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The title compound, K
2[H
7CrMo
6O
24]·8H
2O, contains an unexpectedly protonated polyanion, [H
7CrMo
6O
24]
2- in the B series Anderson-type heteropolyoxomolybdate. It was obtained by recrystallizing K
3[H
6CrMo
6O
24]·
nH
2O at pH 1.80. The asymmetric unit contains two crystallographically independent polyanions that have
Ci (
) symmetry. Six O atoms of the central CrO
6 octahedron and one atom of an edge-shared MoO
6 octahedron are protonated.
Supporting information
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
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 |
Mr = 1241.02 | F(000) = 1186 |
Triclinic, P1 | Dx = 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 | Rint = 0.025 |
Detector resolution: 10.00 pixels mm-1 | θmax = 26.0°, θmin = 1.9° |
φ and ω scans | h = −12→12 |
Absorption correction: multi-scan (SADABS; Sheldrick, 1999) | k = −13→13 |
Tmin = 0.380, Tmax = 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(Fo2) + (0.0228P)2 + 4.6144P] where P = (Fo2 + 2Fc2)/3 |
S = 1.19 | (Δ/σ)max < 0.001 |
5360 reflections | Δρmax = 0.85 e Å−3 |
408 parameters | Δρmin = −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 | Uiso*/Ueq | 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—O25Wiv | 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—O24Tv | 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—O19Tvi | 2.804 (3) |
Mo1—O6Bi | 1.965 (3) | K2—O8Tvii | 2.855 (3) |
Mo2—O2C | 2.295 (3) | K2—O28W | 2.862 (4) |
Mo2—O3C | 2.283 (3) | K2—O30Wviii | 2.895 (5) |
Mo2—O4B | 1.915 (3) | K2—O10Tix | 2.896 (3) |
Mo2—O5B | 1.986 (3) | K2—O9Tix | 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—O25Wiv | 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—O24Tv | 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—O19Tvi | 138.11 (12) |
O10T—Mo2—O4B | 98.82 (14) | O29W—K2—O8Tvii | 67.46 (11) |
O9T—Mo2—O4B | 104.08 (14) | O29W—K2—O28W | 73.30 (11) |
O10T—Mo2—O5B | 98.71 (14) | O29W—K2—O30Wviii | 79.63 (15) |
O9T—Mo2—O5B | 95.24 (14) | O29W—K2—O10Tix | 63.81 (11) |
O4B—Mo2—O5B | 149.31 (13) | O29W—K2—O9Tix | 110.84 (11) |
O10T—Mo2—O3C | 93.19 (13) | O17B—K2—O9Tix | 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···O22Tx | 0.73 (5) | 2.10 (5) | 2.796 (4) | 160 (5) |
O5B—H5···O16Biv | 0.71 (8) | 1.79 (8) | 2.475 (4) | 163 (13) |
O13C—H13···O12Tiv | 0.98 | 1.81 | 2.733 (4) | 155 |
O16B—H16···O5Biv | 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···O31Wvii | 0.96 | 1.83 | 2.719 (5) | 153 |
O28W—H28A···O12Txi | 0.96 | 1.95 | 2.789 (4) | 144 |
O29W—H29A···O11Ti | 0.96 | 2.19 | 2.957 (5) | 136 |
O29W—H29B···O29Wxii | 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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