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The crystal and molecular structure of dipotassium di-μ-oxo-bis[aqua(oxalato-O1,O2)oxomolybdenum(III)] trihydrate, K2­[Mo2O4(C2O4)2(H2O)2]·3H2O, has been determined from X-ray diffraction data. In the dimeric anion, which has approximate twofold symmetry, each Mo atom is in a distorted octahedral coordination, being bonded to one terminal oxo-O atom, two bridging O atoms, two O atoms from the oxalato ligand and one from the water mol­ecule. Bond lengths trans to the multiple-bonded terminal oxo ligand are larger than those in the cis position, confirming the trans influence as a generally valid rule.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100002547/av1030sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100002547/av1030Isup2.hkl
Contains datablock I

CCDC reference: 146032

Computing details top

Data collection: STADI4 (Stoe & Cie, 1996); cell refinement: STADI4; data reduction: X-RED (Stoe & Cie, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLUTON (Spek, 1982) and ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

dipotassium di-µ-oxo-bis[aqua(oxalato-O1,O2)oxomolybdenum(III)] trihydrate top
Crystal data top
K2[Mo2O4(C2O4)2(H2O)2]·3H2OZ = 8
Mr = 600.20F(000) = 2336
Triclinic, P1Dx = 2.523 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71069 Å
a = 12.2683 (10) ÅCell parameters from 30 reflections
b = 15.0622 (17) Åθ = 8–17°
c = 18.2824 (17) ŵ = 2.20 mm1
α = 81.818 (9)°T = 293 K
β = 71.050 (7)°Prism, red
γ = 85.001 (9)°0.30 × 0.27 × 0.25 mm
V = 3159.7 (5) Å3
Data collection top
Philips PW1100 updated by Stoe
diffractometer
θmax = 30.1°, θmin = 2.3°
Radiation source: fine-focus sealed tubeh = 1617
Graphite monochromatork = 2021
ω/θ scansl = 025
18345 measured reflections3 standard reflections every 90 min
18254 independent reflections intensity decay: 24.2%
7507 reflections with I > 2σ(I)
Refinement top
Refinement on F2Primary atom site location: heavy-atom method
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.049Hydrogen site location: difference Fourier map
wR(F2) = 0.106H-atom parameters not refined
S = 0.93Calculated w = 1/[σ2(Fo2) + (0.065P)2]
where P = (Fo2 + 2Fc2)/3
18254 reflections(Δ/σ)max = 0.003
907 parametersΔρmax = 1.51 e Å3
0 restraintsΔρmin = 1.14 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Mo110.64581 (5)0.36223 (4)0.56566 (4)0.02044 (16)
Mo120.62107 (5)0.36345 (4)0.43129 (4)0.02111 (16)
O110.6331 (4)0.4726 (3)0.5737 (3)0.0323 (13)
O120.6171 (4)0.4735 (3)0.4010 (3)0.0326 (13)
O130.6479 (4)0.2133 (3)0.5969 (3)0.0286 (12)
O140.6385 (4)0.2169 (3)0.4263 (3)0.0303 (13)
O150.5452 (4)0.3336 (4)0.6866 (3)0.0270 (12)
O160.7263 (4)0.3420 (4)0.3152 (3)0.0303 (13)
O170.7556 (4)0.3432 (3)0.4662 (3)0.0264 (13)
O180.5133 (4)0.3401 (3)0.5344 (3)0.0248 (12)
O190.5773 (5)0.1004 (4)0.6888 (3)0.0420 (15)
O1100.4993 (4)0.2306 (4)0.7913 (3)0.0314 (13)
O1110.8072 (4)0.2416 (4)0.2322 (3)0.0360 (14)
O1120.7366 (5)0.1077 (4)0.3570 (3)0.0424 (15)
O1130.4832 (4)0.3465 (4)0.3871 (3)0.0292 (13)
H110.42500.35430.40360.035*
H120.49670.30630.35030.035*
O1140.7901 (4)0.3414 (4)0.6064 (3)0.0345 (14)
H130.78130.31430.65280.041*
H140.86160.35870.58260.041*
C110.5930 (6)0.1810 (5)0.6644 (4)0.0244 (16)
C120.5408 (6)0.2523 (5)0.7203 (4)0.0234 (18)
C130.7066 (6)0.1873 (5)0.3646 (5)0.0265 (17)
C140.7503 (6)0.2631 (6)0.2978 (4)0.0262 (18)
Mo210.14510 (5)0.36083 (4)0.56520 (4)0.01970 (16)
Mo220.12443 (5)0.36243 (4)0.42996 (4)0.01974 (15)
O210.1350 (4)0.4707 (3)0.5722 (3)0.0323 (13)
O220.1254 (4)0.4732 (3)0.3981 (3)0.0310 (13)
O230.1598 (4)0.2114 (3)0.5974 (3)0.0280 (12)
O240.1210 (4)0.2174 (3)0.4285 (3)0.0243 (11)
O250.0402 (4)0.3304 (3)0.6839 (3)0.0259 (12)
O260.2332 (4)0.3312 (3)0.3170 (3)0.0267 (12)
O270.2572 (4)0.3383 (3)0.4661 (3)0.0228 (11)
O280.0133 (4)0.3417 (3)0.5322 (3)0.0239 (12)
O290.1169 (4)0.1009 (3)0.6968 (3)0.0308 (12)
O2100.0008 (4)0.2296 (3)0.7911 (3)0.0285 (13)
O2110.1885 (5)0.1015 (4)0.3617 (3)0.0377 (14)
O2120.2996 (4)0.2273 (4)0.2365 (3)0.0313 (13)
O2130.0155 (4)0.3567 (3)0.3815 (3)0.0283 (13)
H210.08050.35900.40300.034*
H220.00240.30530.35200.034*
O2140.2860 (4)0.3475 (4)0.6116 (3)0.0336 (14)
H230.27540.30860.65540.040*
H240.35370.36110.58010.040*
C210.1121 (6)0.1802 (5)0.6688 (4)0.0225 (16)
C220.0444 (6)0.2523 (5)0.7199 (5)0.0243 (18)
C230.1815 (7)0.1816 (5)0.3688 (4)0.0255 (17)
C240.2456 (6)0.2511 (5)0.3010 (5)0.0267 (18)
Mo310.56900 (5)0.35719 (4)1.06688 (4)0.02159 (16)
Mo320.72350 (5)0.35992 (4)0.93278 (4)0.02157 (16)
O310.5482 (4)0.4672 (4)1.0751 (3)0.0339 (14)
O320.7311 (4)0.4701 (4)0.9032 (3)0.0324 (13)
O330.5617 (4)0.2076 (3)1.0972 (3)0.0305 (13)
O340.7506 (4)0.2128 (3)0.9289 (3)0.0301 (13)
O350.5601 (4)0.3273 (4)1.1871 (3)0.0290 (13)
O360.7364 (4)0.3353 (4)0.8182 (3)0.0309 (13)
O370.7358 (4)0.3372 (3)1.0357 (3)0.0262 (12)
O380.5604 (4)0.3386 (3)0.9659 (3)0.0253 (12)
O390.5393 (5)0.0955 (4)1.1947 (3)0.0399 (14)
O3100.5263 (5)0.2252 (4)1.2912 (3)0.0319 (13)
O3110.7741 (4)0.2360 (4)0.7324 (3)0.0319 (13)
O3120.7740 (5)0.1029 (4)0.8558 (3)0.0431 (15)
O3130.9104 (4)0.3479 (4)0.8863 (3)0.0355 (14)
H310.91880.33170.93640.043*
H320.94320.42600.85930.043*
O3140.3881 (4)0.3384 (4)1.1100 (3)0.0360 (15)
H330.32990.34521.09390.043*
H340.36000.31031.16090.043*
C310.5488 (6)0.1751 (5)1.1692 (5)0.0293 (19)
C320.5450 (6)0.2486 (5)1.2215 (4)0.0231 (17)
C330.7610 (6)0.1805 (6)0.8647 (4)0.0255 (18)
C340.7568 (6)0.2554 (5)0.7991 (5)0.0247 (18)
Mo411.07590 (5)0.36453 (4)1.06078 (4)0.02022 (15)
Mo421.23165 (5)0.36446 (4)0.92694 (4)0.02041 (15)
O411.0559 (4)0.4752 (3)1.0669 (3)0.0303 (13)
O421.2380 (4)0.4752 (3)0.8945 (3)0.0292 (12)
O431.0781 (5)0.2151 (3)1.0911 (3)0.0308 (13)
O441.2559 (4)0.2168 (3)0.9279 (3)0.0271 (12)
O451.0650 (4)0.3363 (3)1.1824 (3)0.0243 (12)
O461.2491 (4)0.3355 (3)0.8112 (3)0.0274 (12)
O471.2435 (4)0.3461 (3)1.0308 (3)0.0221 (11)
O481.0680 (4)0.3424 (3)0.9607 (3)0.0250 (12)
O491.0795 (5)0.1033 (4)1.1872 (3)0.0393 (14)
O4101.0211 (4)0.2347 (4)1.2870 (3)0.0295 (13)
O4111.2459 (6)0.1038 (4)0.8631 (3)0.0473 (16)
O4121.2813 (5)0.2295 (4)0.7318 (3)0.0364 (14)
O4131.4165 (4)0.3518 (4)0.8844 (3)0.0297 (13)
H411.43640.32030.84980.036*
H421.44060.35460.91830.036*
O4140.8970 (5)0.3430 (4)1.1023 (3)0.0352 (16)
H430.8730.3221.1430.042*
H440.8580.3571.0760.042*
C411.0711 (6)0.1827 (5)1.1602 (4)0.0211 (15)
C421.0505 (6)0.2566 (5)1.2158 (4)0.0258 (18)
C431.2545 (7)0.1834 (6)0.8691 (5)0.032 (2)
C441.2616 (6)0.2545 (5)0.7968 (5)0.0251 (19)
K10.9118 (2)0.49703 (16)0.75164 (13)0.0592 (6)
K20.5704 (2)0.49875 (16)0.25073 (14)0.0620 (7)
K30.03505 (14)0.05368 (12)0.65508 (11)0.0378 (4)
K40.70006 (18)0.03065 (14)0.78047 (12)0.0494 (5)
K50.34568 (17)0.03380 (14)0.71462 (12)0.0476 (5)
K60.00855 (18)0.05198 (14)0.85836 (13)0.0525 (5)
K70.6658 (2)0.05955 (16)0.52713 (15)0.0827 (9)
K80.3486 (4)0.0496 (2)0.9773 (3)0.174 (2)
OW10.8501 (6)0.0525 (4)0.4737 (3)0.0540 (18)
H1A0.85650.08290.41500.081*
H1B0.90260.08810.50240.081*
OW21.1260 (7)0.4977 (5)0.7505 (5)0.079 (2)
H2A1.18280.45560.72920.119*
H2B1.16350.54300.76910.119*
OW30.8688 (5)0.0832 (4)0.6621 (4)0.0609 (19)
H3A0.81760.12710.70700.091*
H3B0.83930.01100.64590.091*
OW40.3562 (7)0.4953 (6)0.2460 (5)0.089 (3)
H4A0.31660.44920.29970.133*
H4B0.40500.55750.25210.133*
OW50.1130 (5)0.1575 (4)0.4920 (4)0.0580 (19)
H5A0.19640.18440.47000.087*
H5B0.13580.10480.55420.087*
OW60.4100 (5)0.1491 (5)0.5552 (4)0.0587 (18)
H6A0.33450.17230.57000.088*
H6B0.45900.20210.55940.088*
OW70.3686 (7)0.1411 (5)1.0538 (4)0.072 (2)
H7A0.43830.14510.99850.108*
H7B0.29500.16731.03940.108*
OW80.1824 (6)0.0814 (5)0.8307 (5)0.090 (3)
H8A0.14510.11640.87590.135*
H8B0.22430.02160.83580.135*
OW90.5367 (7)0.0753 (5)0.5983 (5)0.095 (3)
H9A0.54090.14940.61090.142*
H9B0.54060.04200.64630.142*
OW100.5078 (7)0.0664 (6)0.8922 (7)0.139 (5)
H10A0.53190.10250.84520.209*
H10B0.41730.08180.92460.209*
OW110.9308 (9)0.1534 (6)1.0016 (6)0.116 (4)
H11A0.95350.12361.05980.173*
H11B0.93250.10590.96120.173*
OW120.1459 (13)0.0442 (6)0.9793 (6)0.173 (6)
H12A0.15800.09221.02600.259*
H12B0.09560.08980.92490.259*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo110.0155 (3)0.0225 (4)0.0224 (4)0.0014 (3)0.0032 (3)0.0060 (3)
Mo120.0162 (3)0.0240 (4)0.0222 (4)0.0015 (3)0.0039 (3)0.0044 (3)
O110.032 (3)0.034 (3)0.034 (3)0.000 (3)0.009 (2)0.017 (3)
O120.027 (3)0.029 (3)0.035 (3)0.005 (2)0.004 (2)0.002 (3)
O130.029 (3)0.027 (3)0.024 (3)0.002 (2)0.001 (2)0.006 (2)
O140.033 (3)0.028 (3)0.029 (3)0.007 (2)0.004 (2)0.011 (2)
O150.023 (3)0.030 (3)0.025 (3)0.001 (2)0.003 (2)0.010 (2)
O160.023 (3)0.036 (3)0.028 (3)0.002 (2)0.000 (2)0.010 (3)
O170.017 (3)0.034 (3)0.025 (3)0.003 (2)0.000 (2)0.006 (2)
O180.011 (2)0.028 (3)0.035 (3)0.003 (2)0.005 (2)0.007 (2)
O190.047 (4)0.026 (3)0.048 (4)0.006 (3)0.008 (3)0.000 (3)
O1100.027 (3)0.040 (3)0.026 (3)0.002 (3)0.005 (2)0.006 (3)
O1110.034 (3)0.045 (4)0.026 (3)0.000 (3)0.003 (2)0.011 (3)
O1120.040 (3)0.029 (3)0.052 (4)0.007 (3)0.006 (3)0.013 (3)
O1130.015 (2)0.046 (3)0.033 (3)0.003 (2)0.011 (2)0.020 (3)
O1140.020 (3)0.056 (4)0.028 (3)0.008 (3)0.011 (2)0.005 (3)
C110.023 (4)0.027 (4)0.024 (4)0.006 (3)0.005 (3)0.007 (3)
C120.017 (4)0.036 (5)0.015 (4)0.008 (3)0.002 (3)0.006 (4)
C130.016 (3)0.030 (4)0.032 (4)0.002 (3)0.004 (3)0.010 (3)
C140.013 (3)0.042 (5)0.023 (4)0.003 (3)0.002 (3)0.013 (4)
Mo210.0163 (3)0.0218 (4)0.0202 (3)0.0012 (3)0.0034 (3)0.0055 (3)
Mo220.0177 (3)0.0208 (4)0.0199 (3)0.0019 (3)0.0037 (3)0.0048 (3)
O210.032 (3)0.028 (3)0.035 (3)0.000 (2)0.007 (2)0.008 (3)
O220.034 (3)0.025 (3)0.036 (3)0.006 (2)0.012 (2)0.001 (2)
O230.037 (3)0.026 (3)0.021 (3)0.001 (2)0.008 (2)0.004 (2)
O240.025 (3)0.023 (3)0.020 (3)0.003 (2)0.000 (2)0.003 (2)
O250.030 (3)0.022 (3)0.022 (3)0.001 (2)0.003 (2)0.007 (2)
O260.029 (3)0.024 (3)0.026 (3)0.007 (2)0.004 (2)0.005 (2)
O270.014 (2)0.029 (3)0.026 (3)0.001 (2)0.004 (2)0.009 (2)
O280.017 (3)0.031 (3)0.026 (3)0.001 (2)0.008 (2)0.010 (2)
O290.034 (3)0.024 (3)0.034 (3)0.001 (2)0.010 (2)0.001 (2)
O2100.031 (3)0.031 (3)0.018 (3)0.001 (2)0.001 (2)0.004 (2)
O2110.050 (4)0.025 (3)0.035 (3)0.000 (3)0.008 (3)0.010 (2)
O2120.028 (3)0.036 (3)0.026 (3)0.002 (2)0.003 (2)0.005 (3)
O2130.023 (3)0.026 (3)0.035 (3)0.005 (2)0.006 (2)0.010 (2)
O2140.016 (3)0.045 (3)0.039 (3)0.007 (2)0.010 (2)0.002 (3)
C210.022 (3)0.023 (4)0.024 (4)0.000 (3)0.009 (3)0.004 (3)
C220.020 (4)0.022 (4)0.034 (5)0.005 (3)0.010 (3)0.011 (4)
C230.029 (4)0.027 (4)0.021 (4)0.004 (3)0.012 (3)0.004 (3)
C240.022 (4)0.031 (4)0.027 (4)0.003 (3)0.009 (3)0.006 (4)
Mo310.0188 (3)0.0269 (4)0.0212 (4)0.0019 (3)0.0083 (3)0.0045 (3)
Mo320.0188 (3)0.0265 (4)0.0215 (4)0.0003 (3)0.0077 (3)0.0068 (3)
O310.034 (3)0.030 (3)0.037 (3)0.001 (3)0.010 (3)0.007 (3)
O320.029 (3)0.036 (3)0.029 (3)0.005 (2)0.006 (2)0.000 (3)
O330.033 (3)0.026 (3)0.032 (3)0.002 (2)0.009 (2)0.007 (2)
O340.032 (3)0.027 (3)0.031 (3)0.005 (2)0.014 (3)0.001 (3)
O350.037 (3)0.030 (3)0.023 (3)0.002 (2)0.009 (2)0.010 (2)
O360.028 (3)0.036 (3)0.027 (3)0.003 (2)0.010 (2)0.003 (3)
O370.020 (3)0.035 (3)0.023 (3)0.001 (2)0.006 (2)0.007 (2)
O380.023 (3)0.037 (3)0.021 (3)0.001 (2)0.011 (2)0.009 (2)
O390.051 (4)0.030 (3)0.042 (3)0.003 (3)0.019 (3)0.003 (3)
O3100.043 (3)0.035 (3)0.020 (3)0.005 (3)0.012 (2)0.004 (2)
O3110.038 (3)0.043 (3)0.020 (3)0.009 (3)0.012 (2)0.020 (3)
O3120.053 (4)0.024 (3)0.048 (4)0.003 (3)0.009 (3)0.008 (3)
O3130.027 (3)0.043 (4)0.036 (3)0.003 (3)0.008 (3)0.008 (3)
O3140.017 (3)0.061 (4)0.028 (3)0.007 (3)0.009 (2)0.006 (3)
C310.023 (4)0.025 (4)0.035 (5)0.005 (3)0.001 (3)0.002 (4)
C320.015 (3)0.032 (4)0.027 (4)0.003 (3)0.010 (3)0.010 (4)
C330.020 (4)0.034 (5)0.024 (4)0.008 (3)0.005 (3)0.006 (4)
C340.021 (4)0.029 (5)0.028 (5)0.011 (3)0.014 (3)0.009 (4)
Mo410.0192 (3)0.0233 (4)0.0203 (3)0.0006 (3)0.0087 (3)0.0046 (3)
Mo420.0196 (3)0.0232 (4)0.0200 (3)0.0002 (3)0.0081 (3)0.0041 (3)
O410.027 (3)0.028 (3)0.039 (3)0.005 (2)0.013 (2)0.011 (3)
O420.035 (3)0.019 (3)0.037 (3)0.004 (2)0.014 (2)0.003 (2)
O430.050 (3)0.024 (3)0.022 (3)0.004 (2)0.014 (2)0.007 (2)
O440.035 (3)0.022 (3)0.026 (3)0.003 (2)0.012 (2)0.007 (2)
O450.030 (3)0.023 (3)0.024 (3)0.001 (2)0.014 (2)0.004 (2)
O460.041 (3)0.025 (3)0.017 (3)0.004 (2)0.009 (2)0.006 (2)
O470.020 (2)0.034 (3)0.017 (3)0.001 (2)0.008 (2)0.010 (2)
O480.020 (3)0.033 (3)0.027 (3)0.002 (2)0.014 (2)0.007 (2)
O490.055 (4)0.027 (3)0.038 (3)0.003 (3)0.019 (3)0.002 (3)
O4100.033 (3)0.036 (3)0.022 (3)0.003 (2)0.011 (2)0.006 (2)
O4110.077 (5)0.028 (3)0.040 (4)0.011 (3)0.020 (3)0.006 (3)
O4120.042 (3)0.046 (4)0.027 (3)0.006 (3)0.015 (3)0.011 (3)
O4130.019 (3)0.048 (3)0.031 (3)0.001 (2)0.011 (2)0.026 (3)
O4140.021 (3)0.058 (4)0.028 (3)0.005 (3)0.013 (2)0.006 (3)
C410.018 (3)0.029 (4)0.015 (3)0.003 (3)0.003 (3)0.010 (3)
C420.027 (4)0.029 (4)0.020 (4)0.001 (3)0.005 (3)0.003 (3)
C430.031 (4)0.029 (5)0.030 (5)0.001 (4)0.000 (4)0.010 (4)
C440.016 (4)0.034 (5)0.028 (5)0.007 (3)0.008 (3)0.008 (4)
K10.0679 (15)0.0556 (15)0.0459 (13)0.0074 (12)0.0130 (11)0.0115 (11)
K20.0819 (17)0.0491 (14)0.0478 (13)0.0064 (12)0.0144 (12)0.0047 (11)
K30.0321 (9)0.0302 (9)0.0449 (11)0.0019 (7)0.0060 (8)0.0014 (8)
K40.0546 (12)0.0398 (11)0.0539 (13)0.0022 (9)0.0149 (10)0.0140 (10)
K50.0437 (11)0.0440 (12)0.0543 (13)0.0025 (9)0.0135 (9)0.0075 (10)
K60.0489 (12)0.0412 (11)0.0569 (14)0.0016 (9)0.0072 (10)0.0026 (10)
K70.101 (2)0.0383 (13)0.0671 (16)0.0098 (13)0.0332 (14)0.0096 (12)
K80.157 (3)0.060 (2)0.193 (4)0.019 (2)0.102 (3)0.013 (2)
OW10.092 (5)0.032 (4)0.035 (4)0.007 (3)0.023 (3)0.005 (3)
OW20.084 (6)0.056 (5)0.107 (6)0.001 (4)0.041 (5)0.015 (4)
OW30.054 (4)0.048 (4)0.089 (5)0.009 (3)0.026 (4)0.031 (4)
OW40.095 (6)0.072 (6)0.089 (6)0.018 (5)0.029 (5)0.029 (5)
OW50.038 (3)0.043 (4)0.090 (5)0.001 (3)0.010 (3)0.025 (4)
OW60.045 (4)0.063 (5)0.059 (5)0.004 (3)0.003 (3)0.017 (4)
OW70.086 (6)0.063 (5)0.083 (6)0.000 (4)0.047 (5)0.010 (4)
OW80.054 (5)0.054 (5)0.165 (9)0.007 (4)0.021 (5)0.052 (5)
OW90.082 (6)0.060 (5)0.133 (8)0.032 (5)0.026 (5)0.018 (5)
OW100.058 (5)0.094 (7)0.213 (11)0.008 (5)0.019 (6)0.098 (7)
OW110.172 (10)0.075 (6)0.137 (9)0.022 (6)0.101 (8)0.027 (6)
OW120.313 (17)0.059 (7)0.096 (8)0.066 (9)0.016 (9)0.007 (6)
Geometric parameters (Å, º) top
Mo11—O111.679 (5)O33—C311.301 (9)
Mo11—O171.922 (5)O34—C331.298 (9)
Mo11—O181.958 (4)O35—C321.259 (9)
Mo11—O1142.117 (5)O36—C341.282 (9)
Mo11—O152.155 (5)O39—C311.225 (9)
Mo11—O132.235 (5)O310—C321.223 (8)
Mo11—Mo122.5686 (10)O311—C341.241 (8)
Mo12—O121.674 (5)O312—C331.192 (9)
Mo12—O181.924 (5)O313—H310.951
Mo12—O171.941 (5)O313—H321.255
Mo12—O1132.145 (4)O314—H330.850
Mo12—O162.148 (5)O314—H340.932
Mo12—O142.212 (5)C31—C321.551 (10)
O13—C111.248 (8)C33—C341.537 (10)
O14—C131.278 (8)Mo41—O411.678 (5)
O15—C121.286 (9)Mo41—O481.939 (5)
O16—C141.259 (9)Mo41—O471.953 (5)
O19—C111.241 (9)Mo41—O4142.115 (5)
O110—C121.237 (8)Mo41—O452.166 (5)
O111—C141.248 (8)Mo41—O432.241 (5)
O112—C131.236 (9)Mo41—Mo422.5695 (10)
O113—H110.686Mo42—O421.688 (5)
O113—H120.935Mo42—O471.930 (4)
O114—H130.864Mo42—O481.943 (4)
O114—H140.886Mo42—O4132.146 (5)
C11—C121.541 (10)Mo42—O462.160 (5)
C13—O1121.236 (9)Mo42—O442.217 (5)
C13—C141.539 (10)O43—C411.266 (8)
Mo21—O211.669 (5)O44—C431.254 (9)
Mo21—O271.940 (5)O45—C421.266 (8)
Mo21—O281.955 (4)O46—C441.271 (9)
Mo21—O252.140 (5)O49—C411.236 (8)
Mo21—O2142.142 (5)O410—C421.236 (8)
Mo21—O232.250 (5)O411—C431.235 (9)
Mo21—Mo222.5627 (9)O412—C441.240 (8)
Mo22—O221.686 (5)O413—H410.806
Mo22—O281.924 (5)O413—H420.775
Mo22—O271.936 (4)O414—H430.75
Mo22—O262.155 (5)O414—H440.78
Mo22—O2132.185 (5)C41—C421.562 (10)
Mo22—O242.192 (5)C42—O4101.236 (8)
O23—C211.282 (8)C43—C441.563 (11)
O24—C231.267 (9)C44—C431.563 (11)
O25—C221.270 (8)OW1—H1A1.203
O26—C241.266 (9)OW1—H1B1.028
O29—C211.235 (8)OW2—H2A0.925
O210—C221.247 (8)OW2—H2B1.008
O211—C231.225 (9)OW3—H3A1.120
O212—C241.237 (9)OW3—H3B1.277
O213—H210.766OW4—H4A1.112
O213—H220.979OW4—H4B1.193
O214—H230.902OW5—H5A1.233
O214—H240.866OW5—H5B1.256
C21—C221.540 (10)OW6—H6A0.928
C23—C241.546 (10)OW6—H6B1.066
Mo31—O311.675 (5)OW7—H7A1.090
Mo31—O381.944 (5)OW7—H7B1.050
Mo31—O371.946 (5)OW8—H8A0.918
Mo31—O3142.129 (5)OW8—H8B1.105
Mo31—O352.149 (5)OW9—H9A1.107
Mo31—O332.245 (5)OW9—H9B1.087
Mo31—Mo322.5635 (10)OW10—H10A0.923
Mo32—O321.672 (5)OW10—H10B1.097
Mo32—O371.916 (5)OW11—H11A1.202
Mo32—O381.935 (5)OW11—H11B1.094
Mo32—O362.132 (5)OW12—H12A1.017
Mo32—O3132.172 (5)OW12—H12B1.250
Mo32—O342.220 (5)
K1···OW22.622 (8)K4···O193.025 (7)
K1···O22i2.887 (6)K4···O3122.947 (7)
K1···O45ii3.008 (6)K5···OW82.885 (8)
K1···O253.040 (6)K5···O4112.901 (6)
K1···O213i3.057 (5)K5···O39v2.941 (6)
K1···OW4i3.265 (9)K5···OW63.072 (7)
K1···O26i3.341 (6)K5···OW93.131 (9)
K1···O322.933 (5)K5···O192.966 (7)
K1···O363.227 (6)K5···O1123.050 (7)
K1···O3133.083 (6)K5···O293.002 (6)
K2···OW42.663 (9)K5···O4123.018 (6)
K2···O42iii2.923 (6)K6···OW122.724 (10)
K2···O15i2.975 (6)K6···OW82.772 (8)
K2···O35iv3.008 (6)K6···O3122.926 (7)
K2···O413iii3.069 (6)K6···O49v2.986 (6)
K2···O46i3.309 (5)K6···OW113.060 (10)
K2···O31iv3.412 (6)K6···O4113.111 (7)
K2···O11i3.424 (6)K6···O292.834 (5)
K2···O122.951 (7)K6···O2102.789 (5)
K2···O163.242 (6)K7···OW92.607 (7)
K2···O1133.112 (5)K7···OW12.699 (7)
K3···OW12.693 (6)K7···O1122.945 (6)
K3···OW32.757 (7)K7···OW53.042 (7)
K3···O49v2.790 (6)K7···OW63.216 (7)
K3···O410vi2.839 (6)K7···O132.758 (6)
K3···O211vi3.015 (6)K7···O142.854 (6)
K3···OW5vi3.140 (7)K7···O192.935 (7)
K3···O1122.795 (6)K8···OW102.671 (8)
K3···0292.901 (6)K8···OW12viii2.690 (16)
K4···O2112.826 (6)K8···O33v2.866 (6)
K4···OW32.927 (7)K8···O34v2.902 (6)
K4···OW102.998 (11)K8···O312v2.958 (7)
K4···O2123.021 (6)K8···O39v3.147 (7)
K4···O49vii3.033 (6)K8···O4113.334 (8)
K4···O39v3.049 (6)K8···OW10v3.368 (13)
K4···OW7v3.132 (8)K8···OW73.429 (8)
O11—Mo11—O17108.7 (2)O31—Mo31—O3591.2 (2)
O11—Mo11—O18104.2 (2)O38—Mo31—O35158.8 (2)
O17—Mo11—O1893.6 (2)O37—Mo31—O3589.9 (2)
O11—Mo11—O11493.4 (2)O314—Mo31—O3584.5 (2)
O17—Mo11—O11484.8 (2)O31—Mo31—O33161.2 (2)
O18—Mo11—O114161.9 (2)O38—Mo31—O3386.8 (2)
O11—Mo11—O1590.5 (2)O37—Mo31—O3385.8 (2)
O17—Mo11—O15158.7 (2)O314—Mo31—O3377.8 (2)
O18—Mo11—O1590.31 (19)O35—Mo31—O3372.6 (2)
O114—Mo11—O1585.05 (19)O32—Mo32—O37109.2 (2)
O11—Mo11—O13161.3 (2)O32—Mo32—O38104.3 (2)
O17—Mo11—O1387.8 (2)O37—Mo32—O3894.8 (2)
O18—Mo11—O1382.8 (2)O32—Mo32—O3690.1 (2)
O114—Mo11—O1379.1 (2)O37—Mo32—O36158.6 (2)
O15—Mo11—O1371.98 (19)O38—Mo32—O3689.27 (19)
O12—Mo12—O18109.4 (2)O32—Mo32—O31388.6 (2)
O12—Mo12—O17104.9 (2)O37—Mo32—O31388.8 (2)
O18—Mo12—O1794.07 (19)O38—Mo32—O313164.6 (2)
O12—Mo12—O11389.8 (2)O36—Mo32—O31382.2 (2)
O18—Mo12—O11387.68 (19)O32—Mo32—O34159.9 (2)
O17—Mo12—O113163.6 (2)O37—Mo32—O3486.7 (2)
O12—Mo12—O1688.6 (2)O38—Mo32—O3485.9 (2)
O18—Mo12—O16159.7 (2)O36—Mo32—O3472.6 (2)
O17—Mo12—O1690.16 (19)O313—Mo32—O3479.2 (2)
O113—Mo12—O1682.86 (18)C31—O33—Mo31117.6 (5)
O12—Mo12—O14159.4 (2)C33—O34—Mo32119.3 (5)
O18—Mo12—O1488.0 (2)C32—O35—Mo31121.0 (5)
O17—Mo12—O1484.1 (2)C34—O36—Mo32120.4 (5)
O113—Mo12—O1479.7 (2)Mo32—O37—Mo3183.17 (19)
O16—Mo12—O1472.7 (2)Mo32—O38—Mo3182.73 (18)
C11—O13—Mo11119.2 (5)Mo32—O313—H3193.1
C13—O14—Mo12118.6 (5)Mo32—O313—H32106.0
C12—O15—Mo11119.9 (5)H31—O313—H32110.7
C14—O16—Mo12119.6 (5)Mo31—O314—H33139.4
Mo11—O17—Mo1283.36 (18)Mo31—O314—H34115.9
Mo12—O18—Mo1182.86 (16)H33—O314—H34104.5
Mo12—O113—H11129.2O39—C31—O33124.8 (8)
Mo12—O113—H12117.5O39—C31—C32122.3 (8)
H11—O113—H12109.8O33—C31—C32112.9 (7)
Mo11—O114—H13119.0O310—C32—O35126.8 (7)
Mo11—O114—H14128.6O310—C32—C31117.6 (7)
H13—O114—H14112.3O35—C32—C31115.6 (7)
O19—C11—O13126.9 (8)O312—C33—O34125.6 (8)
O19—C11—C12119.4 (7)O312—C33—C34122.9 (7)
O13—C11—C12113.7 (6)O34—C33—C34111.5 (7)
O110—C12—O15124.7 (7)O311—C34—O36124.7 (7)
O110—C12—C11121.0 (7)O311—C34—C33119.3 (7)
O15—C12—C11114.3 (6)O36—C34—C33116.0 (7)
O112—C13—O14125.9 (7)O41—Mo41—O48108.6 (2)
O112—C13—C14121.9 (7)O41—Mo41—O47103.1 (2)
O14—C13—C14112.2 (7)O48—Mo41—O4794.05 (19)
O111—C14—O16125.9 (7)O41—Mo41—O41493.1 (2)
O111—C14—C13117.9 (7)O48—Mo41—O41485.4 (2)
O16—C14—C13116.2 (7)O47—Mo41—O414163.0 (2)
O21—Mo21—O27109.2 (2)O41—Mo41—O4591.6 (2)
O21—Mo21—O28103.7 (2)O48—Mo41—O45157.9 (2)
O27—Mo21—O2893.54 (19)O47—Mo41—O4589.93 (18)
O21—Mo21—O2592.2 (2)O414—Mo41—O4584.5 (2)
O27—Mo21—O25157.0 (2)O41—Mo41—O43162.9 (2)
O28—Mo21—O2589.11 (19)O48—Mo41—O4386.3 (2)
O21—Mo21—O21489.2 (2)O47—Mo41—O4383.5 (2)
O27—Mo21—O21487.17 (19)O414—Mo41—O4379.5 (2)
O28—Mo21—O214165.9 (2)O45—Mo41—O4372.47 (18)
O25—Mo21—O21484.91 (19)O42—Mo42—O47109.0 (2)
O21—Mo21—O23160.4 (2)O42—Mo42—O48104.0 (2)
O27—Mo21—O2385.06 (19)O47—Mo42—O4894.65 (19)
O28—Mo21—O2388.2 (2)O42—Mo42—O41389.6 (2)
O25—Mo21—O2372.22 (19)O47—Mo42—O41387.38 (19)
O214—Mo21—O2377.87 (19)O48—Mo42—O413164.6 (2)
O22—Mo22—O28109.6 (2)O42—Mo42—O4689.8 (2)
O22—Mo22—O27105.1 (2)O47—Mo42—O46158.5 (2)
O28—Mo22—O2794.65 (19)O48—Mo42—O4690.5 (2)
O22—Mo22—O2691.4 (2)O413—Mo42—O4682.36 (19)
O28—Mo22—O26157.2 (2)O42—Mo42—O44160.8 (2)
O27—Mo22—O2688.24 (19)O47—Mo42—O4486.8 (2)
O22—Mo22—O21386.6 (2)O48—Mo42—O4484.9 (2)
O28—Mo22—O21388.17 (19)O413—Mo42—O4480.0 (2)
O27—Mo22—O213166.15 (19)O46—Mo42—O4472.87 (19)
O26—Mo22—O21384.03 (18)C41—O43—Mo41118.7 (5)
O22—Mo22—O24159.2 (2)C43—O44—Mo42118.4 (5)
O28—Mo22—O2485.15 (19)C42—O45—Mo41119.2 (5)
O27—Mo22—O2487.68 (19)C44—O46—Mo42119.6 (5)
O26—Mo22—O2472.32 (18)Mo42—O47—Mo4182.84 (17)
O213—Mo22—O2479.04 (19)Mo41—O48—Mo4282.89 (17)
C21—O23—Mo21117.6 (5)Mo42—O413—H41109.6
C23—O24—Mo22119.9 (4)Mo42—O413—H42109.1
C22—O25—Mo21120.7 (5)H41—O413—H42130.8
C24—O26—Mo22120.2 (5)Mo41—O414—H43117
Mo22—O27—Mo2182.78 (17)Mo41—O414—H44122
Mo22—O28—Mo2182.68 (17)H43—O414—H44122
Mo22—O213—H21127.6O49—C41—O43128.9 (7)
Mo22—O213—H22110.3O49—C41—C42118.4 (6)
H21—O213—H22105.3O43—C41—C42112.7 (6)
Mo21—O214—H23114.7O410—C42—O45125.0 (8)
Mo21—O214—H24118.0O410—C42—C41119.6 (7)
H23—O214—H24122.7O45—C42—C41115.4 (6)
O29—C21—O23125.8 (7)O411—C43—O44128.2 (8)
O29—C21—C22120.8 (7)O411—C43—C44118.3 (8)
O23—C21—C22113.3 (6)O44—C43—C44113.5 (7)
O210—C22—O25126.4 (7)O412—C44—O46125.7 (7)
O210—C22—C21118.4 (7)O412—C44—C43119.8 (7)
O25—C22—C21115.2 (7)O46—C44—C43114.5 (7)
O211—C23—O24125.9 (7)H1A—OW1—H1B111.8
O211—C23—C24121.3 (7)H2A—OW2—H2B107.4
O24—C23—C24112.8 (7)H3A—OW3—H3B128.3
O212—C24—O26125.1 (7)H4A—OW4—H4B117.5
O212—C24—C23120.2 (7)H5A—OW5—H5B115.3
O26—C24—C23114.7 (7)H6A—OW6—H6B104.0
O31—Mo31—O38108.2 (2)H7A—OW7—H7B104.9
O31—Mo31—O37104.2 (2)H8A—OW8—H8B117.5
O38—Mo31—O3793.5 (2)H9A—OW9—H9B112.6
O31—Mo31—O31491.5 (2)H10A—OW10—H10B111.7
O38—Mo31—O31486.4 (2)H11A—OW11—H11B117.1
O37—Mo31—O314163.5 (2)H12A—OW12—H12B100.7
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+2, y+1, z+2; (iii) x+2, y+1, z+1; (iv) x, y, z1; (v) x+1, y, z+2; (vi) x, y, z+1; (vii) x+2, y, z+2; (viii) x, y, z+2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O113—H11···O270.6862.0212.683 (6)162.7
O113—H12···O310iv0.9351.6842.615 (7)173.4
O114—H13···O3110.8641.7222.566 (7)165.0
O114—H14···O28ix0.8861.8032.632 (7)154.8
O213—H21···O17x0.7661.9822.740 (6)170.1
O213—H22···O410xi0.9791.6462.612 (7)168.2
O214—H23···O412x0.9021.7182.610 (8)169.7
O214—H24···O180.8661.8802.686 (6)154.2
O313—H31···O480.9512.0432.692 (7)124.0
O313—H31···O370.9512.3882.865 (7)110.6
O313—H32···O41ii1.2552.1493.012 (8)122.2
O314—H33···O47x0.8501.8012.616 (7)160.1
O314—H34···O212xii0.9321.7402.630 (7)158.4
O413—H41···O110ix0.8061.8062.589 (7)163.6
O413—H42···O38ix0.7751.9192.633 (6)152.9
O414—H43···O111xii0.751.872.598 (8)163
O414—H44···O370.781.932.650 (7)153
OW1—H1A···O23xiii1.2032.0162.912 (8)127.7
OW1—H1A···O29xiii1.2032.0173.192 (8)164.5
OW1—H1B···O24xiii1.0282.1522.913 (7)129.2
OW1—H1B···O211xiii1.0282.3582.886 (8)110.7
OW2—H2A···O460.9252.4383.025 (10)121.4
OW2—H2B···O16iii1.0082.3453.013 (9)122.9
OW3—H3A···O3111.1201.7582.775 (8)148.5
OW3—H3B···O211xiii1.2771.7903.050 (8)167.8
OW4—H4A···O261.1122.0622.921 (9)131.6
OW4—H4A···O221.1122.4833.263 (10)126.0
OW4—H4B···O15i1.1932.3383.472 (10)157.8
OW5—H5A···O17x1.2332.4093.158 (8)116.4
OW5—H5B···OW3x1.2561.9713.094 (10)146.1
OW6—H6A···O230.9282.0883.011 (8)173.0
OW6—H6B···O181.0662.1793.168 (8)153.5
OW7—H7A···OW101.0902.3063.201 (15)138.2
OW7—H7B···O44x1.0502.2553.092 (8)135.4
OW8—H8A···OW11v0.9182.1393.009 (14)158.0
OW8—H8B···O411x1.1052.0813.145 (9)160.8
OW9—H9A···O310v1.1071.9522.786 (9)129.2
OW9—H9B···O191.0872.5063.465 (11)146.6
OW10—H10A···O1100.9232.1052.883 (9)141.2
OW10—H10B···OW71.0972.5153.201 (15)119.5
OW11—H11A···OW8v1.2022.2023.009 (14)121.5
OW11—H11A···O431.2022.3923.074 (10)113.4
OW11—H11B···OW12ix1.0942.4713.316 (13)133.1
OW12—H12A···O411v1.0171.9532.788 (12)137.3
OW12—H12A···O44v1.0172.2273.054 (10)137.4
OW12—H12B···O43v1.2501.9332.975 (11)137.2
OW12—H12B···O49v1.2502.0333.124 (12)143.1
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+2, y+1, z+2; (iii) x+2, y+1, z+1; (iv) x, y, z1; (v) x+1, y, z+2; (ix) x+1, y, z; (x) x1, y, z; (xi) x1, y, z1; (xii) x, y, z+1; (xiii) x+1, y, z+1.
 

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