Disodium chromium(III) hexamolyb­do­iodate(VII) 24-hydrate, Na2Cr[IMo6O24]·24H2O

Rosu, C.; Weakley, T.J.R.

doi:10.1107/S0108270100005229

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Disodium chromium(III) hexamolybdoiodate(VII) 24-hydrate, Na₂Cr[IMo₆O₂₄]·24H₂O

C. Rosu and T. J. R. Weakley

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 $\overline 3$ m 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.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100005229/qb0206sup1.cif Contains datablocks global, I
	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 IMo₆O₂₄^5- 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.

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]·24H₂O	F(000) = 1566.00
M_r = 1616.87	D_x = 2.511 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
a = 10.3829 (7) Å	Cell parameters from 25 reflections
b = 14.0871 (12) Å	θ = 14.0–14.9°
c = 14.9994 (14) Å	µ = 2.82 mm⁻¹
β = 102.931 (9)°	T = 295 K
V = 2138.2 (3) Å³	Block, violet
Z = 2	0.29 × 0.23 × 0.18 mm

Data collection top

Enraf-Nonius CAD-4 diffractometer	4697 reflections with I > σ(I)
Radiation source: sealed X-ray tube	R_int = 0.011
Graphite monochromator	θ_max = 30.0°, θ_min = 2.0°
ω–2θ scans	h = −14→14
Absorption correction: ψ scan (North et al., 1968)	k = 0→19
T_min = 0.480, T_max = 0.545	l = −20→21
6570 measured reflections	3 standard reflections every 300 reflections
6210 independent reflections	intensity decay: 0.0%

Refinement top

Refinement on F²	0 constraints
Least-squares matrix: full	H-atom parameters not defined
R[F² > 2σ(F²)] = 0.034	w = 4F_o²/[σ²(I) + (0.020I)²]
wR(F²) = 0.050	(Δ/σ)_max = 0.022
S = 1.86	Δρ_max = 1.21 (1.07 Å from I) e Å⁻³
6210 reflections	Δρ_min = −1.11 (0.79 Å from Mo1) e Å⁻³
276 parameters	Extinction correction: Zachariasen (1967), equ(3) Acta Cryst. (1968) A24, p. 213
0 restraints	Extinction coefficient: 5.5E-7 (2)

Crystal data top

CrNa₂[IMo₆O₂₄]·24H₂O	V = 2138.2 (3) Å³
M_r = 1616.87	Z = 2
Monoclinic, P2₁/n	Mo Kα radiation
a = 10.3829 (7) Å	µ = 2.82 mm⁻¹
b = 14.0871 (12) Å	T = 295 K
c = 14.9994 (14) Å	0.29 × 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)	R_int = 0.011
T_min = 0.480, T_max = 0.545	3 standard reflections every 300 reflections
6570 measured reflections	intensity decay: 0.0%
6210 independent reflections

Refinement top

R[F² > 2σ(F²)] = 0.034	0 restraints
wR(F²) = 0.050	H-atom parameters not defined
S = 1.86	Δρ_max = 1.21 (1.07 Å from I) e Å⁻³
6210 reflections	Δρ_min = −1.11 (0.79 Å from Mo1) e Å⁻³
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

	x	y	z	U_iso*/U_eq	Occ. (<1)
I	0.5000	0.5000	0.5000	0.01617 (6)
Mo1	0.39295 (3)	0.37860 (2)	0.308259 (19)	0.02484 (8)
Mo2	0.49649 (3)	0.26577 (2)	0.50429 (2)	0.02550 (8)
Mo3	0.60153 (3)	0.38491 (2)	0.696128 (19)	0.02436 (8)
Cr	0.0000	0.0000	0.5000	0.02341 (18)
Na	−0.00217 (14)	0.37363 (11)	0.49923 (10)	0.0379 (4)
O1	0.3492 (2)	0.49931 (14)	0.40221 (15)	0.0207 (5)
O2	0.5653 (2)	0.40086 (15)	0.43816 (14)	0.0206 (5)
O3	0.4314 (2)	0.40580 (16)	0.56525 (14)	0.0208 (5)
O4	0.2401 (3)	0.3805 (2)	0.23744 (19)	0.0435 (8)
O5	0.3534 (2)	0.30167 (16)	0.40399 (16)	0.0280 (6)
O6	0.4881 (3)	0.30240 (19)	0.26157 (18)	0.0379 (8)
O7	0.4652 (3)	0.49536 (15)	0.26970 (16)	0.0277 (6)
O8	0.4081 (3)	0.1970 (2)	0.5615 (2)	0.0440 (8)
O9	0.5840 (3)	0.19116 (19)	0.45142 (19)	0.0430 (8)
O10	0.6404 (2)	0.30282 (16)	0.60310 (15)	0.0272 (6)
O11	0.5028 (3)	0.31276 (19)	0.74427 (18)	0.0378 (8)
O12	0.7537 (3)	0.3846 (2)	0.76716 (19)	0.0412 (8)
O13	0.0650 (3)	0.0421 (2)	0.62724 (18)	0.0330 (8)	0.880
O13A	−0.059 (3)	0.042 (2)	0.3752 (19)	0.058 (7)*	0.120
O14	−0.1173 (3)	0.1113 (2)	0.4748 (2)	0.0345 (8)	0.880
O14A	0.123 (4)	0.101 (2)	0.504 (2)	0.069 (9)*	0.120
O15	0.1429 (3)	0.0725 (2)	0.4648 (2)	0.0332 (8)	0.880
O15A	−0.139 (3)	0.080 (2)	0.525 (2)	0.058 (7)*	0.120
O16	0.1898 (4)	0.3879 (3)	0.6194 (3)	0.0792 (14)
O17	0.0825 (3)	0.49959 (18)	0.4169 (2)	0.0393 (8)
O18	−0.1960 (3)	0.3802 (4)	0.3799 (3)	0.0834 (15)
O19	0.1055 (3)	0.25618 (18)	0.41992 (18)	0.0340 (7)
O20	−0.1095 (3)	0.25942 (17)	0.58231 (17)	0.0325 (7)
O21	0.1414 (4)	0.4886 (3)	0.0572 (3)	0.0728 (13)
O22	0.2415 (5)	0.3379 (4)	0.8124 (3)	0.1072 (17)
O23A	0.0060 (14)	0.4992 (8)	0.7815 (9)	0.114 (4)*	0.450
O23	0.0159 (7)	0.4405 (6)	0.7742 (5)	0.070 (2)*	0.550
O24	0.1889 (5)	0.5965 (4)	0.8061 (4)	0.0569 (13)*	0.650
O24A	0.2405 (10)	0.6579 (7)	0.8097 (7)	0.058 (3)*	0.350

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
I	0.0165 (2)	0.0170 (2)	0.0156 (1)	0.0001 (1)	0.0048 (1)	0.0003 (1)
Mo1	0.0287 (2)	0.0261 (2)	0.0197 (2)	−0.0019 (1)	0.0055 (2)	−0.0039 (1)
Mo2	0.0315 (2)	0.0194 (2)	0.0272 (2)	−0.0009 (1)	0.0098 (1)	0.0006 (1)
Mo3	0.0278 (2)	0.0261 (2)	0.0194 (2)	0.0028 (1)	0.0058 (1)	0.0040 (1)
Cr	0.0282 (4)	0.0200 (3)	0.0251 (4)	−0.0010 (3)	0.0125 (3)	−0.0013 (3)
Na	0.0370 (9)	0.0353 (9)	0.0445 (9)	0.0005 (7)	0.0158 (7)	0.0012 (7)
O1	0.018 (1)	0.024 (1)	0.019 (1)	0.000 (1)	0.002 (1)	0.000 (1)
O2	0.022 (1)	0.020 (1)	0.021 (1)	0.002 (1)	0.007 (1)	−0.001 (1)
O3	0.022 (1)	0.022 (1)	0.020 (1)	−0.002 (1)	0.008 (1)	0.003 (1)
O4	0.040 (2)	0.049 (2)	0.035 (2)	−0.007 (2)	−0.006 (2)	−0.002 (1)
O5	0.029 (2)	0.026 (1)	0.029 (1)	−0.008 (1)	0.007 (1)	−0.003 (1)
O6	0.051 (2)	0.033 (2)	0.033 (2)	0.004 (1)	0.017 (2)	−0.006 (1)
O7	0.034 (2)	0.029 (2)	0.023 (1)	0.001 (1)	0.015 (1)	−0.001 (1)
O8	0.052 (2)	0.038 (2)	0.044 (2)	−0.016 (2)	0.015 (2)	0.007 (1)
O9	0.055 (2)	0.033 (2)	0.044 (2)	0.013 (2)	0.016 (2)	−0.006 (1)
O10	0.030 (2)	0.025 (1)	0.027 (1)	0.008 (1)	0.007 (1)	0.003 (1)
O11	0.046 (2)	0.038 (2)	0.033 (2)	−0.002 (1)	0.015 (2)	0.010 (1)
O12	0.038 (2)	0.048 (2)	0.032 (2)	0.007 (2)	−0.003 (2)	0.001 (1)
O13	0.041 (2)	0.038 (2)	0.024 (2)	−0.010 (2)	0.015 (2)	−0.006 (1)
O14	0.039 (2)	0.027 (2)	0.039 (2)	0.005 (1)	0.012 (2)	0.000 (1)
O15	0.036 (2)	0.028 (2)	0.043 (2)	−0.005 (1)	0.024 (2)	−0.001 (2)
O16	0.036 (2)	0.150 (4)	0.054 (2)	0.007 (2)	0.016 (2)	0.010 (2)
O17	0.030 (2)	0.042 (2)	0.049 (2)	0.000 (1)	0.016 (2)	0.001 (2)
O18	0.033 (2)	0.164 (5)	0.054 (2)	0.006 (2)	0.012 (2)	0.009 (2)
O19	0.033 (2)	0.032 (2)	0.039 (2)	−0.005 (1)	0.013 (1)	−0.004 (1)
O20	0.036 (2)	0.030 (2)	0.033 (2)	0.005 (1)	0.012 (1)	0.002 (1)
O21	0.048 (2)	0.074 (3)	0.102 (3)	−0.015 (2)	0.028 (2)	−0.016 (2)
O22	0.142 (4)	0.137 (4)	0.044 (2)	−0.081 (4)	0.024 (3)	−0.008 (2)

Geometric parameters (Å, º) top

I—O1	1.890 (2)	Mo3—O7ⁱ	1.935 (2)
I—O2	1.885 (2)	Mo3—O10	1.923 (2)
I—O3	1.881 (2)	Mo3—O11	1.714 (3)
Mo1—O1	2.317 (2)	Mo3—O12	1.697 (3)
Mo1—O2	2.353 (2)	Cr—O13	1.968 (3)
Mo1—O4	1.701 (3)	Cr—O13A	1.93 (3)
Mo1—O5	1.915 (2)	Cr—O14	1.969 (3)
Mo1—O6	1.711 (3)	Cr—O14A	1.90 (3)
Mo1—O7	1.948 (2)	Cr—O15	1.968 (3)
Mo2—O2	2.331 (2)	Cr—O15A	1.93 (3)
Mo2—O3	2.337 (2)	Na—O16	2.378 (4)
Mo2—O5	1.930 (2)	Na—O17	2.435 (3)
Mo2—O8	1.694 (3)	Na—O17ⁱⁱ	2.437 (3)
Mo2—O9	1.697 (3)	Na—O18	2.377 (4)
Mo2—O10	1.926 (2)	Na—O19	2.449 (3)
Mo3—O1ⁱ	2.331 (2)	Na—O20	2.451 (3)
Mo3—O3	2.347 (2)

O1···O17	2.827 (4)	O13A···O22^iv	2.68 (3)
O2···O18ⁱⁱⁱ	2.821 (4)	O13A···O24^iv	3.24 (3)
O3···O16	2.816 (4)	O13A···O19	3.46 (3)
O4···O23Aⁱⁱ	3.026 (14)	O13A···O24A^iv	3.51 (3)
O4···O21	3.072 (5)	O14···O20	2.627 (4)
O4···O10^iv	3.297 (4)	O14···O22^iv	2.645 (5)
O5···O19	2.715 (3)	O14···O19	3.323 (4)
O5···O12^iv	3.350 (4)	O14···O21^x	3.343 (5)
O6···O20^v	2.792 (4)	O14A···O19	2.52 (3)
O6···O13^v	3.196 (4)	O14A···O24A^vii	2.94 (4)
O6···O22^v	3.242 (5)	O14A···O24^vii	3.07 (4)
O6···O24Aⁱ	3.278 (10)	O14A···O21^viii	3.21 (4)
O6···O23^v	3.436 (8)	O15···O21^viii	2.618 (5)
O6···O18ⁱⁱⁱ	3.536 (5)	O15···O19	2.680 (4)
O7···O13^v	2.629 (3)	O15···O24^vii	3.504 (6)
O7···O13A^vi	2.66 (3)	O15···O24A^vii	3.538 (10)
O8···O24A^vii	2.784 (10)	O15A···O21^x	2.62 (3)
O8···O24^vii	2.803 (6)	O15A···O20	2.66 (3)
O8···O14A	3.19 (4)	O15A···O22^iv	3.36 (3)
O8···O15	3.312 (4)	O16···O22	2.910 (5)
O8···O21^viii	3.411 (5)	O16···O23	3.328 (8)
O8···O19	3.477 (4)	O16···O24A^vii	3.437 (11)
O8···O21^ix	3.575 (5)	O17···O23Aⁱⁱ	2.912 (14)
O9···O22^v	2.952 (5)	O17···O23ⁱⁱ	2.943 (8)
O9···O21^ix	2.977 (5)	O18···O24ⁱⁱ	2.827 (7)
O9···O23^v	3.188 (8)	O18···O24Aⁱⁱ	2.829 (10)
O9···O14ⁱⁱⁱ	3.244 (4)	O18···O22^iv	3.254 (7)
O9···O15Aⁱⁱⁱ	3.24 (3)	O21···O21^xi	3.068 (8)
O9···O20ⁱⁱⁱ	3.480 (4)	O21···O23Aⁱⁱ	3.143 (14)
O10···O20ⁱⁱⁱ	2.752 (3)	O21···O23ⁱⁱ	3.450 (8)
O11···O19^ix	2.786 (4)	O22···O23	2.703 (10)
O11···O13A^ix	3.00 (3)	O22···O24A^vii	3.158 (12)
O11···O22	3.126 (6)	O22···O23A	3.294 (15)
O11···O24A^vii	3.299 (10)	O23A···O24	2.305 (15)
O11···O16	3.531 (5)	O23A···O24A	3.263 (17)
O12···O23ⁱⁱⁱ	2.812 (8)	O23···O24	2.811 (9)
O12···O23Aⁱⁱⁱ	3.042 (14)	I···Mo2	3.3006 (3)
O12···O21ⁱ	3.167 (5)	I···Mo1	3.3167 (3)
O12···O15^ix	3.465 (4)	I···Mo3	3.3175 (3)
O13···O24A^vii	2.603 (10)	Mo1···Mo2	3.3036 (4)
O13···O24^vii	2.640 (6)	Mo1···Mo3ⁱ	3.3328 (4)
O13···O22^vii	3.510 (5)	Mo2···Mo3	3.2987 (4)
O13···O20	3.545 (4)

O1—I—O1ⁱ	180.00	O7ⁱ—Mo3—O11	97.01 (11)
O1—I—O2	86.61 (9)	O7ⁱ—Mo3—O12	100.01 (12)
O1—I—O3	93.20 (9)	O10—Mo3—O11	101.04 (12)
O2—I—O2ⁱ	180.00	O10—Mo3—O12	97.88 (12)
O2—I—O3	87.31 (10)	O11—Mo3—O12	107.16 (14)
O3—I—O3ⁱ	180.00	O13—Cr—O13^xii	180.00
O1—Mo1—O2	67.34 (8)	O13—Cr—O13A^xii	35.5 (9)
O1—Mo1—O4	94.93 (12)	O13—Cr—O14	90.54 (13)
O1—Mo1—O5	81.69 (9)	O13—Cr—O15	89.30 (12)
O1—Mo1—O6	156.75 (11)	O13A—Cr—O13A^xii	180.00
O1—Mo1—O7	72.65 (8)	O13A—Cr—O14A	82.6 (13)
O2—Mo1—O4	160.98 (12)	O13A—Cr—O15A	85.3 (12)
O2—Mo1—O5	72.86 (9)	O14—Cr—O14^xii	180.00
O2—Mo1—O6	91.20 (11)	O14—Cr—O15	90.36 (13)
O2—Mo1—O7	82.04 (9)	O14A—Cr—O14A^xii	180.00
O4—Mo1—O5	98.66 (12)	O14A—Cr—O15A	94.8 (15)
O4—Mo1—O6	107.32 (14)	O15—Cr—O15^xii	180.00
O4—Mo1—O7	99.70 (12)	O15A—Cr—O15A^xii	180.00
O5—Mo1—O6	101.06 (12)	O16—Na—O17	89.23 (13)
O5—Mo1—O7	149.48 (10)	O16—Na—O17ⁱⁱ	82.65 (13)
O6—Mo1—O7	96.46 (11)	O16—Na—O18	172.90 (19)
O2—Mo2—O3	67.68 (8)	O16—Na—O19	91.67 (13)
O2—Mo2—O5	73.14 (9)	O16—Na—O20	93.98 (13)
O2—Mo2—O8	159.21 (12)	O17—Na—O17ⁱⁱ	86.09 (11)
O2—Mo2—O9	93.43 (11)	O17—Na—O18	86.03 (13)
O2—Mo2—O10	81.22 (9)	O17—Na—O19	89.44 (10)
O3—Mo2—O5	81.04 (9)	O17—Na—O20	173.20 (11)
O3—Mo2—O8	92.74 (12)	O17ⁱⁱ—Na—O18	91.74 (14)
O3—Mo2—O9	159.62 (11)	O17ⁱⁱ—Na—O19	172.81 (11)
O3—Mo2—O10	73.31 (8)	O17ⁱⁱ—Na—O20	88.37 (10)
O5—Mo2—O8	97.76 (12)	O18—Na—O19	93.57 (13)
O5—Mo2—O9	101.36 (12)	O18—Na—O20	90.20 (13)
O5—Mo2—O10	149.08 (10)	O19—Na—O20	96.46 (10)
O8—Mo2—O9	106.83 (16)	I—O1—Mo1	103.58 (9)
O8—Mo2—O10	100.38 (12)	I—O1—Mo3ⁱ	103.10 (9)
O9—Mo2—O10	97.08 (12)	Mo1—O1—Mo3ⁱ	91.61 (8)
O1ⁱ—Mo3—O3	67.27 (8)	I—O2—Mo1	102.46 (9)
O1ⁱ—Mo3—O7ⁱ	72.54 (9)	I—O2—Mo2	102.55 (9)
O1ⁱ—Mo3—O10	81.39 (9)	Mo1—O2—Mo2	89.71 (8)
O1ⁱ—Mo3—O11	156.65 (11)	I—O3—Mo2	102.45 (9)
O1ⁱ—Mo3—O12	95.37 (11)	I—O3—Mo3	102.82 (9)
O3—Mo3—O7ⁱ	82.26 (10)	Mo2—O3—Mo3	89.54 (8)
O3—Mo3—O10	73.11 (9)	Mo1—O5—Mo2	118.43 (12)
O3—Mo3—O11	91.01 (11)	Mo1—O7—Mo3ⁱ	118.22 (12)
O3—Mo3—O12	161.15 (11)	Mo2—O10—Mo3	117.94 (12)
O7ⁱ—Mo3—O10	149.51 (10)	Na—O17—Naⁱⁱ	93.91 (11)

I—O1—Mo1—O2	−0.87 (8)	Mo2—O3—I—O2	0.13 (9)
I—O1—Mo1—O4	172.02 (12)	Mo2—O3—I—O2ⁱ	−179.87 (9)
I—O1—Mo1—O5	73.96 (11)	Mo2—O3—I—O3ⁱ	−179.87 (9)
I—O1—Mo1—O6	−24.7 (3)	Mo2—O3—Mo3—O1ⁱ	103.57 (8)
I—O1—Mo1—O7	−89.34 (12)	Mo2—O3—Mo3—O7ⁱ	177.82 (9)
I—O1—Mo3ⁱ—O3ⁱ	0.90 (8)	Mo2—O3—Mo3—O10	16.00 (8)
I—O1—Mo3ⁱ—O7	89.68 (11)	Mo2—O3—Mo3—O11	−85.23 (11)
I—O1—Mo3ⁱ—O10ⁱ	−74.32 (10)	Mo2—O3—Mo3—O12	79.5 (3)
I—O1—Mo3ⁱ—O11ⁱ	23.6 (3)	Mo2—O5—Mo1—O1	−90.55 (13)
I—O1—Mo3ⁱ—O12ⁱ	−171.50 (12)	Mo2—O5—Mo1—O2	−21.80 (11)
I—O1ⁱ—Mo1ⁱ—O2ⁱ	0.87 (8)	Mo2—O5—Mo1—O4	175.70 (14)
I—O1ⁱ—Mo1ⁱ—O4ⁱ	−172.02 (12)	Mo2—O5—Mo1—O6	66.03 (15)
I—O1ⁱ—Mo1ⁱ—O5ⁱ	−73.96 (11)	Mo2—O5—Mo1—O7	−57.8 (3)
I—O1ⁱ—Mo1ⁱ—O6ⁱ	24.7 (3)	Mo2—O10—Mo3—O1ⁱ	−90.99 (13)
I—O1ⁱ—Mo1ⁱ—O7ⁱ	89.34 (12)	Mo2—O10—Mo3—O3	−22.24 (11)
I—O1ⁱ—Mo3—O3	−0.90 (8)	Mo2—O10—Mo3—O7ⁱ	−59.8 (3)
I—O1ⁱ—Mo3—O7ⁱ	−89.68 (11)	Mo2—O10—Mo3—O11	65.44 (15)
I—O1ⁱ—Mo3—O10	74.32 (10)	Mo2—O10—Mo3—O12	174.73 (14)
I—O1ⁱ—Mo3—O11	−23.6 (3)	Mo3—O1ⁱ—I—O1	174.73 (14)
I—O1ⁱ—Mo3—O12	171.50 (12)	Mo3—O1ⁱ—I—O2	−86.08 (10)
I—O2—Mo1—O1	0.87 (8)	Mo3—O1ⁱ—I—O2ⁱ	93.92 (10)
I—O2—Mo1—O4	−21.4 (4)	Mo3—O1ⁱ—I—O3	1.04 (9)
I—O2—Mo1—O5	−87.11 (11)	Mo3—O1ⁱ—I—O3ⁱ	−178.96 (9)
I—O2—Mo1—O6	171.68 (11)	Mo3—O1ⁱ—Mo1ⁱ—O2ⁱ	−103.02 (9)
I—O2—Mo1—O7	75.33 (10)	Mo3—O1ⁱ—Mo1ⁱ—O4ⁱ	84.09 (12)
I—O2—Mo2—O3	0.12 (8)	Mo3—O1ⁱ—Mo1ⁱ—O5ⁱ	−177.85 (9)
I—O2—Mo2—O5	87.16 (11)	Mo3—O1ⁱ—Mo1ⁱ—O6ⁱ	−79.2 (3)
I—O2—Mo2—O8	20.8 (4)	Mo3—O1ⁱ—Mo1ⁱ—O7ⁱ	−14.55 (9)
I—O2—Mo2—O9	−172.00 (12)	Mo3—O3—I—O1	178.97 (9)
I—O2—Mo2—O10	−75.36 (10)	Mo3—O3—I—O1ⁱ	−1.03 (9)
I—O2ⁱ—Mo1ⁱ—O1ⁱ	−0.87 (8)	Mo3—O3—I—O2	92.52 (10)
I—O2ⁱ—Mo1ⁱ—O4ⁱ	21.4 (4)	Mo3—O3—I—O2ⁱ	−87.48 (10)
I—O2ⁱ—Mo1ⁱ—O5ⁱ	87.11 (11)	Mo3—O3—I—O3ⁱ	−87.48 (10)
I—O2ⁱ—Mo1ⁱ—O6ⁱ	−171.68 (11)	Mo3—O3—Mo2—O2	−103.14 (9)
I—O2ⁱ—Mo1ⁱ—O7ⁱ	−75.33 (10)	Mo3—O3—Mo2—O5	−178.51 (9)
I—O2ⁱ—Mo2ⁱ—O3ⁱ	−0.12 (8)	Mo3—O3—Mo2—O8	84.06 (11)
I—O2ⁱ—Mo2ⁱ—O5ⁱ	−87.16 (11)	Mo3—O3—Mo2—O9	−80.0 (3)
I—O2ⁱ—Mo2ⁱ—O8ⁱ	−20.8 (4)	Mo3—O3—Mo2—O10	−15.96 (8)
I—O2ⁱ—Mo2ⁱ—O9ⁱ	172.00 (12)	Mo3—O7ⁱ—Mo1ⁱ—O1ⁱ	20.08 (12)
I—O2ⁱ—Mo2ⁱ—O10ⁱ	75.36 (10)	Mo3—O7ⁱ—Mo1ⁱ—O2ⁱ	88.74 (14)
I—O3—Mo2—O2	−0.12 (8)	Mo3—O7ⁱ—Mo1ⁱ—O4ⁱ	−72.09 (17)
I—O3—Mo2—O5	−75.48 (10)	Mo3—O7ⁱ—Mo1ⁱ—O5ⁱ	54.1 (3)
I—O3—Mo2—O8	−172.91 (12)	Mo3—O7ⁱ—Mo1ⁱ—O6ⁱ	179.05 (15)
I—O3—Mo2—O9	23.0 (4)	Mo3—O10—Mo2—O2	91.54 (12)
I—O3—Mo2—O10	87.07 (11)	Mo3—O10—Mo2—O3	22.32 (11)
I—O3—Mo3—O1ⁱ	0.90 (8)	Mo3—O10—Mo2—O5	57.5 (2)
I—O3—Mo3—O7ⁱ	75.16 (10)	Mo3—O10—Mo2—O8	−67.44 (16)
I—O3—Mo3—O10	−86.67 (11)	Mo3—O10—Mo2—O9	−176.07 (14)
I—O3—Mo3—O11	172.10 (12)	O13—Cr—O13^xii—O13A	−35.5 (10)
I—O3—Mo3—O12	−23.2 (4)	O13—Cr—O14—O15A	−55.8 (19)
I—O3ⁱ—Mo2ⁱ—O2ⁱ	0.12 (8)	O13—Cr—O14^xii—O15A^xii	−124.2 (19)
I—O3ⁱ—Mo2ⁱ—O5ⁱ	75.48 (10)	O13—Cr—O14A—O15	145 (3)
I—O3ⁱ—Mo2ⁱ—O8ⁱ	172.91 (12)	O13—Cr—O14A^xii—O15^xii	35 (3)
I—O3ⁱ—Mo2ⁱ—O9ⁱ	−23.0 (4)	O13—Cr—O15—O14A	−33 (3)
I—O3ⁱ—Mo2ⁱ—O10ⁱ	−87.07 (11)	O13—Cr—O15^xii—O14A^xii	−147 (3)
I—O3ⁱ—Mo3ⁱ—O1	−0.90 (8)	O13—Cr—O15A—O14	121.2 (18)
I—O3ⁱ—Mo3ⁱ—O7	−75.16 (10)	O13—Cr—O15A^xii—O14^xii	58.8 (18)
I—O3ⁱ—Mo3ⁱ—O10ⁱ	86.67 (11)	O13—O13A^xii—Cr—O13A	58.8 (18)
I—O3ⁱ—Mo3ⁱ—O11ⁱ	−172.10 (12)	O13—O13A^xii—Cr—O14	−41.4 (15)
I—O3ⁱ—Mo3ⁱ—O12ⁱ	23.2 (4)	O13—O13A^xii—Cr—O14^xii	138.6 (15)
Mo1—O1—I—O1ⁱ	23.2 (4)	O13—O13A^xii—Cr—O14A	39.2 (16)
Mo1—O1—I—O2	1.01 (9)	O13—O13A^xii—Cr—O14A^xii	−140.8 (16)
Mo1—O1—I—O2ⁱ	−178.99 (9)	O13—O13A^xii—Cr—O15	59.8 (13)
Mo1—O1—I—O3	−86.11 (10)	O13—O13A^xii—Cr—O15^xii	−120.2 (13)
Mo1—O1—I—O3ⁱ	93.89 (10)	O13—O13A^xii—Cr—O15A	−56.3 (15)
Mo1—O1—Mo3ⁱ—O3ⁱ	−103.44 (9)	O13—O13A^xii—Cr—O15A^xii	123.7 (15)
Mo1—O1—Mo3ⁱ—O7	−14.66 (9)	O13A—Cr—O14—O15A	147 (2)
Mo1—O1—Mo3ⁱ—O10ⁱ	−178.66 (9)	O13A—Cr—O14^xii—O15A^xii	33 (2)
Mo1—O1—Mo3ⁱ—O11ⁱ	−80.7 (3)	O13A—Cr—O14A—O15	−58 (3)
Mo1—O1—Mo3ⁱ—O12ⁱ	84.16 (12)	O13A—Cr—O14A^xii—O15^xii	−122 (3)
Mo1—O2—I—O1	−0.99 (9)	O13A—Cr—O15—O14A	117 (3)
Mo1—O2—I—O1ⁱ	179.01 (9)	O13A—Cr—O15^xii—O14A^xii	63 (3)
Mo1—O2—I—O2ⁱ	179.01 (9)	O13A—Cr—O15A—O14	−28.9 (18)
Mo1—O2—I—O3	92.38 (10)	O13A—Cr—O15A^xii—O14^xii	−151.1 (18)
Mo1—O2—I—O3ⁱ	−87.62 (10)	O13A—O13^xii—Cr—O14	35.4 (14)
Mo1—O2—Mo2—O3	−102.59 (9)	O13A—O13^xii—Cr—O14^xii	−144.6 (14)
Mo1—O2—Mo2—O5	−15.54 (8)	O13A—O13^xii—Cr—O14A	−41.8 (18)
Mo1—O2—Mo2—O8	−81.9 (3)	O13A—O13^xii—Cr—O14A^xii	138.2 (18)
Mo1—O2—Mo2—O9	85.29 (12)	O13A—O13^xii—Cr—O15	−54.9 (14)
Mo1—O2—Mo2—O10	−178.06 (9)	O13A—O13^xii—Cr—O15^xii	125.1 (14)
Mo1—O5—Mo2—O2	21.98 (11)	O13A—O13^xii—Cr—O15A	59.0 (17)
Mo1—O5—Mo2—O3	91.25 (13)	O13A—O13^xii—Cr—O15A^xii	−121.0 (17)
Mo1—O5—Mo2—O8	−177.18 (14)	O14—Cr—O14^xii—O15A^xii	−121.0 (17)
Mo1—O5—Mo2—O9	−68.19 (16)	O14—Cr—O14A—O15	−120 (3)
Mo1—O5—Mo2—O10	57.3 (2)	O14—Cr—O14A^xii—O15^xii	−60 (3)
Mo1—O7—Mo3ⁱ—O1	19.97 (12)	O14—Cr—O15—O14A	58 (3)
Mo1—O7—Mo3ⁱ—O3ⁱ	88.50 (14)	O14—Cr—O15^xii—O14A^xii	122 (3)
Mo1—O7—Mo3ⁱ—O10ⁱ	52.5 (3)	O14—O15A—Cr—O14A	53.3 (19)
Mo1—O7—Mo3ⁱ—O11ⁱ	178.56 (15)	O14—O15A—Cr—O14A^xii	−126.7 (19)
Mo1—O7—Mo3ⁱ—O12ⁱ	−72.56 (17)	O14—O15A—Cr—O15	38 (2)
Mo2—O2—I—O1	−93.50 (10)	O14—O15A—Cr—O15^xii	−142 (2)
Mo2—O2—I—O1ⁱ	86.50 (10)	O14—O15A—Cr—O15A^xii	−142 (2)
Mo2—O2—I—O2ⁱ	86.50 (10)	O14A—Cr—O14—O15A	−125 (2)
Mo2—O2—I—O3	−0.13 (9)	O14A—Cr—O14^xii—O15A^xii	−55 (2)
Mo2—O2—I—O3ⁱ	179.87 (9)	O14A—Cr—O14A^xii—O15^xii	−55 (2)
Mo2—O2—Mo1—O1	103.67 (8)	O14A—O15—Cr—O15^xii	−55 (2)
Mo2—O2—Mo1—O4	81.4 (3)	O14A—O15—Cr—O15A	41 (3)
Mo2—O2—Mo1—O5	15.69 (8)	O14A—O15—Cr—O15A^xii	−139 (3)
Mo2—O2—Mo1—O6	−85.52 (10)	O15—Cr—O14—O15A	−145.1 (19)
Mo2—O2—Mo1—O7	178.13 (9)	O15—Cr—O14^xii—O15A^xii	−34.9 (19)
Mo2—O3—I—O1	86.58 (10)	O15—O14A—Cr—O15A	−143 (3)
Mo2—O3—I—O1ⁱ	−93.42 (10)	O15—O14A—Cr—O15A^xii	37 (3)

Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x, −y+1, −z+1; (iii) x+1, y, z; (iv) x−1/2, −y+1/2, z−1/2; (v) x+1/2, −y+1/2, z−1/2; (vi) −x+1/2, y+1/2, −z+1/2; (vii) −x+1/2, y−1/2, −z+3/2; (viii) −x+1/2, y−1/2, −z+1/2; (ix) x+1/2, −y+1/2, z+1/2; (x) x−1/2, −y+1/2, z+1/2; (xi) −x, −y+1, −z; (xii) −x, −y, −z+1.

Experimental details

Crystal data
Chemical formula	CrNa₂[IMo₆O₂₄]·24H₂O
M_r	1616.87
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	295
a, b, c (Å)	10.3829 (7), 14.0871 (12), 14.9994 (14)
β (°)	102.931 (9)
V (Å³)	2138.2 (3)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	2.82
Crystal size (mm)	0.29 × 0.23 × 0.18

Data collection
Diffractometer	Enraf-Nonius CAD-4 diffractometer
Absorption correction	ψ scan (North et al., 1968)
T_min, T_max	0.480, 0.545
No. of measured, independent and observed [I > σ(I)] reflections	6570, 6210, 4697
R_int	0.011
(sin θ/λ)_max (Å⁻¹)	0.703

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.034, 0.050, 1.86
No. of reflections	6210
No. of parameters	276
H-atom treatment	H-atom parameters not defined
Δρ_max, Δρ_min (e Å⁻³)	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—O1	1.890 (2)	Mo3—O7ⁱ	1.935 (2)
I—O2	1.885 (2)	Mo3—O10	1.923 (2)
I—O3	1.881 (2)	Mo3—O11	1.714 (3)
Mo1—O1	2.317 (2)	Mo3—O12	1.697 (3)
Mo1—O2	2.353 (2)	Cr—O13	1.968 (3)
Mo1—O4	1.701 (3)	Cr—O13A	1.93 (3)
Mo1—O5	1.915 (2)	Cr—O14	1.969 (3)
Mo1—O6	1.711 (3)	Cr—O14A	1.90 (3)
Mo1—O7	1.948 (2)	Cr—O15	1.968 (3)
Mo2—O2	2.331 (2)	Cr—O15A	1.93 (3)
Mo2—O3	2.337 (2)	Na—O16	2.378 (4)
Mo2—O5	1.930 (2)	Na—O17	2.435 (3)
Mo2—O8	1.694 (3)	Na—O17ⁱⁱ	2.437 (3)
Mo2—O9	1.697 (3)	Na—O18	2.377 (4)
Mo2—O10	1.926 (2)	Na—O19	2.449 (3)
Mo3—O1ⁱ	2.331 (2)	Na—O20	2.451 (3)
Mo3—O3	2.347 (2)

O1—I—O1ⁱ	180.00	O7ⁱ—Mo3—O11	97.01 (11)
O1—I—O2	86.61 (9)	O7ⁱ—Mo3—O12	100.01 (12)
O1—I—O3	93.20 (9)	O10—Mo3—O11	101.04 (12)
O2—I—O2ⁱ	180.00	O10—Mo3—O12	97.88 (12)
O2—I—O3	87.31 (10)	O11—Mo3—O12	107.16 (14)
O3—I—O3ⁱ	180.00	O13—Cr—O13ⁱⁱⁱ	180.00
O1—Mo1—O2	67.34 (8)	O13—Cr—O13Aⁱⁱⁱ	35.5 (9)
O1—Mo1—O4	94.93 (12)	O13—Cr—O14	90.54 (13)
O1—Mo1—O5	81.69 (9)	O13—Cr—O15	89.30 (12)
O1—Mo1—O6	156.75 (11)	O13A—Cr—O13Aⁱⁱⁱ	180.00
O1—Mo1—O7	72.65 (8)	O13A—Cr—O14A	82.6 (13)
O2—Mo1—O4	160.98 (12)	O13A—Cr—O15A	85.3 (12)
O2—Mo1—O5	72.86 (9)	O14—Cr—O14ⁱⁱⁱ	180.00
O2—Mo1—O6	91.20 (11)	O14—Cr—O15	90.36 (13)
O2—Mo1—O7	82.04 (9)	O14A—Cr—O14Aⁱⁱⁱ	180.00
O4—Mo1—O5	98.66 (12)	O14A—Cr—O15A	94.8 (15)
O4—Mo1—O6	107.32 (14)	O15—Cr—O15ⁱⁱⁱ	180.00
O4—Mo1—O7	99.70 (12)	O15A—Cr—O15Aⁱⁱⁱ	180.00
O5—Mo1—O6	101.06 (12)	O16—Na—O17	89.23 (13)
O5—Mo1—O7	149.48 (10)	O16—Na—O17ⁱⁱ	82.65 (13)
O6—Mo1—O7	96.46 (11)	O16—Na—O18	172.90 (19)
O2—Mo2—O3	67.68 (8)	O16—Na—O19	91.67 (13)
O2—Mo2—O5	73.14 (9)	O16—Na—O20	93.98 (13)
O2—Mo2—O8	159.21 (12)	O17—Na—O17ⁱⁱ	86.09 (11)
O2—Mo2—O9	93.43 (11)	O17—Na—O18	86.03 (13)
O2—Mo2—O10	81.22 (9)	O17—Na—O19	89.44 (10)
O3—Mo2—O5	81.04 (9)	O17—Na—O20	173.20 (11)
O3—Mo2—O8	92.74 (12)	O17ⁱⁱ—Na—O18	91.74 (14)
O3—Mo2—O9	159.62 (11)	O17ⁱⁱ—Na—O19	172.81 (11)
O3—Mo2—O10	73.31 (8)	O17ⁱⁱ—Na—O20	88.37 (10)
O5—Mo2—O8	97.76 (12)	O18—Na—O19	93.57 (13)
O5—Mo2—O9	101.36 (12)	O18—Na—O20	90.20 (13)
O5—Mo2—O10	149.08 (10)	O19—Na—O20	96.46 (10)
O8—Mo2—O9	106.83 (16)	I—O1—Mo1	103.58 (9)
O8—Mo2—O10	100.38 (12)	I—O1—Mo3ⁱ	103.10 (9)
O9—Mo2—O10	97.08 (12)	Mo1—O1—Mo3ⁱ	91.61 (8)
O1ⁱ—Mo3—O3	67.27 (8)	I—O2—Mo1	102.46 (9)
O1ⁱ—Mo3—O7ⁱ	72.54 (9)	I—O2—Mo2	102.55 (9)
O1ⁱ—Mo3—O10	81.39 (9)	Mo1—O2—Mo2	89.71 (8)
O1ⁱ—Mo3—O11	156.65 (11)	I—O3—Mo2	102.45 (9)
O1ⁱ—Mo3—O12	95.37 (11)	I—O3—Mo3	102.82 (9)
O3—Mo3—O7ⁱ	82.26 (10)	Mo2—O3—Mo3	89.54 (8)
O3—Mo3—O10	73.11 (9)	Mo1—O5—Mo2	118.43 (12)
O3—Mo3—O11	91.01 (11)	Mo1—O7—Mo3ⁱ	118.22 (12)
O3—Mo3—O12	161.15 (11)	Mo2—O10—Mo3	117.94 (12)
O7ⁱ—Mo3—O10	149.51 (10)	Na—O17—Naⁱⁱ	93.91 (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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Disodium chromium(III) hexamolyb­do­iodate(VII) 24-hydrate, Na2Cr[IMo6O24]·24H2O

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Disodium chromium(III) hexamolybdoiodate(VII) 24-hydrate, Na₂Cr[IMo₆O₂₄]·24H₂O