Bis[1,1′-(butane-1,4-di­yl)diimidazolium] δ-octa­molybdate(VI)

The title compound, (C₁₀H₁₆N₄)₂[δ-Mo₈O₂₆], was synthesized by a hydro­thermal reaction. The structure consists of a centrosymmetric δ-octa­molybdate anion and two 1,1′-(butane-1,4-di­yl)bis­(imidazolium) cations for charge balance. The anions and cations are linked by N—H...O hydrogen bonds, generating a three-dimensional supra­molecular structure.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.004 Å
• R factor = 0.021
• wR factor = 0.048
• Data-to-parameter ratio = 17.3

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  Mo1    -   O9_a    ..       5.74 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  Mo2    -   O10     ..       5.14 su

Alert level G
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature        293 K
PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature .        293 K
PLAT794_ALERT_5_G Check Predicted Bond Valency for Mo1         (6)       6.03
PLAT794_ALERT_5_G Check Predicted Bond Valency for Mo2         (6)       5.83
PLAT794_ALERT_5_G Check Predicted Bond Valency for Mo3         (6)       5.99
PLAT794_ALERT_5_G Check Predicted Bond Valency for Mo4         (6)       5.86
PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints .......          2

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

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

---

S1. Comment

Recently, much of work has been focused on the polyoxometalate with different neutral ligands. In this paper, the structure of the title compound, (I), is described (Fig. 1).

The compound (I) contains a centrosymmetric δ-octamolybdate anion (Allis et al., 2004; Bridgeman, 2002) and two 1,1'-(butane-1,4-diyl)bis(imidazolium) cations. As shown in Fig. 2, each cation connects three anions through hydrogen bonds (Table 2), while each anion links six cations (Fig. 3). All anions and cations are linked each other in this mode to give a three-dimensional supramolecular structure. The Mo—O bond distances and angles are in normal range (Kalpana & Vidyasagar, 2005) (Table 1).

Related literature

For related structures, see: Allis et al. (2004); Bridgeman (2002); Kalpana & Vidyasagar (2005). For the ligand synthesis, see: Ma et al. (2003).

S2. Experimental

1,1'-(Butane-1,4-diyl)bis(imidazole) was synthesized according to the method reported by Ma et al. (2003). A mixture of 1,1'-(butane-1,4-diyl)bis(imidazole) (0.190 g, 0.1 mmol), Na₂MoO₄.2H₂O (0.242 g, 1.0 mmol) and H₂O (10 ml) was adjusted to pH ≈ 4 with HNO₃ (1 mol L^-1) and then transferred to and sealed in a 25 ml Teflon-lined stainless steel container. The container was heated to 423 K for 72 h, then cooled to room temperature. Colorless crystals of (I) were collected (yield 58.3% based on Na₂MoO₄.2H₂O). Analysis calculated for C₂₀H₃₂Mo₈N₈O₂₆: C 15.32, H 2.06, N 7.15%; found: C 15.30, H 2.07, N 7.18%.

S3. Refinement

All H atoms on C atoms were positioned geometrically and refined as riding, with C—H = 0.93 (CH), 0.97 Å (CH₂) and U_iso(H) = 1.2U_eq(C). The H atoms bonded to N atoms were located on a difference Fourier map and refined isotropically with a distance restraint of 0.86 (3) Å.

Computing details

Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL-Plus (Sheldrick, 1990); software used to prepare material for publication: SHELXL97.

Figures

	Fig. 1. The structures of the anion and cation of (I). Displacement ellipsoids are drawn at the 30% probability level. H atoms have been omitted for clarity.
	Fig. 2. The hydrogen bonds around the 1,1'-(butane-1,4-diyl)bis(imidazole) ligand. Dashed lines denote hydrogen bonds. Only the H atoms involving hydrogen bonds have been shown. [Symmetry codes: (ii) -x + 1, -y + 1, -z + 1; (iii) -x + 3/2, y + 1/2, -z + 1/2; (iv) x, y, z - 1.]
	Fig. 3. The hydrogen bonds around the octamolybdate anion. Dashed lines denote hydrogen bonds. Only the H atoms involving hydrogen bonds have been shown.

Bis[1,1'-(butane-1,4-diyl)diimidazolium] δ-octamolybdate(VI)

Crystal data

(C10H16N4)2[Mo8O26]	F(000) = 1504
Mr = 1568.06	Dx = 2.530 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 10235 reflections
a = 12.252 (3) Å	θ = 2.2–28.4°
b = 13.766 (3) Å	µ = 2.45 mm^−1
c = 12.405 (4) Å	T = 293 K
β = 100.371 (4)°	Block, colourless
V = 2058.1 (9) Å^3	0.40 × 0.32 × 0.28 mm
Z = 2

Data collection

Bruker SMART APEX CCD area-detector diffractometer	4979 independent reflections
Radiation source: fine-focus sealed tube	4400 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.022
φ and ω scans	θmax = 28.4°, θmin = 2.2°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −16→12
Tmin = 0.405, Tmax = 0.512	k = −18→16
12476 measured reflections	l = −16→15

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) = 0.048	H atoms treated by a mixture of independent and constrained refinement
S = 1.03	w = 1/[σ^2(Fo^2) + (0.0222P)^2 + 0.1238P] where P = (Fo^2 + 2Fc^2)/3
4979 reflections	(Δ/σ)max = 0.002
288 parameters	Δρmax = 0.34 e Å^−3
2 restraints	Δρmin = −0.63 e Å^−3

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Mo1	0.754292 (17)	1.019021 (14)	0.622942 (17)	0.02690 (6)
Mo2	0.455430 (16)	0.935845 (13)	0.613148 (16)	0.02382 (5)
Mo3	0.420322 (17)	0.803161 (14)	0.358359 (17)	0.02803 (6)
Mo4	0.687630 (18)	0.785795 (14)	0.499020 (17)	0.02708 (6)
O8	0.45559 (16)	0.90491 (13)	0.74631 (15)	0.0406 (4)
O10	0.48032 (14)	0.82703 (11)	0.54413 (14)	0.0303 (4)
O1	0.65759 (14)	0.67556 (12)	0.55209 (15)	0.0354 (4)
O7	0.56208 (13)	1.02931 (11)	0.61139 (14)	0.0284 (4)
O5	0.88155 (15)	1.01901 (14)	0.58946 (17)	0.0419 (5)
O11	0.41126 (16)	0.68162 (12)	0.37685 (17)	0.0452 (5)
O6	0.77946 (16)	1.01455 (12)	0.76203 (15)	0.0380 (4)
O12	0.39766 (17)	0.82020 (15)	0.22085 (16)	0.0461 (5)
O2	0.80695 (16)	0.76876 (14)	0.44952 (17)	0.0436 (5)
O13	0.28365 (13)	0.84549 (11)	0.39446 (14)	0.0302 (4)
O9	0.32230 (14)	0.98175 (12)	0.56067 (14)	0.0320 (4)
O4	0.58508 (14)	0.81338 (12)	0.37603 (14)	0.0306 (4)
N1	0.5128 (2)	0.38184 (18)	0.3352 (2)	0.0499 (6)
C7	0.5839 (2)	0.77486 (18)	0.0168 (2)	0.0416 (7)
H7A	0.5988	0.7377	−0.0454	0.050*
H7B	0.5043	0.7751	0.0143	0.050*
C1	0.5719 (3)	0.3377 (2)	0.2674 (3)	0.0499 (8)
H1	0.5733	0.2716	0.2523	0.060*
O3	0.71282 (15)	0.88071 (11)	0.60380 (14)	0.0352 (4)
N3	0.62268 (18)	0.87472 (15)	0.00892 (18)	0.0347 (5)
N2	0.60261 (18)	0.49305 (14)	0.27097 (18)	0.0322 (5)
C8	0.6744 (3)	0.9098 (2)	−0.0680 (3)	0.0476 (7)
H8	0.6948	0.8748	−0.1254	0.057*
C9	0.6086 (2)	0.94964 (19)	0.0782 (2)	0.0423 (7)
H9	0.5751	0.9452	0.1396	0.051*
C6	0.6404 (2)	0.72714 (18)	0.1215 (2)	0.0384 (6)
H6A	0.6394	0.7712	0.1823	0.046*
H6B	0.7172	0.7143	0.1169	0.046*
C3	0.5309 (2)	0.4750 (2)	0.3355 (2)	0.0420 (7)
H3	0.4985	0.5210	0.3748	0.050*
C2	0.6282 (3)	0.4077 (2)	0.2261 (3)	0.0466 (7)
H2	0.6757	0.3995	0.1763	0.056*
C4	0.6455 (2)	0.58912 (19)	0.2472 (2)	0.0421 (7)
H4A	0.7233	0.5830	0.2422	0.051*
H4B	0.6403	0.6327	0.3075	0.051*
C5	0.5841 (2)	0.63262 (19)	0.1429 (2)	0.0382 (6)
H5A	0.5076	0.6449	0.1493	0.046*
H5B	0.5846	0.5880	0.0825	0.046*
C10	0.6510 (3)	1.0294 (2)	0.0423 (3)	0.0487 (7)
H10	0.6524	1.0910	0.0731	0.058*
N4	0.6918 (2)	1.00341 (19)	−0.0483 (2)	0.0517 (7)
H1N	0.466 (2)	0.360 (2)	0.373 (2)	0.063 (10)*
H4N	0.724 (3)	1.047 (2)	−0.081 (3)	0.085 (13)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Mo1	0.02472 (11)	0.02370 (10)	0.03129 (12)	0.00105 (8)	0.00240 (8)	−0.00177 (8)
Mo2	0.02711 (11)	0.02013 (10)	0.02486 (11)	−0.00093 (8)	0.00640 (8)	0.00104 (7)
Mo3	0.03107 (12)	0.02043 (10)	0.03198 (12)	0.00099 (8)	0.00405 (9)	−0.00463 (8)
Mo4	0.03080 (12)	0.02067 (10)	0.03081 (12)	0.00111 (8)	0.00835 (9)	0.00170 (8)
O8	0.0557 (12)	0.0381 (10)	0.0283 (10)	−0.0024 (9)	0.0080 (9)	0.0029 (8)
O10	0.0346 (9)	0.0238 (8)	0.0323 (9)	0.0015 (7)	0.0055 (7)	0.0014 (7)
O1	0.0393 (10)	0.0226 (8)	0.0469 (11)	0.0027 (7)	0.0150 (9)	0.0044 (7)
O7	0.0279 (9)	0.0206 (7)	0.0374 (10)	−0.0001 (6)	0.0072 (7)	−0.0023 (7)
O5	0.0294 (10)	0.0454 (11)	0.0520 (12)	0.0045 (8)	0.0103 (9)	0.0049 (9)
O11	0.0467 (12)	0.0237 (9)	0.0649 (14)	0.0004 (8)	0.0087 (10)	−0.0057 (9)
O6	0.0442 (11)	0.0334 (9)	0.0346 (10)	−0.0002 (8)	0.0021 (8)	−0.0010 (8)
O12	0.0522 (12)	0.0514 (11)	0.0336 (11)	0.0079 (10)	0.0045 (9)	−0.0056 (9)
O2	0.0352 (11)	0.0460 (11)	0.0524 (13)	0.0027 (9)	0.0155 (9)	0.0076 (9)
O13	0.0270 (9)	0.0230 (8)	0.0398 (10)	−0.0032 (7)	0.0046 (7)	−0.0011 (7)
O9	0.0301 (9)	0.0344 (9)	0.0331 (10)	0.0027 (7)	0.0100 (7)	−0.0021 (7)
O4	0.0317 (9)	0.0304 (8)	0.0309 (9)	0.0050 (7)	0.0090 (7)	−0.0013 (7)
N1	0.0540 (16)	0.0433 (14)	0.0546 (17)	−0.0089 (12)	0.0161 (13)	0.0132 (12)
C7	0.0443 (17)	0.0320 (13)	0.0453 (17)	−0.0079 (12)	−0.0003 (13)	0.0026 (12)
C1	0.058 (2)	0.0252 (13)	0.064 (2)	−0.0010 (13)	0.0045 (16)	0.0032 (13)
O3	0.0397 (10)	0.0234 (8)	0.0395 (10)	0.0029 (7)	−0.0011 (8)	−0.0007 (7)
N3	0.0385 (12)	0.0307 (11)	0.0348 (12)	−0.0046 (9)	0.0069 (9)	0.0048 (9)
N2	0.0365 (12)	0.0255 (10)	0.0363 (12)	−0.0001 (9)	0.0107 (9)	0.0028 (9)
C8	0.0488 (18)	0.0539 (18)	0.0417 (17)	−0.0024 (14)	0.0127 (14)	0.0039 (14)
C9	0.0519 (18)	0.0346 (14)	0.0409 (17)	−0.0032 (13)	0.0097 (13)	0.0012 (12)
C6	0.0433 (16)	0.0315 (13)	0.0403 (16)	−0.0073 (11)	0.0071 (12)	0.0022 (11)
C3	0.0416 (16)	0.0440 (16)	0.0433 (17)	0.0020 (13)	0.0159 (13)	−0.0015 (13)
C2	0.0534 (18)	0.0331 (14)	0.058 (2)	0.0030 (13)	0.0236 (15)	−0.0082 (13)
C4	0.0506 (18)	0.0314 (13)	0.0437 (17)	−0.0121 (12)	0.0067 (13)	0.0014 (12)
C5	0.0433 (16)	0.0298 (13)	0.0426 (16)	−0.0082 (11)	0.0101 (12)	0.0005 (11)
C10	0.0542 (19)	0.0342 (14)	0.0522 (19)	−0.0058 (13)	−0.0057 (15)	0.0037 (13)
N4	0.0512 (16)	0.0470 (15)	0.0561 (17)	−0.0175 (13)	0.0076 (13)	0.0185 (13)

Geometric parameters (Å, º)

Mo1—O5	1.6843 (18)	C7—C6	1.508 (4)
Mo1—O6	1.6983 (18)	C7—H7A	0.9700
Mo1—O13^i	1.9249 (15)	C7—H7B	0.9700
Mo1—O3	1.9738 (16)	C1—C2	1.339 (4)
Mo1—O9^i	2.3020 (18)	C1—H1	0.9300
Mo1—O7	2.3377 (16)	N3—C8	1.328 (3)
Mo2—O8	1.7055 (18)	N3—C9	1.373 (3)
Mo2—O9	1.7611 (17)	N2—C3	1.315 (3)
Mo2—O10	1.7788 (16)	N2—C2	1.360 (3)
Mo2—O7	1.8367 (16)	N2—C4	1.473 (3)
Mo3—O12	1.6945 (19)	C8—N4	1.322 (4)
Mo3—O11	1.6952 (17)	C8—H8	0.9300
Mo3—O13	1.9010 (16)	C9—C10	1.325 (4)
Mo3—O4	1.9959 (17)	C9—H9	0.9300
Mo3—O10	2.3128 (17)	C6—C5	1.518 (3)
Mo3—O7^i	2.3403 (15)	C6—H6A	0.9700
Mo4—O2	1.7007 (18)	C6—H6B	0.9700
Mo4—O1	1.7202 (16)	C3—H3	0.9300
Mo4—O3	1.8296 (17)	C2—H2	0.9300
Mo4—O4	1.8331 (17)	C4—C5	1.500 (4)
O7—Mo3^i	2.3403 (15)	C4—H4A	0.9700
O13—Mo1^i	1.9249 (15)	C4—H4B	0.9700
O9—Mo1^i	2.3020 (18)	C5—H5A	0.9700
N1—C3	1.302 (4)	C5—H5B	0.9700
N1—C1	1.350 (4)	C10—N4	1.357 (4)
N1—H1N	0.86 (3)	C10—H10	0.9300
C7—N3	1.464 (3)	N4—H4N	0.86 (3)
O5—Mo1—O6	104.11 (10)	N3—C7—C6	111.2 (2)
O5—Mo1—O13^i	100.84 (8)	N3—C7—H7A	109.4
O6—Mo1—O13^i	98.34 (8)	C6—C7—H7A	109.4
O5—Mo1—O3	101.53 (8)	N3—C7—H7B	109.4
O6—Mo1—O3	94.76 (8)	C6—C7—H7B	109.4
O13^i—Mo1—O3	150.39 (7)	H7A—C7—H7B	108.0
O5—Mo1—O9^i	89.23 (8)	C2—C1—N1	106.6 (2)
O6—Mo1—O9^i	166.45 (8)	C2—C1—H1	126.7
O13^i—Mo1—O9^i	81.16 (7)	N1—C1—H1	126.7
O3—Mo1—O9^i	80.00 (7)	Mo4—O3—Mo1	141.37 (10)
O5—Mo1—O7	162.17 (8)	C8—N3—C9	107.9 (2)
O6—Mo1—O7	93.50 (8)	C8—N3—C7	126.3 (2)
O13^i—Mo1—O7	73.39 (6)	C9—N3—C7	125.8 (2)
O3—Mo1—O7	79.42 (6)	C3—N2—C2	108.3 (2)
O9^i—Mo1—O7	73.32 (6)	C3—N2—C4	126.4 (2)
O8—Mo2—O9	106.68 (9)	C2—N2—C4	125.3 (2)
O8—Mo2—O10	106.59 (8)	N4—C8—N3	107.6 (3)
O9—Mo2—O10	110.60 (8)	N4—C8—H8	126.2
O8—Mo2—O7	108.04 (9)	N3—C8—H8	126.2
O9—Mo2—O7	110.97 (7)	C10—C9—N3	108.1 (3)
O10—Mo2—O7	113.59 (7)	C10—C9—H9	125.9
O12—Mo3—O11	105.66 (10)	N3—C9—H9	125.9
O12—Mo3—O13	101.72 (9)	C7—C6—C5	111.8 (2)
O11—Mo3—O13	100.88 (8)	C7—C6—H6A	109.3
O12—Mo3—O4	94.59 (9)	C5—C6—H6A	109.3
O11—Mo3—O4	98.30 (8)	C7—C6—H6B	109.3
O13—Mo3—O4	150.33 (7)	C5—C6—H6B	109.3
O12—Mo3—O10	161.53 (8)	H6A—C6—H6B	107.9
O11—Mo3—O10	91.27 (8)	N1—C3—N2	108.5 (2)
O13—Mo3—O10	81.79 (7)	N1—C3—H3	125.8
O4—Mo3—O10	75.33 (6)	N2—C3—H3	125.8
O12—Mo3—O7^i	91.07 (8)	C1—C2—N2	107.1 (3)
O11—Mo3—O7^i	163.21 (8)	C1—C2—H2	126.5
O13—Mo3—O7^i	73.73 (6)	N2—C2—H2	126.5
O4—Mo3—O7^i	81.42 (6)	N2—C4—C5	112.9 (2)
O10—Mo3—O7^i	72.34 (6)	N2—C4—H4A	109.0
O2—Mo4—O1	105.88 (9)	C5—C4—H4A	109.0
O2—Mo4—O3	107.99 (9)	N2—C4—H4B	109.0
O1—Mo4—O3	112.24 (8)	C5—C4—H4B	109.0
O2—Mo4—O4	103.47 (9)	H4A—C4—H4B	107.8
O1—Mo4—O4	109.84 (8)	C4—C5—C6	108.7 (2)
O3—Mo4—O4	116.49 (7)	C4—C5—H5A	110.0
Mo2—O10—Mo3	123.22 (8)	C6—C5—H5A	110.0
Mo2—O7—Mo1	131.90 (8)	C4—C5—H5B	110.0
Mo2—O7—Mo3^i	137.19 (8)	C6—C5—H5B	110.0
Mo1—O7—Mo3^i	89.26 (5)	H5A—C5—H5B	108.3
Mo3—O13—Mo1^i	118.41 (8)	C9—C10—N4	106.6 (3)
Mo2—O9—Mo1^i	123.34 (8)	C9—C10—H10	126.7
Mo4—O4—Mo3	127.22 (9)	N4—C10—H10	126.7
C3—N1—C1	109.6 (2)	C8—N4—C10	109.8 (2)
C3—N1—H1N	118 (2)	C8—N4—H4N	132 (3)
C1—N1—H1N	132 (2)	C10—N4—H4N	118 (3)
O8—Mo2—O10—Mo3	153.57 (10)	O12—Mo3—O4—Mo4	−170.00 (11)
O9—Mo2—O10—Mo3	37.97 (12)	O11—Mo3—O4—Mo4	−63.41 (12)
O7—Mo2—O10—Mo3	−87.57 (11)	O13—Mo3—O4—Mo4	66.47 (18)
O12—Mo3—O10—Mo2	52.1 (3)	O10—Mo3—O4—Mo4	25.73 (10)
O11—Mo3—O10—Mo2	−151.20 (11)	O7^i—Mo3—O4—Mo4	99.61 (11)
O13—Mo3—O10—Mo2	−50.39 (10)	C3—N1—C1—C2	0.4 (4)
O4—Mo3—O10—Mo2	110.56 (10)	O2—Mo4—O3—Mo1	61.40 (17)
O7^i—Mo3—O10—Mo2	25.06 (9)	O1—Mo4—O3—Mo1	177.73 (14)
O8—Mo2—O7—Mo1	81.32 (13)	O4—Mo4—O3—Mo1	−54.42 (18)
O9—Mo2—O7—Mo1	−162.05 (10)	O5—Mo1—O3—Mo4	−62.11 (17)
O10—Mo2—O7—Mo1	−36.70 (14)	O6—Mo1—O3—Mo4	−167.57 (16)
O8—Mo2—O7—Mo3^i	−79.26 (14)	O13^i—Mo1—O3—Mo4	76.3 (2)
O9—Mo2—O7—Mo3^i	37.36 (15)	O9^i—Mo1—O3—Mo4	25.03 (15)
O10—Mo2—O7—Mo3^i	162.72 (11)	O7—Mo1—O3—Mo4	99.74 (16)
O5—Mo1—O7—Mo2	105.1 (2)	C6—C7—N3—C8	118.5 (3)
O6—Mo1—O7—Mo2	−83.91 (12)	C6—C7—N3—C9	−63.8 (4)
O13^i—Mo1—O7—Mo2	178.43 (13)	C9—N3—C8—N4	−0.3 (3)
O3—Mo1—O7—Mo2	10.29 (11)	C7—N3—C8—N4	177.8 (3)
O9^i—Mo1—O7—Mo2	92.90 (12)	C8—N3—C9—C10	0.5 (3)
O5—Mo1—O7—Mo3^i	−88.0 (2)	C7—N3—C9—C10	−177.6 (3)
O6—Mo1—O7—Mo3^i	83.03 (7)	N3—C7—C6—C5	167.6 (2)
O13^i—Mo1—O7—Mo3^i	−14.63 (6)	C1—N1—C3—N2	−1.3 (4)
O3—Mo1—O7—Mo3^i	177.23 (7)	C2—N2—C3—N1	1.7 (3)
O9^i—Mo1—O7—Mo3^i	−100.16 (6)	C4—N2—C3—N1	179.6 (3)
O12—Mo3—O13—Mo1^i	−67.03 (12)	N1—C1—C2—N2	0.6 (4)
O11—Mo3—O13—Mo1^i	−175.73 (10)	C3—N2—C2—C1	−1.4 (3)
O4—Mo3—O13—Mo1^i	54.92 (18)	C4—N2—C2—C1	−179.3 (3)
O10—Mo3—O13—Mo1^i	94.55 (9)	C3—N2—C4—C5	−96.4 (3)
O7^i—Mo3—O13—Mo1^i	20.64 (8)	C2—N2—C4—C5	81.1 (3)
O8—Mo2—O9—Mo1^i	−155.56 (10)	N2—C4—C5—C6	−175.5 (2)
O10—Mo2—O9—Mo1^i	−40.03 (12)	C7—C6—C5—C4	179.3 (2)
O7—Mo2—O9—Mo1^i	86.98 (11)	N3—C9—C10—N4	−0.5 (4)
O2—Mo4—O4—Mo3	160.04 (11)	N3—C8—N4—C10	0.0 (4)
O1—Mo4—O4—Mo3	47.35 (12)	C9—C10—N4—C8	0.3 (4)
O3—Mo4—O4—Mo3	−81.65 (12)

Symmetry code: (i) −x+1, −y+2, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1N···O1^ii	0.86 (3)	1.98 (3)	2.826 (3)	171 (3)
N4—H4N···O1^iii	0.86 (3)	2.27 (3)	3.009 (3)	143 (4)
N4—H4N···O6^iv	0.86 (3)	2.22 (4)	2.761 (3)	121 (3)

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