Bis(hexane-1,6-diaminium) di-μ₅-hydrogenphosphato-penta-μ₂-oxo-penta­kis[dioxomolybdenum(VI)] dihydrate

The reaction of hexane-1,6-diamine with sodium molybdate and phospho­ric acid yields the title salt, (C₆H₁₈N₂)₂[Mo₅(HPO₄)₂O₁₅]·2H₂O. Two penta­molybdate anions are linked by hydrogen bonds to form a dimer; the dimers are incorporated into the network structure through hydrogen bonds involving the hexane-1,6-diaminium cations and uncoordinated water mol­ecules.

Key indicators

• Single-crystal X-ray study
• T = 298 K
• Mean [sigma](C-C) = 0.005 Å
• R factor = 0.021
• wR factor = 0.052
• Data-to-parameter ratio = 16.3

checkCIF/PLATON results

No syntax errors found



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 .....................       0.98
PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given .......          ?
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....       2.34
PLAT480_ALERT_4_C Long H...A H-Bond Reported H4C    ..  O7      ..       2.66 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H2C    ..  O1      ..       2.62 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H2C    ..  O15     ..       2.66 Ang.
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         56
            O22 -MO5 -O4  -P1    -14.30  0.60   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         91
            O9  -MO1 -O7  -P2    -32.50  0.70   1.555   1.555   1.555   1.555
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          4
PLAT731_ALERT_1_C Bond    Calc     0.85(3), Rep   0.846(10) ......       3.00 su-Rat
              O1W  -H1WA    1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.85(3), Rep   0.848(10) ......       3.00 su-Rat
              O2W  -H2WA    1.555   1.555
PLAT731_ALERT_1_C Bond    Calc     0.85(3), Rep   0.846(10) ......       3.00 su-Rat
              O2W  -H2WB    1.555   1.555
PLAT732_ALERT_1_C Angle   Calc      110(4), Rep   109.9(17) ......       2.35 su-Rat
              H2WA -O2W  -H2WB    1.555   1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.85(3), Rep   0.848(10) ......       3.00 su-Rat
              O2W  -H3#     1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.85(3), Rep   0.846(10) ......       3.00 su-Rat
              O1W  -H1#     1.555   1.555
PLAT735_ALERT_1_C D-H     Calc     0.85(3), Rep   0.846(10) ......       3.00 su-Rat
              O2W  -H4#     1.555   1.555
PLAT736_ALERT_1_C H...A   Calc     1.99(3), Rep   1.990(11) ......       2.73 su-Rat
              H3#  -O18     1.555   1.655
PLAT736_ALERT_1_C H...A   Calc     1.93(3), Rep   1.930(12) ......       2.50 su-Rat
              H1#  -O2W     1.555   1.556
PLAT736_ALERT_1_C H...A   Calc     1.94(3), Rep   1.944(11) ......       2.73 su-Rat
              H4#  -O9      1.555   1.555
PLAT752_ALERT_4_C Angle   Calc      112.00, Rep  112.43(15) ......  Senseless su
              P2   -O5   -H2      1.555   1.555   1.555

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

  11 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   1 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
   9 ALERT type 4 Improvement, methodology, query or suggestion

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S1. Comment

Pentamolybdates with five-unit MoO₆ octahedra have been reported for pentakis(trioxomolybdophosphate) polyanions in which octahedrons 1 and 2, 2 and 3, 3 and 4, and 4 and 5 share an edge, and octahedrons 1 and 5 have only one common vertex (Harrison et al., 1997a,b). The reaction of 2,5-dimethylpiperazine with phosphoric acid yields the 2,5-dimethylpiperazinium salt of the anionic cluster, which has a hydroxyl group on the P atom. (Zhang et al., 2004). With hexane-1,6-diamine as the structure-directing reagent, the similar reaction affords the title pentamolybdate compound, (C₆H₁₈N₂)₂ [Mo₅O₁₅(HPO₄)₂]^.2H₂O) (I) (Fig. 1). The tetraanions are linked via hydrogen bonds involving the H atom of the hydrogenphosphate group into a dimer (Fig. 2). The dimers are incorporated into the network structure through hydrogen bonds involving the hexane-1,6-diamine cations and uncoordinated water molecules.

S2. Experimental

A mixture of sodium molybdate dihydrate (0.192 g, 0.88 mmol), hexane-1,6-diamine (0.055 g, 0.47 mmol), 1,10-phenanthroline monohydrate (0.059 g, 0.30 mmol), 85% phosphoric acid (0.17 g, 1.47 mmol)and water (6 ml) in the molar ratio of 3:1.6:1:4.9:1100 was sealed in a 15 ml Teflon-lined stainless-steel bomb, which was heated at 175 °C for 6 days. The bomb was cooled to room temperature, affording prismatic crystals in 50% yield. Anal. Calc. for C₁₂H₄₂Mo₅N₄O₂₅P₂: C 12.17, H 3.58, N 4.73%. Found: C 12.02, H 3.72, N 4.59%.

S3. Refinement

The water and phosphate H atoms were located from the Fourier map. The H atoms belonging to organic groups were placed at calculated positions (N—H = 0.89, C—H = 0.97 Å) and refined using the riding model approximation, with U_iso = 1.2 or 1.5 times U_eq(parent atom).

Computing details

Data collection: SMART (Bruker, 2001); cell refinement: SMART; data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

Figures

	Fig. 1. ORTEPII (Johnson, 1976) plot of (I), with displacement ellipsoids drawn at the 50% probability level. H atoms are drawn as spheres of arbitrary radii.
	Fig. 2. ORTEPII (Johnson, 1976) plot illustrating the octamolybdate dimer formed by hydrogen bonds (dashed lines). H atoms are drawn as spheres of arbitrary radii.

Bis(hexane-1,6-diaminium) di-µ₅-hydrogenphosphato-penta-µ₂-oxo-pentakis[dioxomolybdenum(VI)] dihydrate

Crystal data

(C6H18N2)2[Mo5(HPO4)2O15]·2H2O	Z = 2
Mr = 1184.14	F(000) = 1164
Triclinic, P1	Dx = 2.278 Mg m^−3
a = 11.0814 (13) Å	Mo Kα radiation, λ = 0.71073 Å
b = 11.9500 (14) Å	Cell parameters from 3258 reflections
c = 14.2178 (17) Å	θ = 2.2–28.3°
α = 103.038 (2)°	µ = 1.96 mm^−1
β = 100.388 (2)°	T = 298 K
γ = 103.746 (1)°	Block, white
V = 1726.4 (4) Å^3	0.30 × 0.30 × 0.19 mm

Data collection

Bruker APEX area-detector diffractometer	7331 independent reflections
Radiation source: fine-focus sealed tube	6893 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.018
ϕ and ω scans	θmax = 27.0°, θmin = 1.5°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −13→14
Tmin = 0.592, Tmax = 0.708	k = −15→15
18401 measured reflections	l = −18→18

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)] = 0.021	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.052	H atoms treated by a mixture of independent and constrained refinement
S = 1.06	w = 1/[σ^2(Fo^2) + (0.021P)^2 + 1.6423P] where P = (Fo^2 + 2Fc^2)/3
7331 reflections	(Δ/σ)max = 0.001
451 parameters	Δρmax = 0.64 e Å^−3
6 restraints	Δρmin = −0.46 e Å^−3

Special details

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
Mo1	0.724772 (19)	0.360740 (19)	0.348093 (15)	0.01855 (5)
Mo2	0.53546 (2)	0.078184 (19)	0.304419 (16)	0.02015 (5)
Mo3	0.225995 (19)	0.074755 (18)	0.232153 (15)	0.01856 (5)
Mo4	0.217794 (19)	0.345237 (19)	0.195145 (15)	0.01871 (5)
Mo5	0.52000 (2)	0.512165 (18)	0.223109 (15)	0.01866 (5)
P1	0.45983 (6)	0.22159 (5)	0.12942 (4)	0.01660 (12)
P2	0.43636 (6)	0.33866 (5)	0.38983 (4)	0.01543 (12)
O1	0.45500 (17)	0.11628 (16)	0.03979 (13)	0.0249 (4)
H1	0.5049	0.1327	0.0029	0.065 (13)*
O1W	0.6463 (2)	0.16511 (18)	0.95445 (15)	0.0309 (4)
H1WA	0.703 (3)	0.160 (3)	1.0008 (15)	0.052 (11)*
H1WB	0.637 (3)	0.111 (2)	0.9017 (12)	0.034 (9)*
O2	0.55020 (15)	0.21797 (15)	0.22398 (12)	0.0198 (3)
O2W	0.8528 (2)	0.17444 (19)	0.10083 (16)	0.0368 (5)
H2WA	0.9289 (16)	0.203 (3)	0.097 (3)	0.063 (13)*
H2WB	0.841 (3)	0.214 (3)	0.1541 (17)	0.063 (13)*
O3	0.32002 (15)	0.19707 (15)	0.13870 (12)	0.0187 (3)
O4	0.50726 (16)	0.34130 (15)	0.11062 (12)	0.0208 (4)
O5	0.35231 (16)	0.37264 (15)	0.46248 (13)	0.0226 (4)
H2	0.3750	0.4471	0.4916	0.041 (10)*
O6	0.40236 (16)	0.20198 (14)	0.35778 (12)	0.0188 (3)
O7	0.57780 (15)	0.39604 (15)	0.44037 (12)	0.0194 (3)
O8	0.40437 (16)	0.38843 (15)	0.30014 (12)	0.0183 (3)
O9	0.82151 (17)	0.31874 (17)	0.27289 (14)	0.0267 (4)
O10	0.83611 (17)	0.45132 (17)	0.45370 (14)	0.0287 (4)
O11	0.67468 (16)	0.21641 (15)	0.38761 (12)	0.0216 (4)
O12	0.6122 (2)	−0.00165 (19)	0.23628 (15)	0.0373 (5)
O13	0.5099 (2)	0.00901 (17)	0.39514 (15)	0.0342 (5)
O14	0.36751 (16)	0.01253 (15)	0.21385 (12)	0.0212 (4)
O15	0.11610 (17)	−0.00877 (16)	0.12241 (13)	0.0278 (4)
O16	0.17400 (18)	0.01270 (17)	0.31888 (14)	0.0286 (4)
O17	0.17370 (16)	0.21828 (15)	0.25862 (12)	0.0201 (3)
O18	0.10220 (18)	0.28353 (18)	0.08482 (14)	0.0307 (4)
O19	0.15779 (19)	0.43939 (17)	0.26878 (15)	0.0304 (4)
O20	0.33801 (16)	0.45774 (16)	0.15374 (13)	0.0221 (4)
O21	0.58025 (18)	0.58097 (16)	0.14150 (14)	0.0282 (4)
O22	0.51737 (18)	0.63009 (16)	0.31554 (14)	0.0280 (4)
O23	0.66273 (16)	0.46972 (15)	0.29003 (13)	0.0214 (4)
N1	0.0573 (2)	0.3145 (2)	0.40678 (16)	0.0256 (5)
H1C	−0.0111	0.3105	0.3610	0.038*
H1D	0.1159	0.2938	0.3769	0.038*
H1E	0.0899	0.3891	0.4466	0.038*
N2	0.1629 (2)	0.0741 (2)	0.93726 (16)	0.0283 (5)
H2C	0.2117	0.1042	0.9993	0.042*
H2D	0.1578	−0.0032	0.9155	0.042*
H2E	0.0848	0.0817	0.9362	0.042*
N3	−0.3215 (2)	0.4244 (2)	−0.00251 (17)	0.0317 (5)
H3C	−0.3651	0.3470	−0.0204	0.048*
H3D	−0.3105	0.4473	−0.0565	0.048*
H3E	−0.3650	0.4675	0.0293	0.048*
N4	0.3816 (2)	0.7737 (2)	0.41853 (17)	0.0314 (5)
H4C	0.3811	0.7780	0.4818	0.047*
H4D	0.4263	0.8443	0.4147	0.047*
H4E	0.4175	0.7175	0.3953	0.047*
C1	0.0194 (3)	0.2316 (3)	0.4662 (3)	0.0468 (9)
H1A	−0.0178	0.1508	0.4219	0.056*
H1B	−0.0464	0.2534	0.4968	0.056*
C2	0.1265 (3)	0.2318 (3)	0.5451 (2)	0.0425 (8)
H2A	0.1657	0.3133	0.5876	0.051*
H2B	0.1907	0.2074	0.5140	0.051*
C3	0.0900 (3)	0.1519 (3)	0.6089 (3)	0.0472 (9)
H3A	0.0144	0.1657	0.6290	0.057*
H3B	0.0663	0.0692	0.5685	0.057*
C4	0.1890 (3)	0.1667 (4)	0.6995 (3)	0.0489 (9)
H4A	0.2197	0.2508	0.7370	0.059*
H4B	0.2610	0.1437	0.6797	0.059*
C5	0.1412 (3)	0.0926 (3)	0.7671 (2)	0.0385 (7)
H5A	0.0534	0.0917	0.7668	0.046*
H5B	0.1418	0.0105	0.7408	0.046*
C6	0.2209 (3)	0.1406 (3)	0.8716 (2)	0.0312 (6)
H6A	0.2279	0.2251	0.8961	0.037*
H6B	0.3065	0.1331	0.8734	0.037*
C7	−0.1948 (3)	0.4437 (3)	0.0643 (2)	0.0348 (6)
H7A	−0.1487	0.3953	0.0297	0.042*
H7B	−0.2074	0.4168	0.1223	0.042*
C8	−0.1148 (3)	0.5731 (3)	0.0983 (2)	0.0349 (7)
H8A	−0.1586	0.6213	0.1359	0.042*
H8B	−0.1049	0.6013	0.0405	0.042*
C9	0.0169 (3)	0.5892 (3)	0.1629 (2)	0.0350 (7)
H9A	0.0069	0.5709	0.2246	0.042*
H9B	0.0551	0.5321	0.1287	0.042*
C10	0.1075 (3)	0.7148 (3)	0.1872 (2)	0.0376 (7)
H10A	0.0696	0.7713	0.2224	0.045*
H10B	0.1152	0.7334	0.1252	0.045*
C11	0.2420 (3)	0.7337 (3)	0.2500 (2)	0.0337 (6)
H11A	0.2735	0.6677	0.2224	0.040*
H11B	0.2987	0.8070	0.2458	0.040*
C12	0.2466 (3)	0.7421 (3)	0.3576 (2)	0.0361 (7)
H12A	0.2072	0.8026	0.3838	0.043*
H12B	0.1978	0.6658	0.3628	0.043*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Mo1	0.01493 (10)	0.02068 (11)	0.01843 (10)	0.00477 (8)	0.00259 (8)	0.00399 (8)
Mo2	0.02343 (11)	0.01749 (11)	0.01932 (11)	0.00776 (8)	0.00317 (8)	0.00447 (8)
Mo3	0.01823 (10)	0.01624 (10)	0.01991 (11)	0.00280 (8)	0.00532 (8)	0.00440 (8)
Mo4	0.01631 (10)	0.02157 (11)	0.02016 (11)	0.00621 (8)	0.00441 (8)	0.00893 (8)
Mo5	0.01861 (10)	0.01741 (10)	0.02020 (11)	0.00409 (8)	0.00480 (8)	0.00697 (8)
P1	0.0164 (3)	0.0182 (3)	0.0144 (3)	0.0042 (2)	0.0044 (2)	0.0035 (2)
P2	0.0165 (3)	0.0152 (3)	0.0141 (3)	0.0045 (2)	0.0039 (2)	0.0033 (2)
O1	0.0271 (10)	0.0240 (9)	0.0198 (9)	0.0044 (7)	0.0097 (7)	−0.0008 (7)
O1W	0.0340 (11)	0.0297 (11)	0.0253 (10)	0.0082 (9)	0.0092 (9)	0.0000 (8)
O2	0.0180 (8)	0.0214 (9)	0.0193 (8)	0.0049 (7)	0.0030 (7)	0.0067 (7)
O2W	0.0329 (12)	0.0362 (12)	0.0362 (12)	0.0069 (9)	0.0090 (9)	0.0029 (9)
O3	0.0158 (8)	0.0214 (9)	0.0183 (8)	0.0043 (7)	0.0043 (6)	0.0054 (7)
O4	0.0229 (9)	0.0211 (9)	0.0186 (8)	0.0051 (7)	0.0073 (7)	0.0058 (7)
O5	0.0229 (9)	0.0206 (9)	0.0218 (9)	0.0042 (7)	0.0096 (7)	0.0001 (7)
O6	0.0220 (9)	0.0164 (8)	0.0170 (8)	0.0054 (7)	0.0034 (7)	0.0038 (6)
O7	0.0179 (8)	0.0203 (9)	0.0168 (8)	0.0040 (7)	0.0026 (6)	0.0018 (7)
O8	0.0187 (8)	0.0183 (8)	0.0189 (8)	0.0050 (7)	0.0047 (6)	0.0074 (7)
O9	0.0224 (9)	0.0327 (10)	0.0265 (9)	0.0105 (8)	0.0080 (7)	0.0068 (8)
O10	0.0223 (9)	0.0300 (10)	0.0260 (10)	0.0043 (8)	−0.0009 (7)	0.0017 (8)
O11	0.0204 (9)	0.0230 (9)	0.0207 (9)	0.0081 (7)	0.0014 (7)	0.0061 (7)
O12	0.0402 (12)	0.0353 (11)	0.0371 (12)	0.0222 (10)	0.0080 (9)	0.0010 (9)
O13	0.0430 (12)	0.0276 (10)	0.0298 (10)	0.0062 (9)	0.0026 (9)	0.0127 (8)
O14	0.0229 (9)	0.0164 (8)	0.0216 (9)	0.0055 (7)	0.0039 (7)	0.0016 (7)
O15	0.0245 (9)	0.0257 (10)	0.0255 (10)	0.0013 (8)	0.0022 (7)	0.0017 (8)
O16	0.0312 (10)	0.0262 (10)	0.0290 (10)	0.0036 (8)	0.0111 (8)	0.0111 (8)
O17	0.0193 (8)	0.0220 (9)	0.0223 (9)	0.0075 (7)	0.0085 (7)	0.0084 (7)
O18	0.0234 (10)	0.0391 (11)	0.0271 (10)	0.0043 (8)	0.0002 (8)	0.0140 (9)
O19	0.0356 (11)	0.0312 (11)	0.0365 (11)	0.0194 (9)	0.0174 (9)	0.0160 (9)
O20	0.0200 (9)	0.0246 (9)	0.0240 (9)	0.0069 (7)	0.0046 (7)	0.0120 (7)
O21	0.0303 (10)	0.0253 (10)	0.0299 (10)	0.0043 (8)	0.0094 (8)	0.0117 (8)
O22	0.0287 (10)	0.0240 (10)	0.0299 (10)	0.0084 (8)	0.0069 (8)	0.0040 (8)
O23	0.0177 (8)	0.0203 (9)	0.0252 (9)	0.0039 (7)	0.0042 (7)	0.0072 (7)
N1	0.0237 (11)	0.0311 (12)	0.0247 (11)	0.0097 (9)	0.0074 (9)	0.0101 (9)
N2	0.0292 (12)	0.0304 (12)	0.0228 (11)	0.0072 (10)	0.0046 (9)	0.0056 (9)
N3	0.0288 (12)	0.0400 (14)	0.0286 (12)	0.0069 (10)	0.0086 (10)	0.0160 (11)
N4	0.0408 (14)	0.0295 (13)	0.0227 (11)	0.0107 (10)	0.0056 (10)	0.0064 (10)
C1	0.0331 (17)	0.062 (2)	0.048 (2)	0.0025 (15)	0.0065 (14)	0.0366 (18)
C2	0.0347 (17)	0.054 (2)	0.0374 (17)	0.0020 (14)	0.0031 (13)	0.0269 (15)
C3	0.0407 (18)	0.056 (2)	0.0403 (18)	−0.0016 (16)	0.0008 (14)	0.0291 (16)
C4	0.0321 (17)	0.074 (3)	0.0449 (19)	0.0063 (16)	0.0078 (14)	0.0373 (19)
C5	0.0277 (15)	0.054 (2)	0.0333 (16)	0.0042 (14)	0.0024 (12)	0.0247 (15)
C6	0.0321 (15)	0.0293 (15)	0.0343 (15)	0.0089 (12)	0.0105 (12)	0.0111 (12)
C7	0.0345 (16)	0.0350 (16)	0.0340 (16)	0.0090 (13)	0.0019 (12)	0.0143 (13)
C8	0.0372 (16)	0.0300 (15)	0.0355 (16)	0.0124 (13)	−0.0006 (13)	0.0102 (12)
C9	0.0357 (16)	0.0305 (15)	0.0380 (16)	0.0114 (13)	0.0007 (13)	0.0128 (13)
C10	0.0415 (17)	0.0292 (15)	0.0370 (17)	0.0083 (13)	−0.0006 (13)	0.0097 (13)
C11	0.0365 (16)	0.0313 (15)	0.0302 (15)	0.0065 (12)	0.0043 (12)	0.0091 (12)
C12	0.0350 (16)	0.0391 (17)	0.0336 (16)	0.0089 (13)	0.0109 (13)	0.0094 (13)

Geometric parameters (Å, º)

Mo1—O10	1.7066 (18)	N1—H1E	0.8900
Mo1—O9	1.7238 (18)	N2—C6	1.490 (3)
Mo1—O23	1.8857 (17)	N2—H2C	0.8900
Mo1—O11	1.9218 (17)	N2—H2D	0.8900
Mo1—O7	2.3236 (17)	N2—H2E	0.8900
Mo1—O2	2.3683 (17)	N3—C7	1.481 (4)
Mo2—O12	1.6841 (19)	N3—H3C	0.8900
Mo2—O13	1.7114 (19)	N3—H3D	0.8900
Mo2—O14	1.9297 (17)	N3—H3E	0.8900
Mo2—O11	1.9383 (17)	N4—C12	1.499 (4)
Mo2—O2	2.2191 (17)	N4—H4C	0.8900
Mo2—O6	2.4236 (17)	N4—H4D	0.8900
Mo3—O16	1.6936 (18)	N4—H4E	0.8900
Mo3—O15	1.7170 (18)	C1—C2	1.478 (4)
Mo3—O17	1.9180 (17)	C1—H1A	0.9700
Mo3—O14	1.9220 (17)	C1—H1B	0.9700
Mo3—O6	2.3292 (16)	C2—C3	1.496 (4)
Mo3—O3	2.3747 (16)	C2—H2A	0.9700
Mo4—O19	1.6968 (19)	C2—H2B	0.9700
Mo4—O18	1.7174 (18)	C3—C4	1.480 (4)
Mo4—O20	1.9280 (17)	C3—H3A	0.9700
Mo4—O17	1.9440 (17)	C3—H3B	0.9700
Mo4—O8	2.1913 (16)	C4—C5	1.528 (4)
Mo4—O3	2.3879 (17)	C4—H4A	0.9700
Mo5—O22	1.7063 (18)	C4—H4B	0.9700
Mo5—O21	1.7079 (18)	C5—C6	1.489 (4)
Mo5—O23	1.9289 (17)	C5—H5A	0.9700
Mo5—O20	1.9578 (17)	C5—H5B	0.9700
Mo5—O4	2.2484 (17)	C6—H6A	0.9700
Mo5—O8	2.3161 (16)	C6—H6B	0.9700
P1—O4	1.5033 (18)	C7—C8	1.505 (4)
P1—O2	1.5406 (17)	C7—H7A	0.9700
P1—O3	1.5424 (17)	C7—H7B	0.9700
P1—O1	1.5590 (18)	C8—C9	1.521 (4)
P2—O7	1.5179 (17)	C8—H8A	0.9700
P2—O6	1.5256 (17)	C8—H8B	0.9700
P2—O8	1.5442 (17)	C9—C10	1.518 (4)
P2—O5	1.5610 (17)	C9—H9A	0.9700
O1—H1	0.85	C9—H9B	0.9700
O1W—H1WA	0.846 (10)	C10—C11	1.529 (4)
O1W—H1WB	0.845 (10)	C10—H10A	0.9700
O2W—H2WA	0.848 (10)	C10—H10B	0.9700
O2W—H2WB	0.846 (10)	C11—C12	1.500 (4)
O5—H2	0.85	C11—H11A	0.9700
N1—C1	1.477 (4)	C11—H11B	0.9700
N1—H1C	0.8900	C12—H12A	0.9700
N1—H1D	0.8900	C12—H12B	0.9700
O10—Mo1—O9	101.29 (9)	P2—O8—Mo5	135.76 (10)
O10—Mo1—O23	103.53 (8)	Mo4—O8—Mo5	96.64 (6)
O9—Mo1—O23	101.97 (8)	Mo1—O11—Mo2	122.07 (9)
O10—Mo1—O11	100.32 (8)	Mo3—O14—Mo2	123.03 (9)
O9—Mo1—O11	99.12 (8)	Mo3—O17—Mo4	123.95 (9)
O23—Mo1—O11	144.15 (7)	Mo4—O20—Mo5	120.13 (8)
O10—Mo1—O7	84.24 (8)	Mo1—O23—Mo5	149.26 (10)
O9—Mo1—O7	173.49 (8)	C1—N1—H1C	109.5
O23—Mo1—O7	79.85 (7)	C1—N1—H1D	109.5
O11—Mo1—O7	76.33 (7)	H1C—N1—H1D	109.5
O10—Mo1—O2	168.47 (8)	C1—N1—H1E	109.5
O9—Mo1—O2	86.77 (7)	H1C—N1—H1E	109.5
O23—Mo1—O2	82.56 (7)	H1D—N1—H1E	109.5
O11—Mo1—O2	70.01 (6)	C6—N2—H2C	109.5
O7—Mo1—O2	87.27 (6)	C6—N2—H2D	109.5
O12—Mo2—O13	105.07 (11)	H2C—N2—H2D	109.5
O12—Mo2—O14	97.53 (9)	C6—N2—H2E	109.5
O13—Mo2—O14	99.55 (9)	H2C—N2—H2E	109.5
O12—Mo2—O11	102.21 (9)	H2D—N2—H2E	109.5
O13—Mo2—O11	97.30 (8)	C7—N3—H3C	109.5
O14—Mo2—O11	149.66 (7)	C7—N3—H3D	109.5
O12—Mo2—O2	94.98 (9)	H3C—N3—H3D	109.5
O13—Mo2—O2	159.33 (8)	C7—N3—H3E	109.5
O14—Mo2—O2	82.43 (7)	H3C—N3—H3E	109.5
O11—Mo2—O2	73.17 (7)	H3D—N3—H3E	109.5
O12—Mo2—O6	163.84 (8)	C12—N4—H4C	109.5
O13—Mo2—O6	88.94 (8)	C12—N4—H4D	109.5
O14—Mo2—O6	71.77 (6)	H4C—N4—H4D	109.5
O11—Mo2—O6	83.54 (6)	C12—N4—H4E	109.5
O2—Mo2—O6	72.02 (6)	H4C—N4—H4E	109.5
O16—Mo3—O15	104.09 (9)	H4D—N4—H4E	109.5
O16—Mo3—O17	100.42 (8)	N1—C1—C2	113.8 (3)
O15—Mo3—O17	100.96 (8)	N1—C1—H1A	108.8
O16—Mo3—O14	102.62 (8)	C2—C1—H1A	108.8
O15—Mo3—O14	99.43 (8)	N1—C1—H1B	108.8
O17—Mo3—O14	144.29 (7)	C2—C1—H1B	108.8
O16—Mo3—O6	88.14 (8)	H1A—C1—H1B	107.7
O15—Mo3—O6	167.30 (7)	C1—C2—C3	114.9 (3)
O17—Mo3—O6	79.77 (7)	C1—C2—H2A	108.5
O14—Mo3—O6	74.14 (6)	C3—C2—H2A	108.5
O16—Mo3—O3	168.26 (8)	C1—C2—H2B	108.5
O15—Mo3—O3	86.73 (7)	C3—C2—H2B	108.5
O17—Mo3—O3	72.62 (6)	H2A—C2—H2B	107.5
O14—Mo3—O3	79.65 (7)	C4—C3—C2	116.2 (3)
O6—Mo3—O3	81.38 (6)	C4—C3—H3A	108.2
O19—Mo4—O18	105.28 (10)	C2—C3—H3A	108.2
O19—Mo4—O20	100.98 (8)	C4—C3—H3B	108.2
O18—Mo4—O20	98.91 (8)	C2—C3—H3B	108.2
O19—Mo4—O17	93.77 (8)	H3A—C3—H3B	107.4
O18—Mo4—O17	99.22 (8)	C3—C4—C5	113.6 (3)
O20—Mo4—O17	152.65 (7)	C3—C4—H4A	108.8
O19—Mo4—O8	96.40 (8)	C5—C4—H4A	108.8
O18—Mo4—O8	158.05 (8)	C3—C4—H4B	108.8
O20—Mo4—O8	73.18 (7)	C5—C4—H4B	108.8
O17—Mo4—O8	82.45 (7)	H4A—C4—H4B	107.7
O19—Mo4—O3	162.13 (8)	C6—C5—C4	112.6 (3)
O18—Mo4—O3	87.93 (8)	C6—C5—H5A	109.1
O20—Mo4—O3	88.50 (7)	C4—C5—H5A	109.1
O17—Mo4—O3	71.90 (6)	C6—C5—H5B	109.1
O8—Mo4—O3	71.68 (6)	C4—C5—H5B	109.1
O22—Mo5—O21	102.74 (9)	H5A—C5—H5B	107.8
O22—Mo5—O23	99.89 (8)	C5—C6—N2	110.8 (2)
O21—Mo5—O23	103.82 (8)	C5—C6—H6A	109.5
O22—Mo5—O20	98.68 (8)	N2—C6—H6A	109.5
O21—Mo5—O20	99.12 (8)	C5—C6—H6B	109.5
O23—Mo5—O20	146.33 (7)	N2—C6—H6B	109.5
O22—Mo5—O4	172.44 (8)	H6A—C6—H6B	108.1
O21—Mo5—O4	84.63 (8)	N3—C7—C8	112.8 (2)
O23—Mo5—O4	79.68 (7)	N3—C7—H7A	109.0
O20—Mo5—O4	78.28 (7)	C8—C7—H7A	109.0
O22—Mo5—O8	86.93 (8)	N3—C7—H7B	109.0
O21—Mo5—O8	166.56 (8)	C8—C7—H7B	109.0
O23—Mo5—O8	83.35 (6)	H7A—C7—H7B	107.8
O20—Mo5—O8	69.86 (6)	C7—C8—C9	111.6 (2)
O4—Mo5—O8	85.52 (6)	C7—C8—H8A	109.3
O4—P1—O2	108.78 (10)	C9—C8—H8A	109.3
O4—P1—O3	111.58 (10)	C7—C8—H8B	109.3
O2—P1—O3	111.37 (9)	C9—C8—H8B	109.3
O4—P1—O1	111.49 (10)	H8A—C8—H8B	108.0
O2—P1—O1	109.49 (10)	C10—C9—C8	113.5 (2)
O3—P1—O1	104.08 (10)	C10—C9—H9A	108.9
O7—P2—O6	111.68 (10)	C8—C9—H9A	108.9
O7—P2—O8	107.91 (10)	C10—C9—H9B	108.9
O6—P2—O8	111.56 (9)	C8—C9—H9B	108.9
O7—P2—O5	110.65 (10)	H9A—C9—H9B	107.7
O6—P2—O5	106.89 (10)	C9—C10—C11	115.1 (2)
O8—P2—O5	108.12 (10)	C9—C10—H10A	108.5
P1—O1—H1	116.5	C11—C10—H10A	108.5
H1WA—O1W—H1WB	109.7 (16)	C9—C10—H10B	108.5
P1—O2—Mo2	129.90 (10)	C11—C10—H10B	108.5
P1—O2—Mo1	134.60 (10)	H10A—C10—H10B	107.5
Mo2—O2—Mo1	94.76 (6)	C12—C11—C10	113.4 (3)
H2WA—O2W—H2WB	109.9 (17)	C12—C11—H11A	108.9
P1—O3—Mo3	125.64 (9)	C10—C11—H11A	108.9
P1—O3—Mo4	126.03 (9)	C12—C11—H11B	108.9
Mo3—O3—Mo4	91.42 (6)	C10—C11—H11B	108.9
P1—O4—Mo5	120.72 (9)	H11A—C11—H11B	107.7
P2—O5—H2	112.43 (15)	N4—C12—C11	111.7 (2)
P2—O6—Mo3	125.09 (9)	N4—C12—H12A	109.3
P2—O6—Mo2	128.16 (9)	C11—C12—H12A	109.3
Mo3—O6—Mo2	90.82 (6)	N4—C12—H12B	109.3
P2—O7—Mo1	117.78 (9)	C11—C12—H12B	109.3
P2—O8—Mo4	127.48 (9)	H12A—C12—H12B	107.9
O4—P1—O2—Mo2	175.08 (11)	O9—Mo1—O7—P2	−32.5 (7)
O3—P1—O2—Mo2	51.70 (15)	O23—Mo1—O7—P2	74.25 (11)
O1—P1—O2—Mo2	−62.86 (14)	O11—Mo1—O7—P2	−78.76 (11)
O4—P1—O2—Mo1	7.59 (16)	O2—Mo1—O7—P2	−8.67 (10)
O3—P1—O2—Mo1	−115.80 (13)	O7—P2—O8—Mo4	−179.50 (11)
O1—P1—O2—Mo1	129.65 (13)	O6—P2—O8—Mo4	57.47 (14)
O12—Mo2—O2—P1	87.98 (14)	O5—P2—O8—Mo4	−59.79 (14)
O13—Mo2—O2—P1	−106.0 (2)	O7—P2—O8—Mo5	5.49 (16)
O14—Mo2—O2—P1	−8.97 (13)	O6—P2—O8—Mo5	−117.53 (13)
O11—Mo2—O2—P1	−170.74 (14)	O5—P2—O8—Mo5	125.21 (13)
O6—Mo2—O2—P1	−82.19 (13)	O19—Mo4—O8—P2	81.04 (13)
O12—Mo2—O2—Mo1	−100.92 (9)	O18—Mo4—O8—P2	−107.9 (2)
O13—Mo2—O2—Mo1	65.1 (2)	O20—Mo4—O8—P2	−179.39 (14)
O14—Mo2—O2—Mo1	162.13 (7)	O17—Mo4—O8—P2	−11.93 (12)
O11—Mo2—O2—Mo1	0.35 (6)	O3—Mo4—O8—P2	−85.30 (12)
O6—Mo2—O2—Mo1	88.90 (6)	O19—Mo4—O8—Mo5	−102.47 (8)
O10—Mo1—O2—P1	136.2 (4)	O18—Mo4—O8—Mo5	68.6 (2)
O9—Mo1—O2—P1	−89.04 (14)	O20—Mo4—O8—Mo5	−2.89 (6)
O23—Mo1—O2—P1	13.48 (14)	O17—Mo4—O8—Mo5	164.56 (7)
O11—Mo1—O2—P1	170.04 (15)	O3—Mo4—O8—Mo5	91.19 (6)
O7—Mo1—O2—P1	93.59 (14)	O22—Mo5—O8—P2	−80.68 (15)
O10—Mo1—O2—Mo2	−34.2 (4)	O21—Mo5—O8—P2	142.8 (3)
O9—Mo1—O2—Mo2	100.56 (8)	O23—Mo5—O8—P2	19.66 (14)
O23—Mo1—O2—Mo2	−156.92 (7)	O20—Mo5—O8—P2	178.92 (16)
O11—Mo1—O2—Mo2	−0.36 (6)	O4—Mo5—O8—P2	99.77 (14)
O7—Mo1—O2—Mo2	−76.81 (6)	O22—Mo5—O8—Mo4	103.31 (8)
O4—P1—O3—Mo3	−152.13 (10)	O21—Mo5—O8—Mo4	−33.2 (3)
O2—P1—O3—Mo3	−30.36 (14)	O23—Mo5—O8—Mo4	−156.35 (7)
O1—P1—O3—Mo3	87.51 (12)	O20—Mo5—O8—Mo4	2.90 (6)
O4—P1—O3—Mo4	−28.13 (14)	O4—Mo5—O8—Mo4	−76.24 (6)
O2—P1—O3—Mo4	93.64 (12)	O10—Mo1—O11—Mo2	173.99 (10)
O1—P1—O3—Mo4	−148.49 (11)	O9—Mo1—O11—Mo2	−82.67 (11)
O16—Mo3—O3—P1	80.8 (4)	O23—Mo1—O11—Mo2	42.84 (18)
O15—Mo3—O3—P1	−121.69 (13)	O7—Mo1—O11—Mo2	92.57 (10)
O17—Mo3—O3—P1	135.75 (13)	O2—Mo1—O11—Mo2	0.49 (8)
O14—Mo3—O3—P1	−21.48 (11)	O12—Mo2—O11—Mo1	91.05 (12)
O6—Mo3—O3—P1	53.85 (11)	O13—Mo2—O11—Mo1	−161.73 (11)
O16—Mo3—O3—Mo4	−57.1 (4)	O14—Mo2—O11—Mo1	−38.4 (2)
O15—Mo3—O3—Mo4	100.43 (8)	O2—Mo2—O11—Mo1	−0.51 (9)
O17—Mo3—O3—Mo4	−2.13 (6)	O6—Mo2—O11—Mo1	−73.64 (10)
O14—Mo3—O3—Mo4	−159.36 (7)	O16—Mo3—O14—Mo2	−79.76 (12)
O6—Mo3—O3—Mo4	−84.04 (6)	O15—Mo3—O14—Mo2	173.37 (11)
O19—Mo4—O3—P1	−97.5 (3)	O17—Mo3—O14—Mo2	49.21 (17)
O18—Mo4—O3—P1	124.09 (12)	O6—Mo3—O14—Mo2	4.60 (9)
O20—Mo4—O3—P1	25.11 (12)	O3—Mo3—O14—Mo2	88.48 (10)
O17—Mo4—O3—P1	−135.52 (13)	O12—Mo2—O14—Mo3	−172.03 (12)
O8—Mo4—O3—P1	−47.66 (11)	O13—Mo2—O14—Mo3	81.21 (12)
O19—Mo4—O3—Mo3	40.1 (3)	O11—Mo2—O14—Mo3	−41.6 (2)
O18—Mo4—O3—Mo3	−98.28 (8)	O2—Mo2—O14—Mo3	−77.98 (10)
O20—Mo4—O3—Mo3	162.74 (7)	O6—Mo2—O14—Mo3	−4.48 (9)
O17—Mo4—O3—Mo3	2.11 (6)	O16—Mo3—O17—Mo4	173.41 (11)
O8—Mo4—O3—Mo3	89.97 (6)	O15—Mo3—O17—Mo4	−79.87 (12)
O2—P1—O4—Mo5	−61.12 (13)	O14—Mo3—O17—Mo4	43.88 (18)
O3—P1—O4—Mo5	62.14 (13)	O6—Mo3—O17—Mo4	87.24 (10)
O1—P1—O4—Mo5	178.05 (10)	O3—Mo3—O17—Mo4	3.16 (9)
O22—Mo5—O4—P1	−14.3 (6)	O19—Mo4—O17—Mo3	−172.24 (11)
O21—Mo5—O4—P1	178.31 (13)	O18—Mo4—O17—Mo3	81.60 (12)
O23—Mo5—O4—P1	73.19 (11)	O20—Mo4—O17—Mo3	−49.4 (2)
O20—Mo5—O4—P1	−81.19 (11)	O8—Mo4—O17—Mo3	−76.28 (10)
O8—Mo5—O4—P1	−10.85 (11)	O3—Mo4—O17—Mo3	−3.15 (9)
O7—P2—O6—Mo3	−156.91 (10)	O19—Mo4—O20—Mo5	97.37 (11)
O8—P2—O6—Mo3	−36.06 (14)	O18—Mo4—O20—Mo5	−155.04 (11)
O5—P2—O6—Mo3	81.93 (12)	O17—Mo4—O20—Mo5	−24.0 (2)
O7—P2—O6—Mo2	−31.86 (14)	O8—Mo4—O20—Mo5	3.93 (9)
O8—P2—O6—Mo2	88.99 (12)	O3—Mo4—O20—Mo5	−67.37 (10)
O5—P2—O6—Mo2	−153.01 (11)	O22—Mo5—O20—Mo4	−87.27 (11)
O16—Mo3—O6—P2	−119.46 (13)	O21—Mo5—O20—Mo4	168.23 (11)
O15—Mo3—O6—P2	75.9 (4)	O23—Mo5—O20—Mo4	35.59 (19)
O17—Mo3—O6—P2	−18.52 (11)	O4—Mo5—O20—Mo4	85.70 (10)
O14—Mo3—O6—P2	136.86 (13)	O8—Mo5—O20—Mo4	−3.79 (8)
O3—Mo3—O6—P2	55.24 (11)	O10—Mo1—O23—Mo5	−137.74 (19)
O16—Mo3—O6—Mo2	100.61 (8)	O9—Mo1—O23—Mo5	117.37 (19)
O15—Mo3—O6—Mo2	−64.0 (4)	O11—Mo1—O23—Mo5	−7.4 (3)
O17—Mo3—O6—Mo2	−158.45 (7)	O7—Mo1—O23—Mo5	−56.25 (19)
O14—Mo3—O6—Mo2	−3.07 (6)	O2—Mo1—O23—Mo5	32.29 (19)
O3—Mo3—O6—Mo2	−84.69 (6)	O22—Mo5—O23—Mo1	110.6 (2)
O12—Mo2—O6—P2	−84.7 (3)	O21—Mo5—O23—Mo1	−143.56 (19)
O13—Mo2—O6—P2	124.74 (13)	O20—Mo5—O23—Mo1	−12.0 (3)
O14—Mo2—O6—P2	−134.84 (13)	O4—Mo5—O23—Mo1	−61.76 (19)
O11—Mo2—O6—P2	27.27 (12)	O8—Mo5—O23—Mo1	24.88 (19)
O2—Mo2—O6—P2	−47.08 (11)	N1—C1—C2—C3	177.9 (3)
O12—Mo2—O6—Mo3	53.2 (3)	C1—C2—C3—C4	−169.0 (4)
O13—Mo2—O6—Mo3	−97.32 (8)	C2—C3—C4—C5	173.7 (3)
O14—Mo2—O6—Mo3	3.10 (6)	C3—C4—C5—C6	−158.4 (3)
O11—Mo2—O6—Mo3	165.21 (7)	C4—C5—C6—N2	173.8 (3)
O2—Mo2—O6—Mo3	90.86 (6)	N3—C7—C8—C9	−177.4 (3)
O6—P2—O7—Mo1	61.39 (12)	C7—C8—C9—C10	172.1 (3)
O8—P2—O7—Mo1	−61.56 (12)	C8—C9—C10—C11	−178.7 (3)
O5—P2—O7—Mo1	−179.66 (9)	C9—C10—C11—C12	−74.7 (4)
O10—Mo1—O7—P2	179.13 (12)	C10—C11—C12—N4	−173.9 (2)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N4—H4C···O11^i	0.89	2.05	2.917 (3)	163
N4—H4C···O13^i	0.89	2.60	3.077 (3)	114
N4—H4C···O7^i	0.89	2.66	3.207 (3)	121
N4—H4D···O13^ii	0.89	2.07	2.955 (3)	173
N4—H4E···O22	0.89	2.02	2.871 (3)	160
N1—H1C···O9^iii	0.89	2.08	2.961 (3)	171
N1—H1D···O17	0.89	2.01	2.831 (3)	153
N1—H1D···O5	0.89	2.53	3.088 (3)	122
N1—H1E···O10^i	0.89	1.98	2.871 (3)	175
N2—H2C···O3^iv	0.89	2.03	2.912 (3)	171
N2—H2C···O1^iv	0.89	2.62	3.169 (3)	121
N2—H2C···O15^iv	0.89	2.66	3.099 (3)	112
N2—H2D···O2W^v	0.89	1.98	2.853 (3)	167
N2—H2E···O15^vi	0.89	2.12	2.915 (3)	149
N3—H3C···O1W^vii	0.89	2.16	2.940 (3)	146
N3—H3D···O20^viii	0.89	2.00	2.826 (3)	153
N3—H3E···O21^iii	0.89	2.13	2.987 (3)	163
O2W—H2WA···O18^ix	0.85 (1)	1.99 (1)	2.835 (3)	174 (4)
O1W—H1WA···O2W^iv	0.85 (1)	1.93 (1)	2.764 (3)	169 (4)
O1W—H1WB···O14^v	0.85 (1)	1.93 (1)	2.771 (3)	175 (3)
O2W—H2WB···O9	0.85 (1)	1.94 (1)	2.787 (3)	174 (4)
O1—H1···O1W^x	0.85	1.817	2.639 (3)	163.06
O5—H2···O7^i	0.85	1.805	2.650 (2)	176.97

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