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The title compound can be formulated as [Cr(H2O)6][Na2(H2O)10][IMo6O24]·8H2O. The anion has the I atom on an inversion centre and has close to \overline 3m symmetry, with I-O bond lengths in the range 1.881-1.890 (2) Å and Mo-O bond lengths in the ranges 1.697 (3)-1.714 (3), 1.915 (2)-1.948 (2) and 2.317 (2)-2.357 (2) Å.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100005229/qb0206sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100005229/qb0206Isup2.hkl
Contains datablock I

Comment top

This work forms part of an investigation into the interaction of transition metal cations and polyoxometalate anions. The IMo6O245- anion lies on a crystal inversion centre, in an orientation such that the cell is pseudo-body-centered. Its non-crystallographic symmetry is close to 3 m and its dimensions are very similar to those of the anion in CoNa3[IMo6O24].14H2O (Rosu & Dickman, 1999) and in K5[IMo6O24]·5H2O (Kondo et al., 1980). The Mo atoms are coplanar to within 0.007 (1) Å, whereas in CoNa3[IMo6O24].14H2O, the Co2+ and Na+ cations are coordinated to the anion, the Na+ ions in the present structure are present in discrete, centrosymmetric [Na2(H2O)10]2+ units, and despite the preparation at 373 K, O atoms of anions have not replaced water in the kinetically inert [Cr(H2O)6]3+ groups.

Experimental top

The pH of a slurry containing 15 g Na5[IMo6O24].16.5H2O (Rosu & Dickman, 1999) and 4 g Cr(NO3)3·9H2O in 100 ml water was adjusted to 6. The mixture was heated to reflux for 30 min and filtered while hot. The filtrate was allowed to evaporate at room temperature for 3 d to give 11.7 g of violet crystals. Found (calculated) for CrNa2[IMo6O24].24H2O: Na 2.8 (2.8), Cr 3.2 (3.2), Mo 35.5 (35.6), H2O 26.7% (26.7%). The crystal used for data collection was glued to a glass fibre.

Refinement top

The intensity data were corrected for absorption (azimuthal scans). Structure solution used an SIR92 E map (Altomare et al., 1994). Alternative positions were found for the three independent water molecules bonded to Cr, and for two non-coordinated waters. Atoms other than minor-occupancy water molecules were refined anisotropically. H atoms of water molecules could not be located with confidence and no attempt was made to model them. The value of a secondary extinction parameter was refined.

Computing details top

Data collection: CAD-4-PC Diffractometer Software (Enraf-Nonius, 1993); cell refinement: CAD-4-PC Diffractometer Software; data reduction: TEXSAN (Molecular Structure Corporation, 1997); program(s) used to solve structure: TEXSAN; program(s) used to refine structure: TEXSAN; software used to prepare material for publication: TEXSAN.

(I) top
Crystal data top
CrNa2[IMo6O24]·24H2OF(000) = 1566.00
Mr = 1616.87Dx = 2.511 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
a = 10.3829 (7) ÅCell parameters from 25 reflections
b = 14.0871 (12) Åθ = 14.0–14.9°
c = 14.9994 (14) ŵ = 2.82 mm1
β = 102.931 (9)°T = 295 K
V = 2138.2 (3) Å3Block, violet
Z = 20.29 × 0.23 × 0.18 mm
Data collection top
Enraf-Nonius CAD-4
diffractometer
4697 reflections with I > σ(I)
Radiation source: sealed X-ray tubeRint = 0.011
Graphite monochromatorθmax = 30.0°, θmin = 2.0°
ω–2θ scansh = 1414
Absorption correction: ψ scan
(North et al., 1968)
k = 019
Tmin = 0.480, Tmax = 0.545l = 2021
6570 measured reflections3 standard reflections every 300 reflections
6210 independent reflections intensity decay: 0.0%
Refinement top
Refinement on F20 constraints
Least-squares matrix: fullH-atom parameters not defined
R[F2 > 2σ(F2)] = 0.034 w = 4Fo2/[σ2(I) + (0.020I)2]
wR(F2) = 0.050(Δ/σ)max = 0.022
S = 1.86Δρmax = 1.21 (1.07 Å from I) e Å3
6210 reflectionsΔρmin = 1.11 (0.79 Å from Mo1) e Å3
276 parametersExtinction correction: Zachariasen (1967), equ(3) Acta Cryst. (1968) A24, p. 213
0 restraintsExtinction coefficient: 5.5E-7 (2)
Crystal data top
CrNa2[IMo6O24]·24H2OV = 2138.2 (3) Å3
Mr = 1616.87Z = 2
Monoclinic, P21/nMo Kα radiation
a = 10.3829 (7) ŵ = 2.82 mm1
b = 14.0871 (12) ÅT = 295 K
c = 14.9994 (14) Å0.29 × 0.23 × 0.18 mm
β = 102.931 (9)°
Data collection top
Enraf-Nonius CAD-4
diffractometer
4697 reflections with I > σ(I)
Absorption correction: ψ scan
(North et al., 1968)
Rint = 0.011
Tmin = 0.480, Tmax = 0.5453 standard reflections every 300 reflections
6570 measured reflections intensity decay: 0.0%
6210 independent reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0340 restraints
wR(F2) = 0.050H-atom parameters not defined
S = 1.86Δρmax = 1.21 (1.07 Å from I) e Å3
6210 reflectionsΔρmin = 1.11 (0.79 Å from Mo1) e Å3
276 parameters
Special details top

Experimental. The preliminary cell determination indicated a C-centered monoclinic cell with a, b and c equal to 16.217, 14.087, 10.383 Å, and β equal to 115.65 Å, and data were originally collected on this basis in the ±h,+k,+l quadrant. Subsequently it was realised that the C-centering was false and the missing data were collected from the same crystal but, through an oversight, in the +h,+k,±l quadrant. The cell was transformed after data reduction to the present (P21/n) one. As a result, some independent reflections in the structure factor list have positive h and some have negative h.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
I0.50000.50000.50000.01617 (6)
Mo10.39295 (3)0.37860 (2)0.308259 (19)0.02484 (8)
Mo20.49649 (3)0.26577 (2)0.50429 (2)0.02550 (8)
Mo30.60153 (3)0.38491 (2)0.696128 (19)0.02436 (8)
Cr0.00000.00000.50000.02341 (18)
Na0.00217 (14)0.37363 (11)0.49923 (10)0.0379 (4)
O10.3492 (2)0.49931 (14)0.40221 (15)0.0207 (5)
O20.5653 (2)0.40086 (15)0.43816 (14)0.0206 (5)
O30.4314 (2)0.40580 (16)0.56525 (14)0.0208 (5)
O40.2401 (3)0.3805 (2)0.23744 (19)0.0435 (8)
O50.3534 (2)0.30167 (16)0.40399 (16)0.0280 (6)
O60.4881 (3)0.30240 (19)0.26157 (18)0.0379 (8)
O70.4652 (3)0.49536 (15)0.26970 (16)0.0277 (6)
O80.4081 (3)0.1970 (2)0.5615 (2)0.0440 (8)
O90.5840 (3)0.19116 (19)0.45142 (19)0.0430 (8)
O100.6404 (2)0.30282 (16)0.60310 (15)0.0272 (6)
O110.5028 (3)0.31276 (19)0.74427 (18)0.0378 (8)
O120.7537 (3)0.3846 (2)0.76716 (19)0.0412 (8)
O130.0650 (3)0.0421 (2)0.62724 (18)0.0330 (8)0.880
O13A0.059 (3)0.042 (2)0.3752 (19)0.058 (7)*0.120
O140.1173 (3)0.1113 (2)0.4748 (2)0.0345 (8)0.880
O14A0.123 (4)0.101 (2)0.504 (2)0.069 (9)*0.120
O150.1429 (3)0.0725 (2)0.4648 (2)0.0332 (8)0.880
O15A0.139 (3)0.080 (2)0.525 (2)0.058 (7)*0.120
O160.1898 (4)0.3879 (3)0.6194 (3)0.0792 (14)
O170.0825 (3)0.49959 (18)0.4169 (2)0.0393 (8)
O180.1960 (3)0.3802 (4)0.3799 (3)0.0834 (15)
O190.1055 (3)0.25618 (18)0.41992 (18)0.0340 (7)
O200.1095 (3)0.25942 (17)0.58231 (17)0.0325 (7)
O210.1414 (4)0.4886 (3)0.0572 (3)0.0728 (13)
O220.2415 (5)0.3379 (4)0.8124 (3)0.1072 (17)
O23A0.0060 (14)0.4992 (8)0.7815 (9)0.114 (4)*0.450
O230.0159 (7)0.4405 (6)0.7742 (5)0.070 (2)*0.550
O240.1889 (5)0.5965 (4)0.8061 (4)0.0569 (13)*0.650
O24A0.2405 (10)0.6579 (7)0.8097 (7)0.058 (3)*0.350
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
I0.0165 (2)0.0170 (2)0.0156 (1)0.0001 (1)0.0048 (1)0.0003 (1)
Mo10.0287 (2)0.0261 (2)0.0197 (2)0.0019 (1)0.0055 (2)0.0039 (1)
Mo20.0315 (2)0.0194 (2)0.0272 (2)0.0009 (1)0.0098 (1)0.0006 (1)
Mo30.0278 (2)0.0261 (2)0.0194 (2)0.0028 (1)0.0058 (1)0.0040 (1)
Cr0.0282 (4)0.0200 (3)0.0251 (4)0.0010 (3)0.0125 (3)0.0013 (3)
Na0.0370 (9)0.0353 (9)0.0445 (9)0.0005 (7)0.0158 (7)0.0012 (7)
O10.018 (1)0.024 (1)0.019 (1)0.000 (1)0.002 (1)0.000 (1)
O20.022 (1)0.020 (1)0.021 (1)0.002 (1)0.007 (1)0.001 (1)
O30.022 (1)0.022 (1)0.020 (1)0.002 (1)0.008 (1)0.003 (1)
O40.040 (2)0.049 (2)0.035 (2)0.007 (2)0.006 (2)0.002 (1)
O50.029 (2)0.026 (1)0.029 (1)0.008 (1)0.007 (1)0.003 (1)
O60.051 (2)0.033 (2)0.033 (2)0.004 (1)0.017 (2)0.006 (1)
O70.034 (2)0.029 (2)0.023 (1)0.001 (1)0.015 (1)0.001 (1)
O80.052 (2)0.038 (2)0.044 (2)0.016 (2)0.015 (2)0.007 (1)
O90.055 (2)0.033 (2)0.044 (2)0.013 (2)0.016 (2)0.006 (1)
O100.030 (2)0.025 (1)0.027 (1)0.008 (1)0.007 (1)0.003 (1)
O110.046 (2)0.038 (2)0.033 (2)0.002 (1)0.015 (2)0.010 (1)
O120.038 (2)0.048 (2)0.032 (2)0.007 (2)0.003 (2)0.001 (1)
O130.041 (2)0.038 (2)0.024 (2)0.010 (2)0.015 (2)0.006 (1)
O140.039 (2)0.027 (2)0.039 (2)0.005 (1)0.012 (2)0.000 (1)
O150.036 (2)0.028 (2)0.043 (2)0.005 (1)0.024 (2)0.001 (2)
O160.036 (2)0.150 (4)0.054 (2)0.007 (2)0.016 (2)0.010 (2)
O170.030 (2)0.042 (2)0.049 (2)0.000 (1)0.016 (2)0.001 (2)
O180.033 (2)0.164 (5)0.054 (2)0.006 (2)0.012 (2)0.009 (2)
O190.033 (2)0.032 (2)0.039 (2)0.005 (1)0.013 (1)0.004 (1)
O200.036 (2)0.030 (2)0.033 (2)0.005 (1)0.012 (1)0.002 (1)
O210.048 (2)0.074 (3)0.102 (3)0.015 (2)0.028 (2)0.016 (2)
O220.142 (4)0.137 (4)0.044 (2)0.081 (4)0.024 (3)0.008 (2)
Geometric parameters (Å, º) top
I—O11.890 (2)Mo3—O7i1.935 (2)
I—O21.885 (2)Mo3—O101.923 (2)
I—O31.881 (2)Mo3—O111.714 (3)
Mo1—O12.317 (2)Mo3—O121.697 (3)
Mo1—O22.353 (2)Cr—O131.968 (3)
Mo1—O41.701 (3)Cr—O13A1.93 (3)
Mo1—O51.915 (2)Cr—O141.969 (3)
Mo1—O61.711 (3)Cr—O14A1.90 (3)
Mo1—O71.948 (2)Cr—O151.968 (3)
Mo2—O22.331 (2)Cr—O15A1.93 (3)
Mo2—O32.337 (2)Na—O162.378 (4)
Mo2—O51.930 (2)Na—O172.435 (3)
Mo2—O81.694 (3)Na—O17ii2.437 (3)
Mo2—O91.697 (3)Na—O182.377 (4)
Mo2—O101.926 (2)Na—O192.449 (3)
Mo3—O1i2.331 (2)Na—O202.451 (3)
Mo3—O32.347 (2)
O1···O172.827 (4)O13A···O22iv2.68 (3)
O2···O18iii2.821 (4)O13A···O24iv3.24 (3)
O3···O162.816 (4)O13A···O193.46 (3)
O4···O23Aii3.026 (14)O13A···O24Aiv3.51 (3)
O4···O213.072 (5)O14···O202.627 (4)
O4···O10iv3.297 (4)O14···O22iv2.645 (5)
O5···O192.715 (3)O14···O193.323 (4)
O5···O12iv3.350 (4)O14···O21x3.343 (5)
O6···O20v2.792 (4)O14A···O192.52 (3)
O6···O13v3.196 (4)O14A···O24Avii2.94 (4)
O6···O22v3.242 (5)O14A···O24vii3.07 (4)
O6···O24Ai3.278 (10)O14A···O21viii3.21 (4)
O6···O23v3.436 (8)O15···O21viii2.618 (5)
O6···O18iii3.536 (5)O15···O192.680 (4)
O7···O13v2.629 (3)O15···O24vii3.504 (6)
O7···O13Avi2.66 (3)O15···O24Avii3.538 (10)
O8···O24Avii2.784 (10)O15A···O21x2.62 (3)
O8···O24vii2.803 (6)O15A···O202.66 (3)
O8···O14A3.19 (4)O15A···O22iv3.36 (3)
O8···O153.312 (4)O16···O222.910 (5)
O8···O21viii3.411 (5)O16···O233.328 (8)
O8···O193.477 (4)O16···O24Avii3.437 (11)
O8···O21ix3.575 (5)O17···O23Aii2.912 (14)
O9···O22v2.952 (5)O17···O23ii2.943 (8)
O9···O21ix2.977 (5)O18···O24ii2.827 (7)
O9···O23v3.188 (8)O18···O24Aii2.829 (10)
O9···O14iii3.244 (4)O18···O22iv3.254 (7)
O9···O15Aiii3.24 (3)O21···O21xi3.068 (8)
O9···O20iii3.480 (4)O21···O23Aii3.143 (14)
O10···O20iii2.752 (3)O21···O23ii3.450 (8)
O11···O19ix2.786 (4)O22···O232.703 (10)
O11···O13Aix3.00 (3)O22···O24Avii3.158 (12)
O11···O223.126 (6)O22···O23A3.294 (15)
O11···O24Avii3.299 (10)O23A···O242.305 (15)
O11···O163.531 (5)O23A···O24A3.263 (17)
O12···O23iii2.812 (8)O23···O242.811 (9)
O12···O23Aiii3.042 (14)I···Mo23.3006 (3)
O12···O21i3.167 (5)I···Mo13.3167 (3)
O12···O15ix3.465 (4)I···Mo33.3175 (3)
O13···O24Avii2.603 (10)Mo1···Mo23.3036 (4)
O13···O24vii2.640 (6)Mo1···Mo3i3.3328 (4)
O13···O22vii3.510 (5)Mo2···Mo33.2987 (4)
O13···O203.545 (4)
O1—I—O1i180.00O7i—Mo3—O1197.01 (11)
O1—I—O286.61 (9)O7i—Mo3—O12100.01 (12)
O1—I—O393.20 (9)O10—Mo3—O11101.04 (12)
O2—I—O2i180.00O10—Mo3—O1297.88 (12)
O2—I—O387.31 (10)O11—Mo3—O12107.16 (14)
O3—I—O3i180.00O13—Cr—O13xii180.00
O1—Mo1—O267.34 (8)O13—Cr—O13Axii35.5 (9)
O1—Mo1—O494.93 (12)O13—Cr—O1490.54 (13)
O1—Mo1—O581.69 (9)O13—Cr—O1589.30 (12)
O1—Mo1—O6156.75 (11)O13A—Cr—O13Axii180.00
O1—Mo1—O772.65 (8)O13A—Cr—O14A82.6 (13)
O2—Mo1—O4160.98 (12)O13A—Cr—O15A85.3 (12)
O2—Mo1—O572.86 (9)O14—Cr—O14xii180.00
O2—Mo1—O691.20 (11)O14—Cr—O1590.36 (13)
O2—Mo1—O782.04 (9)O14A—Cr—O14Axii180.00
O4—Mo1—O598.66 (12)O14A—Cr—O15A94.8 (15)
O4—Mo1—O6107.32 (14)O15—Cr—O15xii180.00
O4—Mo1—O799.70 (12)O15A—Cr—O15Axii180.00
O5—Mo1—O6101.06 (12)O16—Na—O1789.23 (13)
O5—Mo1—O7149.48 (10)O16—Na—O17ii82.65 (13)
O6—Mo1—O796.46 (11)O16—Na—O18172.90 (19)
O2—Mo2—O367.68 (8)O16—Na—O1991.67 (13)
O2—Mo2—O573.14 (9)O16—Na—O2093.98 (13)
O2—Mo2—O8159.21 (12)O17—Na—O17ii86.09 (11)
O2—Mo2—O993.43 (11)O17—Na—O1886.03 (13)
O2—Mo2—O1081.22 (9)O17—Na—O1989.44 (10)
O3—Mo2—O581.04 (9)O17—Na—O20173.20 (11)
O3—Mo2—O892.74 (12)O17ii—Na—O1891.74 (14)
O3—Mo2—O9159.62 (11)O17ii—Na—O19172.81 (11)
O3—Mo2—O1073.31 (8)O17ii—Na—O2088.37 (10)
O5—Mo2—O897.76 (12)O18—Na—O1993.57 (13)
O5—Mo2—O9101.36 (12)O18—Na—O2090.20 (13)
O5—Mo2—O10149.08 (10)O19—Na—O2096.46 (10)
O8—Mo2—O9106.83 (16)I—O1—Mo1103.58 (9)
O8—Mo2—O10100.38 (12)I—O1—Mo3i103.10 (9)
O9—Mo2—O1097.08 (12)Mo1—O1—Mo3i91.61 (8)
O1i—Mo3—O367.27 (8)I—O2—Mo1102.46 (9)
O1i—Mo3—O7i72.54 (9)I—O2—Mo2102.55 (9)
O1i—Mo3—O1081.39 (9)Mo1—O2—Mo289.71 (8)
O1i—Mo3—O11156.65 (11)I—O3—Mo2102.45 (9)
O1i—Mo3—O1295.37 (11)I—O3—Mo3102.82 (9)
O3—Mo3—O7i82.26 (10)Mo2—O3—Mo389.54 (8)
O3—Mo3—O1073.11 (9)Mo1—O5—Mo2118.43 (12)
O3—Mo3—O1191.01 (11)Mo1—O7—Mo3i118.22 (12)
O3—Mo3—O12161.15 (11)Mo2—O10—Mo3117.94 (12)
O7i—Mo3—O10149.51 (10)Na—O17—Naii93.91 (11)
I—O1—Mo1—O20.87 (8)Mo2—O3—I—O20.13 (9)
I—O1—Mo1—O4172.02 (12)Mo2—O3—I—O2i179.87 (9)
I—O1—Mo1—O573.96 (11)Mo2—O3—I—O3i179.87 (9)
I—O1—Mo1—O624.7 (3)Mo2—O3—Mo3—O1i103.57 (8)
I—O1—Mo1—O789.34 (12)Mo2—O3—Mo3—O7i177.82 (9)
I—O1—Mo3i—O3i0.90 (8)Mo2—O3—Mo3—O1016.00 (8)
I—O1—Mo3i—O789.68 (11)Mo2—O3—Mo3—O1185.23 (11)
I—O1—Mo3i—O10i74.32 (10)Mo2—O3—Mo3—O1279.5 (3)
I—O1—Mo3i—O11i23.6 (3)Mo2—O5—Mo1—O190.55 (13)
I—O1—Mo3i—O12i171.50 (12)Mo2—O5—Mo1—O221.80 (11)
I—O1i—Mo1i—O2i0.87 (8)Mo2—O5—Mo1—O4175.70 (14)
I—O1i—Mo1i—O4i172.02 (12)Mo2—O5—Mo1—O666.03 (15)
I—O1i—Mo1i—O5i73.96 (11)Mo2—O5—Mo1—O757.8 (3)
I—O1i—Mo1i—O6i24.7 (3)Mo2—O10—Mo3—O1i90.99 (13)
I—O1i—Mo1i—O7i89.34 (12)Mo2—O10—Mo3—O322.24 (11)
I—O1i—Mo3—O30.90 (8)Mo2—O10—Mo3—O7i59.8 (3)
I—O1i—Mo3—O7i89.68 (11)Mo2—O10—Mo3—O1165.44 (15)
I—O1i—Mo3—O1074.32 (10)Mo2—O10—Mo3—O12174.73 (14)
I—O1i—Mo3—O1123.6 (3)Mo3—O1i—I—O1174.73 (14)
I—O1i—Mo3—O12171.50 (12)Mo3—O1i—I—O286.08 (10)
I—O2—Mo1—O10.87 (8)Mo3—O1i—I—O2i93.92 (10)
I—O2—Mo1—O421.4 (4)Mo3—O1i—I—O31.04 (9)
I—O2—Mo1—O587.11 (11)Mo3—O1i—I—O3i178.96 (9)
I—O2—Mo1—O6171.68 (11)Mo3—O1i—Mo1i—O2i103.02 (9)
I—O2—Mo1—O775.33 (10)Mo3—O1i—Mo1i—O4i84.09 (12)
I—O2—Mo2—O30.12 (8)Mo3—O1i—Mo1i—O5i177.85 (9)
I—O2—Mo2—O587.16 (11)Mo3—O1i—Mo1i—O6i79.2 (3)
I—O2—Mo2—O820.8 (4)Mo3—O1i—Mo1i—O7i14.55 (9)
I—O2—Mo2—O9172.00 (12)Mo3—O3—I—O1178.97 (9)
I—O2—Mo2—O1075.36 (10)Mo3—O3—I—O1i1.03 (9)
I—O2i—Mo1i—O1i0.87 (8)Mo3—O3—I—O292.52 (10)
I—O2i—Mo1i—O4i21.4 (4)Mo3—O3—I—O2i87.48 (10)
I—O2i—Mo1i—O5i87.11 (11)Mo3—O3—I—O3i87.48 (10)
I—O2i—Mo1i—O6i171.68 (11)Mo3—O3—Mo2—O2103.14 (9)
I—O2i—Mo1i—O7i75.33 (10)Mo3—O3—Mo2—O5178.51 (9)
I—O2i—Mo2i—O3i0.12 (8)Mo3—O3—Mo2—O884.06 (11)
I—O2i—Mo2i—O5i87.16 (11)Mo3—O3—Mo2—O980.0 (3)
I—O2i—Mo2i—O8i20.8 (4)Mo3—O3—Mo2—O1015.96 (8)
I—O2i—Mo2i—O9i172.00 (12)Mo3—O7i—Mo1i—O1i20.08 (12)
I—O2i—Mo2i—O10i75.36 (10)Mo3—O7i—Mo1i—O2i88.74 (14)
I—O3—Mo2—O20.12 (8)Mo3—O7i—Mo1i—O4i72.09 (17)
I—O3—Mo2—O575.48 (10)Mo3—O7i—Mo1i—O5i54.1 (3)
I—O3—Mo2—O8172.91 (12)Mo3—O7i—Mo1i—O6i179.05 (15)
I—O3—Mo2—O923.0 (4)Mo3—O10—Mo2—O291.54 (12)
I—O3—Mo2—O1087.07 (11)Mo3—O10—Mo2—O322.32 (11)
I—O3—Mo3—O1i0.90 (8)Mo3—O10—Mo2—O557.5 (2)
I—O3—Mo3—O7i75.16 (10)Mo3—O10—Mo2—O867.44 (16)
I—O3—Mo3—O1086.67 (11)Mo3—O10—Mo2—O9176.07 (14)
I—O3—Mo3—O11172.10 (12)O13—Cr—O13xii—O13A35.5 (10)
I—O3—Mo3—O1223.2 (4)O13—Cr—O14—O15A55.8 (19)
I—O3i—Mo2i—O2i0.12 (8)O13—Cr—O14xii—O15Axii124.2 (19)
I—O3i—Mo2i—O5i75.48 (10)O13—Cr—O14A—O15145 (3)
I—O3i—Mo2i—O8i172.91 (12)O13—Cr—O14Axii—O15xii35 (3)
I—O3i—Mo2i—O9i23.0 (4)O13—Cr—O15—O14A33 (3)
I—O3i—Mo2i—O10i87.07 (11)O13—Cr—O15xii—O14Axii147 (3)
I—O3i—Mo3i—O10.90 (8)O13—Cr—O15A—O14121.2 (18)
I—O3i—Mo3i—O775.16 (10)O13—Cr—O15Axii—O14xii58.8 (18)
I—O3i—Mo3i—O10i86.67 (11)O13—O13Axii—Cr—O13A58.8 (18)
I—O3i—Mo3i—O11i172.10 (12)O13—O13Axii—Cr—O1441.4 (15)
I—O3i—Mo3i—O12i23.2 (4)O13—O13Axii—Cr—O14xii138.6 (15)
Mo1—O1—I—O1i23.2 (4)O13—O13Axii—Cr—O14A39.2 (16)
Mo1—O1—I—O21.01 (9)O13—O13Axii—Cr—O14Axii140.8 (16)
Mo1—O1—I—O2i178.99 (9)O13—O13Axii—Cr—O1559.8 (13)
Mo1—O1—I—O386.11 (10)O13—O13Axii—Cr—O15xii120.2 (13)
Mo1—O1—I—O3i93.89 (10)O13—O13Axii—Cr—O15A56.3 (15)
Mo1—O1—Mo3i—O3i103.44 (9)O13—O13Axii—Cr—O15Axii123.7 (15)
Mo1—O1—Mo3i—O714.66 (9)O13A—Cr—O14—O15A147 (2)
Mo1—O1—Mo3i—O10i178.66 (9)O13A—Cr—O14xii—O15Axii33 (2)
Mo1—O1—Mo3i—O11i80.7 (3)O13A—Cr—O14A—O1558 (3)
Mo1—O1—Mo3i—O12i84.16 (12)O13A—Cr—O14Axii—O15xii122 (3)
Mo1—O2—I—O10.99 (9)O13A—Cr—O15—O14A117 (3)
Mo1—O2—I—O1i179.01 (9)O13A—Cr—O15xii—O14Axii63 (3)
Mo1—O2—I—O2i179.01 (9)O13A—Cr—O15A—O1428.9 (18)
Mo1—O2—I—O392.38 (10)O13A—Cr—O15Axii—O14xii151.1 (18)
Mo1—O2—I—O3i87.62 (10)O13A—O13xii—Cr—O1435.4 (14)
Mo1—O2—Mo2—O3102.59 (9)O13A—O13xii—Cr—O14xii144.6 (14)
Mo1—O2—Mo2—O515.54 (8)O13A—O13xii—Cr—O14A41.8 (18)
Mo1—O2—Mo2—O881.9 (3)O13A—O13xii—Cr—O14Axii138.2 (18)
Mo1—O2—Mo2—O985.29 (12)O13A—O13xii—Cr—O1554.9 (14)
Mo1—O2—Mo2—O10178.06 (9)O13A—O13xii—Cr—O15xii125.1 (14)
Mo1—O5—Mo2—O221.98 (11)O13A—O13xii—Cr—O15A59.0 (17)
Mo1—O5—Mo2—O391.25 (13)O13A—O13xii—Cr—O15Axii121.0 (17)
Mo1—O5—Mo2—O8177.18 (14)O14—Cr—O14xii—O15Axii121.0 (17)
Mo1—O5—Mo2—O968.19 (16)O14—Cr—O14A—O15120 (3)
Mo1—O5—Mo2—O1057.3 (2)O14—Cr—O14Axii—O15xii60 (3)
Mo1—O7—Mo3i—O119.97 (12)O14—Cr—O15—O14A58 (3)
Mo1—O7—Mo3i—O3i88.50 (14)O14—Cr—O15xii—O14Axii122 (3)
Mo1—O7—Mo3i—O10i52.5 (3)O14—O15A—Cr—O14A53.3 (19)
Mo1—O7—Mo3i—O11i178.56 (15)O14—O15A—Cr—O14Axii126.7 (19)
Mo1—O7—Mo3i—O12i72.56 (17)O14—O15A—Cr—O1538 (2)
Mo2—O2—I—O193.50 (10)O14—O15A—Cr—O15xii142 (2)
Mo2—O2—I—O1i86.50 (10)O14—O15A—Cr—O15Axii142 (2)
Mo2—O2—I—O2i86.50 (10)O14A—Cr—O14—O15A125 (2)
Mo2—O2—I—O30.13 (9)O14A—Cr—O14xii—O15Axii55 (2)
Mo2—O2—I—O3i179.87 (9)O14A—Cr—O14Axii—O15xii55 (2)
Mo2—O2—Mo1—O1103.67 (8)O14A—O15—Cr—O15xii55 (2)
Mo2—O2—Mo1—O481.4 (3)O14A—O15—Cr—O15A41 (3)
Mo2—O2—Mo1—O515.69 (8)O14A—O15—Cr—O15Axii139 (3)
Mo2—O2—Mo1—O685.52 (10)O15—Cr—O14—O15A145.1 (19)
Mo2—O2—Mo1—O7178.13 (9)O15—Cr—O14xii—O15Axii34.9 (19)
Mo2—O3—I—O186.58 (10)O15—O14A—Cr—O15A143 (3)
Mo2—O3—I—O1i93.42 (10)O15—O14A—Cr—O15Axii37 (3)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y+1, z+1; (iii) x+1, y, z; (iv) x1/2, y+1/2, z1/2; (v) x+1/2, y+1/2, z1/2; (vi) x+1/2, y+1/2, z+1/2; (vii) x+1/2, y1/2, z+3/2; (viii) x+1/2, y1/2, z+1/2; (ix) x+1/2, y+1/2, z+1/2; (x) x1/2, y+1/2, z+1/2; (xi) x, y+1, z; (xii) x, y, z+1.

Experimental details

Crystal data
Chemical formulaCrNa2[IMo6O24]·24H2O
Mr1616.87
Crystal system, space groupMonoclinic, P21/n
Temperature (K)295
a, b, c (Å)10.3829 (7), 14.0871 (12), 14.9994 (14)
β (°) 102.931 (9)
V3)2138.2 (3)
Z2
Radiation typeMo Kα
µ (mm1)2.82
Crystal size (mm)0.29 × 0.23 × 0.18
Data collection
DiffractometerEnraf-Nonius CAD-4
diffractometer
Absorption correctionψ scan
(North et al., 1968)
Tmin, Tmax0.480, 0.545
No. of measured, independent and
observed [I > σ(I)] reflections
6570, 6210, 4697
Rint0.011
(sin θ/λ)max1)0.703
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.034, 0.050, 1.86
No. of reflections6210
No. of parameters276
H-atom treatmentH-atom parameters not defined
Δρmax, Δρmin (e Å3)1.21 (1.07 Å from I), 1.11 (0.79 Å from Mo1)

Computer programs: CAD-4-PC Diffractometer Software (Enraf-Nonius, 1993), CAD-4-PC Diffractometer Software, TEXSAN (Molecular Structure Corporation, 1997), TEXSAN.

Selected geometric parameters (Å, º) top
I—O11.890 (2)Mo3—O7i1.935 (2)
I—O21.885 (2)Mo3—O101.923 (2)
I—O31.881 (2)Mo3—O111.714 (3)
Mo1—O12.317 (2)Mo3—O121.697 (3)
Mo1—O22.353 (2)Cr—O131.968 (3)
Mo1—O41.701 (3)Cr—O13A1.93 (3)
Mo1—O51.915 (2)Cr—O141.969 (3)
Mo1—O61.711 (3)Cr—O14A1.90 (3)
Mo1—O71.948 (2)Cr—O151.968 (3)
Mo2—O22.331 (2)Cr—O15A1.93 (3)
Mo2—O32.337 (2)Na—O162.378 (4)
Mo2—O51.930 (2)Na—O172.435 (3)
Mo2—O81.694 (3)Na—O17ii2.437 (3)
Mo2—O91.697 (3)Na—O182.377 (4)
Mo2—O101.926 (2)Na—O192.449 (3)
Mo3—O1i2.331 (2)Na—O202.451 (3)
Mo3—O32.347 (2)
O1—I—O1i180.00O7i—Mo3—O1197.01 (11)
O1—I—O286.61 (9)O7i—Mo3—O12100.01 (12)
O1—I—O393.20 (9)O10—Mo3—O11101.04 (12)
O2—I—O2i180.00O10—Mo3—O1297.88 (12)
O2—I—O387.31 (10)O11—Mo3—O12107.16 (14)
O3—I—O3i180.00O13—Cr—O13iii180.00
O1—Mo1—O267.34 (8)O13—Cr—O13Aiii35.5 (9)
O1—Mo1—O494.93 (12)O13—Cr—O1490.54 (13)
O1—Mo1—O581.69 (9)O13—Cr—O1589.30 (12)
O1—Mo1—O6156.75 (11)O13A—Cr—O13Aiii180.00
O1—Mo1—O772.65 (8)O13A—Cr—O14A82.6 (13)
O2—Mo1—O4160.98 (12)O13A—Cr—O15A85.3 (12)
O2—Mo1—O572.86 (9)O14—Cr—O14iii180.00
O2—Mo1—O691.20 (11)O14—Cr—O1590.36 (13)
O2—Mo1—O782.04 (9)O14A—Cr—O14Aiii180.00
O4—Mo1—O598.66 (12)O14A—Cr—O15A94.8 (15)
O4—Mo1—O6107.32 (14)O15—Cr—O15iii180.00
O4—Mo1—O799.70 (12)O15A—Cr—O15Aiii180.00
O5—Mo1—O6101.06 (12)O16—Na—O1789.23 (13)
O5—Mo1—O7149.48 (10)O16—Na—O17ii82.65 (13)
O6—Mo1—O796.46 (11)O16—Na—O18172.90 (19)
O2—Mo2—O367.68 (8)O16—Na—O1991.67 (13)
O2—Mo2—O573.14 (9)O16—Na—O2093.98 (13)
O2—Mo2—O8159.21 (12)O17—Na—O17ii86.09 (11)
O2—Mo2—O993.43 (11)O17—Na—O1886.03 (13)
O2—Mo2—O1081.22 (9)O17—Na—O1989.44 (10)
O3—Mo2—O581.04 (9)O17—Na—O20173.20 (11)
O3—Mo2—O892.74 (12)O17ii—Na—O1891.74 (14)
O3—Mo2—O9159.62 (11)O17ii—Na—O19172.81 (11)
O3—Mo2—O1073.31 (8)O17ii—Na—O2088.37 (10)
O5—Mo2—O897.76 (12)O18—Na—O1993.57 (13)
O5—Mo2—O9101.36 (12)O18—Na—O2090.20 (13)
O5—Mo2—O10149.08 (10)O19—Na—O2096.46 (10)
O8—Mo2—O9106.83 (16)I—O1—Mo1103.58 (9)
O8—Mo2—O10100.38 (12)I—O1—Mo3i103.10 (9)
O9—Mo2—O1097.08 (12)Mo1—O1—Mo3i91.61 (8)
O1i—Mo3—O367.27 (8)I—O2—Mo1102.46 (9)
O1i—Mo3—O7i72.54 (9)I—O2—Mo2102.55 (9)
O1i—Mo3—O1081.39 (9)Mo1—O2—Mo289.71 (8)
O1i—Mo3—O11156.65 (11)I—O3—Mo2102.45 (9)
O1i—Mo3—O1295.37 (11)I—O3—Mo3102.82 (9)
O3—Mo3—O7i82.26 (10)Mo2—O3—Mo389.54 (8)
O3—Mo3—O1073.11 (9)Mo1—O5—Mo2118.43 (12)
O3—Mo3—O1191.01 (11)Mo1—O7—Mo3i118.22 (12)
O3—Mo3—O12161.15 (11)Mo2—O10—Mo3117.94 (12)
O7i—Mo3—O10149.51 (10)Na—O17—Naii93.91 (11)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y+1, z+1; (iii) x, y, z+1.
 

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