Bis(4,4′-bipyridinium) bis­(μ₅-hydrogen phosphate)penta­kis(μ₂-oxido)deca­oxido­penta­molybdate dihydrate

The title compound, (bipyH₂)₂[H₂Mo₅O₂₃P₂]·2H₂O or (C₁₀H₁₀N₂)₂[Mo₅O₁₅(HPO₄)₂]·2H₂O, contains the heteropoly­anion [P₂Mo₅O₂₁(OH)₂]⁴⁻, two diprotonated 4,4′-bipyridine (bipy) molecules as cations and two water mol­ecules. The heteropolyanion is built up from five MoO₆ octa­hedra sharing four common edges and one common corner. The heteropolyanion has approximate noncrystallographic twofold rotation symmetry, the axis running through one Mo and one O atom. Five bridging O atoms between molybdenum centers connect the distorted MoO₆ octa­hedra to form a ring system, with ten Mo—O distances having an average value of 1.923 (2) Å. Six O atoms of the PO₃(OH) tetra­hedra above and below the ring stabilize the polyanionic framework. The ten Mo—OP bond lengths differ markedly, between 2.219 (2) and 2.461 (2) Å. The ten short terminal Mo—O distances average 1.706 (2) Å. The P—O bond lengths range between 1.513 (2) and 1.567 (2) Å. The crystal packing exhibits a great number of N—H...O and O—H...O inter­molecular classical hydrogen bonds, which link the cations, water mol­ecules and polyanions to form a three-dimensional framework.

Key indicators

• Single-crystal X-ray study
• T = 170 K
• Mean [sigma](C-C) = 0.004 Å
• R factor = 0.020
• wR factor = 0.052
• Data-to-parameter ratio = 15.4

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT415_ALERT_2_B Short Inter D-H..H-X       H2A    ..  H6A     ..       1.93 Ang.
PLAT417_ALERT_2_B Short Inter D-H..H-D       H4     ..  H5B     ..       1.70 Ang.
PLAT417_ALERT_2_B Short Inter D-H..H-D       H5B    ..  H22     ..       1.52 Ang.
PLAT432_ALERT_2_B Short Inter X...Y Contact  O1     ..  C7      ..       2.90 Ang.
PLAT432_ALERT_2_B Short Inter X...Y Contact  O19    ..  C13     ..       2.91 Ang.

Alert level C
PLAT063_ALERT_3_C Crystal Probably too Large for Beam Size .......       0.62 mm
PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical .          ?
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  Mo4    -   O17     ..       5.57 su
PLAT432_ALERT_2_C Short Inter X...Y Contact  O7     ..  C12     ..       2.95 Ang.
PLAT432_ALERT_2_C Short Inter X...Y Contact  O8     ..  C16     ..       2.99 Ang.
PLAT432_ALERT_2_C Short Inter X...Y Contact  O19    ..  C18     ..       2.94 Ang.
PLAT432_ALERT_2_C Short Inter X...Y Contact  O19    ..  C20     ..       2.96 Ang.
PLAT432_ALERT_2_C Short Inter X...Y Contact  O21    ..  C15     ..       2.94 Ang.
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         30
            O1  -MO2 -O9  -P2     -4.40  0.90   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         95
            O19 -MO5 -O14 -P1     19.60  0.50   1.555   1.555   1.555   1.555

Alert level G
PLAT793_ALERT_1_G Check the Absolute Configuration of P1     = ...          R
PLAT794_ALERT_5_G Check Predicted Bond Valency for Mo1         (6)       6.03
PLAT794_ALERT_5_G Check Predicted Bond Valency for Mo2         (6)       5.99
PLAT794_ALERT_5_G Check Predicted Bond Valency for Mo3         (6)       5.77
PLAT794_ALERT_5_G Check Predicted Bond Valency for Mo4         (6)       6.03
PLAT794_ALERT_5_G Check Predicted Bond Valency for Mo5         (6)       6.01

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

   2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
  11 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
   2 ALERT type 4 Improvement, methodology, query or suggestion
   5 ALERT type 5 Informative message, check

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S1. Comment

Recently, many research activities have focused on the synthesis of open-framework metal phosphates with organic ligands because of their interesting structural chemistry and potential applications (Haushalter & Mundi, 1992; Lii et al., 1998; Wang et al., 1995). Many metal complexes containing polymolybdates have been synthesized and characterized (Luo et al., 2003; Wu et al., 2002). During our ongoing studies of related materials, we obtained the title compound (Fig.1). The unit cell contains two protonated 4,4'-bipyridine molecules, an (H₂P₂Mo₅O₂₃)^4- anion and two water molecules. The heteropolyanion of (H₂P₂Mo₅O₂₃)^4- is built up from five MoO₆ octahedra (Fig. 2) sharing four common edges and one common corner, capped by two PO₃(OH) tetrahedra. All the Mo atoms exhibit a 6⁺ oxidation state and possess distorted octahedral geometry. The Mo—O and P—O distances are in the range 1.693 (2)–2.461 (2) Å and 1.513 (2)–1.567 (2) Å. It is interesting to note that the protonated 4,4'-bipyridine cations and the water molecules play important roles for the crystal packing arrangement by linking (H₂P₂Mo₅O₂₃)^4- anions via numerous N—H^···O and O—H^···O hydrogen-bonds. There are two types of protonated 4,4'-bipyridine molecules and two kinds of lattice-waters in the crystal packing. For example, O1W links two (H₂P₂Mo₅O₂₃)^4- anions by three O—H^···O(terminal oxygen) hydrogen bonds. However, O2W links two heteropolyanions via O—H^···O(terminal oxygen) and O—H^···O(double-bridging oxygen) hydrogen bonds. Similar to the lattice-water, the ligand 4,4-bpy with atoms N1 and N2 links two (H₂P₂Mo₅O₂₃)^4- anions by N—H^···O(terminal oxygen) and an N—H^···O(double-bridging oxygen) hydrogen-bonds, and the other 4,4-bpy ligand with atoms N3 and N4 have two N—H^···O(double- bridging oxygen) hydrogen bonds and an N—H^···O(terminal oxygen) hydrogen bond. The crystal packing exhibits a great number of N—H^···O and O—H^···O intra- and intermolecular classic hydrogen bonds, which link the cations, water molecules and the polyanions to form a three-dimensional framework (Fig. 3). The most important geometric parameters of the title compound are listed for one example Mo-complex in Table 1. The classic hydrogen bonding interactions are given in Table 2. Ten weak intermolecular C—H^···O hydrogen bonding contacts are not considered for clarity.

Related literature

For related literature see: Haushalter & Mundi (1992); Lii et al., (1998); Wang et al., (1995); Wu et al. (2002).

For related literature, see: Luo et al. (2003).

S2. Experimental

All reagents were used as purchased without further purification. The synthesis was carried out in a rational way from a mixture of H₂MoO₄ (2 mmol 0.324 g). 4,4'-bipyridine(4 mmol 0.674 g), H₃PO₄(0.2 mmol 85wt%) and H₂O(12 mmol). The mixture was loaded in a Teflon-lined autoclave (23 ml capacity) and was heated at 443k for 5 d under autogenous pressure. The solid product was collected by filtration, washed with water and dried at room temperature. Colorless crystals of the title compound were isolated.

S3. Refinement

The structure was solved by direct methods and refined on F² using the SHELXTL97 software package. The hydrogen atoms that are bonded to water oxygen, nitrogen and carbon atoms were placed geometrically, with O—H, N—H and C—H distances of 0.98 Å for water, 0.88 Å for N atoms and 0.95 Å for C atoms of the pyridinium moieties, and U_iso(H) = 1.2U_eq for (O), (N) and (C) atoms, respectively. The H atoms of O1W and O2W were located in a difference Fourier map and refined with O—H distances approximately equal to 0.98 Å. Atoms H5B and H5C of O1W were treated as disordered and their site occupation set 1/2 due to similar electron density peaks. Finally, the coordinates of H5A, H5B, and H5C of O1W were fixed to stabilize the refinement. The hydroxyl H atoms of the phosphate groups were from difference Fourier maps, they were finally refined with isotropic displacement parameters, using a rotation mode with the HFIX 147 instruction of SHELXL97, with O—H distances 0.84 Å and U_iso(H21, H22) = 1.5U_eq for O4 and O7, respectively. More details and interpretation of the hydrogen bonding situation are given in the _exptl_special_details. All non-hydrogen atoms were refined with anisotropic thermal parameters.

Computing details

Data collection: RAPID-AUTO (Rigaku, 2004); cell refinement: RAPID-AUTO; data reduction: RAPID-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 1999); software used to prepare material for publication: SHELXTL.

Figures

	Fig. 1. : The molecular structure of the title compound, with atom labels and with displacement ellipsoids drawn at the 50% probability level, for non-H atoms.
	Fig. 2. : The polyanion of the title compound, viewed approximately upon the five-membered Mo skeleton to show the non-crystallographic twofold axis symmetry, the axis running through Mo4 and O11.
	Fig. 3. : A packing diagram of the title compound, viewed along the a axis. Dashed lines indicate hydrogen bonds of the type N—H^···O and O—H^···O.

bis(4,4'-bipyridinium) bis(µ₅-hydrogen phosphate)pentakis(µ₂-oxido)decaoxidopentamolybdate dihydrate

Crystal data

(C10H10N2)2[Mo5O15(HPO4)2]·2H2O	F(000) = 4912
Mr = 1264.09	Dx = 2.462 Mg m^−3
Orthorhombic, Pbca	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2ab	Cell parameters from 58657 reflections
a = 11.823 (2) Å	θ = 3.1–27.5°
b = 18.307 (4) Å	µ = 1.99 mm^−1
c = 31.517 (6) Å	T = 170 K
V = 6821 (2) Å^3	Needle, colorless
Z = 8	0.62 × 0.10 × 0.06 mm

Data collection

Rigaku R-AXIS SPIDER diffractometer	6885 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.032
Graphite monochromator	θmax = 27.5°, θmin = 3.1°
ω oscillation scans	h = −15→13
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	k = −23→23
Tmin = 0.788, Tmax = 0.888	l = −40→40
58657 measured reflections	2 standard reflections every 150 reflections
7810 independent reflections	intensity decay: none

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.020	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.052	H-atom parameters constrained
S = 1.04	w = 1/[σ^2(Fo^2) + (0.0232P)^2 + 8.9692P] where P = (Fo^2 + 2Fc^2)/3
7810 reflections	(Δ/σ)max = 0.001
507 parameters	Δρmax = 0.55 e Å^−3
0 restraints	Δρmin = −0.53 e Å^−3

Special details

Experimental. Due to short H···H contacts detected with PLATON, atoms H4, H5B and H22 were omitted in a test-refinement and could be located at approximate positions as before. Additionally, a third H-atom at O1W could be found. Atom H22 at O7 of the second HPO₄ moiety could be rotated away from a short H5B···H22 contact of 1.52 Å by using the BUMP instruction of SHELXL97. But then H22 lost its good donor property for the hydrogen bonding contact O7—H22···O1W. Atom H5B is a bifurcated donor for the contacts O1W—H5B···O7 and O1W—H5B···N4. The third H-atom H5C is a donor for the contact O1W—H5C···O23. It is thinkable that there is a kind of flip-flop disorder of H-atoms between H5b, H22 and also H4 of the bipyridine. We decided to reduce the problem by leaving atoms H5B and H5C at their observed positions with site occupation 1/2 each. The possibility of H-atom migration and tautomeric situations can lead to the observed H···H collisions in the measured subcell. The structure can be seen as a superstructure with different hydrogen bonds in adjacent subcells or as a statistical distribution of alternately protonated (O1W) and deprotonated (N4, O7) atoms. Some weak C—H···O hydrogen bonding contacts with Hbipy as donor molecules and terminal oxygen atoms of the polyanion as acceptors were also observed with PLATON. The classic hydrogen bonds including alternative bonds with H5B and H5C as donors are shown in the Table of hydrogen bonding geometry.

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 (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Mo1	0.673842 (17)	0.395894 (11)	0.164003 (6)	0.01949 (5)
Mo2	0.222060 (17)	0.435677 (11)	0.110922 (6)	0.01973 (5)
Mo3	0.300879 (18)	0.259156 (12)	0.092842 (7)	0.02377 (5)
Mo4	0.568983 (17)	0.235361 (11)	0.129289 (6)	0.01836 (5)
Mo5	0.488850 (17)	0.531167 (11)	0.136063 (7)	0.01990 (5)
P1	0.49905 (5)	0.39040 (3)	0.071272 (19)	0.01954 (12)
P2	0.39585 (5)	0.35973 (3)	0.182165 (18)	0.01672 (11)
O1	0.19088 (17)	0.46367 (11)	0.06076 (6)	0.0326 (4)
O2	0.37835 (14)	0.36919 (9)	0.08454 (5)	0.0219 (3)
O3	0.24558 (18)	0.18901 (11)	0.12105 (8)	0.0445 (5)
O4	0.51165 (18)	0.36254 (11)	0.02472 (6)	0.0348 (5)
H21	0.5561	0.3900	0.0114	0.052*
O5	0.26267 (18)	0.24150 (13)	0.04182 (7)	0.0436 (5)
O6	0.80289 (15)	0.38793 (11)	0.14037 (6)	0.0323 (4)
O7	0.40830 (16)	0.34044 (10)	0.23039 (5)	0.0273 (4)
H22	0.4292	0.3777	0.2438	0.041*
O8	0.70150 (17)	0.41885 (11)	0.21538 (6)	0.0329 (4)
O9	0.28124 (14)	0.39508 (9)	0.17575 (5)	0.0211 (3)
O10	0.63370 (14)	0.29609 (9)	0.17264 (5)	0.0220 (3)
O11	0.33624 (14)	0.50730 (9)	0.12380 (5)	0.0224 (4)
O12	0.45737 (15)	0.22831 (9)	0.08715 (5)	0.0236 (4)
O13	0.40575 (14)	0.28766 (9)	0.15824 (5)	0.0212 (3)
O14	0.51224 (15)	0.47256 (9)	0.07319 (5)	0.0236 (4)
O15	0.64225 (14)	0.49222 (9)	0.14026 (5)	0.0213 (3)
O16	0.51736 (17)	0.60912 (10)	0.10865 (6)	0.0336 (4)
O17	0.58737 (14)	0.35249 (9)	0.09946 (5)	0.0217 (3)
O18	0.48900 (14)	0.41418 (9)	0.17009 (5)	0.0202 (3)
O19	0.47497 (15)	0.56183 (10)	0.18699 (6)	0.0281 (4)
O20	0.54467 (15)	0.15868 (10)	0.15847 (6)	0.0264 (4)
O21	0.19002 (14)	0.33318 (10)	0.10747 (6)	0.0246 (4)
O22	0.69131 (15)	0.21350 (10)	0.10217 (6)	0.0263 (4)
O23	0.10681 (15)	0.46518 (10)	0.13920 (6)	0.0293 (4)
O1W	0.0081 (2)	0.45867 (14)	0.22711 (7)	0.0484 (6)
H5A	0.0746	0.4565	0.2450	0.058*
H5B	−0.0590	0.4580	0.2444	0.058*	0.50
H5C	0.0365	0.4571	0.1983	0.058*	0.50
O2W	0.1367 (2)	0.07679 (19)	0.03045 (8)	0.0781 (10)
H6A	0.2105	0.0628	0.0180	0.094*
H6B	0.1396	0.0637	0.0609	0.094*
N1	1.1584 (2)	0.70730 (15)	−0.05533 (7)	0.0388 (6)
H1	1.2067	0.7286	−0.0726	0.047*
N2	0.7791 (2)	0.53924 (13)	0.08094 (7)	0.0304 (5)
H2	0.7310	0.5176	0.0982	0.036*
N3	1.10428 (19)	0.30064 (13)	0.19184 (8)	0.0331 (5)
H3	1.1565	0.3317	0.1835	0.040*
N4	0.6958 (2)	0.05518 (14)	0.25719 (9)	0.0415 (6)
H4	0.6442	0.0236	0.2655	0.050*
C1	1.1859 (3)	0.64345 (19)	−0.03824 (9)	0.0388 (7)
H1A	1.2567	0.6216	−0.0448	0.047*
C2	1.1126 (2)	0.60884 (16)	−0.01112 (9)	0.0315 (6)
H2A	1.1324	0.5633	0.0013	0.038*
C3	1.0093 (2)	0.64131 (14)	−0.00206 (7)	0.0225 (5)
C4	0.9837 (2)	0.70774 (16)	−0.02057 (9)	0.0339 (6)
H4A	0.9134	0.7308	−0.0148	0.041*
C5	1.0605 (3)	0.74020 (18)	−0.04738 (10)	0.0417 (7)
H5	1.0437	0.7859	−0.0601	0.050*
C6	0.7391 (2)	0.57677 (16)	0.04779 (9)	0.0311 (6)
H6	0.6598	0.5798	0.0432	0.037*
C7	0.8120 (2)	0.61103 (15)	0.02029 (8)	0.0262 (5)
H7	0.7837	0.6382	−0.0031	0.031*
C8	0.9276 (2)	0.60545 (13)	0.02716 (7)	0.0213 (5)
C9	0.9667 (2)	0.56597 (14)	0.06186 (8)	0.0270 (5)
H9	1.0456	0.5614	0.0670	0.032*
C10	0.8895 (2)	0.53352 (15)	0.08870 (9)	0.0306 (6)
H10	0.9152	0.5070	0.1128	0.037*
C11	1.1214 (2)	0.26356 (15)	0.22744 (9)	0.0291 (6)
H11	1.1880	0.2714	0.2437	0.035*
C12	1.0420 (2)	0.21368 (14)	0.24067 (8)	0.0253 (5)
H12	1.0539	0.1865	0.2660	0.030*
C13	0.9441 (2)	0.20307 (13)	0.21692 (8)	0.0219 (5)
C14	0.9291 (2)	0.24402 (16)	0.17998 (9)	0.0313 (6)
H14	0.8629	0.2382	0.1633	0.038*
C15	1.0119 (2)	0.29308 (18)	0.16812 (10)	0.0375 (7)
H15	1.0030	0.3214	0.1431	0.045*
C16	0.7041 (2)	0.07013 (16)	0.21599 (10)	0.0356 (7)
H16	0.6547	0.0473	0.1962	0.043*
C17	0.7839 (2)	0.11843 (15)	0.20234 (9)	0.0294 (6)
H17	0.7901	0.1295	0.1730	0.035*
C18	0.8559 (2)	0.15142 (14)	0.23123 (8)	0.0240 (5)
C19	0.8440 (2)	0.13527 (17)	0.27439 (9)	0.0337 (6)
H19	0.8914	0.1579	0.2949	0.040*
C20	0.7622 (3)	0.08594 (19)	0.28668 (10)	0.0422 (7)
H20	0.7530	0.0738	0.3158	0.051*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Mo1	0.01621 (10)	0.02008 (10)	0.02219 (10)	−0.00188 (7)	0.00135 (8)	0.00065 (8)
Mo2	0.01688 (10)	0.02155 (10)	0.02075 (10)	0.00192 (7)	0.00012 (8)	0.00032 (8)
Mo3	0.01946 (10)	0.02123 (11)	0.03062 (11)	−0.00034 (8)	−0.00211 (9)	−0.00514 (8)
Mo4	0.01718 (10)	0.01714 (10)	0.02077 (10)	0.00070 (7)	0.00317 (8)	−0.00003 (7)
Mo5	0.01883 (10)	0.01682 (10)	0.02407 (10)	−0.00144 (7)	0.00478 (8)	−0.00049 (8)
P1	0.0208 (3)	0.0208 (3)	0.0170 (3)	0.0005 (2)	0.0042 (2)	0.0008 (2)
P2	0.0161 (3)	0.0168 (3)	0.0172 (3)	−0.0008 (2)	0.0034 (2)	0.0014 (2)
O1	0.0368 (11)	0.0358 (11)	0.0253 (9)	0.0069 (9)	−0.0058 (8)	0.0010 (8)
O2	0.0181 (8)	0.0215 (8)	0.0259 (8)	0.0009 (7)	0.0031 (7)	0.0000 (7)
O3	0.0312 (11)	0.0299 (11)	0.0724 (15)	−0.0077 (9)	0.0030 (11)	0.0052 (10)
O4	0.0471 (12)	0.0362 (11)	0.0212 (9)	−0.0060 (9)	0.0104 (9)	−0.0043 (8)
O5	0.0348 (11)	0.0538 (14)	0.0422 (12)	0.0135 (10)	−0.0133 (10)	−0.0234 (10)
O6	0.0196 (9)	0.0342 (10)	0.0433 (11)	0.0016 (8)	0.0054 (8)	0.0061 (9)
O7	0.0356 (10)	0.0265 (9)	0.0199 (8)	0.0025 (8)	0.0009 (8)	0.0034 (7)
O8	0.0393 (11)	0.0321 (10)	0.0271 (9)	−0.0067 (9)	−0.0053 (8)	−0.0007 (8)
O9	0.0176 (8)	0.0234 (9)	0.0222 (8)	0.0003 (6)	0.0037 (7)	0.0029 (7)
O10	0.0220 (8)	0.0210 (8)	0.0229 (8)	0.0004 (7)	−0.0002 (7)	0.0016 (7)
O11	0.0199 (8)	0.0203 (8)	0.0272 (9)	0.0020 (7)	0.0025 (7)	0.0006 (7)
O12	0.0234 (9)	0.0233 (9)	0.0242 (8)	0.0023 (7)	0.0001 (7)	−0.0056 (7)
O13	0.0216 (8)	0.0186 (8)	0.0233 (8)	−0.0008 (7)	0.0049 (7)	−0.0018 (7)
O14	0.0275 (9)	0.0212 (9)	0.0219 (8)	−0.0006 (7)	0.0044 (7)	0.0024 (7)
O15	0.0172 (8)	0.0201 (8)	0.0264 (8)	−0.0031 (6)	0.0053 (7)	0.0014 (7)
O16	0.0355 (11)	0.0233 (10)	0.0421 (11)	−0.0030 (8)	0.0092 (9)	0.0046 (8)
O17	0.0183 (8)	0.0231 (8)	0.0237 (8)	0.0009 (7)	0.0027 (7)	0.0014 (7)
O18	0.0175 (8)	0.0173 (8)	0.0259 (8)	−0.0022 (6)	0.0020 (7)	0.0010 (7)
O19	0.0245 (9)	0.0283 (10)	0.0315 (9)	−0.0022 (7)	0.0050 (8)	−0.0094 (8)
O20	0.0278 (9)	0.0223 (9)	0.0293 (9)	−0.0012 (7)	0.0033 (8)	0.0035 (7)
O21	0.0160 (8)	0.0255 (9)	0.0323 (9)	−0.0018 (7)	0.0009 (7)	−0.0022 (7)
O22	0.0243 (9)	0.0246 (9)	0.0300 (9)	0.0025 (7)	0.0095 (8)	0.0010 (7)
O23	0.0206 (9)	0.0343 (10)	0.0331 (10)	0.0052 (8)	0.0008 (8)	−0.0014 (8)
O1W	0.0473 (14)	0.0580 (15)	0.0398 (12)	0.0031 (11)	0.0049 (10)	0.0056 (11)
O2W	0.0599 (17)	0.127 (3)	0.0471 (15)	0.0313 (18)	0.0066 (13)	0.0466 (17)
N1	0.0390 (14)	0.0514 (16)	0.0259 (12)	−0.0203 (12)	0.0101 (11)	0.0036 (11)
N2	0.0302 (12)	0.0294 (12)	0.0314 (12)	−0.0051 (9)	0.0138 (10)	0.0022 (10)
N3	0.0209 (11)	0.0327 (12)	0.0458 (14)	−0.0022 (9)	0.0081 (10)	0.0101 (11)
N4	0.0327 (13)	0.0318 (13)	0.0598 (17)	−0.0071 (11)	0.0152 (13)	0.0056 (12)
C1	0.0270 (14)	0.0536 (19)	0.0358 (15)	−0.0034 (13)	0.0124 (13)	−0.0033 (14)
C2	0.0282 (14)	0.0348 (15)	0.0316 (14)	−0.0001 (11)	0.0080 (12)	0.0024 (11)
C3	0.0210 (12)	0.0274 (13)	0.0191 (11)	−0.0056 (10)	0.0020 (10)	−0.0020 (9)
C4	0.0302 (14)	0.0318 (14)	0.0397 (15)	−0.0005 (12)	0.0057 (12)	0.0054 (12)
C5	0.0482 (19)	0.0388 (17)	0.0382 (16)	−0.0099 (14)	0.0037 (15)	0.0121 (13)
C6	0.0222 (13)	0.0364 (15)	0.0347 (14)	−0.0035 (11)	0.0053 (12)	−0.0026 (12)
C7	0.0230 (13)	0.0321 (14)	0.0234 (12)	−0.0020 (10)	0.0009 (10)	−0.0005 (10)
C8	0.0220 (12)	0.0207 (12)	0.0211 (11)	−0.0022 (9)	0.0049 (10)	−0.0029 (9)
C9	0.0231 (13)	0.0279 (13)	0.0299 (13)	0.0016 (10)	0.0038 (11)	0.0025 (11)
C10	0.0327 (15)	0.0310 (14)	0.0281 (13)	0.0003 (11)	0.0049 (12)	0.0062 (11)
C11	0.0218 (12)	0.0298 (14)	0.0357 (14)	0.0006 (10)	0.0018 (11)	−0.0015 (11)
C12	0.0244 (12)	0.0239 (12)	0.0276 (12)	0.0021 (10)	0.0021 (10)	0.0001 (10)
C13	0.0221 (12)	0.0196 (11)	0.0239 (11)	0.0022 (9)	0.0052 (10)	−0.0018 (9)
C14	0.0236 (13)	0.0400 (16)	0.0303 (14)	−0.0012 (11)	−0.0012 (11)	0.0065 (12)
C15	0.0301 (15)	0.0444 (17)	0.0380 (15)	−0.0010 (13)	0.0040 (12)	0.0174 (13)
C16	0.0285 (14)	0.0295 (14)	0.0489 (17)	−0.0025 (11)	0.0062 (13)	−0.0090 (13)
C17	0.0244 (13)	0.0289 (13)	0.0348 (14)	0.0008 (11)	0.0044 (11)	−0.0053 (11)
C18	0.0196 (12)	0.0215 (12)	0.0308 (12)	0.0033 (9)	0.0042 (10)	0.0001 (10)
C19	0.0265 (14)	0.0435 (17)	0.0313 (14)	−0.0006 (12)	0.0039 (12)	0.0077 (12)
C20	0.0342 (16)	0.0523 (19)	0.0401 (16)	0.0019 (14)	0.0115 (14)	0.0157 (15)

Geometric parameters (Å, º)

Mo1—O6	1.7041 (19)	N1—C5	1.328 (4)
Mo1—O8	1.7045 (19)	N1—H1	0.88
Mo1—O10	1.9073 (17)	N2—C10	1.332 (4)
Mo1—O15	1.9518 (17)	N2—C6	1.337 (4)
Mo1—O18	2.2191 (17)	N2—H2	0.88
Mo1—O17	2.4114 (17)	N3—C11	1.327 (4)
Mo2—O1	1.7024 (19)	N3—C15	1.330 (4)
Mo2—O23	1.7155 (18)	N3—H3	0.88
Mo2—O21	1.9174 (18)	N4—C16	1.331 (4)
Mo2—O11	1.9251 (18)	N4—C20	1.341 (4)
Mo2—O9	2.2839 (17)	N4—H4	0.88
Mo2—O2	2.3637 (17)	C1—C2	1.372 (4)
Mo3—O3	1.693 (2)	C1—H1A	0.95
Mo3—O5	1.701 (2)	C2—C3	1.389 (4)
Mo3—O21	1.9409 (18)	C2—H2A	0.95
Mo3—O12	1.9427 (18)	C3—C4	1.382 (4)
Mo3—O2	2.2283 (17)	C3—C8	1.487 (3)
Mo3—O13	2.4613 (17)	C4—C5	1.376 (4)
Mo4—O20	1.7026 (17)	C4—H4A	0.95
Mo4—O22	1.7270 (17)	C5—H5	0.95
Mo4—O12	1.8766 (18)	C6—C7	1.374 (4)
Mo4—O10	1.9204 (17)	C6—H6	0.95
Mo4—O13	2.3396 (17)	C7—C8	1.387 (4)
Mo4—O17	2.3515 (17)	C7—H7	0.95
Mo5—O16	1.7020 (18)	C8—C9	1.390 (4)
Mo5—O19	1.7084 (18)	C9—C10	1.379 (4)
Mo5—O11	1.8962 (18)	C9—H9	0.95
Mo5—O15	1.9532 (17)	C10—H10	0.95
Mo5—O14	2.2703 (17)	C11—C12	1.374 (4)
Mo5—O18	2.3952 (17)	C11—H11	0.95
P1—O14	1.5134 (18)	C12—C13	1.391 (4)
P1—O17	1.5365 (18)	C12—H12	0.95
P1—O2	1.5369 (17)	C13—C14	1.396 (4)
P1—O4	1.5606 (18)	C13—C18	1.479 (3)
P2—O9	1.5152 (17)	C14—C15	1.380 (4)
P2—O13	1.5242 (17)	C14—H14	0.95
P2—O18	1.5333 (17)	C15—H15	0.95
P2—O7	1.5674 (17)	C16—C17	1.363 (4)
O4—H21	0.84	C16—H16	0.95
O7—H22	0.84	C17—C18	1.385 (4)
O1W—H5A	0.97	C17—H17	0.95
O1W—H5B	0.96	C18—C19	1.399 (4)
O1W—H5C	0.97	C19—C20	1.379 (4)
O2W—H6A	0.99	C19—H19	0.95
O2W—H6B	0.99	C20—H20	0.95
N1—C1	1.328 (4)
O6—Mo1—O8	105.34 (10)	P2—O9—Mo2	122.16 (9)
O6—Mo1—O10	101.73 (8)	Mo1—O10—Mo4	123.52 (9)
O8—Mo1—O10	98.53 (8)	Mo5—O11—Mo2	150.13 (10)
O6—Mo1—O15	94.65 (8)	Mo4—O12—Mo3	125.75 (9)
O8—Mo1—O15	100.26 (8)	P2—O13—Mo4	127.63 (10)
O10—Mo1—O15	150.77 (7)	P2—O13—Mo3	123.99 (9)
O6—Mo1—O18	158.81 (8)	Mo4—O13—Mo3	90.12 (6)
O8—Mo1—O18	93.99 (8)	P1—O14—Mo5	119.48 (9)
O10—Mo1—O18	83.52 (7)	Mo1—O15—Mo5	122.24 (8)
O15—Mo1—O18	73.04 (6)	P1—O17—Mo4	125.47 (9)
O6—Mo1—O17	89.01 (8)	P1—O17—Mo1	128.83 (10)
O8—Mo1—O17	164.57 (8)	Mo4—O17—Mo1	90.13 (6)
O10—Mo1—O17	72.50 (6)	P2—O18—Mo1	129.10 (10)
O15—Mo1—O17	83.87 (6)	P2—O18—Mo5	133.78 (10)
O18—Mo1—O17	72.85 (6)	Mo1—O18—Mo5	95.56 (6)
O1—Mo2—O23	102.46 (9)	Mo2—O21—Mo3	124.29 (9)
O1—Mo2—O21	101.49 (9)	H5A—O1W—H5B	109.9
O23—Mo2—O21	100.41 (8)	H5A—O1W—H5C	105.2
O1—Mo2—O11	98.20 (9)	H5B—O1W—H5C	144.7
O23—Mo2—O11	103.47 (8)	H6A—O2W—H6B	106.9
O21—Mo2—O11	144.79 (7)	C1—N1—C5	122.5 (3)
O1—Mo2—O9	174.32 (8)	C1—N1—H1	118.8
O23—Mo2—O9	83.16 (8)	C5—N1—H1	118.8
O21—Mo2—O9	78.04 (7)	C10—N2—C6	122.0 (2)
O11—Mo2—O9	79.53 (7)	C10—N2—H2	119.0
O1—Mo2—O2	89.87 (8)	C6—N2—H2	119.0
O23—Mo2—O2	164.98 (8)	C11—N3—C15	123.2 (2)
O21—Mo2—O2	68.32 (6)	C11—N3—H3	118.4
O11—Mo2—O2	82.92 (7)	C15—N3—H3	118.4
O9—Mo2—O2	84.70 (6)	C16—N4—C20	123.2 (3)
O3—Mo3—O5	104.46 (12)	C16—N4—H4	118.4
O3—Mo3—O21	98.28 (9)	C20—N4—H4	118.4
O5—Mo3—O21	100.25 (9)	N1—C1—C2	120.3 (3)
O3—Mo3—O12	101.29 (9)	N1—C1—H1A	119.9
O5—Mo3—O12	96.34 (9)	C2—C1—H1A	119.9
O21—Mo3—O12	150.23 (7)	C1—C2—C3	119.1 (3)
O3—Mo3—O2	154.95 (9)	C1—C2—H2A	120.5
O5—Mo3—O2	99.78 (10)	C3—C2—H2A	120.5
O21—Mo3—O2	70.99 (7)	C4—C3—C2	118.8 (2)
O12—Mo3—O2	81.98 (7)	C4—C3—C8	120.5 (2)
O3—Mo3—O13	85.16 (9)	C2—C3—C8	120.7 (2)
O5—Mo3—O13	164.92 (9)	C5—C4—C3	119.7 (3)
O21—Mo3—O13	89.61 (7)	C5—C4—H4A	120.2
O12—Mo3—O13	70.08 (6)	C3—C4—H4A	120.2
O2—Mo3—O13	72.52 (6)	N1—C5—C4	119.7 (3)
O20—Mo4—O22	102.57 (9)	N1—C5—H5	120.2
O20—Mo4—O12	101.94 (8)	C4—C5—H5	120.2
O22—Mo4—O12	102.86 (8)	N2—C6—C7	120.4 (3)
O20—Mo4—O10	99.22 (8)	N2—C6—H6	119.8
O22—Mo4—O10	98.78 (8)	C7—C6—H6	119.8
O12—Mo4—O10	145.43 (7)	C6—C7—C8	119.1 (2)
O20—Mo4—O13	89.28 (7)	C6—C7—H7	120.5
O22—Mo4—O13	168.14 (7)	C8—C7—H7	120.5
O12—Mo4—O13	73.99 (7)	C7—C8—C9	119.3 (2)
O10—Mo4—O13	79.29 (7)	C7—C8—C3	120.7 (2)
O20—Mo4—O17	169.55 (7)	C9—C8—C3	120.0 (2)
O22—Mo4—O17	86.33 (7)	C10—C9—C8	119.1 (3)
O12—Mo4—O17	81.07 (7)	C10—C9—H9	120.4
O10—Mo4—O17	73.72 (7)	C8—C9—H9	120.4
O13—Mo4—O17	81.89 (6)	N2—C10—C9	120.1 (3)
O16—Mo5—O19	102.73 (9)	N2—C10—H10	119.9
O16—Mo5—O11	106.15 (9)	C9—C10—H10	119.9
O19—Mo5—O11	100.13 (8)	N3—C11—C12	119.5 (3)
O16—Mo5—O15	99.01 (8)	N3—C11—H11	120.2
O19—Mo5—O15	98.37 (8)	C12—C11—H11	120.2
O11—Mo5—O15	144.41 (7)	C11—C12—C13	119.8 (2)
O16—Mo5—O14	85.93 (8)	C11—C12—H12	120.1
O19—Mo5—O14	170.78 (8)	C13—C12—H12	120.1
O11—Mo5—O14	80.16 (7)	C12—C13—C14	118.6 (2)
O15—Mo5—O14	76.91 (7)	C12—C13—C18	120.8 (2)
O16—Mo5—O18	167.66 (8)	C14—C13—C18	120.5 (2)
O19—Mo5—O18	82.72 (8)	C15—C14—C13	119.0 (3)
O11—Mo5—O18	83.45 (6)	C15—C14—H14	120.5
O15—Mo5—O18	69.06 (6)	C13—C14—H14	120.5
O14—Mo5—O18	88.17 (6)	N3—C15—C14	119.8 (3)
O14—P1—O17	110.84 (10)	N3—C15—H15	120.1
O14—P1—O2	109.63 (10)	C14—C15—H15	120.1
O17—P1—O2	111.07 (9)	N4—C16—C17	119.5 (3)
O14—P1—O4	110.65 (11)	N4—C16—H16	120.2
O17—P1—O4	109.33 (11)	C17—C16—H16	120.2
O2—P1—O4	105.19 (11)	C16—C17—C18	120.1 (3)
O9—P2—O13	111.86 (10)	C16—C17—H17	120.0
O9—P2—O18	109.36 (10)	C18—C17—H17	120.0
O13—P2—O18	112.63 (10)	C17—C18—C19	119.0 (2)
O9—P2—O7	108.03 (10)	C17—C18—C13	120.8 (2)
O13—P2—O7	106.11 (10)	C19—C18—C13	120.2 (2)
O18—P2—O7	108.65 (10)	C20—C19—C18	118.8 (3)
P1—O2—Mo3	129.94 (10)	C20—C19—H19	120.6
P1—O2—Mo2	133.75 (10)	C18—C19—H19	120.6
Mo3—O2—Mo2	95.91 (6)	N4—C20—C19	119.4 (3)
P1—O4—H21	109.5	N4—C20—H20	120.3
P2—O7—H22	109.5	C19—C20—H20	120.3
O14—P1—O2—Mo3	−176.12 (11)	O11—Mo5—O15—Mo1	−39.14 (17)
O17—P1—O2—Mo3	−53.29 (15)	O14—Mo5—O15—Mo1	−90.36 (10)
O4—P1—O2—Mo3	64.89 (15)	O18—Mo5—O15—Mo1	2.73 (8)
O14—P1—O2—Mo2	−5.27 (16)	O14—P1—O17—Mo4	155.65 (10)
O17—P1—O2—Mo2	117.56 (13)	O2—P1—O17—Mo4	33.52 (14)
O4—P1—O2—Mo2	−124.26 (14)	O4—P1—O17—Mo4	−82.12 (13)
O3—Mo3—O2—P1	110.1 (2)	O14—P1—O17—Mo1	30.40 (15)
O5—Mo3—O2—P1	−84.55 (14)	O2—P1—O17—Mo1	−91.73 (13)
O21—Mo3—O2—P1	177.89 (15)	O4—P1—O17—Mo1	152.64 (11)
O12—Mo3—O2—P1	10.55 (13)	O20—Mo4—O17—P1	−89.7 (4)
O13—Mo3—O2—P1	82.10 (13)	O22—Mo4—O17—P1	121.51 (13)
O3—Mo3—O2—Mo2	−63.3 (2)	O12—Mo4—O17—P1	17.86 (11)
O5—Mo3—O2—Mo2	102.08 (8)	O10—Mo4—O17—P1	−138.24 (13)
O21—Mo3—O2—Mo2	4.52 (6)	O13—Mo4—O17—P1	−57.09 (11)
O12—Mo3—O2—Mo2	−162.82 (7)	O20—Mo4—O17—Mo1	50.8 (4)
O13—Mo3—O2—Mo2	−91.27 (6)	O22—Mo4—O17—Mo1	−98.01 (7)
O1—Mo2—O2—P1	79.95 (15)	O12—Mo4—O17—Mo1	158.35 (7)
O23—Mo2—O2—P1	−134.6 (3)	O10—Mo4—O17—Mo1	2.25 (6)
O21—Mo2—O2—P1	−177.62 (16)	O13—Mo4—O17—Mo1	83.40 (6)
O11—Mo2—O2—P1	−18.33 (13)	O6—Mo1—O17—P1	−121.35 (13)
O9—Mo2—O2—P1	−98.41 (14)	O8—Mo1—O17—P1	79.9 (3)
O1—Mo2—O2—Mo3	−107.09 (8)	O10—Mo1—O17—P1	136.03 (13)
O23—Mo2—O2—Mo3	38.4 (3)	O15—Mo1—O17—P1	−26.56 (12)
O21—Mo2—O2—Mo3	−4.66 (7)	O18—Mo1—O17—P1	47.55 (11)
O11—Mo2—O2—Mo3	154.63 (7)	O6—Mo1—O17—Mo4	100.35 (8)
O9—Mo2—O2—Mo3	74.56 (6)	O8—Mo1—O17—Mo4	−58.4 (3)
O13—P2—O9—Mo2	−64.72 (13)	O10—Mo1—O17—Mo4	−2.28 (6)
O18—P2—O9—Mo2	60.76 (13)	O15—Mo1—O17—Mo4	−164.87 (6)
O7—P2—O9—Mo2	178.85 (10)	O18—Mo1—O17—Mo4	−90.76 (6)
O1—Mo2—O9—P2	−4.4 (9)	O9—P2—O18—Mo1	−171.70 (11)
O23—Mo2—O9—P2	−176.36 (13)	O13—P2—O18—Mo1	−46.66 (15)
O21—Mo2—O9—P2	81.43 (12)	O7—P2—O18—Mo1	70.59 (14)
O11—Mo2—O9—P2	−71.25 (11)	O9—P2—O18—Mo5	−9.58 (16)
O2—Mo2—O9—P2	12.51 (11)	O13—P2—O18—Mo5	115.46 (13)
O6—Mo1—O10—Mo4	−81.83 (12)	O7—P2—O18—Mo5	−127.29 (13)
O8—Mo1—O10—Mo4	170.45 (11)	O6—Mo1—O18—P2	112.6 (2)
O15—Mo1—O10—Mo4	40.9 (2)	O8—Mo1—O18—P2	−91.35 (14)
O18—Mo1—O10—Mo4	77.36 (10)	O10—Mo1—O18—P2	6.79 (12)
O17—Mo1—O10—Mo4	3.35 (9)	O15—Mo1—O18—P2	169.12 (14)
O20—Mo4—O10—Mo1	−175.50 (11)	O17—Mo1—O18—P2	80.43 (12)
O22—Mo4—O10—Mo1	80.13 (11)	O6—Mo1—O18—Mo5	−54.5 (2)
O12—Mo4—O10—Mo1	−48.27 (18)	O8—Mo1—O18—Mo5	101.52 (8)
O13—Mo4—O10—Mo1	−88.00 (10)	O10—Mo1—O18—Mo5	−160.34 (7)
O17—Mo4—O10—Mo1	−3.41 (9)	O15—Mo1—O18—Mo5	1.99 (6)
O16—Mo5—O11—Mo2	139.11 (19)	O17—Mo1—O18—Mo5	−86.70 (6)
O19—Mo5—O11—Mo2	−114.3 (2)	O16—Mo5—O18—P2	−153.0 (3)
O15—Mo5—O11—Mo2	5.9 (3)	O19—Mo5—O18—P2	89.92 (14)
O14—Mo5—O11—Mo2	56.30 (19)	O11—Mo5—O18—P2	−11.21 (13)
O18—Mo5—O11—Mo2	−32.97 (19)	O15—Mo5—O18—P2	−168.19 (15)
O1—Mo2—O11—Mo5	−114.2 (2)	O14—Mo5—O18—P2	−91.51 (14)
O23—Mo2—O11—Mo5	140.78 (19)	O16—Mo5—O18—Mo1	13.2 (4)
O21—Mo2—O11—Mo5	9.4 (3)	O19—Mo5—O18—Mo1	−103.93 (8)
O9—Mo2—O11—Mo5	60.50 (19)	O11—Mo5—O18—Mo1	154.94 (7)
O2—Mo2—O11—Mo5	−25.39 (19)	O15—Mo5—O18—Mo1	−2.04 (6)
O20—Mo4—O12—Mo3	83.35 (12)	O14—Mo5—O18—Mo1	74.64 (6)
O22—Mo4—O12—Mo3	−170.60 (11)	O1—Mo2—O21—Mo3	91.66 (12)
O10—Mo4—O12—Mo3	−43.20 (19)	O23—Mo2—O21—Mo3	−163.19 (11)
O13—Mo4—O12—Mo3	−2.40 (10)	O11—Mo2—O21—Mo3	−31.05 (19)
O17—Mo4—O12—Mo3	−86.47 (11)	O9—Mo2—O21—Mo3	−82.55 (11)
O3—Mo3—O12—Mo4	−78.23 (14)	O2—Mo2—O21—Mo3	6.45 (9)
O5—Mo3—O12—Mo4	175.61 (13)	O3—Mo3—O21—Mo2	149.94 (13)
O21—Mo3—O12—Mo4	51.9 (2)	O5—Mo3—O21—Mo2	−103.64 (13)
O2—Mo3—O12—Mo4	76.57 (11)	O12—Mo3—O21—Mo2	19.2 (2)
O13—Mo3—O12—Mo4	2.34 (9)	O2—Mo3—O21—Mo2	−6.72 (10)
O9—P2—O13—Mo4	149.46 (10)	O13—Mo3—O21—Mo2	64.89 (11)
O18—P2—O13—Mo4	25.80 (15)	C5—N1—C1—C2	−0.2 (5)
O7—P2—O13—Mo4	−92.95 (13)	N1—C1—C2—C3	0.4 (4)
O9—P2—O13—Mo3	27.92 (13)	C1—C2—C3—C4	−0.2 (4)
O18—P2—O13—Mo3	−95.74 (12)	C1—C2—C3—C8	180.0 (3)
O7—P2—O13—Mo3	145.51 (10)	C2—C3—C4—C5	−0.1 (4)
O20—Mo4—O13—P2	123.86 (13)	C8—C3—C4—C5	179.7 (3)
O22—Mo4—O13—P2	−57.4 (4)	C1—N1—C5—C4	−0.1 (5)
O12—Mo4—O13—P2	−133.50 (13)	C3—C4—C5—N1	0.2 (5)
O10—Mo4—O13—P2	24.33 (12)	C10—N2—C6—C7	0.1 (4)
O17—Mo4—O13—P2	−50.53 (12)	N2—C6—C7—C8	0.7 (4)
O20—Mo4—O13—Mo3	−101.10 (7)	C6—C7—C8—C9	−0.6 (4)
O22—Mo4—O13—Mo3	77.7 (4)	C6—C7—C8—C3	179.6 (2)
O12—Mo4—O13—Mo3	1.54 (6)	C4—C3—C8—C7	35.2 (4)
O10—Mo4—O13—Mo3	159.37 (7)	C2—C3—C8—C7	−145.0 (3)
O17—Mo4—O13—Mo3	84.51 (6)	C4—C3—C8—C9	−144.6 (3)
O3—Mo3—O13—P2	−120.11 (13)	C2—C3—C8—C9	35.2 (4)
O5—Mo3—O13—P2	109.4 (3)	C7—C8—C9—C10	−0.2 (4)
O21—Mo3—O13—P2	−21.76 (11)	C3—C8—C9—C10	179.6 (2)
O12—Mo3—O13—P2	136.03 (12)	C6—N2—C10—C9	−0.9 (4)
O2—Mo3—O13—P2	48.40 (11)	C8—C9—C10—N2	1.0 (4)
O3—Mo3—O13—Mo4	102.35 (9)	C15—N3—C11—C12	1.2 (4)
O5—Mo3—O13—Mo4	−28.1 (4)	N3—C11—C12—C13	−0.7 (4)
O21—Mo3—O13—Mo4	−159.31 (7)	C11—C12—C13—C14	−0.2 (4)
O12—Mo3—O13—Mo4	−1.52 (6)	C11—C12—C13—C18	−178.0 (2)
O2—Mo3—O13—Mo4	−89.15 (6)	C12—C13—C14—C15	0.5 (4)
O17—P1—O14—Mo5	−61.89 (13)	C18—C13—C14—C15	178.4 (3)
O2—P1—O14—Mo5	61.08 (13)	C11—N3—C15—C14	−0.9 (5)
O4—P1—O14—Mo5	176.65 (11)	C13—C14—C15—N3	0.0 (5)
O16—Mo5—O14—P1	179.84 (13)	C20—N4—C16—C17	0.5 (5)
O19—Mo5—O14—P1	19.6 (5)	N4—C16—C17—C18	0.2 (4)
O11—Mo5—O14—P1	−72.97 (12)	C16—C17—C18—C19	−1.0 (4)
O15—Mo5—O14—P1	79.61 (12)	C16—C17—C18—C13	179.0 (2)
O18—Mo5—O14—P1	10.69 (11)	C12—C13—C18—C17	−154.0 (2)
O6—Mo1—O15—Mo5	159.52 (11)	C14—C13—C18—C17	28.2 (4)
O8—Mo1—O15—Mo5	−93.95 (11)	C12—C13—C18—C19	26.0 (4)
O10—Mo1—O15—Mo5	35.3 (2)	C14—C13—C18—C19	−151.8 (3)
O18—Mo1—O15—Mo5	−2.88 (9)	C17—C18—C19—C20	1.2 (4)
O17—Mo1—O15—Mo5	71.02 (10)	C13—C18—C19—C20	−178.9 (3)
O16—Mo5—O15—Mo1	−174.01 (11)	C16—N4—C20—C19	−0.4 (5)
O19—Mo5—O15—Mo1	81.58 (11)	C18—C19—C20—N4	−0.5 (5)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H5A···O8^i	0.97	2.07	3.008 (3)	162
O1W—H5B···N4^ii	0.96	2.44	3.135 (4)	129
O2W—H6A···O1^iii	0.99	2.54	3.059 (3)	112
O2W—H6B···O11^iii	0.99	2.25	3.221 (3)	166
O2W—H6B···O16^iii	0.99	2.53	3.121 (4)	118
N1—H1···O22^iv	0.88	1.86	2.728 (3)	170
N3—H3···O9^v	0.88	1.89	2.761 (3)	169
N3—H3···O21^v	0.88	2.43	2.907 (3)	115
N4—H4···O19^vi	0.88	2.17	2.680 (3)	116
N4—H4···O1W^iii	0.88	2.47	3.135 (4)	132
O4—H21···O2W^vii	0.84	1.74	2.538 (3)	159
O7—H22···O1W^viii	0.84	1.98	2.805 (3)	169
N2—H2···O15	0.88	1.75	2.618 (3)	166
O1W—H5C···O23	0.97	2.05	3.009 (3)	173

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