Bis(amino­{[iminio(morpholino)meth­yl]amino}iminium) bis­(amino­{[imino­(morpholino)meth­yl]amino}iminium) tetra­cosa­oxidotellurohexa­molybdate(6-) tetra­hydrate

The title compound, (H₂ABOB)₂(HABOB)₂[Te^VIMo^VI₆O₂₄]·4H₂O, consists of an Anderson-type heteropolyanion, [Te^VIMo^VI₆O₂₄]^6-, two monoprotonated ABOB cations, two diprotonated ABOB cations and four water mol­ecules (ABOB = N-amidino-4-morpholincarboxamidine). The hetero­polyanion [Te^VIMo^VI₆O₂₄]^6- is located on an inversion center. Electrostatic forces and hydrogen-bonding inter­actions among the [Te^VIMo^VI₆O₂₄]^6-anions, the water mol­ecules and the ABOB cations result in a three-dimensional supra­molecular structure.

Key indicators

• Single-crystal X-ray study
• T = 298 K
• Mean [sigma](C-C) = 0.005 Å
• R factor = 0.025
• wR factor = 0.056
• Data-to-parameter ratio = 13.0

checkCIF/PLATON results

No syntax errors found



Datablock: I


Alert level B
PLAT432_ALERT_2_B Short Inter X...Y Contact  O4     ..  C8      ..       2.90 Ang.

Alert level C
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  Te1    -   Mo1     ..       5.96 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  Te1    -   Mo3     ..       7.14 su
PLAT414_ALERT_2_C Short Intra D-H..H-X       H9A    ..  H17     ..       1.94 Ang.
PLAT420_ALERT_2_C D-H Without Acceptor       N6     -   H12    ...          ?
PLAT432_ALERT_2_C Short Inter X...Y Contact  O9     ..  C11     ..       2.94 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H2     ..  O12     ..       2.61 Ang.

Alert level G
PLAT794_ALERT_5_G Check Predicted Bond Valency for Te1         (6)       5.86
PLAT794_ALERT_5_G Check Predicted Bond Valency for Mo1         (6)       5.94
PLAT794_ALERT_5_G Check Predicted Bond Valency for Mo2         (6)       5.98
PLAT794_ALERT_5_G Check Predicted Bond Valency for Mo3         (6)       5.99

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

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   6 ALERT type 2 Indicator that the structure model may be wrong or deficient
   0 ALERT type 3 Indicator that the structure quality may be low
   1 ALERT type 4 Improvement, methodology, query or suggestion
   4 ALERT type 5 Informative message, check

---

S1. Comment

N-Amidino-4-morpholincarboxamidine (ABOB) is an effective broad-spectrum antiviral medicine to influenza, chickenpox and measles. In our chemical studies (Chen et al., 2007; Li et al., 2005; Liu et al., 2004), we found it is a versatile ligand capable of interacting with different types of polyanions. As a part of our ongoing work, we have investigated the reaction of ABOB and the Anderson type [Te^VIMo^VI₆O₂₄]^6- polyanion to give a compound formulated as (H₂ABOB)₂(HABOB)₂[Te^VIMo^VI₆O₂₄]^.4H₂O (I).

The compound consists of [Te^VIMo^VI₆O₂₄]^6-, protonated ABOB, and lattice water molecules. The three-dimensional supramolecular structure is formed by electrostatic forces and hydrogen bonding interactions among these components (Fig. 1). The [Te^VIMo^VI₆O₂₄]^6- anion lies on an inversion center and is close to having D_{3 d} symmetry. It is made up of six MoO₆ octahedra surrounding one TeO₆ octahedron by entirely edge-shared contacts; bond lengths and angles are in accordance with those of reported examples (Drewes et al., 2004; Gao et al., 2006) The diprotonated ABOB acquires two protons with its two imine groups (N2, N4). The monoprotonated ABOB acquires two protons with two imine groups (N6, N9) as well but loses one proton on the third imine groups (N8). Electrostatic forces and hydrogen bonding interactions result in a three-dimensional supramolecular structure (Figure 2, Figure 3). The hydrogen-bond donors are the protonated imines groups and water molecules whereas the acceptors are mostly the O atoms of the Anderson type polyanion.

Related literature

Similar structures have been reported, see: Chen et al. (2007); Li et al. (2005); Liu et al. (2004); Drewes et al. (2004); Gao et al. (2006). For the synthesis of the [Te^VI^Mo^VI^~6Õ~24~]^6-^ polyanion see Saito (1994).

S2. Experimental

A mixture of Na₆[Te^VIMo^VI₆O₂₄]^6-.22H₂O (0.32 g, 0.2 mmol) (Saito, 1994)) and ABOB (0.21 g, 1.2 mmol) in water (30 ml) treated with dilute hydrochloric acid to pH 5–6. The solution was stirred for 2 h. It was then filtered; the filtrate was set aside for the formation of crystals after two weeks; yield 65% based on Te.

S3. Refinement

The H atoms on water molecules, amine, and protonated imine groups were located in a difference Fourier map, and refined with distance restraints of with O–H = 0.85 Å, N–H = 0.90 Å and U_iso(H) = 1.2 U_eq(O,N). Those on C atoms are placed in calculated positions and refined in the riding model approximation with C–H = 0.97 Å and U_iso(H) = 1.2U_eq(C).

Computing details

Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO; data reduction: PROCESS-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 1998); software used to prepare material for publication: SHELXTL (Bruker, 2001).

Figures

	Fig. 1. ORTEP view of (I) with displacement ellipsoids drawn at 50% probability level. [Symmetry code: (i) 2 - x, 2 - y, -z.]
	Fig. 2. Hydrogen bonds (yellow dotted line) around a polyanion which is represented as polyhedra.
	Fig. 3. The crystal packing in a unit cell, with hydrogen bonds showed as yellow dotted line and polyanions represented as polyhedra.

Bis(amino{[iminio(morpholino)methyl]amino}iminium) bis(amino{[imino(morpholino)methyl]amino}iminium) tetracosaoxidotellurohexamolybdate(6-) tetrahydrate

Crystal data

(C6H15N5O)2(C6H14N5O)2[TeMo6O24].4H2O	F(000) = 1820
Mr = 1850.21	Dx = 2.205 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 875 reflections
a = 15.722 (3) Å	θ = 3.1–25.0°
b = 9.2364 (18) Å	µ = 1.93 mm^−1
c = 19.256 (4) Å	T = 298 K
β = 94.67 (3)°	Block, white
V = 2787.0 (10) Å^3	0.24 × 0.24 × 0.22 mm
Z = 2

Data collection

Rigaku R-AXIS RAPID IP diffractometer	4883 independent reflections
Radiation source: fine-focus sealed tube	4465 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.030
Detector resolution: 0 pixels mm^-1	θmax = 25.0°, θmin = 3.1°
ω scans	h = −18→18
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	k = −10→10
Tmin = 0.643, Tmax = 0.657	l = −22→22
20771 measured reflections

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.025	H-atom parameters constrained
wR(F^2) = 0.056	w = 1/[σ^2(Fo^2) + (0.0189P)^2 + 3.249P] where P = (Fo^2 + 2Fc^2)/3
S = 1.09	(Δ/σ)max = 0.002
4883 reflections	Δρmax = 0.63 e Å^−3
377 parameters	Δρmin = −0.86 e Å^−3
0 restraints	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.00488 (13)

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
Te1	1.0000	1.0000	0.0000	0.01336 (7)
Mo1	0.840705 (14)	0.97463 (2)	−0.121498 (12)	0.01725 (8)
Mo2	0.962462 (15)	1.03579 (3)	0.163987 (12)	0.01902 (8)
Mo3	0.804183 (14)	1.00883 (2)	0.045455 (12)	0.01829 (8)
O1	1.06718 (11)	0.87503 (19)	−0.05424 (9)	0.0177 (4)
O2	0.89805 (11)	0.88611 (19)	−0.01551 (9)	0.0166 (4)
O3	0.96442 (11)	1.09343 (19)	−0.08720 (9)	0.0176 (4)
O4	0.91282 (14)	1.1756 (2)	0.20215 (11)	0.0333 (5)
O5	0.92935 (12)	0.8616 (2)	−0.15719 (9)	0.0212 (4)
O6	0.75632 (13)	1.1543 (2)	0.08024 (11)	0.0330 (5)
O7	0.76252 (12)	0.8424 (2)	−0.12693 (11)	0.0276 (5)
O8	0.72660 (13)	0.8813 (2)	0.02944 (11)	0.0323 (5)
O9	0.99343 (13)	0.9194 (2)	0.22975 (10)	0.0296 (5)
O10	0.79802 (11)	1.09461 (19)	−0.04971 (9)	0.0192 (4)
O11	0.81680 (13)	1.0896 (2)	−0.18973 (10)	0.0293 (5)
O12	0.86502 (12)	0.9258 (2)	0.12556 (9)	0.0219 (4)
O13	0.51701 (15)	0.1569 (3)	−0.10142 (15)	0.0582 (8)
O14	0.70371 (14)	1.0881 (2)	0.31912 (13)	0.0397 (6)
O1W	0.96255 (14)	0.6375 (2)	0.11550 (12)	0.0370 (5)
H1	0.9889	0.7141	0.1055	0.044*
H2	0.9140	0.6556	0.1301	0.044*
O2W	1.07989 (17)	0.4426 (3)	0.18435 (15)	0.0540 (7)
H3	1.0676	0.3607	0.1661	0.065*
H4	1.0434	0.4979	0.1629	0.065*
N1	0.83492 (18)	0.6090 (3)	−0.03895 (14)	0.0344 (6)
H5	0.8712	0.6705	−0.0155	0.041*
H6	0.7979	0.6376	−0.0744	0.041*
N2	0.90623 (15)	0.4192 (3)	0.01555 (13)	0.0282 (6)
H7	0.9353	0.4823	0.0441	0.034*
H8	0.9136	0.3237	0.0232	0.034*
N3	0.79856 (16)	0.3705 (3)	−0.06762 (13)	0.0277 (6)
H9	0.8008	0.2776	−0.0534	0.033*
N4	0.75224 (18)	0.4803 (3)	−0.17227 (14)	0.0354 (6)
H10	0.8071	0.5025	−0.1774	0.042*
H11	0.7113	0.5017	−0.2061	0.042*
N5	0.65933 (16)	0.3408 (3)	−0.11197 (13)	0.0300 (6)
N6	1.0938 (2)	0.7734 (4)	0.45693 (18)	0.0577 (9)
H12	1.0669	0.7843	0.4961	0.069*
H13	1.1469	0.7363	0.4607	0.069*
N7	1.08581 (17)	0.7464 (3)	0.33860 (16)	0.0453 (8)
H14	1.1380	0.7059	0.3425	0.054*
H15	1.0642	0.7675	0.2950	0.054*
N8	0.96948 (16)	0.8341 (3)	0.39610 (14)	0.0358 (6)
N9	0.90343 (17)	0.6720 (3)	0.31506 (16)	0.0418 (7)
H16	0.9432	0.6051	0.3279	0.050*
H17	0.8657	0.6575	0.2780	0.050*
N10	0.84324 (15)	0.8936 (3)	0.33528 (13)	0.0263 (5)
C1	0.5878 (2)	0.1522 (4)	−0.05053 (19)	0.0438 (9)
H1A	0.6283	0.0799	−0.0637	0.053*
H1B	0.5684	0.1246	−0.0058	0.053*
C2	0.5475 (2)	0.1889 (5)	−0.1672 (2)	0.0537 (10)
H2A	0.4998	0.1879	−0.2026	0.064*
H2B	0.5872	0.1140	−0.1788	0.064*
C3	0.5913 (2)	0.3336 (4)	−0.16842 (18)	0.0416 (8)
H3A	0.6151	0.3470	−0.2129	0.050*
H3B	0.5502	0.4103	−0.1629	0.050*
C4	0.6308 (2)	0.2974 (4)	−0.04428 (17)	0.0381 (8)
H4A	0.5912	0.3689	−0.0288	0.046*
H4B	0.6794	0.2925	−0.0099	0.046*
C5	0.7344 (2)	0.4006 (3)	−0.11897 (15)	0.0263 (6)
C6	0.84770 (18)	0.4686 (3)	−0.03086 (15)	0.0228 (6)
C7	0.7724 (2)	1.1139 (4)	0.3706 (2)	0.0452 (9)
H7A	0.7575	1.0754	0.4149	0.054*
H7B	0.7806	1.2175	0.3761	0.054*
C8	0.6910 (2)	0.9357 (3)	0.31187 (19)	0.0371 (8)
H8A	0.6423	0.9178	0.2788	0.045*
H8B	0.6784	0.8954	0.3564	0.045*
C9	0.76780 (19)	0.8614 (4)	0.28752 (17)	0.0320 (7)
H9A	0.7582	0.7577	0.2858	0.038*
H9B	0.7774	0.8942	0.2409	0.038*
C10	0.8540 (2)	1.0472 (4)	0.35268 (18)	0.0367 (8)
H10A	0.8746	1.0980	0.3133	0.044*
H10B	0.8964	1.0573	0.3919	0.044*
C11	0.90742 (19)	0.8001 (3)	0.34730 (16)	0.0288 (7)
C12	1.0479 (2)	0.7821 (4)	0.39541 (19)	0.0372 (8)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Te1	0.01484 (13)	0.01183 (12)	0.01295 (13)	−0.00084 (8)	−0.00163 (9)	0.00035 (9)
Mo1	0.01854 (13)	0.01554 (13)	0.01677 (13)	−0.00164 (9)	−0.00401 (9)	0.00015 (9)
Mo2	0.02178 (14)	0.02072 (14)	0.01437 (13)	−0.00030 (9)	0.00025 (9)	−0.00023 (9)
Mo3	0.01674 (13)	0.01865 (13)	0.01923 (13)	−0.00111 (9)	0.00005 (9)	0.00082 (9)
O1	0.0194 (9)	0.0156 (9)	0.0179 (9)	0.0014 (7)	0.0009 (7)	−0.0018 (8)
O2	0.0170 (9)	0.0144 (9)	0.0179 (9)	−0.0031 (7)	−0.0019 (7)	0.0007 (7)
O3	0.0196 (9)	0.0168 (9)	0.0157 (9)	−0.0010 (7)	−0.0036 (7)	0.0028 (8)
O4	0.0345 (12)	0.0342 (12)	0.0315 (11)	0.0043 (9)	0.0054 (9)	−0.0070 (10)
O5	0.0244 (10)	0.0188 (9)	0.0201 (9)	−0.0027 (8)	−0.0005 (8)	−0.0035 (8)
O6	0.0318 (12)	0.0371 (12)	0.0298 (11)	0.0105 (9)	0.0017 (9)	−0.0031 (10)
O7	0.0233 (10)	0.0250 (10)	0.0334 (11)	−0.0050 (8)	−0.0051 (9)	−0.0030 (9)
O8	0.0286 (12)	0.0341 (12)	0.0329 (11)	−0.0120 (9)	−0.0046 (9)	0.0071 (10)
O9	0.0335 (12)	0.0330 (12)	0.0216 (10)	−0.0047 (9)	−0.0028 (9)	0.0083 (9)
O10	0.0194 (10)	0.0149 (9)	0.0226 (9)	0.0018 (7)	−0.0021 (7)	0.0017 (8)
O11	0.0361 (12)	0.0257 (11)	0.0245 (11)	0.0008 (9)	−0.0077 (9)	0.0050 (9)
O12	0.0221 (10)	0.0234 (10)	0.0202 (10)	−0.0035 (8)	0.0014 (8)	0.0042 (8)
O13	0.0313 (14)	0.076 (2)	0.0657 (18)	−0.0082 (13)	−0.0048 (12)	0.0279 (16)
O14	0.0301 (12)	0.0254 (11)	0.0622 (16)	0.0041 (9)	−0.0047 (11)	0.0019 (11)
O1W	0.0405 (13)	0.0229 (11)	0.0482 (14)	−0.0051 (9)	0.0074 (11)	−0.0027 (11)
O2W	0.0557 (17)	0.0388 (14)	0.0658 (18)	−0.0077 (12)	−0.0047 (14)	0.0036 (14)
N1	0.0478 (17)	0.0171 (12)	0.0358 (15)	−0.0010 (11)	−0.0125 (12)	0.0008 (11)
N2	0.0320 (14)	0.0203 (12)	0.0307 (14)	−0.0021 (10)	−0.0074 (11)	0.0000 (11)
N3	0.0379 (15)	0.0123 (11)	0.0306 (13)	−0.0008 (10)	−0.0105 (11)	0.0038 (10)
N4	0.0389 (16)	0.0341 (15)	0.0312 (15)	−0.0047 (12)	−0.0085 (12)	0.0095 (12)
N5	0.0314 (14)	0.0328 (14)	0.0249 (13)	0.0016 (11)	−0.0042 (11)	0.0049 (11)
N6	0.0385 (18)	0.078 (2)	0.053 (2)	0.0157 (17)	−0.0173 (15)	0.0055 (19)
N7	0.0240 (15)	0.060 (2)	0.0519 (19)	0.0129 (13)	0.0017 (13)	0.0115 (16)
N8	0.0272 (14)	0.0463 (17)	0.0325 (14)	0.0086 (12)	−0.0049 (11)	−0.0024 (13)
N9	0.0308 (15)	0.0335 (15)	0.0598 (19)	0.0085 (12)	−0.0045 (14)	−0.0079 (14)
N10	0.0199 (12)	0.0285 (13)	0.0299 (13)	0.0014 (10)	−0.0011 (10)	−0.0025 (11)
C1	0.0363 (19)	0.052 (2)	0.043 (2)	0.0019 (16)	0.0027 (16)	0.0171 (18)
C2	0.041 (2)	0.068 (3)	0.049 (2)	−0.0111 (19)	−0.0164 (17)	0.012 (2)
C3	0.0325 (18)	0.055 (2)	0.0356 (18)	0.0014 (16)	−0.0110 (14)	0.0133 (17)
C4	0.0416 (19)	0.046 (2)	0.0274 (17)	0.0097 (15)	0.0064 (14)	0.0049 (16)
C5	0.0373 (17)	0.0163 (14)	0.0239 (15)	0.0037 (12)	−0.0062 (12)	0.0000 (12)
C6	0.0293 (15)	0.0156 (13)	0.0237 (14)	−0.0022 (11)	0.0028 (12)	0.0002 (12)
C7	0.044 (2)	0.0358 (19)	0.056 (2)	0.0023 (16)	0.0007 (17)	−0.0128 (18)
C8	0.0277 (17)	0.0307 (17)	0.052 (2)	0.0008 (13)	−0.0016 (15)	0.0033 (16)
C9	0.0257 (16)	0.0342 (17)	0.0352 (17)	−0.0002 (13)	−0.0037 (13)	−0.0047 (15)
C10	0.0341 (18)	0.0343 (18)	0.0407 (19)	−0.0018 (14)	−0.0024 (14)	−0.0083 (15)
C11	0.0226 (15)	0.0345 (17)	0.0295 (16)	0.0014 (12)	0.0040 (12)	0.0045 (14)
C12	0.0279 (17)	0.0330 (17)	0.049 (2)	0.0014 (14)	−0.0065 (15)	0.0101 (16)

Geometric parameters (Å, º)

Te1—O2	1.9202 (17)	N3—C5	1.382 (4)
Te1—O2^i	1.9202 (17)	N3—H9	0.9000
Te1—O1	1.9283 (17)	N4—C5	1.312 (4)
Te1—O1^i	1.9283 (17)	N4—H10	0.8998
Te1—O3	1.9298 (17)	N4—H11	0.9000
Te1—O3^i	1.9298 (17)	N5—C5	1.320 (4)
Mo1—O11	1.7075 (19)	N5—C3	1.464 (4)
Mo1—O7	1.7298 (19)	N5—C4	1.468 (4)
Mo1—O5	1.9131 (19)	N6—C12	1.339 (4)
Mo1—O10	1.9339 (18)	N6—H12	0.9001
Mo1—O3	2.2834 (18)	N6—H13	0.9000
Mo1—O2	2.3123 (18)	N7—C12	1.329 (4)
Mo2—O9	1.702 (2)	N7—H14	0.9001
Mo2—O4	1.706 (2)	N7—H15	0.9001
Mo2—O12	1.9343 (19)	N8—C12	1.324 (4)
Mo2—O5^i	1.9606 (19)	N8—C11	1.336 (4)
Mo2—O1^i	2.2806 (18)	N9—C11	1.335 (4)
Mo2—O3^i	2.2823 (18)	N9—H16	0.8999
Mo3—O6	1.704 (2)	N9—H17	0.9000
Mo3—O8	1.706 (2)	N10—C11	1.334 (4)
Mo3—O12	1.9084 (19)	N10—C10	1.464 (4)
Mo3—O10	1.9916 (18)	N10—C9	1.471 (4)
Mo3—O2	2.2634 (18)	C1—C4	1.503 (5)
Mo3—O1^i	2.2835 (18)	C1—H1A	0.9700
O1—Mo2^i	2.2806 (18)	C1—H1B	0.9700
O1—Mo3^i	2.2835 (18)	C2—C3	1.504 (5)
O3—Mo2^i	2.2823 (18)	C2—H2A	0.9700
O5—Mo2^i	1.9606 (18)	C2—H2B	0.9700
O13—C2	1.422 (5)	C3—H3A	0.9700
O13—C1	1.422 (4)	C3—H3B	0.9700
O14—C7	1.426 (4)	C4—H4A	0.9700
O14—C8	1.427 (4)	C4—H4B	0.9700
O1W—H1	0.8500	C7—C10	1.488 (5)
O1W—H2	0.8500	C7—H7A	0.9700
O2W—H3	0.8499	C7—H7B	0.9700
O2W—H4	0.8500	C8—C9	1.497 (4)
N1—C6	1.319 (4)	C8—H8A	0.9700
N1—H5	0.8999	C8—H8B	0.9700
N1—H6	0.9001	C9—H9A	0.9700
N2—C6	1.311 (4)	C9—H9B	0.9700
N2—H7	0.9001	C10—H10A	0.9700
N2—H8	0.9000	C10—H10B	0.9700
N3—C6	1.353 (4)
O2—Te1—O2^i	180.0	C6—N3—C5	126.3 (2)
O2—Te1—O1	94.30 (8)	C6—N3—H9	118.2
O2^i—Te1—O1	85.70 (8)	C5—N3—H9	114.6
O2—Te1—O1^i	85.70 (8)	C5—N4—H10	118.8
O2^i—Te1—O1^i	94.30 (8)	C5—N4—H11	120.2
O1—Te1—O1^i	180.00 (8)	H10—N4—H11	120.5
O2—Te1—O3	86.01 (8)	C5—N5—C3	123.3 (3)
O2^i—Te1—O3	93.99 (8)	C5—N5—C4	123.1 (3)
O1—Te1—O3	85.94 (8)	C3—N5—C4	112.9 (3)
O1^i—Te1—O3	94.06 (8)	C12—N6—H12	118.6
O2—Te1—O3^i	93.99 (8)	C12—N6—H13	121.6
O2^i—Te1—O3^i	86.01 (8)	H12—N6—H13	118.1
O1—Te1—O3^i	94.06 (8)	C12—N7—H14	120.1
O1^i—Te1—O3^i	85.94 (8)	C12—N7—H15	123.6
O3—Te1—O3^i	180.00 (10)	H14—N7—H15	116.1
O11—Mo1—O7	106.37 (10)	C12—N8—C11	122.3 (3)
O11—Mo1—O5	100.61 (9)	C11—N9—H16	118.4
O7—Mo1—O5	97.36 (9)	C11—N9—H17	120.3
O11—Mo1—O10	97.24 (9)	H16—N9—H17	120.9
O7—Mo1—O10	99.29 (9)	C11—N10—C10	121.1 (3)
O5—Mo1—O10	151.01 (8)	C11—N10—C9	122.5 (3)
O11—Mo1—O3	93.01 (9)	C10—N10—C9	114.3 (2)
O7—Mo1—O3	160.24 (8)	O13—C1—C4	110.4 (3)
O5—Mo1—O3	74.79 (7)	O13—C1—H1A	109.6
O10—Mo1—O3	81.66 (7)	C4—C1—H1A	109.6
O11—Mo1—O2	160.86 (8)	O13—C1—H1B	109.6
O7—Mo1—O2	91.60 (8)	C4—C1—H1B	109.6
O5—Mo1—O2	83.17 (7)	H1A—C1—H1B	108.1
O10—Mo1—O2	72.83 (7)	O13—C2—C3	112.7 (3)
O3—Mo1—O2	69.69 (6)	O13—C2—H2A	109.1
O9—Mo2—O4	105.72 (10)	C3—C2—H2A	109.1
O9—Mo2—O12	97.04 (9)	O13—C2—H2B	109.1
O4—Mo2—O12	100.74 (9)	C3—C2—H2B	109.1
O9—Mo2—O5^i	99.08 (9)	H2A—C2—H2B	107.8
O4—Mo2—O5^i	95.33 (9)	N5—C3—C2	109.7 (3)
O12—Mo2—O5^i	153.20 (8)	N5—C3—H3A	109.7
O9—Mo2—O1^i	160.41 (8)	C2—C3—H3A	109.7
O4—Mo2—O1^i	93.42 (9)	N5—C3—H3B	109.7
O12—Mo2—O1^i	74.90 (7)	C2—C3—H3B	109.7
O5^i—Mo2—O1^i	82.91 (7)	H3A—C3—H3B	108.2
O9—Mo2—O3^i	91.31 (9)	N5—C4—C1	109.9 (3)
O4—Mo2—O3^i	161.30 (9)	N5—C4—H4A	109.7
O12—Mo2—O3^i	84.42 (7)	C1—C4—H4A	109.7
O5^i—Mo2—O3^i	73.98 (7)	N5—C4—H4B	109.7
O1^i—Mo2—O3^i	70.38 (6)	C1—C4—H4B	109.7
O6—Mo3—O8	106.47 (11)	H4A—C4—H4B	108.2
O6—Mo3—O12	101.97 (9)	N4—C5—N5	124.4 (3)
O8—Mo3—O12	99.94 (9)	N4—C5—N3	118.8 (3)
O6—Mo3—O10	93.33 (9)	N5—C5—N3	116.7 (3)
O8—Mo3—O10	97.35 (9)	N2—C6—N1	121.0 (3)
O12—Mo3—O10	152.52 (8)	N2—C6—N3	117.5 (3)
O6—Mo3—O2	157.88 (9)	N1—C6—N3	121.4 (3)
O8—Mo3—O2	92.71 (9)	O14—C7—C10	112.8 (3)
O12—Mo3—O2	85.01 (7)	O14—C7—H7A	109.0
O10—Mo3—O2	72.96 (7)	C10—C7—H7A	109.0
O6—Mo3—O1^i	90.99 (9)	O14—C7—H7B	109.0
O8—Mo3—O1^i	162.53 (9)	C10—C7—H7B	109.0
O12—Mo3—O1^i	75.30 (7)	H7A—C7—H7B	107.8
O10—Mo3—O1^i	81.82 (7)	O14—C8—C9	111.9 (3)
O2—Mo3—O1^i	70.29 (6)	O14—C8—H8A	109.2
Te1—O1—Mo2^i	101.89 (8)	C9—C8—H8A	109.2
Te1—O1—Mo3^i	101.51 (8)	O14—C8—H8B	109.2
Mo2^i—O1—Mo3^i	90.68 (7)	C9—C8—H8B	109.2
Te1—O2—Mo3	102.49 (8)	H8A—C8—H8B	107.9
Te1—O2—Mo1	101.78 (8)	N10—C9—C8	110.0 (3)
Mo3—O2—Mo1	93.26 (7)	N10—C9—H9A	109.7
Te1—O3—Mo2^i	101.78 (8)	C8—C9—H9A	109.7
Te1—O3—Mo1	102.51 (8)	N10—C9—H9B	109.7
Mo2^i—O3—Mo1	91.35 (6)	C8—C9—H9B	109.7
Mo1—O5—Mo2^i	114.94 (9)	H9A—C9—H9B	108.2
Mo1—O10—Mo3	115.85 (9)	N10—C10—C7	111.7 (3)
Mo3—O12—Mo2	115.31 (9)	N10—C10—H10A	109.3
C2—O13—C1	108.6 (3)	C7—C10—H10A	109.3
C7—O14—C8	109.0 (2)	N10—C10—H10B	109.3
H1—O1W—H2	112.3	C7—C10—H10B	109.3
H3—O2W—H4	102.2	H10A—C10—H10B	107.9
C6—N1—H5	118.5	N10—C11—N9	119.1 (3)
C6—N1—H6	117.5	N10—C11—N8	118.0 (3)
H5—N1—H6	122.6	N9—C11—N8	122.6 (3)
C6—N2—H7	119.0	N8—C12—N7	125.3 (3)
C6—N2—H8	121.8	N8—C12—N6	116.6 (3)
H7—N2—H8	118.8	N7—C12—N6	117.9 (3)
O2—Te1—O1—Mo2^i	86.08 (8)	O10—Mo1—O5—Mo2^i	−56.2 (2)
O2^i—Te1—O1—Mo2^i	−93.92 (8)	O3—Mo1—O5—Mo2^i	−19.37 (8)
O3—Te1—O1—Mo2^i	0.40 (7)	O2—Mo1—O5—Mo2^i	−90.12 (10)
O3^i—Te1—O1—Mo2^i	−179.60 (7)	O11—Mo1—O10—Mo3	177.24 (10)
O2—Te1—O1—Mo3^i	179.25 (7)	O7—Mo1—O10—Mo3	69.26 (11)
O2^i—Te1—O1—Mo3^i	−0.75 (7)	O5—Mo1—O10—Mo3	−55.0 (2)
O3—Te1—O1—Mo3^i	93.57 (8)	O3—Mo1—O10—Mo3	−90.76 (10)
O3^i—Te1—O1—Mo3^i	−86.43 (8)	O2—Mo1—O10—Mo3	−19.54 (8)
O1—Te1—O2—Mo3	179.24 (7)	O6—Mo3—O10—Mo1	−177.72 (11)
O1^i—Te1—O2—Mo3	−0.76 (7)	O8—Mo3—O10—Mo1	−70.63 (12)
O3—Te1—O2—Mo3	−95.14 (8)	O12—Mo3—O10—Mo1	58.1 (2)
O3^i—Te1—O2—Mo3	84.86 (8)	O2—Mo3—O10—Mo1	19.96 (8)
O1—Te1—O2—Mo1	−84.69 (8)	O1^i—Mo3—O10—Mo1	91.76 (10)
O1^i—Te1—O2—Mo1	95.31 (8)	O6—Mo3—O12—Mo2	−70.74 (12)
O3—Te1—O2—Mo1	0.92 (7)	O8—Mo3—O12—Mo2	179.91 (11)
O3^i—Te1—O2—Mo1	−179.08 (7)	O10—Mo3—O12—Mo2	51.7 (2)
O6—Mo3—O2—Te1	34.3 (3)	O2—Mo3—O12—Mo2	88.02 (10)
O8—Mo3—O2—Te1	−175.22 (9)	O1^i—Mo3—O12—Mo2	17.12 (9)
O12—Mo3—O2—Te1	−75.47 (8)	O9—Mo2—O12—Mo3	−178.97 (11)
O10—Mo3—O2—Te1	87.92 (9)	O4—Mo2—O12—Mo3	73.50 (12)
O1^i—Mo3—O2—Te1	0.68 (6)	O5^i—Mo2—O12—Mo3	−52.3 (2)
O6—Mo3—O2—Mo1	−68.6 (2)	O1^i—Mo2—O12—Mo3	−17.17 (9)
O8—Mo3—O2—Mo1	81.95 (9)	O3^i—Mo2—O12—Mo3	−88.33 (10)
O12—Mo3—O2—Mo1	−178.30 (7)	C2—O13—C1—C4	62.7 (4)
O10—Mo3—O2—Mo1	−14.91 (6)	C1—O13—C2—C3	−61.4 (4)
O1^i—Mo3—O2—Mo1	−102.15 (7)	C5—N5—C3—C2	140.0 (3)
O11—Mo1—O2—Te1	−27.3 (3)	C4—N5—C3—C2	−49.8 (4)
O7—Mo1—O2—Te1	172.66 (9)	O13—C2—C3—N5	54.6 (4)
O5—Mo1—O2—Te1	75.44 (8)	C5—N5—C4—C1	−137.4 (3)
O10—Mo1—O2—Te1	−88.10 (9)	C3—N5—C4—C1	52.3 (4)
O3—Mo1—O2—Te1	−0.83 (6)	O13—C1—C4—N5	−58.5 (4)
O11—Mo1—O2—Mo3	76.2 (3)	C3—N5—C5—N4	11.6 (5)
O7—Mo1—O2—Mo3	−83.85 (8)	C4—N5—C5—N4	−157.6 (3)
O5—Mo1—O2—Mo3	178.93 (7)	C3—N5—C5—N3	−165.4 (3)
O10—Mo1—O2—Mo3	15.38 (6)	C4—N5—C5—N3	25.3 (4)
O3—Mo1—O2—Mo3	102.65 (7)	C6—N3—C5—N4	55.3 (4)
O2—Te1—O3—Mo2^i	−95.00 (8)	C6—N3—C5—N5	−127.5 (3)
O2^i—Te1—O3—Mo2^i	85.00 (8)	C5—N3—C6—N2	−179.4 (3)
O1—Te1—O3—Mo2^i	−0.40 (7)	C5—N3—C6—N1	3.6 (5)
O1^i—Te1—O3—Mo2^i	179.60 (7)	C8—O14—C7—C10	59.6 (4)
O2—Te1—O3—Mo1	−0.94 (7)	C7—O14—C8—C9	−62.0 (4)
O2^i—Te1—O3—Mo1	179.06 (7)	C11—N10—C9—C8	148.7 (3)
O1—Te1—O3—Mo1	93.67 (8)	C10—N10—C9—C8	−47.8 (4)
O1^i—Te1—O3—Mo1	−86.33 (8)	O14—C8—C9—N10	56.0 (4)
O11—Mo1—O3—Te1	172.42 (9)	C11—N10—C10—C7	−150.2 (3)
O7—Mo1—O3—Te1	−18.7 (3)	C9—N10—C10—C7	46.0 (4)
O5—Mo1—O3—Te1	−87.41 (9)	O14—C7—C10—N10	−51.7 (4)
O10—Mo1—O3—Te1	75.53 (8)	C10—N10—C11—N9	−162.6 (3)
O2—Mo1—O3—Te1	0.83 (6)	C9—N10—C11—N9	−0.1 (4)
O11—Mo1—O3—Mo2^i	−85.20 (9)	C10—N10—C11—N8	23.3 (4)
O7—Mo1—O3—Mo2^i	83.6 (2)	C9—N10—C11—N8	−174.2 (3)
O5—Mo1—O3—Mo2^i	14.98 (7)	C12—N8—C11—N10	−154.6 (3)
O10—Mo1—O3—Mo2^i	177.91 (7)	C12—N8—C11—N9	31.6 (5)
O2—Mo1—O3—Mo2^i	103.21 (7)	C11—N8—C12—N7	30.2 (5)
O11—Mo1—O5—Mo2^i	70.89 (11)	C11—N8—C12—N6	−154.1 (3)
O7—Mo1—O5—Mo2^i	179.14 (10)

Symmetry code: (i) −x+2, −y+2, −z.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H6···O7	0.90	2.20	2.916 (3)	137
N1—H5···O2	0.90	2.04	2.769 (3)	138
N2—H8···O1^ii	0.90	1.95	2.840 (3)	172
N2—H7···O1W	0.90	2.01	2.877 (3)	162
N3—H9···O10^iii	0.90	1.69	2.571 (3)	165
N4—H11···O11^iv	0.90	2.18	2.965 (3)	146
N4—H10···O2W^ii	0.90	1.86	2.762 (4)	177
N9—H17···O14^v	0.90	2.18	3.067 (4)	167
N7—H15···O9	0.90	2.14	2.925 (4)	146
N7—H14···O7^vi	0.90	2.05	2.921 (3)	164
N6—H13···O8^vi	0.90	2.06	2.806 (4)	140
O1W—H1···O3^i	0.85	1.97	2.810 (3)	172
O1W—H2···O12	0.85	2.61	3.087 (3)	117
O1W—H2···O14^v	0.85	2.25	3.027 (3)	152
O2W—H3···O5^ii	0.85	2.06	2.860 (3)	156
O2W—H4···O1W	0.85	1.98	2.829 (4)	176

Symmetry codes: (i) −x+2, −y+2, −z; (ii) −x+2, −y+1, −z; (iii) x, y−1, z; (iv) −x+3/2, y−1/2, −z−1/2; (v) −x+3/2, y−1/2, −z+1/2; (vi) x+1/2, −y+3/2, z+1/2.