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In the title compound, (C2H10N2)3[Mo5O15(PO4)2]·3H2O, the heteropolymolybdate anion adopts its usual structure, consisting of five edge-sharing and corner-sharing distorted MoO6 octa­hedra and two corner-sharing PO4 tetra­hedra. A large number of O—H...O and N—H...O hydrogen bonds helps to consolidate the crystal packing.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806018976/hb2054sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806018976/hb2054Isup2.hkl
Contains datablock I

CCDC reference: 610789

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](C-C) = 0.005 Å
  • Disorder in solvent or counterion
  • R factor = 0.025
  • wR factor = 0.069
  • Data-to-parameter ratio = 11.4

checkCIF/PLATON results

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Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.96 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 25.00 Perc. PLAT432_ALERT_2_C Short Inter X...Y Contact O14 .. C5A .. 3.00 Ang. PLAT432_ALERT_2_C Short Inter X...Y Contact O15 .. C6 .. 2.95 Ang. PLAT432_ALERT_2_C Short Inter X...Y Contact O22 .. C3B .. 2.99 Ang. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 7
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 8 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 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 1 ALERT type 3 Indicator that the structure quality may be low 3 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2000); program(s) used to refine structure: SHELXL97 (Sheldrick, 2000); molecular graphics: SHELXTL/PC (Sheldrick, 1999); software used to prepare material for publication: SHELXTL/PC.

Tris(ethylenediammonium) di-µ5-phosphato-penta-µ2-oxo- decaoxopentamolybdenum(VI) trihydrate top
Crystal data top
(C2H10N2)3[Mo5O15(PO4)2]·3H2OZ = 2
Mr = 1150.05F(000) = 1124
Triclinic, P1Dx = 2.511 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.014 (4) ÅCell parameters from 6589 reflections
b = 10.699 (4) Åθ = 2.3–27.1°
c = 17.543 (7) ŵ = 2.22 mm1
α = 78.611 (7)°T = 298 K
β = 80.228 (6)°Block, colorless
γ = 67.198 (6)°0.50 × 0.40 × 0.20 mm
V = 1520.8 (11) Å3
Data collection top
Bruker SMART 1K CCD area-detector
diffractometer
5211 independent reflections
Radiation source: fine-focus sealed tube5075 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.019
ω scansθmax = 25.1°, θmin = 2.1°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2000)
h = 1010
Tmin = 0.403, Tmax = 0.665k = 1212
6233 measured reflectionsl = 1120
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.026H-atom parameters constrained
wR(F2) = 0.070 w = 1/[σ2(Fo2) + (0.0123P)2 + 3.1377P]
where P = (Fo2 + 2Fc2)/3
S = 1.12(Δ/σ)max = 0.003
5211 reflectionsΔρmax = 0.64 e Å3
459 parametersΔρmin = 0.71 e Å3
16 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0064 (3)
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
xyzUiso*/UeqOcc. (<1)
Mo10.43372 (4)0.01744 (3)0.352231 (19)0.02318 (10)
Mo20.26841 (4)0.32386 (3)0.419032 (18)0.02269 (10)
Mo30.14921 (4)0.57502 (3)0.267433 (19)0.02313 (10)
Mo40.19319 (4)0.43324 (3)0.104986 (19)0.02577 (10)
Mo50.31573 (4)0.08698 (3)0.153145 (19)0.02467 (10)
P10.05920 (11)0.28154 (9)0.28675 (5)0.01974 (19)
P20.48838 (11)0.28853 (9)0.23037 (5)0.0211 (2)
O10.1060 (3)0.3198 (3)0.33351 (16)0.0291 (6)
O20.1982 (3)0.2215 (2)0.34105 (15)0.0238 (5)
O30.0715 (3)0.4128 (2)0.23236 (14)0.0228 (5)
O40.0857 (3)0.1730 (2)0.23423 (15)0.0240 (5)
O50.6113 (3)0.3473 (3)0.18472 (17)0.0337 (6)
O60.5692 (3)0.1446 (3)0.27457 (16)0.0264 (6)
O70.3762 (3)0.3847 (2)0.29042 (15)0.0238 (5)
O80.3809 (3)0.2731 (2)0.17293 (15)0.0245 (5)
O90.3927 (3)0.0021 (3)0.25101 (16)0.0278 (6)
O100.4324 (3)0.1405 (3)0.42004 (15)0.0278 (6)
O110.1065 (3)0.4872 (3)0.36984 (15)0.0262 (6)
O120.2357 (3)0.5563 (3)0.16010 (15)0.0276 (6)
O130.1913 (3)0.2571 (3)0.09086 (15)0.0297 (6)
O140.3046 (3)0.0577 (3)0.40806 (17)0.0332 (6)
O150.6177 (3)0.1124 (3)0.36160 (17)0.0339 (6)
O160.1423 (3)0.2984 (3)0.50050 (17)0.0354 (7)
O170.3851 (3)0.3958 (3)0.45157 (17)0.0339 (6)
O180.0471 (3)0.6893 (3)0.25558 (17)0.0342 (6)
O190.2439 (3)0.6770 (3)0.28528 (19)0.0370 (7)
O200.0012 (4)0.5327 (3)0.08187 (17)0.0368 (7)
O210.3164 (4)0.4611 (3)0.02154 (17)0.0360 (7)
O220.2256 (4)0.0190 (3)0.13580 (18)0.0376 (7)
O230.4962 (4)0.0390 (3)0.09310 (18)0.0403 (7)
O240.6354 (4)0.7624 (3)0.06923 (18)0.0477 (8)
H110.60000.84560.07580.071*
H120.70120.75130.02790.071*
O250.1874 (4)0.6914 (4)0.4752 (2)0.0560 (9)
H130.24540.63520.44410.084*
H140.08850.69850.47790.084*
O260.8284 (6)0.9329 (5)0.1514 (4)0.1027 (19)
H150.84580.92080.19900.154*
H160.88800.86110.13150.154*
C10.6030 (5)0.6628 (4)0.2566 (2)0.0298 (8)
H1A0.49820.70490.23650.036*
H1B0.64730.73380.25170.036*
C20.5793 (5)0.6086 (4)0.3424 (2)0.0319 (9)
H2A0.48910.67730.36770.038*
H2B0.55210.52780.34740.038*
C3A0.7320 (14)0.1923 (14)0.0160 (6)0.061 (3)0.565 (7)
H3A10.75180.09620.01700.073*
H3A20.65690.22120.06140.073*
C3B0.7855 (14)0.1668 (13)0.0100 (9)0.062 (4)0.435 (7)
C40.8919 (6)0.2009 (5)0.0279 (3)0.0554 (14)
H4A0.98340.12770.00680.066*
H4B0.89860.28820.00290.066*
C5A0.8362 (12)0.0011 (10)0.4291 (5)0.033 (2)0.565 (7)
H5A10.76170.04350.45460.039*
H5A20.91750.02000.46430.039*
C5B0.9007 (18)0.0274 (14)0.4219 (8)0.043 (3)0.435 (7)
C60.9190 (6)0.0622 (5)0.3569 (3)0.0495 (12)
H6A0.92340.15600.36720.059*
H6B0.84810.01500.31590.059*
N10.7122 (4)0.5570 (3)0.2068 (2)0.0319 (7)
H1C0.81110.52220.22230.048*
H1D0.71640.59560.15710.048*
H1E0.67390.49030.21150.048*
N20.7265 (4)0.5725 (4)0.3831 (2)0.0346 (8)
H2C0.80230.49620.36830.052*
H2D0.70100.55940.43460.052*
H2E0.76370.64060.37060.052*
N3A0.6473 (8)0.2679 (8)0.0534 (5)0.050 (2)0.565 (7)
H3A30.65370.35060.06470.076*
H3A40.54390.27650.04380.076*
H3A50.69320.22220.09380.076*
N4A0.8884 (7)0.1866 (6)0.1146 (4)0.0355 (18)0.565 (7)
H4C0.88990.10350.13610.053*
H4D0.79870.24970.13330.053*
H4E0.97440.19790.12600.053*
N3B0.6335 (11)0.2828 (11)0.0048 (8)0.050 (3)0.435 (7)
N4B0.8700 (10)0.2962 (10)0.0727 (5)0.042 (2)0.435 (7)
N50.7454 (4)0.1507 (4)0.4198 (2)0.0370 (8)
H5A0.79800.19210.38250.056*
H5B0.73630.18120.46470.056*
H5C0.64730.16880.40660.056*
N6A1.0735 (6)0.0667 (5)0.3253 (3)0.0249 (14)0.565 (7)
H6C1.06710.01450.29810.037*
H6D1.11660.13070.29400.037*
H6E1.13550.08660.36380.037*
N6B0.9059 (11)0.0067 (10)0.2795 (6)0.046 (3)0.435 (7)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mo10.02474 (18)0.01730 (16)0.02539 (18)0.00646 (13)0.00169 (13)0.00166 (13)
Mo20.02594 (18)0.02121 (17)0.02050 (17)0.00789 (13)0.00127 (12)0.00461 (13)
Mo30.02293 (17)0.01704 (16)0.02858 (19)0.00727 (13)0.00164 (13)0.00239 (13)
Mo40.03152 (19)0.02402 (18)0.02117 (18)0.01213 (14)0.00117 (13)0.00080 (13)
Mo50.03010 (18)0.02226 (17)0.02276 (18)0.01056 (14)0.00141 (13)0.00728 (13)
P10.0206 (4)0.0176 (4)0.0208 (5)0.0077 (4)0.0001 (3)0.0022 (4)
P20.0208 (4)0.0190 (4)0.0237 (5)0.0084 (4)0.0017 (4)0.0048 (4)
O10.0252 (13)0.0259 (13)0.0351 (15)0.0107 (11)0.0051 (11)0.0059 (12)
O20.0275 (13)0.0196 (12)0.0241 (13)0.0079 (10)0.0047 (10)0.0024 (10)
O30.0261 (13)0.0206 (12)0.0229 (13)0.0111 (10)0.0029 (10)0.0003 (10)
O40.0261 (13)0.0205 (12)0.0269 (13)0.0104 (10)0.0023 (10)0.0036 (10)
O50.0323 (15)0.0295 (14)0.0413 (17)0.0165 (12)0.0082 (12)0.0090 (13)
O60.0229 (13)0.0223 (13)0.0316 (14)0.0067 (10)0.0012 (11)0.0034 (11)
O70.0246 (13)0.0218 (12)0.0242 (13)0.0075 (10)0.0001 (10)0.0060 (10)
O80.0276 (13)0.0215 (12)0.0247 (13)0.0083 (10)0.0032 (11)0.0044 (10)
O90.0292 (14)0.0231 (13)0.0300 (14)0.0070 (11)0.0015 (11)0.0078 (11)
O100.0310 (14)0.0231 (13)0.0274 (14)0.0066 (11)0.0077 (11)0.0026 (11)
O110.0277 (13)0.0219 (13)0.0250 (13)0.0051 (11)0.0008 (10)0.0043 (11)
O120.0344 (14)0.0219 (13)0.0271 (14)0.0146 (11)0.0006 (11)0.0009 (11)
O130.0377 (15)0.0314 (14)0.0236 (14)0.0161 (12)0.0044 (11)0.0040 (11)
O140.0371 (16)0.0299 (14)0.0332 (15)0.0154 (12)0.0003 (12)0.0026 (12)
O150.0326 (15)0.0228 (13)0.0421 (17)0.0052 (12)0.0080 (13)0.0019 (12)
O160.0369 (16)0.0335 (15)0.0298 (15)0.0104 (13)0.0037 (12)0.0021 (12)
O170.0396 (16)0.0366 (15)0.0306 (15)0.0165 (13)0.0065 (12)0.0085 (12)
O180.0309 (15)0.0254 (14)0.0405 (17)0.0062 (12)0.0045 (12)0.0007 (12)
O190.0339 (15)0.0283 (15)0.0537 (19)0.0151 (12)0.0015 (13)0.0115 (14)
O200.0370 (16)0.0381 (16)0.0320 (16)0.0109 (13)0.0058 (13)0.0016 (13)
O210.0427 (17)0.0322 (15)0.0309 (15)0.0168 (13)0.0040 (13)0.0002 (12)
O220.0484 (18)0.0351 (16)0.0378 (17)0.0218 (14)0.0023 (14)0.0128 (13)
O230.0431 (17)0.0426 (17)0.0364 (17)0.0179 (14)0.0127 (13)0.0178 (14)
O240.064 (2)0.0345 (17)0.0323 (17)0.0092 (15)0.0065 (15)0.0063 (14)
O250.049 (2)0.060 (2)0.068 (2)0.0258 (17)0.0066 (17)0.0278 (19)
O260.087 (3)0.085 (3)0.131 (5)0.042 (3)0.049 (3)0.052 (3)
C10.029 (2)0.0227 (18)0.036 (2)0.0080 (16)0.0026 (16)0.0034 (16)
C20.0258 (19)0.029 (2)0.039 (2)0.0094 (16)0.0024 (17)0.0067 (18)
C3A0.082 (5)0.066 (5)0.046 (5)0.030 (4)0.019 (4)0.018 (4)
C3B0.068 (6)0.056 (6)0.056 (6)0.010 (4)0.006 (4)0.017 (4)
C40.065 (3)0.035 (3)0.052 (3)0.012 (2)0.010 (3)0.000 (2)
C5A0.038 (5)0.035 (5)0.027 (4)0.017 (4)0.003 (4)0.002 (3)
C5B0.050 (9)0.039 (7)0.030 (6)0.010 (6)0.007 (6)0.007 (5)
C60.056 (3)0.040 (3)0.044 (3)0.012 (2)0.002 (2)0.007 (2)
N10.0350 (18)0.0275 (17)0.0332 (19)0.0115 (14)0.0049 (15)0.0036 (14)
N20.0381 (19)0.0344 (18)0.0317 (19)0.0130 (16)0.0018 (15)0.0081 (15)
N3A0.029 (4)0.043 (4)0.068 (6)0.018 (3)0.008 (4)0.028 (4)
N4A0.020 (3)0.029 (3)0.055 (4)0.001 (2)0.007 (3)0.016 (3)
N3B0.042 (6)0.057 (7)0.064 (8)0.036 (5)0.019 (5)0.021 (6)
N4B0.040 (5)0.053 (6)0.031 (5)0.013 (4)0.002 (4)0.013 (4)
N50.0319 (18)0.0357 (19)0.045 (2)0.0167 (15)0.0034 (16)0.0063 (17)
N6A0.027 (3)0.016 (3)0.033 (3)0.009 (2)0.004 (2)0.003 (2)
N6B0.036 (5)0.061 (6)0.046 (5)0.026 (4)0.007 (4)0.011 (5)
Geometric parameters (Å, º) top
Mo1—O151.710 (3)C1—N11.500 (5)
Mo1—O141.728 (3)C1—C21.514 (6)
Mo1—O91.924 (3)C1—H1A0.9700
Mo1—O101.936 (3)C1—H1B0.9700
Mo1—O62.278 (3)C2—N21.495 (5)
Mo1—O22.385 (3)C2—H2A0.9700
Mo2—O161.716 (3)C2—H2B0.9700
Mo2—O171.740 (3)C3A—N3A1.473 (8)
Mo2—O101.945 (3)C3A—C41.530 (8)
Mo2—O111.945 (3)C3A—H3A10.9700
Mo2—O22.212 (2)C3A—H3A20.9700
Mo2—O72.372 (3)C3B—C41.442 (9)
Mo3—O191.722 (3)C3B—N3B1.474 (9)
Mo3—O181.737 (3)C4—N4B1.343 (10)
Mo3—O111.907 (3)C4—N4A1.494 (8)
Mo3—O121.930 (3)C4—H4A0.9700
Mo3—O72.285 (3)C4—H4B0.9700
Mo3—O32.323 (2)C5A—N51.478 (10)
Mo4—O201.712 (3)C5A—C61.499 (10)
Mo4—O211.732 (3)C5A—H5A10.9700
Mo4—O131.956 (3)C5A—H5A20.9700
Mo4—O121.958 (3)C5B—C61.580 (15)
Mo4—O82.203 (3)C6—N6A1.395 (7)
Mo4—O32.325 (3)C6—N6B1.411 (11)
Mo5—O221.724 (3)C6—H6A0.9700
Mo5—O231.733 (3)C6—H6B0.9700
Mo5—O91.885 (3)N1—H1C0.8900
Mo5—O131.953 (3)N1—H1D0.8900
Mo5—O42.282 (3)N1—H1E0.8900
Mo5—O82.383 (3)N2—H2C0.8900
P1—O11.517 (3)N2—H2D0.8900
P1—O41.545 (3)N2—H2E0.8900
P1—O21.559 (3)N3A—H3A30.8900
P1—O31.565 (3)N3A—H3A40.8900
P2—O51.518 (3)N3A—H3A50.8900
P2—O61.535 (3)N4A—H4C0.8900
P2—O71.566 (3)N4A—H4D0.8900
P2—O81.582 (3)N4A—H4E0.8900
O24—H110.8453N5—H5A0.8900
O24—H120.8512N5—H5B0.8900
O25—H130.8493N5—H5C0.8900
O25—H140.8588N6A—H6C0.8900
O26—H150.8508N6A—H6D0.8900
O26—H160.8495N6A—H6E0.8900
O15—Mo1—O14101.59 (14)P1—O3—Mo3125.77 (14)
O15—Mo1—O9100.72 (12)P1—O3—Mo4128.93 (14)
O14—Mo1—O997.75 (13)Mo3—O3—Mo493.38 (9)
O15—Mo1—O10103.08 (12)P1—O4—Mo5123.93 (14)
O14—Mo1—O10101.04 (13)P2—O6—Mo1124.73 (14)
O9—Mo1—O10145.83 (11)P2—O7—Mo3127.36 (14)
O15—Mo1—O687.09 (12)P2—O7—Mo2128.64 (14)
O14—Mo1—O6171.31 (11)Mo3—O7—Mo292.72 (9)
O9—Mo1—O680.05 (11)P2—O8—Mo4129.27 (14)
O10—Mo1—O677.07 (11)P2—O8—Mo5133.57 (14)
O15—Mo1—O2171.02 (11)Mo4—O8—Mo595.66 (10)
O14—Mo1—O285.29 (11)Mo5—O9—Mo1149.49 (15)
O9—Mo1—O283.86 (10)Mo1—O10—Mo2121.62 (13)
O10—Mo1—O269.65 (10)Mo3—O11—Mo2122.05 (13)
O6—Mo1—O286.11 (9)Mo3—O12—Mo4120.89 (13)
O16—Mo2—O17103.72 (14)Mo5—O13—Mo4120.96 (13)
O16—Mo2—O10100.57 (13)H11—O24—H12109.4
O17—Mo2—O1096.38 (13)H13—O25—H14109.3
O16—Mo2—O1195.39 (13)H15—O26—H16108.7
O17—Mo2—O11100.83 (13)N1—C1—C2114.7 (3)
O10—Mo2—O11153.00 (11)N1—C1—H1A108.6
O16—Mo2—O297.77 (12)C2—C1—H1A108.6
O17—Mo2—O2157.66 (12)N1—C1—H1B108.6
O10—Mo2—O273.46 (10)C2—C1—H1B108.6
O11—Mo2—O282.96 (10)H1A—C1—H1B107.6
O16—Mo2—O7164.41 (12)N2—C2—C1112.4 (3)
O17—Mo2—O787.06 (12)N2—C2—H2A109.1
O10—Mo2—O789.18 (10)C1—C2—H2A109.1
O11—Mo2—O771.23 (10)N2—C2—H2B109.1
O2—Mo2—O773.21 (9)C1—C2—H2B109.1
O19—Mo3—O18103.13 (14)H2A—C2—H2B107.8
O19—Mo3—O11102.25 (14)N3A—C3A—C4121.3 (8)
O18—Mo3—O1197.50 (12)N3A—C3A—H3A1107.0
O19—Mo3—O1299.16 (13)C4—C3A—H3A1107.0
O18—Mo3—O12100.92 (13)N3A—C3A—H3A2107.0
O11—Mo3—O12147.65 (11)C4—C3A—H3A2107.0
O19—Mo3—O790.42 (12)H3A1—C3A—H3A2106.8
O18—Mo3—O7165.36 (12)C4—C3B—N3B99.5 (8)
O11—Mo3—O773.89 (10)N4B—C4—C3B134.3 (7)
O12—Mo3—O782.03 (10)N4B—C4—N4A50.7 (5)
O19—Mo3—O3168.72 (11)C3B—C4—N4A123.7 (8)
O18—Mo3—O386.62 (12)N4B—C4—C3A112.2 (7)
O11—Mo3—O381.76 (10)N4A—C4—C3A104.2 (6)
O12—Mo3—O373.10 (10)N4B—C4—H4A136.3
O7—Mo3—O380.50 (9)C3B—C4—H4A89.5
O20—Mo4—O21104.29 (14)N4A—C4—H4A110.9
O20—Mo4—O1397.63 (13)C3A—C4—H4A110.9
O21—Mo4—O1399.24 (13)N4B—C4—H4B61.3
O20—Mo4—O12100.19 (13)C3B—C4—H4B110.4
O21—Mo4—O1293.77 (13)N4A—C4—H4B110.9
O13—Mo4—O12154.59 (11)C3A—C4—H4B110.9
O20—Mo4—O8156.82 (12)H4A—C4—H4B108.9
O21—Mo4—O898.25 (12)N5—C5A—C6117.8 (7)
O13—Mo4—O873.19 (10)N5—C5A—H5A1107.9
O12—Mo4—O883.44 (10)C6—C5A—H5A1107.9
O20—Mo4—O384.81 (12)N5—C5A—H5A2107.9
O21—Mo4—O3164.94 (12)C6—C5A—H5A2107.9
O13—Mo4—O391.27 (10)H5A1—C5A—H5A2107.2
O12—Mo4—O372.57 (10)N6A—C6—N6B73.1 (5)
O8—Mo4—O374.38 (9)N6A—C6—C5A122.1 (6)
O22—Mo5—O23102.46 (14)N6B—C6—C5A125.5 (6)
O22—Mo5—O9102.05 (13)N6A—C6—C5B95.6 (7)
O23—Mo5—O999.86 (14)N6B—C6—C5B116.4 (7)
O22—Mo5—O1399.50 (13)N6A—C6—H6A106.8
O23—Mo5—O13100.32 (14)N6B—C6—H6A118.3
O9—Mo5—O13146.37 (11)C5A—C6—H6A106.8
O22—Mo5—O484.66 (12)C5B—C6—H6A124.7
O23—Mo5—O4172.75 (12)N6A—C6—H6B106.8
O9—Mo5—O479.76 (10)C5A—C6—H6B106.8
O13—Mo5—O476.88 (11)C5B—C6—H6B114.1
O22—Mo5—O8166.87 (12)H6A—C6—H6B106.7
O23—Mo5—O886.54 (12)C1—N1—H1C109.5
O9—Mo5—O885.54 (10)C1—N1—H1D109.5
O13—Mo5—O869.18 (10)H1C—N1—H1D109.5
O4—Mo5—O886.21 (9)C1—N1—H1E109.5
O1—P1—O4111.93 (15)H1C—N1—H1E109.5
O1—P1—O2111.61 (15)H1D—N1—H1E109.5
O4—P1—O2107.26 (14)C2—N2—H2C109.5
O1—P1—O3108.60 (15)C2—N2—H2D109.5
O4—P1—O3107.75 (14)H2C—N2—H2D109.5
O2—P1—O3109.59 (14)C2—N2—H2E109.5
O5—P2—O6112.17 (16)H2C—N2—H2E109.5
O5—P2—O7110.13 (15)H2D—N2—H2E109.5
O6—P2—O7108.86 (15)C4—N4A—H4C109.5
O5—P2—O8110.32 (16)C4—N4A—H4D109.5
O6—P2—O8106.07 (14)C4—N4A—H4E109.5
O7—P2—O8109.16 (14)C6—N6A—H6C109.5
P1—O2—Mo2129.46 (14)C6—N6A—H6D109.5
P1—O2—Mo1134.59 (14)C6—N6A—H6E109.5
Mo2—O2—Mo194.87 (9)
O1—P1—O2—Mo267.7 (2)O11—Mo2—O7—Mo32.21 (9)
O4—P1—O2—Mo2169.35 (17)O2—Mo2—O7—Mo390.34 (10)
O3—P1—O2—Mo252.6 (2)O5—P2—O8—Mo470.7 (2)
O1—P1—O2—Mo1127.3 (2)O6—P2—O8—Mo4167.59 (17)
O4—P1—O2—Mo14.4 (2)O7—P2—O8—Mo450.4 (2)
O3—P1—O2—Mo1112.3 (2)O5—P2—O8—Mo5126.76 (19)
O16—Mo2—O2—P187.8 (2)O6—P2—O8—Mo55.1 (2)
O17—Mo2—O2—P1108.2 (3)O7—P2—O8—Mo5112.09 (19)
O10—Mo2—O2—P1173.5 (2)O20—Mo4—O8—P2104.6 (3)
O11—Mo2—O2—P16.76 (19)O21—Mo4—O8—P288.8 (2)
O7—Mo2—O2—P179.21 (19)O13—Mo4—O8—P2174.0 (2)
O16—Mo2—O2—Mo1102.92 (12)O12—Mo4—O8—P24.04 (19)
O17—Mo2—O2—Mo161.2 (3)O3—Mo4—O8—P277.73 (19)
O10—Mo2—O2—Mo14.14 (10)O20—Mo4—O8—Mo562.7 (3)
O11—Mo2—O2—Mo1162.57 (11)O21—Mo4—O8—Mo5103.80 (12)
O7—Mo2—O2—Mo190.11 (10)O13—Mo4—O8—Mo56.58 (10)
O14—Mo1—O2—P183.7 (2)O12—Mo4—O8—Mo5163.33 (11)
O9—Mo1—O2—P114.6 (2)O3—Mo4—O8—Mo589.64 (10)
O10—Mo1—O2—P1172.7 (2)O22—Mo5—O8—P2141.8 (5)
O6—Mo1—O2—P195.0 (2)O23—Mo5—O8—P284.3 (2)
O14—Mo1—O2—Mo2107.88 (12)O9—Mo5—O8—P215.8 (2)
O9—Mo1—O2—Mo2153.79 (11)O13—Mo5—O8—P2173.2 (2)
O10—Mo1—O2—Mo24.25 (10)O4—Mo5—O8—P295.8 (2)
O6—Mo1—O2—Mo273.39 (10)O22—Mo5—O8—Mo424.7 (6)
O1—P1—O3—Mo385.50 (19)O23—Mo5—O8—Mo4109.16 (14)
O4—P1—O3—Mo3153.07 (15)O9—Mo5—O8—Mo4150.65 (11)
O2—P1—O3—Mo336.7 (2)O13—Mo5—O8—Mo46.75 (10)
O1—P1—O3—Mo4142.00 (17)O4—Mo5—O8—Mo470.65 (10)
O4—P1—O3—Mo420.6 (2)O22—Mo5—O9—Mo1143.0 (3)
O2—P1—O3—Mo495.84 (18)O23—Mo5—O9—Mo1111.9 (3)
O19—Mo3—O3—P195.8 (6)O13—Mo5—O9—Mo114.3 (4)
O18—Mo3—O3—P1114.03 (19)O4—Mo5—O9—Mo160.8 (3)
O11—Mo3—O3—P115.94 (17)O8—Mo5—O9—Mo126.2 (3)
O12—Mo3—O3—P1143.47 (19)O15—Mo1—O9—Mo5139.5 (3)
O7—Mo3—O3—P158.98 (17)O14—Mo1—O9—Mo5117.1 (3)
O19—Mo3—O3—Mo449.2 (6)O10—Mo1—O9—Mo55.9 (4)
O18—Mo3—O3—Mo4101.03 (12)O6—Mo1—O9—Mo554.4 (3)
O11—Mo3—O3—Mo4160.88 (10)O2—Mo1—O9—Mo532.7 (3)
O12—Mo3—O3—Mo41.46 (9)O15—Mo1—O10—Mo2168.83 (16)
O7—Mo3—O3—Mo485.95 (9)O14—Mo1—O10—Mo286.37 (18)
O20—Mo4—O3—P1115.9 (2)O9—Mo1—O10—Mo235.8 (3)
O21—Mo4—O3—P1116.1 (4)O6—Mo1—O10—Mo284.96 (16)
O13—Mo4—O3—P118.31 (19)O2—Mo1—O10—Mo25.66 (13)
O12—Mo4—O3—P1141.7 (2)O16—Mo2—O10—Mo1101.02 (18)
O8—Mo4—O3—P153.84 (17)O17—Mo2—O10—Mo1153.69 (17)
O20—Mo4—O3—Mo3100.95 (12)O11—Mo2—O10—Mo124.2 (3)
O21—Mo4—O3—Mo327.1 (5)O2—Mo2—O10—Mo15.97 (14)
O13—Mo4—O3—Mo3161.50 (10)O7—Mo2—O10—Mo166.74 (16)
O12—Mo4—O3—Mo31.45 (9)O19—Mo3—O11—Mo283.67 (17)
O8—Mo4—O3—Mo389.35 (10)O18—Mo3—O11—Mo2171.08 (16)
O1—P1—O4—Mo5179.44 (15)O12—Mo3—O11—Mo246.7 (3)
O2—P1—O4—Mo557.8 (2)O7—Mo3—O11—Mo23.19 (13)
O3—P1—O4—Mo560.10 (19)O3—Mo3—O11—Mo285.62 (15)
O22—Mo5—O4—P1175.24 (19)O16—Mo2—O11—Mo3174.91 (16)
O9—Mo5—O4—P171.94 (18)O17—Mo2—O11—Mo379.98 (17)
O13—Mo5—O4—P183.69 (18)O10—Mo2—O11—Mo348.7 (3)
O8—Mo5—O4—P114.20 (17)O2—Mo2—O11—Mo377.72 (16)
O5—P2—O6—Mo1179.03 (16)O7—Mo2—O11—Mo33.12 (13)
O7—P2—O6—Mo156.9 (2)O19—Mo3—O12—Mo4173.59 (16)
O8—P2—O6—Mo160.5 (2)O18—Mo3—O12—Mo481.01 (17)
O15—Mo1—O6—P2174.8 (2)O11—Mo3—O12—Mo442.6 (3)
O9—Mo1—O6—P273.41 (18)O7—Mo3—O12—Mo484.45 (15)
O10—Mo1—O6—P281.03 (18)O3—Mo3—O12—Mo42.02 (13)
O2—Mo1—O6—P211.03 (17)O20—Mo4—O12—Mo379.19 (17)
O5—P2—O7—Mo384.1 (2)O21—Mo4—O12—Mo3175.56 (16)
O6—P2—O7—Mo3152.54 (16)O13—Mo4—O12—Mo354.7 (3)
O8—P2—O7—Mo337.2 (2)O8—Mo4—O12—Mo377.67 (15)
O5—P2—O7—Mo2142.54 (18)O3—Mo4—O12—Mo32.02 (13)
O6—P2—O7—Mo219.2 (2)O22—Mo5—O13—Mo4164.26 (17)
O8—P2—O7—Mo296.20 (19)O23—Mo5—O13—Mo491.09 (18)
O19—Mo3—O7—P2114.2 (2)O9—Mo5—O13—Mo434.9 (3)
O18—Mo3—O7—P287.7 (5)O4—Mo5—O13—Mo482.08 (16)
O11—Mo3—O7—P2143.1 (2)O8—Mo5—O13—Mo48.84 (13)
O12—Mo3—O7—P215.05 (18)O20—Mo4—O13—Mo5148.85 (17)
O3—Mo3—O7—P259.04 (17)O21—Mo4—O13—Mo5105.24 (18)
O19—Mo3—O7—Mo2100.41 (12)O12—Mo4—O13—Mo514.6 (4)
O18—Mo3—O7—Mo257.6 (5)O8—Mo4—O13—Mo59.34 (14)
O11—Mo3—O7—Mo22.22 (9)O3—Mo4—O13—Mo563.92 (16)
O12—Mo3—O7—Mo2160.40 (11)N1—C1—C2—N272.2 (4)
O3—Mo3—O7—Mo286.31 (9)N3B—C3B—C4—N4B7.4 (18)
O16—Mo2—O7—P2110.5 (4)N3B—C3B—C4—N4A73.1 (12)
O17—Mo2—O7—P2115.07 (19)N3B—C3B—C4—C3A33.9 (14)
O10—Mo2—O7—P218.64 (18)N3A—C3A—C4—N4B95.1 (13)
O11—Mo2—O7—P2142.4 (2)N3A—C3A—C4—C3B64.8 (18)
O2—Mo2—O7—P254.31 (17)N3A—C3A—C4—N4A148.0 (11)
O16—Mo2—O7—Mo334.1 (4)N5—C5A—C6—N6A85.2 (9)
O17—Mo2—O7—Mo3100.28 (12)N5—C5A—C6—N6B6.2 (12)
O10—Mo2—O7—Mo3163.30 (10)N5—C5A—C6—C5B72.5 (15)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N6A—H6E···O14i0.891.972.773 (6)149
N6A—H6D···O19ii0.891.952.739 (6)147
N6A—H6C···O4i0.891.892.772 (6)172
N5—H5C···O100.892.042.865 (5)153
N5—H5B···O14iii0.892.413.002 (5)124
N5—H5B···O25iv0.892.233.003 (5)145
N5—H5A···O1i0.891.892.733 (4)159
N4A—H4E···O22i0.892.543.016 (6)114
N4A—H4E···O13i0.892.243.047 (7)151
N4A—H4E···O4i0.892.222.922 (6)136
N4A—H4D···O50.891.802.678 (6)168
N4A—H4C···O26v0.892.062.898 (8)156
N3A—H3A5···O22vi0.892.243.014 (10)145
N3A—H3A4···O24vii0.891.962.756 (8)149
N3A—H3A3···O21vii0.892.413.204 (9)149
N3A—H3A4···O210.892.523.140 (9)127
N3A—H3A3···O12vii0.892.082.762 (7)133
N2—H2E···O18i0.892.523.171 (5)130
N2—H2E···O15viii0.892.443.087 (5)130
N2—H2D···O17iv0.892.092.945 (5)160
N2—H2C···O1i0.891.922.769 (4)159
N1—H1E···O50.891.982.838 (4)161
N1—H1D···O20i0.892.583.069 (5)116
N1—H1D···O240.892.092.904 (5)151
N1—H1C···O1i0.892.573.138 (4)122
N1—H1C···O3i0.892.203.068 (4)165
O24—H12···O13vii0.852.152.977 (4)165
O24—H11···O23viii0.851.982.818 (4)175
O25—H14···O16ix0.862.042.891 (5)172
O25—H13···O170.852.363.042 (5)137
O26—H15···O18i0.852.362.818 (7)114
Symmetry codes: (i) x+1, y, z; (ii) x+1, y1, z; (iii) x+1, y, z+1; (iv) x+1, y+1, z+1; (v) x, y1, z; (vi) x+1, y, z; (vii) x+1, y+1, z; (viii) x, y+1, z; (ix) x, y+1, z+1.
 

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