Dipotassium hepta­hydrogenhexa­molybdochromate(III) octa­hydrate, the first hepta­protonated Anderson-type polyoxometalate

Lee, U.

doi:10.1107/S1600536806052883

Dipotassium heptahydrogenhexamolybdochromate(III) octahydrate, the first heptaprotonated Anderson-type polyoxometalate

The title compound, K₂[H₇CrMo₆O₂₄]·8H₂O, contains an unexpectedly protonated polyanion, [H₇CrMo₆O₂₄]^2- in the B series Anderson-type heteropolyoxomolybdate. It was obtained by recrystallizing K₃[H₆CrMo₆O₂₄]·nH₂O at pH 1.80. The asymmetric unit contains two crystallographically independent polyanions that have C_i ( $\overline{1}$ ) symmetry. Six O atoms of the central CrO₆ octahedron and one atom of an edge-shared MoO₆ octahedron are protonated.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806052883/bt2216sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536806052883/bt2216Isup2.hkl Contains datablock I

checkCIF report

Key indicators

Single-crystal X-ray study
T = 173 K
Mean (r-O) = 0.003 Å
H-atom completeness 83%
R factor = 0.029
wR factor = 0.073
Data-to-parameter ratio = 13.1

checkCIF/PLATON results

No syntax errors found



Alert level A
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......       O31W

Author Response: : Explained in the _publ_section_exptl_refinement.

PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) .......       O32W

Author Response: : Explained in the _publ_section_exptl_refinement.


Alert level B
CHEMS01_ALERT_1_B  The sum formula contains elements in the wrong order.
            H  precedes Cr
            Sequence must be C, H, then alphabetical.
PLAT222_ALERT_3_B Large Non-Solvent    H     Ueq(max)/Ueq(min) ...       5.00 Ratio

Author Response: : Explained in the _publ_section_exptl_refinement.

PLAT355_ALERT_3_B Long    O-H Bond (0.82A)   O30W   -   H30A   ...       1.09 Ang.

Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings    Differ ....          ?

Author Response: : Because H atoms of H2O(O31w, O32w) were not included.

PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?

Author Response: : Because H atoms of H2O(O31w, O32w) were not included.

PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............       0.50 Ratio

Author Response: : It is no problem.

PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...          ?

Author Response: : Because H atoms of H2O(O31w, O32w) were not included.

PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #          9
              O

Author Response: : Because it is grouping.


Alert level G
FORMU01_ALERT_2_G  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:H23 Cr1 K2 Mo6 O32
            Atom count from the _atom_site data:  H19 Cr1 K2 Mo6 O32
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional?
           From the CIF: _cell_formula_units_Z    2
           From the CIF: _chemical_formula_sum  H23 Cr K2 Mo6 O32
           TEST: Compare cell contents of formula and atom_site data

           atom    Z*formula  cif sites diff
           H         46.00     38.00    8.00
           Cr         2.00      2.00    0.00
           K          4.00      4.00    0.00
           Mo        12.00     12.00    0.00
           O         64.00     64.00    0.00

   2 ALERT level A = In general: serious problem
   3 ALERT level B = Potentially serious problem
   5 ALERT level C = Check and explain
   3 ALERT level G = General alerts; check

   7 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   3 ALERT type 2 Indicator that the structure model may be wrong or deficient
   2 ALERT type 3 Indicator that the structure quality may be low
   1 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997) and DIAMOND (Brandenburg, 1998); software used to prepare material for publication: SHELXL97.

Dipotassium heptahydrogenhexamolybdochromate(III) octahydrate top

Crystal data top

K₂[H₇CrMo₆O₂₄]·8H₂O	Z = 2
M_r = 1241.02	F(000) = 1186
Triclinic, P1	D_x = 2.954 Mg m⁻³
Hall symbol: -p_1	Mo Kα radiation, λ = 0.71073 Å
a = 10.4733 (6) Å	Cell parameters from 5418 reflections
b = 10.8698 (6) Å	θ = 2.3–28.3°
c = 12.6540 (7) Å	µ = 3.40 mm⁻¹
α = 99.309 (1)°	T = 173 K
β = 94.465 (1)°	Block, purple
γ = 99.256 (1)°	0.32 × 0.25 × 0.20 mm
V = 1395.08 (14) Å³

Data collection top

Bruker SMART CCD diffractometer	5360 independent reflections
Radiation source: fine-focus sealed tube	5200 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.025
Detector resolution: 10.00 pixels mm^-1	θ_max = 26.0°, θ_min = 1.9°
φ and ω scans	h = −12→12
Absorption correction: multi-scan (SADABS; Sheldrick, 1999)	k = −13→13
T_min = 0.380, T_max = 0.512	l = −15→15
10855 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)] = 0.029	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.074	w = 1/[σ²(F_o²) + (0.0228P)² + 4.6144P] where P = (F_o² + 2F_c²)/3
S = 1.19	(Δ/σ)_max < 0.001
5360 reflections	Δρ_max = 0.85 e Å⁻³
408 parameters	Δρ_min = −0.85 e Å⁻³
19 restraints	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0065 (2)

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	U_iso*/U_eq	Occ. (<1)
Cr1	0.5000	0.0000	1.0000	0.00920 (19)
Cr2	0.5000	0.5000	0.5000	0.00872 (19)
Mo1	0.23269 (4)	0.13635 (3)	0.99553 (3)	0.01225 (10)
Mo2	0.20800 (3)	−0.17242 (3)	0.90584 (3)	0.01183 (10)
Mo3	0.47641 (4)	−0.31122 (3)	0.92196 (3)	0.01144 (10)
Mo4	0.79231 (3)	0.42377 (3)	0.46277 (3)	0.01091 (10)
Mo5	0.52137 (3)	0.19390 (3)	0.43521 (3)	0.01023 (10)
Mo6	0.23141 (3)	0.27475 (3)	0.46833 (3)	0.01041 (10)
K1	0.06889 (10)	0.02286 (10)	0.66879 (8)	0.0206 (2)
K2	0.92829 (10)	0.58480 (10)	0.77802 (8)	0.0225 (2)
O1C	0.4159 (3)	0.1136 (3)	1.0986 (2)	0.0117 (6)
H1	0.409 (5)	0.102 (5)	1.153 (4)	0.010 (13)*
O2C	0.3523 (3)	0.0068 (3)	0.8952 (2)	0.0118 (6)
H2	0.362 (6)	0.027 (6)	0.844 (5)	0.034 (18)*
O3C	0.3919 (3)	−0.1596 (3)	1.0194 (2)	0.0119 (6)
H3	0.383 (7)	−0.164 (7)	1.086 (5)	0.05 (2)*
O4B	0.1717 (3)	−0.0379 (3)	1.0105 (2)	0.0152 (6)
O5B	0.3370 (3)	−0.2593 (3)	0.8306 (2)	0.0135 (6)
H5	0.324 (11)	−0.275 (11)	0.774 (6)	0.020*	0.50
O6B	0.6223 (3)	−0.2659 (3)	1.0259 (2)	0.0143 (6)
O7T	0.1322 (3)	0.1465 (3)	0.8859 (3)	0.0207 (7)
O8T	0.1740 (3)	0.2123 (3)	1.1050 (3)	0.0208 (7)
O9T	0.1159 (3)	−0.1627 (3)	0.7908 (2)	0.0191 (7)
O10T	0.1270 (3)	−0.2973 (3)	0.9531 (3)	0.0205 (7)
O11T	0.3865 (3)	−0.4278 (3)	0.9733 (2)	0.0187 (7)
O12T	0.5387 (3)	−0.3859 (3)	0.8116 (2)	0.0171 (6)
O13C	0.4145 (3)	0.3517 (3)	0.3921 (2)	0.0109 (6)
H13	0.4041	0.3617	0.3165	0.016*
O14C	0.3524 (3)	0.4486 (3)	0.5815 (2)	0.0108 (6)
H14	0.362 (6)	0.438 (6)	0.637 (5)	0.037 (19)*
O15C	0.3914 (3)	0.6196 (3)	0.4554 (2)	0.0108 (6)
H15	0.373 (6)	0.613 (6)	0.383 (4)	0.034 (16)*
O16B	0.6638 (3)	0.2881 (3)	0.3675 (2)	0.0133 (6)
H16	0.667 (10)	0.282 (10)	0.302 (6)	0.020*	0.50
O17B	0.8274 (3)	0.5774 (3)	0.5674 (2)	0.0124 (6)
O18B	0.3752 (3)	0.1933 (3)	0.5152 (2)	0.0127 (6)
O19T	0.8820 (3)	0.4577 (3)	0.3616 (2)	0.0184 (7)
O20T	0.8744 (3)	0.3341 (3)	0.5323 (3)	0.0200 (7)
O21T	0.6089 (3)	0.1094 (3)	0.5063 (2)	0.0170 (6)
O22T	0.4578 (3)	0.0957 (3)	0.3161 (2)	0.0164 (6)
O23T	0.1364 (3)	0.2370 (3)	0.5654 (2)	0.0166 (6)
O24T	0.1677 (3)	0.1714 (3)	0.3530 (2)	0.0185 (7)
O25W	0.8718 (3)	0.0732 (3)	0.5303 (3)	0.0214 (7)
H25A	0.8723	0.1635	0.5379	0.032*
H25B	0.7872	0.0314	0.5438	0.032*
O26W	0.8491 (3)	0.0647 (3)	0.7784 (3)	0.0246 (7)
H26A	0.8808	0.1035	0.8519	0.037*
H26B	0.8053	−0.0148	0.7763	0.037*
O27W	0.3571 (4)	0.1166 (4)	0.7136 (3)	0.0281 (8)
H27A	0.371 (6)	0.115 (6)	0.652 (5)	0.030 (16)*
H27B	0.338 (7)	0.180 (6)	0.731 (5)	0.04 (2)*
O28W	0.6801 (3)	0.4221 (3)	0.7521 (2)	0.0209 (7)
H28A	0.6207	0.4640	0.7924	0.031*
H28B	0.6894	0.3454	0.7781	0.031*
O29W	0.8744 (4)	0.5441 (4)	0.9819 (3)	0.0391 (10)
H29A	0.7856	0.5513	0.9906	0.059*
H29B	0.8879	0.4607	0.9902	0.059*
O30W	0.0205 (5)	0.3482 (5)	0.7820 (5)	0.0644 (15)
H30A	−0.0690	0.2835	0.7878	0.097*
H30B	0.0844	0.3584	0.8429	0.097*
O31W	0.3600 (3)	0.8232 (3)	1.2193 (2)	0.0221 (7)
O32W	0.3037 (3)	0.3652 (3)	0.7740 (3)	0.0252 (7)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cr1	0.0087 (5)	0.0105 (4)	0.0082 (4)	0.0018 (3)	0.0001 (3)	0.0010 (3)
Cr2	0.0080 (5)	0.0096 (4)	0.0082 (4)	0.0015 (3)	0.0003 (3)	0.0007 (3)
Mo1	0.0115 (2)	0.01436 (19)	0.01122 (17)	0.00437 (14)	0.00056 (13)	0.00140 (13)
Mo2	0.00988 (19)	0.01347 (19)	0.01121 (17)	0.00058 (14)	−0.00043 (13)	0.00162 (13)
Mo3	0.0131 (2)	0.01082 (18)	0.01012 (17)	0.00251 (14)	0.00102 (13)	0.00076 (13)
Mo4	0.00780 (19)	0.01214 (18)	0.01298 (18)	0.00238 (13)	0.00098 (13)	0.00221 (13)
Mo5	0.00980 (19)	0.00992 (18)	0.01067 (17)	0.00208 (13)	0.00022 (13)	0.00104 (13)
Mo6	0.00846 (19)	0.01080 (18)	0.01132 (17)	0.00041 (13)	0.00017 (13)	0.00179 (13)
K1	0.0185 (5)	0.0270 (5)	0.0173 (5)	0.0041 (4)	0.0008 (4)	0.0075 (4)
K2	0.0175 (5)	0.0319 (6)	0.0167 (5)	0.0009 (4)	0.0013 (4)	0.0035 (4)
O1C	0.0143 (16)	0.0148 (15)	0.0068 (14)	0.0045 (12)	0.0023 (11)	0.0014 (11)
O2C	0.0114 (15)	0.0156 (15)	0.0087 (14)	0.0019 (11)	0.0013 (11)	0.0038 (11)
O3C	0.0130 (15)	0.0124 (14)	0.0098 (14)	0.0008 (11)	0.0013 (11)	0.0024 (11)
O4B	0.0145 (16)	0.0179 (15)	0.0131 (14)	0.0029 (12)	0.0031 (11)	0.0017 (11)
O5B	0.0127 (16)	0.0165 (15)	0.0111 (13)	0.0040 (12)	0.0005 (12)	0.0008 (12)
O6B	0.0165 (16)	0.0145 (14)	0.0119 (13)	0.0022 (12)	−0.0008 (11)	0.0034 (11)
O7T	0.0160 (17)	0.0248 (17)	0.0209 (16)	0.0032 (13)	−0.0040 (13)	0.0062 (13)
O8T	0.0201 (18)	0.0229 (17)	0.0204 (16)	0.0079 (13)	0.0065 (13)	0.0009 (13)
O9T	0.0189 (17)	0.0219 (17)	0.0150 (15)	0.0034 (13)	−0.0040 (12)	0.0019 (12)
O10T	0.0171 (17)	0.0214 (17)	0.0226 (16)	0.0000 (13)	0.0026 (13)	0.0061 (13)
O11T	0.0181 (17)	0.0176 (16)	0.0216 (16)	0.0028 (13)	0.0036 (13)	0.0065 (12)
O12T	0.0198 (17)	0.0172 (15)	0.0150 (14)	0.0072 (13)	0.0020 (12)	0.0006 (12)
O13C	0.0092 (15)	0.0132 (14)	0.0099 (13)	0.0020 (11)	−0.0009 (11)	0.0022 (11)
O14C	0.0078 (15)	0.0148 (15)	0.0102 (14)	0.0016 (11)	0.0007 (11)	0.0041 (11)
O15C	0.0099 (15)	0.0129 (14)	0.0095 (13)	0.0022 (11)	−0.0009 (11)	0.0025 (11)
O16B	0.0139 (16)	0.0152 (15)	0.0104 (14)	0.0023 (12)	0.0029 (11)	0.0010 (11)
O17B	0.0113 (15)	0.0119 (14)	0.0134 (14)	0.0014 (11)	0.0000 (11)	0.0021 (11)
O18B	0.0108 (15)	0.0148 (14)	0.0137 (14)	0.0030 (11)	0.0023 (11)	0.0047 (11)
O19T	0.0133 (16)	0.0198 (16)	0.0214 (16)	−0.0004 (12)	0.0063 (12)	0.0028 (12)
O20T	0.0153 (17)	0.0164 (16)	0.0281 (17)	0.0058 (12)	−0.0032 (13)	0.0031 (13)
O21T	0.0133 (16)	0.0148 (15)	0.0239 (16)	0.0033 (12)	0.0005 (12)	0.0060 (12)
O22T	0.0156 (16)	0.0149 (15)	0.0170 (15)	0.0013 (12)	0.0005 (12)	−0.0007 (12)
O23T	0.0131 (16)	0.0179 (15)	0.0189 (15)	0.0002 (12)	0.0029 (12)	0.0059 (12)
O24T	0.0165 (17)	0.0191 (16)	0.0172 (15)	0.0005 (13)	−0.0050 (12)	0.0010 (12)
O25W	0.0184 (17)	0.0197 (16)	0.0269 (17)	0.0053 (13)	0.0005 (13)	0.0051 (13)
O26W	0.027 (2)	0.0262 (18)	0.0192 (16)	0.0025 (15)	0.0050 (14)	0.0022 (13)
O27W	0.041 (2)	0.032 (2)	0.0160 (18)	0.0117 (18)	0.0059 (15)	0.0101 (15)
O28W	0.0256 (19)	0.0207 (16)	0.0178 (15)	0.0073 (14)	0.0034 (13)	0.0037 (12)
O29W	0.040 (2)	0.040 (2)	0.042 (2)	0.0096 (19)	0.0100 (19)	0.0167 (18)
O30W	0.041 (3)	0.043 (3)	0.118 (5)	0.017 (2)	0.012 (3)	0.030 (3)
O31W	0.0300 (19)	0.0216 (17)	0.0133 (14)	−0.0004 (14)	0.0011 (13)	0.0051 (12)
O32W	0.027 (2)	0.0312 (19)	0.0158 (15)	0.0003 (15)	0.0022 (13)	0.0048 (14)

Geometric parameters (Å, º) top

Cr1—O1C	1.969 (3)	Mo6—O24T	1.707 (3)
Cr1—O2C	1.976 (3)	Mo6—O13C	2.310 (3)
Cr1—O3C	1.975 (3)	Mo6—O14C	2.302 (3)
Cr2—O13C	1.974 (3)	Mo6—O17Bⁱⁱ	1.917 (3)
Cr2—O14C	1.980 (3)	Mo6—O18B	1.965 (3)
Cr2—O15C	1.978 (3)	K1—O25Wⁱⁱⁱ	2.783 (3)
Cr1—O1Cⁱ	1.969 (3)	K1—O25W^iv	2.724 (3)
Cr1—O3Cⁱ	1.975 (3)	K1—O9T	2.812 (3)
Cr1—O2Cⁱ	1.976 (3)	K1—O26Wⁱⁱⁱ	2.839 (3)
Cr2—O13Cⁱⁱ	1.974 (3)	K1—O7T	2.833 (3)
Cr2—O15Cⁱⁱ	1.978 (3)	K1—O23T	2.869 (3)
Cr2—O14Cⁱⁱ	1.980 (3)	K1—O24T^v	2.949 (3)
Mo1—O8T	1.704 (3)	K1—O27W	3.004 (4)
Mo1—O7T	1.704 (3)	K1—H27B	3.03 (7)
Mo1—O1C	2.305 (3)	K2—O29W	2.773 (4)
Mo1—O2C	2.324 (3)	K2—O17B	2.773 (3)
Mo1—O4B	1.943 (3)	K2—O19T^vi	2.804 (3)
Mo1—O6Bⁱ	1.965 (3)	K2—O8T^vii	2.855 (3)
Mo2—O2C	2.295 (3)	K2—O28W	2.862 (4)
Mo2—O3C	2.283 (3)	K2—O30W^viii	2.895 (5)
Mo2—O4B	1.915 (3)	K2—O10T^ix	2.896 (3)
Mo2—O5B	1.986 (3)	K2—O9T^ix	3.081 (3)
Mo2—O10T	1.700 (3)	O1C—H1	0.73 (5)
Mo2—O9T	1.710 (3)	O2C—H2	0.72 (5)
Mo3—O11T	1.701 (3)	O3C—H3	0.86 (6)
Mo3—O12T	1.726 (3)	O5B—H5	0.71 (8)
Mo3—O1Cⁱ	2.324 (3)	O13C—H13	0.9800
Mo3—O3C	2.236 (3)	O14C—H14	0.73 (6)
Mo3—O5B	2.000 (3)	O15C—H15	0.91 (5)
Mo3—O6B	1.882 (3)	O16B—H16	0.83 (8)
Mo4—O19T	1.699 (3)	O25W—H25A	0.9700
Mo4—O20T	1.701 (3)	O25W—H25B	0.9700
Mo4—O16B	1.993 (3)	O26W—H26A	0.9666
Mo4—O17B	1.921 (3)	O26W—H26B	0.9064
Mo4—O14Cⁱⁱ	2.309 (3)	O27W—H27A	0.80 (5)
Mo4—O15Cⁱⁱ	2.275 (3)	O27W—H27B	0.75 (6)
Mo5—O21T	1.703 (3)	O28W—H28A	0.9600
Mo5—O22T	1.717 (3)	O28W—H28B	0.9600
Mo5—O13C	2.306 (3)	O29W—H29A	0.9600
Mo5—O15Cⁱⁱ	2.272 (3)	O29W—H29B	0.9600
Mo5—O16B	2.000 (3)	O30W—H30A	1.0930
Mo5—O18B	1.900 (3)	O30W—H30B	0.9600
Mo6—O23T	1.700 (3)

Mo1—O1C—Mo3ⁱ	91.44 (11)	O12T—Mo3—O1Cⁱ	91.94 (13)
Mo2—O2C—Mo1	92.13 (11)	O6B—Mo3—O1Cⁱ	72.69 (11)
Mo3—O3C—Mo2	97.78 (11)	O5B—Mo3—O1Cⁱ	80.51 (12)
Mo2—O4B—Mo1	119.10 (15)	O3C—Mo3—O1Cⁱ	70.39 (11)
Mo2—O5B—Mo3	117.37 (14)	O19T—Mo4—O20T	106.36 (16)
Mo3—O6B—Mo1ⁱ	118.93 (14)	O19T—Mo4—O17B	104.21 (14)
Mo5—O13C—Mo6	92.44 (10)	O20T—Mo4—O17B	98.14 (14)
Mo6—O14C—Mo4ⁱⁱ	91.62 (10)	O19T—Mo4—O16B	94.10 (14)
Mo5ⁱⁱ—O15C—Mo4ⁱⁱ	97.58 (11)	O20T—Mo4—O16B	100.09 (14)
Mo4—O16B—Mo5	117.88 (14)	O17B—Mo4—O16B	149.28 (12)
Mo6ⁱⁱ—O17B—Mo4	118.96 (14)	O19T—Mo4—O15Cⁱⁱ	156.72 (13)
Mo5—O18B—Mo6	119.15 (14)	O20T—Mo4—O15Cⁱⁱ	93.37 (13)
O1Cⁱ—Cr1—O1C	180.000 (1)	O17B—Mo4—O15Cⁱⁱ	84.60 (11)
O1Cⁱ—Cr1—O3C	83.63 (12)	O16B—Mo4—O15Cⁱⁱ	69.87 (11)
O1C—Cr1—O3C	96.37 (13)	O19T—Mo4—O14Cⁱⁱ	91.55 (13)
O1Cⁱ—Cr1—O3Cⁱ	96.37 (12)	O20T—Mo4—O14Cⁱⁱ	161.40 (14)
O1C—Cr1—O3Cⁱ	83.63 (13)	O17B—Mo4—O14Cⁱⁱ	72.02 (11)
O3C—Cr1—O3Cⁱ	180.000 (1)	O16B—Mo4—O14Cⁱⁱ	83.20 (11)
O1Cⁱ—Cr1—O2Cⁱ	83.71 (12)	O15Cⁱⁱ—Mo4—O14Cⁱⁱ	70.41 (10)
O1C—Cr1—O2Cⁱ	96.29 (12)	O21T—Mo5—O22T	106.71 (15)
O3C—Cr1—O2Cⁱ	96.13 (12)	O21T—Mo5—O18B	99.36 (14)
O3Cⁱ—Cr1—O2Cⁱ	83.87 (12)	O22T—Mo5—O18B	102.69 (14)
O1Cⁱ—Cr1—O2C	96.29 (12)	O21T—Mo5—O16B	100.02 (14)
O1C—Cr1—O2C	83.71 (12)	O22T—Mo5—O16B	93.28 (13)
O3C—Cr1—O2C	83.87 (12)	O18B—Mo5—O16B	150.08 (12)
O3Cⁱ—Cr1—O2C	96.13 (12)	O21T—Mo5—O15Cⁱⁱ	92.90 (13)
O2Cⁱ—Cr1—O2C	180.000 (1)	O22T—Mo5—O15Cⁱⁱ	156.32 (12)
O13Cⁱⁱ—Cr2—O13C	180.000 (1)	O18B—Mo5—O15Cⁱⁱ	86.64 (12)
O13Cⁱⁱ—Cr2—O15Cⁱⁱ	96.38 (11)	O16B—Mo5—O15Cⁱⁱ	69.83 (11)
O13C—Cr2—O15Cⁱⁱ	83.62 (11)	O21T—Mo5—O13C	161.40 (12)
O13Cⁱⁱ—Cr2—O15C	83.62 (11)	O22T—Mo5—O13C	91.56 (12)
O13C—Cr2—O15C	96.38 (11)	O18B—Mo5—O13C	72.53 (11)
O15Cⁱⁱ—Cr2—O15C	180.000 (1)	O16B—Mo5—O13C	82.01 (11)
O13Cⁱⁱ—Cr2—O14Cⁱⁱ	83.40 (12)	O15Cⁱⁱ—Mo5—O13C	70.28 (10)
O13C—Cr2—O14Cⁱⁱ	96.60 (12)	O23T—Mo6—O24T	106.31 (15)
O15Cⁱⁱ—Cr2—O14Cⁱⁱ	83.76 (12)	O23T—Mo6—O17Bⁱⁱ	102.60 (14)
O15C—Cr2—O14Cⁱⁱ	96.24 (12)	O24T—Mo6—O17Bⁱⁱ	98.23 (14)
O13Cⁱⁱ—Cr2—O14C	96.60 (12)	O23T—Mo6—O18B	95.69 (13)
O13C—Cr2—O14C	83.40 (12)	O24T—Mo6—O18B	100.28 (14)
O15Cⁱⁱ—Cr2—O14C	96.24 (12)	O17Bⁱⁱ—Mo6—O18B	149.09 (12)
O15C—Cr2—O14C	83.76 (12)	O23T—Mo6—O14C	92.67 (13)
O14Cⁱⁱ—Cr2—O14C	180.00 (11)	O24T—Mo6—O14C	160.38 (13)
O8T—Mo1—O7T	106.52 (16)	O17Bⁱⁱ—Mo6—O14C	72.23 (11)
O8T—Mo1—O4B	99.27 (14)	O18B—Mo6—O14C	82.33 (11)
O7T—Mo1—O4B	100.29 (14)	O23T—Mo6—O13C	158.86 (13)
O8T—Mo1—O6Bⁱ	101.48 (14)	O24T—Mo6—O13C	92.69 (13)
O7T—Mo1—O6Bⁱ	96.72 (14)	O17Bⁱⁱ—Mo6—O13C	83.28 (11)
O4B—Mo1—O6Bⁱ	148.09 (13)	O18B—Mo6—O13C	71.36 (11)
O8T—Mo1—O1C	91.76 (13)	O14C—Mo6—O13C	69.54 (10)
O7T—Mo1—O1C	160.24 (14)	O25Wⁱⁱⁱ—K1—O25W^iv	76.51 (11)
O4B—Mo1—O1C	83.67 (12)	O25Wⁱⁱⁱ—K1—O9T	139.33 (10)
O6Bⁱ—Mo1—O1C	71.78 (11)	O9T—K1—O26Wⁱⁱⁱ	90.95 (10)
O8T—Mo1—O2C	159.40 (13)	O25Wⁱⁱⁱ—K1—O7T	123.85 (10)
O7T—Mo1—O2C	93.41 (14)	O25Wⁱⁱⁱ—K1—O23T	64.16 (10)
O4B—Mo1—O2C	71.45 (11)	O25Wⁱⁱⁱ—K1—O24T^v	68.54 (9)
O6Bⁱ—Mo1—O2C	80.81 (12)	O25Wⁱⁱⁱ—K1—O27W	134.42 (10)
O1C—Mo1—O2C	69.32 (10)	O29W—K2—O17B	146.21 (11)
O10T—Mo2—O9T	105.43 (15)	O29W—K2—O19T^vi	138.11 (12)
O10T—Mo2—O4B	98.82 (14)	O29W—K2—O8T^vii	67.46 (11)
O9T—Mo2—O4B	104.08 (14)	O29W—K2—O28W	73.30 (11)
O10T—Mo2—O5B	98.71 (14)	O29W—K2—O30W^viii	79.63 (15)
O9T—Mo2—O5B	95.24 (14)	O29W—K2—O10T^ix	63.81 (11)
O4B—Mo2—O5B	149.31 (13)	O29W—K2—O9T^ix	110.84 (11)
O10T—Mo2—O3C	93.19 (13)	O17B—K2—O9T^ix	94.22 (9)
O9T—Mo2—O3C	157.66 (13)	Cr1—O1C—Mo1	103.93 (12)
O4B—Mo2—O3C	84.68 (12)	Cr1—O1C—Mo3ⁱ	101.43 (13)
O5B—Mo2—O3C	69.36 (11)	Cr1—O2C—Mo2	102.60 (13)
O10T—Mo2—O2C	161.85 (13)	Cr1—O2C—Mo1	103.03 (12)
O9T—Mo2—O2C	92.30 (13)	Cr1—O3C—Mo3	104.36 (13)
O4B—Mo2—O2C	72.58 (12)	Cr1—O3C—Mo2	103.07 (12)
O5B—Mo2—O2C	83.17 (12)	Cr2—O13C—Mo5	102.45 (11)
O3C—Mo2—O2C	70.45 (10)	Cr2—O13C—Mo6	103.46 (12)
O11T—Mo3—O12T	106.23 (15)	Cr2—O14C—Mo6	103.57 (12)
O11T—Mo3—O6B	100.54 (14)	Cr2—O14C—Mo4ⁱⁱ	102.28 (12)
O12T—Mo3—O6B	102.62 (14)	Cr2—O15C—Mo5ⁱⁱ	103.53 (12)
O11T—Mo3—O5B	100.34 (14)	Cr2—O15C—Mo4ⁱⁱ	103.53 (12)
O12T—Mo3—O5B	92.81 (13)	H25A—O25W—H25B	109.0
O6B—Mo3—O5B	149.31 (12)	H26A—O26W—H26B	109.9
O11T—Mo3—O3C	92.55 (13)	H27A—O27W—H27B	105 (7)
O12T—Mo3—O3C	156.84 (12)	H28A—O28W—H28B	109.5
O6B—Mo3—O3C	86.70 (12)	H29A—O29W—H29B	109.5
O5B—Mo3—O3C	70.13 (11)	H30A—O30W—H30B	113.4
O11T—Mo3—O1Cⁱ	161.70 (13)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1C—H1···O22T^x	0.73 (5)	2.10 (5)	2.796 (4)	160 (5)
O5B—H5···O16B^iv	0.71 (8)	1.79 (8)	2.475 (4)	163 (13)
O13C—H13···O12T^iv	0.98	1.81	2.733 (4)	155
O16B—H16···O5B^iv	0.83 (8)	1.65 (8)	2.475 (4)	175 (11)
O25W—H25B···O21T	0.97	2.22	2.844 (4)	121
O25W—H25A···O20T	0.97	1.86	2.828 (4)	172
O26W—H26A···O4Bⁱ	0.97	2.07	2.755 (4)	127
O27W—H27B···O32W	0.75 (6)	2.10 (6)	2.842 (6)	174 (7)
O28W—H28B···O31W^vii	0.96	1.83	2.719 (5)	153
O28W—H28A···O12T^xi	0.96	1.95	2.789 (4)	144
O29W—H29A···O11Tⁱ	0.96	2.19	2.957 (5)	136
O29W—H29B···O29W^xii	0.96	2.50	2.968 (8)	110
O29W—H29B···O10Tⁱ	0.96	2.01	2.928 (5)	160
O30W—H30B···O32W	0.96	2.51	2.953 (6)	108
O30W—H30B···O7T	0.96	2.57	3.069 (6)	113

Symmetry codes: (i) −x+1, −y, −z+2; (iv) −x+1, −y, −z+1; (vii) −x+1, −y+1, −z+2; (x) x, y, z+1; (xi) x, y+1, z; (xii) −x+2, −y+1, −z+2.

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Dipotassium hepta­hydrogenhexa­molybdochromate(III) octa­hydrate, the first hepta­protonated Anderson-type polyoxometalate

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Key indicators

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Dipotassium heptahydrogenhexamolybdochromate(III) octahydrate, the first heptaprotonated Anderson-type polyoxometalate