)
O12—V2—O23i87.21 (19)V5—O15—V4114.1 (2)
O16—V2—O23i80.67 (16)V2—O16—V5106.85 (18)
O17—V2—O23i81.70 (17)V2—O16—V3i107.5 (2)
O21—V2—O2387.28 (18)V5—O16—V3i99.77 (18)
O12—V2—O23165.75 (19)V2—O17—V3106.32 (19)
O16—V2—O2380.96 (18)V2—O17—V5i107.01 (19)
O17—V2—O2380.48 (17)V3—O17—V5i100.80 (18)
O23i—V2—O2378.60 (17)V2—O21—V4i110.6 (2)
O21—V2—V1145.34 (15)V2i—O23—V2101.40 (17)
O12—V2—V138.44 (14)V2i—O23—V5i93.89 (16)
O16—V2—V189.92 (13)V2—O23—V5i93.55 (16)
O17—V2—V190.03 (13)V2i—O23—V3i92.44 (16)
O23i—V2—V148.78 (12)V2—O23—V3i93.37 (17)
O23—V2—V1127.38 (12)V5i—O23—V3i169.5 (2)
O21—V2—V4i38.63 (14)V2i—O23—V4i171.0 (2)
O12—V2—V4i145.53 (15)V2—O23—V4i87.57 (15)
O16—V2—V4i89.06 (13)V5i—O23—V4i86.48 (15)
O17—V2—V4i89.38 (13)V3i—O23—V4i85.97 (14)
O23i—V2—V4i127.26 (12)V2i—O23—V1i88.08 (15)
O23—V2—V4i48.66 (11)V2—O23—V1i170.5 (2)
V1—V2—V4i176.03 (5)V5i—O23—V1i86.46 (15)
O18—V3—O13104.2 (2)V3i—O23—V1i85.42 (14)
O18—V3—O14102.5 (2)V4i—O23—V1i82.95 (14)
Symmetry code: (i) x, y+2, z+2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1B···O90.822.312.712 (7)111
O1—H1A···O4W0.961.882.737 (8)147
O2W—H2WA···O3W0.852.022.58 (2)123
O4W—H4WB···O200.852.012.855 (8)180
O5W—H5WB···O2W0.852.533.019 (18)118
O1W—H1WB···O11ii0.852.262.781 (7)120
O5W—H5WB···O11ii0.852.443.020 (8)126
O2—H2B···O20ii0.962.513.363 (7)148
O7—H7A···O16ii0.851.922.689 (6)151
O1W—H1WA···O12iii0.852.313.013 (7)140
O2W—H2WA···O21iii0.852.162.838 (14)137
O3W—H3WB···O21iii0.852.613.185 (9)126
O4W—H4WA···O18iii0.852.323.128 (8)159
O5—H5B···O22iii0.962.393.220 (7)145
O7—H7B···O22iii0.852.122.971 (6)174
O8—H8B···O13iii0.962.653.606 (7)173
O3W—H3WA···O6iv0.852.452.991 (9)122
O3W—H3WA···O4iv0.852.613.202 (10)128
O3W—H3WB···O19v0.852.373.190 (10)162
O4W—H4WA···O5Wvi0.852.532.944 (9)111
O5W—H5WA···O18vii0.852.392.912 (8)120
O1—H1B···O1Wvi0.822.092.841 (7)153
O3—H3B···O19vi0.962.593.339 (8)135
O4—H4A···O10vi0.852.362.792 (6)112
O6—H6B···O19vi0.852.092.814 (7)143
O8—H8A···O5Wvi0.962.152.899 (9)134
O8—H8A···O2Wvi0.962.353.087 (15)134
O3—H3B···O20viii0.962.302.814 (7)112
O3—H3A···O18ix0.962.503.198 (7)130
O4—H4A···O2Wx0.852.483.016 (14)122
O4—H4B···O3Wx0.852.232.837 (9)128
O5—H5A···O3Wx0.961.802.748 (10)171
O6—H6A···O14xi0.852.002.731 (6)144
O9—H9A···O17ix0.822.022.761 (6)150
O9—H9B···O21ix0.962.573.140 (7)118
Symmetry codes: (ii) x+1, y1/2, z+3/2; (iii) x, y+3/2, z1/2; (iv) x+1, y+1, z+1; (v) x, y1/2, z+3/2; (vi) x+1, y+1/2, z+3/2; (vii) x+1, y+1, z+2; (viii) x+1, y, z; (ix) x+1, y+2, z+2; (x) x, y+1, z; (xi) x+1, y+3/2, z1/2.

Experimental details

Crystal data
Chemical formula[La(H2O)9]2[V10O28]·8H2O
Mr1703.64
Crystal system, space groupMonoclinic, P21/c
Temperature (K)293
a, b, c (Å)9.818 (2), 11.935 (2), 19.514 (4)
β (°) 98.42 (3)
V3)2262.0 (8)
Z2
Radiation typeMo Kα
µ (mm1)3.94
Crystal size (mm)0.30 × 0.20 × 0.20
Data collection
DiffractometerEnraf-nonius CAD-4
diffractometer
Absorption correctionψ scan
(North et al., 1968)
Tmin, Tmax0.403, 0.456
No. of measured, independent and
observed [I > 2σ(I)] reflections
4226, 3979, 3460
Rint0.034
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.039, 0.124, 1.07
No. of reflections3979
No. of parameters322
No. of restraints1
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.79, 0.79

Computer programs: CAD-4 Operations Manual (Enraf-Nonius, 1977), CAD-4 SDP/VAX (Enraf-Nonius, 1989), TEXSAN (Molecular Structure Corporation, 1989), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 1997), SHELXL97.

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1B···O90.822.312.712 (7)110.5
O1—H1A···O4W0.961.882.737 (8)146.8
O2W—H2WA···O3W0.852.022.58 (2)122.7
O4W—H4WB···O200.852.012.855 (8)180.0
O5W—H5WB···O2W0.852.533.019 (18)117.5
O1W—H1WB···O11i0.852.262.781 (7)120.1
O5W—H5WB···O11i0.852.443.020 (8)126.0
O2—H2B···O20i0.962.513.363 (7)148.1
O7—H7A···O16i0.851.922.689 (6)150.6
O1W—H1WA···O12ii0.852.313.013 (7)139.8
O2W—H2WA···O21ii0.852.162.838 (14)136.5
O3W—H3WB···O21ii0.852.613.185 (9)126.1
O4W—H4WA···O18ii0.852.323.128 (8)158.5
O5—H5B···O22ii0.962.393.220 (7)144.7
O7—H7B···O22ii0.852.122.971 (6)173.6
O8—H8B···O13ii0.962.653.606 (7)173.4
O3W—H3WA···O6iii0.852.452.991 (9)121.8
O3W—H3WA···O4iii0.852.613.202 (10)127.7
O3W—H3WB···O19iv0.852.373.190 (10)162.0
O4W—H4WA···O5Wv0.852.532.944 (9)110.7
O5W—H5WA···O18vi0.852.392.912 (8)120.2
O1—H1B···O1Wv0.822.092.841 (7)152.5
O3—H3B···O19v0.962.593.339 (8)135.2
O4—H4A···O10v0.852.362.792 (6)111.7
O6—H6B···O19v0.852.092.814 (7)143.3
O8—H8A···O5Wv0.962.152.899 (9)133.9
O8—H8A···O2Wv0.962.353.087 (15)133.6
O3—H3B···O20vii0.962.302.814 (7)112.4
O3—H3A···O18viii0.962.503.198 (7)129.8
O4—H4A···O2Wix0.852.483.016 (14)122.2
O4—H4B···O3Wix0.852.232.837 (9)127.9
O5—H5A···O3Wix0.961.802.748 (10)170.5
O6—H6A···O14x0.852.002.731 (6)144.0
O9—H9A···O17viii0.822.022.761 (6)149.8
O9—H9B···O21viii0.962.573.140 (7)118.0
Symmetry codes: (i) x+1, y1/2, z+3/2; (ii) x, y+3/2, z1/2; (iii) x+1, y+1, z+1; (iv) x, y1/2, z+3/2; (v) x+1, y+1/2, z+3/2; (vi) x+1, y+1, z+2; (vii) x+1, y, z; (viii) x+1, y+2, z+2; (ix) x, y+1, z; (x) x+1, y+3/2, z1/2.
 

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