Tris(ethyl-enediammonium) bis-[(2-amino-ethyl)ammonium] bis-[bis-(μ(5)-hydrogen phosphato)penta-μ(2)-oxido-deca-oxido-penta-molybdenum(VI)] deca-hydrate.

The title compound, (C(2)H(10)N(2))(3)(C(2)H(9)N(2))(2)[Mo(5)(HPO(4))(2)O(15)]·10H(2)O, was prepared under hydro-thermal conditions at pH 5.0. The structure contains mono- and diprotonated ethyl-enediamine cations, [Mo(5)O(15)(HPO(4))(2)](4-) anions and uncoord-in-ated water mol-ecules. The [Mo(5)O(15)(HPO(4))(2)](4-) hetero-poly-oxometallate anion is made up of five MoO(6) octa-hedra sharing an edge and forming a ring, which is closed by common corners of the terminal MoO(6) octa-hedron. The ring is topped on both sides by two slightly distorted PO(4) tetra-hedra, sharing three corners with three MoO(6) octa-hedra. The terminal oxygen atoms of the PO(4) units are protonated. Together with the anions, the water mol-ecules and the ethyl-enediammonium cations are involved in N-H⋯O and O-H⋯O hydrogen bonding, forming a three-dimensional supra-molecular network.

Related literature

For background to polyoxometalates, see: Coronado & Gomez-Garcia (1998 ▶); Niu et al. (2009 ▶); Ruether et al. (2003 ▶). For the structure of (C2H10N2)2[Mo5O15(HPO4)2], see: Sun et al. (2003 ▶). For structures containing the [Mo5O15(PO4)2]6− anion, see: Gong et al. (2006 ▶); Skibsted et al. (2000 ▶). For the bond-valence method, see: Brown (2002 ▶).

Experimental

Crystal data

(C2H10N2)3(C2H9N2)2[Mo5(HPO4)2O15]·10H2O

M = 2312.06

Triclinic,

a = 10.0045 (11) Å

b = 10.6625 (12) Å

c = 15.1884 (19) Å

α = 87.405 (2)°

β = 73.119 (1)°

γ = 77.978 (1)°

V = 1516.2 (3) Å3

Z = 1

Mo Kα radiation

μ = 2.23 mm−1

T = 298 K

0.38 × 0.34 × 0.30 mm

Data collection

Siemens SMART CCD area-detector diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.485, T max = 0.554

7582 measured reflections

5253 independent reflections

4015 reflections with I > 2σ(I)

R int = 0.033

Refinement

R[F 2 > 2σ(F 2)] = 0.041

wR(F 2) = 0.114

S = 1.04

5253 reflections

396 parameters

5 restraints

H-atom parameters constrained

Δρmax = 1.28 e Å−3

Δρmin = −1.07 e Å−3

Data collection: SMART (Siemens, 1996 ▶); cell refinement: SAINT (Siemens, 1996 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablocks global, I. DOI: 10.1107/S160053681001545X/wm2326sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S160053681001545X/wm2326Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

(C2H10N2)3(C2H9N2)2[Mo5(HPO4)2O15]·10H2O	Z = 1
Mr = 2312.06	F(000) = 1130
Triclinic, P1	Dx = 2.532 Mg m−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 10.0045 (11) Å	Cell parameters from 5253 reflections
b = 10.6625 (12) Å	θ = 1.4–25.0°
c = 15.1884 (19) Å	µ = 2.23 mm−1
α = 87.405 (2)°	T = 298 K
β = 73.119 (1)°	Block, blue
γ = 77.978 (1)°	0.38 × 0.34 × 0.30 mm
V = 1516.2 (3) Å3

Siemens SMART CCD area-detector diffractometer	5253 independent reflections
Radiation source: fine-focus sealed tube	4015 reflections with I > 2σ(I)
graphite	Rint = 0.033
phi and ω scans	θmax = 25.0°, θmin = 1.4°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −11→11
Tmin = 0.485, Tmax = 0.554	k = −12→12
7582 measured reflections	l = −16→18

Refinement on F2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.041	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.114	H-atom parameters constrained
S = 1.03	w = 1/[σ2(Fo2) + (0.0528P)2 + 3.4931P] where P = (Fo2 + 2Fc2)/3
5253 reflections	(Δ/σ)max = 0.001
396 parameters	Δρmax = 1.28 e Å−3
5 restraints	Δρmin = −1.06 e Å−3

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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.

	x	y	z	Uiso*/Ueq
Mo1	0.68911 (6)	0.98073 (6)	0.29463 (4)	0.01950 (16)
Mo2	0.70040 (6)	0.66797 (6)	0.33717 (4)	0.01926 (16)
Mo3	1.04111 (6)	0.51146 (6)	0.24970 (4)	0.01935 (16)
Mo4	1.25353 (6)	0.72000 (6)	0.16806 (4)	0.01859 (16)
Mo5	1.06247 (6)	1.02104 (6)	0.22185 (4)	0.02026 (17)
P1	0.96988 (18)	0.79447 (17)	0.37213 (12)	0.0172 (4)
P2	0.92311 (18)	0.77833 (17)	0.13393 (12)	0.0173 (4)
O1	0.9504 (5)	0.7503 (5)	0.4712 (3)	0.0252 (11)
H1F	0.9730	0.6690	0.4724	0.030*
O2	0.8247 (5)	0.8134 (4)	0.3492 (3)	0.0194 (10)
O3	1.0838 (4)	0.6931 (4)	0.3051 (3)	0.0165 (10)
O4	1.0145 (5)	0.9234 (4)	0.3588 (3)	0.0204 (11)
O5	0.9720 (5)	0.7288 (5)	0.0357 (3)	0.0253 (11)
H5F	0.9054	0.7121	0.0184	0.030*
O6	0.7953 (5)	0.8908 (4)	0.1520 (3)	0.0196 (10)
O7	0.8823 (5)	0.6662 (4)	0.1989 (3)	0.0185 (10)
O8	1.0447 (5)	0.8278 (4)	0.1577 (3)	0.0203 (10)
O9	0.6217 (5)	1.0335 (5)	0.4066 (3)	0.0306 (12)
O10	0.5760 (5)	1.0780 (5)	0.2421 (3)	0.0276 (12)
O11	0.6061 (5)	0.8291 (4)	0.3003 (3)	0.0198 (10)
O12	0.8564 (5)	1.0536 (5)	0.2577 (3)	0.0247 (11)
O13	0.6085 (5)	0.6714 (5)	0.4513 (3)	0.0317 (13)
O14	0.6344 (6)	0.5618 (5)	0.2884 (4)	0.0328 (13)
O15	0.8706 (5)	0.5525 (4)	0.3514 (3)	0.0210 (11)
O16	1.0008 (5)	0.4019 (5)	0.1883 (4)	0.0297 (12)
O17	1.1447 (5)	0.4220 (5)	0.3112 (4)	0.0307 (12)
O18	1.1771 (5)	0.5751 (4)	0.1505 (3)	0.0207 (11)
O19	1.3806 (5)	0.6492 (5)	0.2178 (4)	0.0325 (13)
O20	1.3464 (5)	0.7417 (5)	0.0556 (3)	0.0299 (12)
O21	1.2370 (5)	0.8958 (5)	0.2099 (3)	0.0219 (11)
O22	1.0926 (6)	1.1388 (5)	0.2799 (4)	0.0321 (13)
O23	1.0943 (5)	1.0763 (5)	0.1119 (3)	0.0320 (13)
O24	0.3296 (8)	0.1763 (7)	0.4162 (5)	0.076 (2)
H24A	0.2419	0.2141	0.4404	0.091*
H24B	0.3264	0.1133	0.3838	0.091*
O25	0.3181 (5)	0.9219 (5)	0.3693 (3)	0.0301 (12)
H25A	0.4032	0.8802	0.3547	0.036*
H25B	0.2831	0.9163	0.3256	0.036*
O26	0.4289 (7)	0.4016 (6)	0.3250 (4)	0.0511 (16)
H26A	0.4839	0.4443	0.3370	0.061*
H26B	0.3799	0.4467	0.2938	0.061*
O27	0.3488 (8)	0.2320 (9)	0.1809 (5)	0.098 (3)
H27A	0.4030	0.1839	0.2099	0.118*
H27B	0.2619	0.2300	0.2124	0.118*
O28	0.2690 (6)	0.2880 (6)	0.0232 (4)	0.0443 (15)
H28A	0.3305	0.3154	0.0406	0.053*
H28B	0.2403	0.2316	0.0625	0.053*
C1	0.3022 (8)	0.5766 (8)	0.9035 (5)	0.0328 (18)*
H1D	0.3735	0.5145	0.8608	0.039*
H1E	0.3418	0.5931	0.9519	0.039*
C2	0.2697 (9)	0.6994 (8)	0.8535 (5)	0.037 (2)*
H2A	0.3583	0.7180	0.8138	0.045*
H2B	0.2112	0.6877	0.8147	0.045*
C3	0.2894 (8)	0.6276 (8)	0.4831 (6)	0.037 (2)
H3A	0.3200	0.6701	0.4251	0.045*
H3B	0.3715	0.5671	0.4917	0.045*
C4	0.2356 (10)	0.7262 (8)	0.5605 (6)	0.043 (2)
H4A	0.1792	0.6900	0.6149	0.052*
H4B	0.3163	0.7477	0.5752	0.052*
C5	0.5516 (8)	1.0024 (8)	0.0280 (5)	0.0295 (18)
H5A	0.6482	0.9898	−0.0128	0.035*
H5B	0.5289	1.0861	0.0574	0.035*
N1	0.1738 (7)	0.5215 (6)	0.9442 (4)	0.0327 (16)
H1A	0.1043	0.5743	0.9849	0.049*
H1B	0.2007	0.4508	0.9739	0.049*
H1C	0.1358	0.4996	0.9021	0.049*
N2	0.1935 (7)	0.8119 (6)	0.9175 (4)	0.0313 (15)
H2C	0.1776	0.8842	0.8863	0.047*
H2D	0.2396	0.8257	0.9571	0.047*
H2E	0.1062	0.7999	0.9507	0.047*
N3	0.1786 (7)	0.5569 (6)	0.4790 (4)	0.0309 (15)
H3C	0.1472	0.5167	0.5312	0.046*
H3D	0.1649	0.5203	0.4333	0.046*
N4	0.1468 (7)	0.8455 (6)	0.5355 (4)	0.0327 (16)
H4C	0.1986	0.8779	0.4852	0.049*
H4D	0.1126	0.9056	0.5792	0.049*
H4E	0.0741	0.8210	0.5231	0.049*
N5	0.5426 (7)	0.9020 (6)	0.0988 (4)	0.0319 (15)
H5C	0.4558	0.9047	0.1371	0.048*
H5D	0.6028	0.9086	0.1306	0.048*
H5E	0.5721	0.8236	0.0713	0.048*

	U11	U22	U33	U12	U13	U23
Mo1	0.0177 (3)	0.0153 (3)	0.0236 (3)	−0.0010 (2)	−0.0049 (3)	0.0023 (2)
Mo2	0.0192 (3)	0.0160 (3)	0.0227 (3)	−0.0047 (3)	−0.0059 (3)	0.0036 (2)
Mo3	0.0209 (3)	0.0136 (3)	0.0234 (3)	−0.0031 (3)	−0.0066 (3)	0.0010 (2)
Mo4	0.0174 (3)	0.0174 (3)	0.0204 (3)	−0.0026 (3)	−0.0052 (2)	0.0006 (2)
Mo5	0.0202 (3)	0.0148 (3)	0.0255 (3)	−0.0046 (3)	−0.0062 (3)	0.0044 (2)
P1	0.0189 (9)	0.0153 (9)	0.0170 (9)	−0.0015 (7)	−0.0059 (7)	0.0003 (7)
P2	0.0183 (9)	0.0173 (10)	0.0165 (9)	−0.0036 (7)	−0.0055 (7)	0.0026 (7)
O1	0.029 (3)	0.020 (3)	0.023 (3)	0.001 (2)	−0.006 (2)	0.001 (2)
O2	0.017 (2)	0.018 (3)	0.023 (3)	−0.002 (2)	−0.007 (2)	0.002 (2)
O3	0.014 (2)	0.013 (2)	0.021 (2)	−0.0014 (19)	−0.0038 (19)	−0.0017 (19)
O4	0.023 (3)	0.015 (3)	0.022 (3)	−0.002 (2)	−0.005 (2)	−0.0026 (19)
O5	0.027 (3)	0.029 (3)	0.021 (3)	−0.008 (2)	−0.007 (2)	0.000 (2)
O6	0.018 (2)	0.022 (3)	0.018 (2)	0.000 (2)	−0.006 (2)	0.002 (2)
O7	0.021 (2)	0.012 (2)	0.023 (3)	−0.007 (2)	−0.005 (2)	0.0036 (19)
O8	0.017 (2)	0.018 (3)	0.027 (3)	−0.006 (2)	−0.008 (2)	0.004 (2)
O9	0.031 (3)	0.027 (3)	0.028 (3)	−0.003 (2)	−0.003 (2)	−0.003 (2)
O10	0.025 (3)	0.020 (3)	0.037 (3)	0.000 (2)	−0.012 (2)	0.005 (2)
O11	0.013 (2)	0.017 (3)	0.028 (3)	−0.001 (2)	−0.005 (2)	0.004 (2)
O12	0.022 (3)	0.017 (3)	0.035 (3)	−0.003 (2)	−0.010 (2)	0.004 (2)
O13	0.029 (3)	0.029 (3)	0.030 (3)	−0.001 (2)	−0.001 (2)	0.003 (2)
O14	0.035 (3)	0.029 (3)	0.041 (3)	−0.015 (3)	−0.017 (3)	0.005 (2)
O15	0.025 (3)	0.015 (3)	0.025 (3)	−0.007 (2)	−0.009 (2)	0.006 (2)
O16	0.030 (3)	0.021 (3)	0.039 (3)	−0.009 (2)	−0.010 (2)	0.002 (2)
O17	0.033 (3)	0.018 (3)	0.044 (3)	−0.001 (2)	−0.019 (3)	0.005 (2)
O18	0.021 (3)	0.018 (3)	0.022 (3)	−0.004 (2)	−0.005 (2)	−0.002 (2)
O19	0.025 (3)	0.027 (3)	0.047 (3)	−0.002 (2)	−0.015 (3)	0.003 (2)
O20	0.029 (3)	0.031 (3)	0.025 (3)	−0.007 (2)	0.000 (2)	−0.003 (2)
O21	0.019 (2)	0.022 (3)	0.024 (3)	−0.005 (2)	−0.005 (2)	0.000 (2)
O22	0.035 (3)	0.025 (3)	0.040 (3)	−0.010 (2)	−0.014 (3)	0.000 (2)
O23	0.034 (3)	0.030 (3)	0.030 (3)	−0.007 (3)	−0.008 (2)	0.014 (2)
O24	0.055 (5)	0.058 (5)	0.094 (6)	−0.007 (4)	0.009 (4)	−0.027 (4)
O25	0.026 (3)	0.033 (3)	0.034 (3)	−0.006 (2)	−0.013 (2)	−0.001 (2)
O26	0.050 (4)	0.044 (4)	0.063 (4)	−0.015 (3)	−0.019 (3)	0.002 (3)
O27	0.059 (5)	0.137 (9)	0.078 (6)	0.019 (5)	−0.020 (5)	0.020 (5)
O28	0.042 (3)	0.032 (4)	0.060 (4)	−0.007 (3)	−0.016 (3)	0.001 (3)
C3	0.028 (4)	0.024 (5)	0.051 (5)	0.002 (4)	−0.003 (4)	0.005 (4)
C4	0.053 (6)	0.039 (6)	0.048 (5)	−0.016 (5)	−0.027 (5)	0.013 (4)
C5	0.035 (4)	0.025 (4)	0.037 (4)	−0.016 (4)	−0.015 (4)	0.006 (3)
N1	0.044 (4)	0.026 (4)	0.025 (3)	−0.003 (3)	−0.007 (3)	0.000 (3)
N2	0.029 (4)	0.025 (4)	0.035 (4)	−0.005 (3)	−0.002 (3)	0.010 (3)
N3	0.048 (4)	0.026 (4)	0.022 (3)	−0.008 (3)	−0.015 (3)	0.006 (3)
N4	0.046 (4)	0.022 (4)	0.031 (4)	−0.010 (3)	−0.008 (3)	−0.009 (3)
N5	0.037 (4)	0.030 (4)	0.034 (4)	−0.010 (3)	−0.015 (3)	−0.003 (3)

Mo1—O9	1.710 (5)	O24—H24B	0.8617
Mo1—O10	1.718 (5)	O25—H25A	0.8451
Mo1—O12	1.917 (5)	O25—H25B	0.8447
Mo1—O11	1.953 (5)	O26—H26A	0.8443
Mo1—O6	2.274 (4)	O26—H26B	0.8435
Mo1—O2	2.285 (4)	O27—H27A	0.8680
Mo2—O13	1.709 (5)	O27—H27B	0.8656
Mo2—O14	1.714 (5)	O28—H28A	0.8421
Mo2—O11	1.924 (4)	O28—H28B	0.8598
Mo2—O15	1.944 (5)	C1—N1	1.482 (10)
Mo2—O2	2.224 (5)	C1—C2	1.508 (10)
Mo2—O7	2.343 (4)	C1—H1D	0.9700
Mo3—O16	1.706 (5)	C1—H1E	0.9700
Mo3—O17	1.711 (5)	C2—N2	1.502 (10)
Mo3—O18	1.919 (5)	C2—H2A	0.9700
Mo3—O15	1.926 (5)	C2—H2B	0.9700
Mo3—O3	2.311 (4)	C3—N3	1.481 (10)
Mo3—O7	2.312 (4)	C3—C4	1.512 (10)
Mo4—O19	1.692 (5)	C3—H3A	0.9700
Mo4—O20	1.722 (5)	C3—H3B	0.9700
Mo4—O18	1.921 (5)	C4—N4	1.494 (10)
Mo4—O21	1.966 (5)	C4—H4A	0.9700
Mo4—O8	2.211 (4)	C4—H4B	0.9700
Mo4—O3	2.322 (4)	C5—N5	1.481 (9)
Mo5—O22	1.690 (5)	C5—C5i	1.525 (14)
Mo5—O23	1.709 (5)	C5—H5A	0.9700
Mo5—O21	1.932 (5)	C5—H5B	0.9700
Mo5—O12	1.933 (5)	N1—H1A	0.8953
Mo5—O4	2.253 (5)	N1—H1B	0.8934
Mo5—O8	2.380 (5)	N1—H1C	0.8952
P1—O4	1.520 (5)	N2—H2C	0.8970
P1—O1	1.526 (5)	N2—H2D	0.8910
P1—O3	1.555 (5)	N2—H2E	0.9044
P1—O2	1.561 (5)	N3—H3C	0.8896
P2—O5	1.511 (5)	N3—H3D	0.8689
P2—O6	1.528 (5)	N4—H4C	0.8901
P2—O8	1.558 (5)	N4—H4D	0.8854
P2—O7	1.560 (5)	N4—H4E	0.8918
O1—H1F	0.8500	N5—H5C	0.8890
O5—H5F	0.8360	N5—H5D	0.8888
O24—H24A	0.8641	N5—H5E	0.9043
O9—Mo1—O10	102.4 (2)	O6—P2—O7	109.2 (3)
O9—Mo1—O12	100.1 (2)	O8—P2—O7	109.4 (3)
O10—Mo1—O12	102.6 (2)	P1—O1—H1F	110.0
O9—Mo1—O11	100.8 (2)	P1—O2—Mo2	129.3 (3)
O10—Mo1—O11	96.4 (2)	P1—O2—Mo1	133.9 (3)
O12—Mo1—O11	147.8 (2)	Mo2—O2—Mo1	96.06 (16)
O9—Mo1—O6	173.2 (2)	P1—O3—Mo3	125.3 (2)
O10—Mo1—O6	84.3 (2)	P1—O3—Mo4	130.2 (3)
O12—Mo1—O6	79.31 (19)	Mo3—O3—Mo4	92.41 (15)
O11—Mo1—O6	77.05 (18)	P1—O4—Mo5	123.0 (3)
O9—Mo1—O2	85.7 (2)	P2—O5—H5F	112.6
O10—Mo1—O2	166.4 (2)	P2—O6—Mo1	121.6 (2)
O12—Mo1—O2	86.43 (18)	P2—O7—Mo3	125.2 (3)
O11—Mo1—O2	71.10 (17)	P2—O7—Mo2	130.2 (3)
O6—Mo1—O2	87.45 (16)	Mo3—O7—Mo2	92.82 (15)
O13—Mo2—O14	104.5 (3)	P2—O8—Mo4	129.5 (3)
O13—Mo2—O11	100.0 (2)	P2—O8—Mo5	134.9 (3)
O14—Mo2—O11	101.2 (2)	Mo4—O8—Mo5	94.63 (16)
O13—Mo2—O15	94.9 (2)	Mo2—O11—Mo1	119.7 (2)
O14—Mo2—O15	98.7 (2)	Mo1—O12—Mo5	146.5 (3)
O11—Mo2—O15	151.31 (19)	Mo3—O15—Mo2	121.2 (2)
O13—Mo2—O2	95.4 (2)	Mo3—O18—Mo4	121.2 (2)
O14—Mo2—O2	160.0 (2)	Mo5—O21—Mo4	120.0 (2)
O11—Mo2—O2	73.01 (18)	H24A—O24—H24B	105.7
O15—Mo2—O2	81.31 (18)	H25A—O25—H25B	108.9
O13—Mo2—O7	162.8 (2)	H26A—O26—H26B	109.4
O14—Mo2—O7	89.0 (2)	H27A—O27—H27B	105.9
O11—Mo2—O7	87.47 (17)	H28A—O28—H28B	106.4
O15—Mo2—O7	72.28 (17)	N1—C1—C2	112.4 (6)
O2—Mo2—O7	71.84 (16)	N1—C1—H1D	109.1
O16—Mo3—O17	104.8 (2)	C2—C1—H1D	109.1
O16—Mo3—O18	98.2 (2)	N1—C1—H1E	109.1
O17—Mo3—O18	103.4 (2)	C2—C1—H1E	109.1
O16—Mo3—O15	102.4 (2)	H1D—C1—H1E	107.9
O17—Mo3—O15	96.2 (2)	N2—C2—C1	113.0 (6)
O18—Mo3—O15	146.9 (2)	N2—C2—H2A	109.0
O16—Mo3—O3	166.0 (2)	C1—C2—H2A	109.0
O17—Mo3—O3	88.1 (2)	N2—C2—H2B	109.0
O18—Mo3—O3	73.27 (17)	C1—C2—H2B	109.0
O15—Mo3—O3	81.00 (18)	H2A—C2—H2B	107.8
O16—Mo3—O7	87.5 (2)	N3—C3—C4	112.0 (7)
O17—Mo3—O7	165.5 (2)	N3—C3—H3A	109.2
O18—Mo3—O7	82.00 (17)	C4—C3—H3A	109.2
O15—Mo3—O7	73.31 (17)	N3—C3—H3B	109.2
O3—Mo3—O7	80.46 (15)	C4—C3—H3B	109.2
O19—Mo4—O20	104.5 (3)	H3A—C3—H3B	107.9
O19—Mo4—O18	100.8 (2)	N4—C4—C3	111.8 (6)
O20—Mo4—O18	99.1 (2)	N4—C4—H4A	109.3
O19—Mo4—O21	96.6 (2)	C3—C4—H4A	109.3
O20—Mo4—O21	95.7 (2)	N4—C4—H4B	109.3
O18—Mo4—O21	153.52 (19)	C3—C4—H4B	109.3
O19—Mo4—O8	158.6 (2)	H4A—C4—H4B	107.9
O20—Mo4—O8	95.8 (2)	N5—C5—C5i	110.7 (8)
O18—Mo4—O8	82.59 (18)	N5—C5—H5A	109.5
O21—Mo4—O8	74.17 (18)	C5i—C5—H5A	109.5
O19—Mo4—O3	88.0 (2)	N5—C5—H5B	109.5
O20—Mo4—O3	166.4 (2)	C5i—C5—H5B	109.5
O18—Mo4—O3	72.96 (17)	H5A—C5—H5B	108.1
O21—Mo4—O3	87.89 (17)	C1—N1—H1A	113.3
O8—Mo4—O3	72.61 (16)	C1—N1—H1B	107.2
O22—Mo5—O23	103.1 (3)	H1A—N1—H1B	107.8
O22—Mo5—O21	100.0 (2)	C1—N1—H1C	113.0
O23—Mo5—O21	99.9 (2)	H1A—N1—H1C	107.1
O22—Mo5—O12	101.7 (2)	H1B—N1—H1C	108.2
O23—Mo5—O12	99.6 (2)	C2—N2—H2C	111.4
O21—Mo5—O12	146.5 (2)	C2—N2—H2D	113.7
O22—Mo5—O4	85.1 (2)	H2C—N2—H2D	108.1
O23—Mo5—O4	171.9 (2)	C2—N2—H2E	110.2
O21—Mo5—O4	78.16 (18)	H2C—N2—H2E	105.6
O12—Mo5—O4	78.63 (18)	H2D—N2—H2E	107.4
O22—Mo5—O8	168.7 (2)	C3—N3—H3C	112.0
O23—Mo5—O8	85.4 (2)	C3—N3—H3D	131.5
O21—Mo5—O8	70.87 (18)	H3C—N3—H3D	110.5
O12—Mo5—O8	83.95 (18)	C4—N4—H4C	109.0
O4—Mo5—O8	86.50 (16)	C4—N4—H4D	114.6
O4—P1—O1	111.1 (3)	H4C—N4—H4D	108.8
O4—P1—O3	109.7 (3)	C4—N4—H4E	105.9
O1—P1—O3	110.0 (3)	H4C—N4—H4E	109.6
O4—P1—O2	106.7 (3)	H4D—N4—H4E	109.0
O1—P1—O2	109.5 (3)	C5—N5—H5C	114.8
O3—P1—O2	109.8 (3)	C5—N5—H5D	108.2
O5—P2—O6	112.9 (3)	H5C—N5—H5D	109.7
O5—P2—O8	110.5 (3)	C5—N5—H5E	109.6
O6—P2—O8	106.4 (3)	H5C—N5—H5E	107.2
O5—P2—O7	108.4 (3)	H5D—N5—H5E	107.0

D—H···A	D—H	H···A	D···A	D—H···A
N5—H5E···O20ii	0.90	2.66	3.075 (8)	109
N5—H5E···O28iii	0.90	2.01	2.796 (9)	144
N5—H5D···O10	0.89	2.45	3.069 (8)	127
N5—H5D···O6	0.89	2.01	2.846 (8)	156
N5—H5C···O21ii	0.89	2.17	3.046 (8)	170
N4—H4E···O1ii	0.89	1.93	2.806 (8)	167
N4—H4D···O12iv	0.89	2.65	3.357 (8)	137
N4—H4D···O22iv	0.89	2.60	3.099 (8)	116
N4—H4D···O4iv	0.89	2.08	2.907 (8)	155
N4—H4C···O25	0.89	1.92	2.803 (8)	171
N3—H3D···O17ii	0.87	2.25	3.117 (8)	176
N3—H3C···O15v	0.89	1.87	2.732 (7)	162
N2—H2E···O23iv	0.90	2.56	3.030 (8)	113
N2—H2E···O5vi	0.90	1.84	2.699 (8)	159
N2—H2D···O20vi	0.89	2.14	2.924 (8)	146
N2—H2C···O6iv	0.90	2.49	3.310 (8)	151
N2—H2C···O12iv	0.90	2.35	3.084 (8)	139
N1—H1C···O7v	0.90	2.46	3.259 (8)	149
N1—H1C···O16v	0.90	2.28	3.011 (8)	138
N1—H1B···O28vii	0.89	1.93	2.819 (8)	173
N1—H1A···O5vi	0.90	1.92	2.772 (8)	159
O28—H28B···O23viii	0.86	2.39	3.157 (8)	149
O28—H28A···O27	0.84	2.31	2.740 (10)	112
O27—H27B···O17ii	0.87	2.46	2.912 (10)	113
O27—H27B···O22viii	0.87	2.11	2.916 (10)	155
O27—H27A···O10ix	0.87	2.03	2.875 (9)	163
O26—H26B···O19ii	0.84	2.40	3.064 (8)	136
O26—H26B···O17ii	0.84	2.36	2.874 (8)	120
O26—H26A···O14	0.84	2.11	2.858 (8)	148
O25—H25B···O21ii	0.84	1.97	2.808 (7)	170
O25—H25B···O4ii	0.84	2.57	3.083 (7)	120
O25—H25A···O11	0.85	1.93	2.745 (7)	163
O24—H24B···O25ix	0.86	2.08	2.868 (9)	151
O24—H24A···O1v	0.86	1.97	2.795 (8)	159
O5—H5F···O28iii	0.84	2.02	2.845 (8)	168
O1—H1F···N3x	0.85	2.18	2.766 (8)	126

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N5—H5E⋯O20i	0.90	2.66	3.075 (8)	109
N5—H5E⋯O28ii	0.90	2.01	2.796 (9)	144
N5—H5D⋯O10	0.89	2.45	3.069 (8)	127
N5—H5D⋯O6	0.89	2.01	2.846 (8)	156
N5—H5C⋯O21i	0.89	2.17	3.046 (8)	170
N4—H4E⋯O1i	0.89	1.93	2.806 (8)	167
N4—H4D⋯O12iii	0.89	2.65	3.357 (8)	137
N4—H4D⋯O22iii	0.89	2.60	3.099 (8)	116
N4—H4D⋯O4iii	0.89	2.08	2.907 (8)	155
N4—H4C⋯O25	0.89	1.92	2.803 (8)	171
N3—H3D⋯O17i	0.87	2.25	3.117 (8)	176
N3—H3C⋯O15iv	0.89	1.87	2.732 (7)	162
N2—H2E⋯O23iii	0.90	2.56	3.030 (8)	113
N2—H2E⋯O5v	0.90	1.84	2.699 (8)	159
N2—H2D⋯O20v	0.89	2.14	2.924 (8)	146
N2—H2C⋯O6iii	0.90	2.49	3.310 (8)	151
N2—H2C⋯O12iii	0.90	2.35	3.084 (8)	139
N1—H1C⋯O7iv	0.90	2.46	3.259 (8)	149
N1—H1C⋯O16iv	0.90	2.28	3.011 (8)	138
N1—H1B⋯O28vi	0.89	1.93	2.819 (8)	173
N1—H1A⋯O5v	0.90	1.92	2.772 (8)	159
O28—H28B⋯O23vii	0.86	2.39	3.157 (8)	149
O28—H28A⋯O27	0.84	2.31	2.740 (10)	112
O27—H27B⋯O17i	0.87	2.46	2.912 (10)	113
O27—H27B⋯O22vii	0.87	2.11	2.916 (10)	155
O27—H27A⋯O10viii	0.87	2.03	2.875 (9)	163
O26—H26B⋯O19i	0.84	2.40	3.064 (8)	136
O26—H26B⋯O17i	0.84	2.36	2.874 (8)	120
O26—H26A⋯O14	0.84	2.11	2.858 (8)	148
O25—H25B⋯O21i	0.84	1.97	2.808 (7)	170
O25—H25B⋯O4i	0.84	2.57	3.083 (7)	120
O25—H25A⋯O11	0.85	1.93	2.745 (7)	163
O24—H24B⋯O25viii	0.86	2.08	2.868 (9)	151
O24—H24A⋯O1iv	0.86	1.97	2.795 (8)	159
O5—H5F⋯O28ii	0.84	2.02	2.845 (8)	168
O1—H1F⋯N3ix	0.85	2.18	2.766 (8)	126

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) ; (vii) ; (viii) ; (ix) .