Tetra­imidazolium bis­(imidazole-κN)di-μ₄-oxido-tetra-μ₃-oxido-hexa-μ₂-oxido-tetra­deca­oxido­octa­molybdate(VI) monohydrate

The anion of the title salt, (C₃H₅N₂)₄[Mo₈O₂₆(C₃H₄N₂)₂]·H₂O, is a centrosymmetric Mo₈O₂₆ species in which two Mo atoms are each coordinated by an imidazole heterocycle. The anion is made up of two MoNO₅ and six MoO₆ edge-sharing octa­hedra. The cations inter­act with the tetra­anion to give rise to a three-dimensional hydrogen-bonded network. The asymmetric unit features three cations, two of which lie on centers of inversion; the solvent water mol­ecule is disordered with respect to one of these two cations.

Key indicators

• Single-crystal X-ray study
• T = 295 K
• Mean [sigma](C-C) = 0.005 Å
• Disorder in solvent or counterion
• R factor = 0.019
• wR factor = 0.050
• Data-to-parameter ratio = 11.9

checkCIF/PLATON results

No syntax errors found



Alert level A
PLAT770_ALERT_2_A Suspect C-H Bond in CIF:      C7     -H1W2    ..       1.38 Ang.

Author Response: The water molecule is disordered with respect to the imidalium ring, and the O1w atom occupies the same position as the N5 atom of the ring.

Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT062_ALERT_4_C Rescale T(min) & T(max) by .....................       0.96
PLAT154_ALERT_1_C The su's on the Cell Angles are Equal  (x 10000)        100 Deg.
PLAT180_ALERT_3_C Check Cell Rounding: # of Values Ending with 0 =          3
PLAT243_ALERT_4_C High  'Solvent' Ueq as Compared to Neighbors for        O1W
PLAT243_ALERT_4_C High  'Solvent' Ueq as Compared to Neighbors for         N5
PLAT302_ALERT_4_C Anion/Solvent Disorder .........................      34.00 Perc.
PLAT432_ALERT_2_C Short Inter X...Y Contact  O13    ..  C6      ..       2.92 Ang.
PLAT432_ALERT_2_C Short Inter X...Y Contact  C3     ..  C7      ..       3.14 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          2

Alert level G
PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints .......         84

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

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

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S1. Comment

The tetraanion of the title salt, tetrakis(imidazolium) bis(imidazole)-octamolybdate monohydrate, was previously identified as tetrakis(dimethylammonium) bis(imidazole)-octamolybdate trihydrate (Martían-Zarza et al., 1993). The anion is made up of two MoNO₅ and six MoO₆ edge-sharing octahedra as two of the molybdenum atoms are coordinated by the neutral N-heterocycles. In the present salt, two of the three cations of the asymmetric unit are disordered over different centers-of-inversion. The cations and tetraanion interact through hydrogen bonds to give rise to a three-dimensional network.

Related literature

For tetrakis(dimethylammonium) bis(imidazole)octamolybdate trihydrate (which has the same anion), see Martían-Zarza et al. (1993).

S2. Experimental

Sodium molybdate dihydrate, Na₂MoO₄^.2H₂O (0.65 g, 2.7 mmol) and ammonium acetate (0.15 g, 2 mmol) were dissolved in 30 ml water. Imidazole (0.10 g, 1.5 mmol) was added and the pH of the mixture adjusted to about 3.8 by the addition of acetic acid. The solution was heated at 333 K for about 12 h. It was then set aside for the growth of faint yellow crystals.

S3. Refinement

Two imidazolium cations are disordered about centers-of-inversion. For these two five-membered rings, the 1,2-related distances were restrained to 1.35±0.01 Å and the 1,3-related ones to 2.18±0.01 Å. The rings were also restrained to be almost planar. The rings are necessarily of half-occupancy only; one of the rings is also disordered with respect to a water molecule. (The presence of water in the compound was confirmed by an infrared spectrum.) The O1w atom occupies the same position as the N5 atom of the ring; the temperature factors of the two atoms were restrained to be identical. Additionally, the anisotropic displacement parameters of all disordered atoms were restrained to be nearly isotropic.

The carbon- and nitrogen-boud hydrogen atoms were placed at calculated positions (C–H 0.95 and N–H 0.86 Å), and were included in the refinement in the riding model approximation, with U(H) set to 1.2 times U_eq(C,N). The hydrogen atoms of the half-occupancy water molecule were placed in chemically sensible positions on the basis of hydrogen bonds but were not refined; their temperature factors were set to 1.5 times U_eq(O).

Computing details

Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT (Bruker, 2005); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2007).

Figures

Fig. 1. Thermal ellipsoid plot of 4[C3H5N2]^+ [(C3H4N2)2O26Mo8]^4-.H2O. The tetraanion lies about a center-of-inversion, and the unlabeled atoms are related to the labeled ones by (i = 2 – x, 1 – y, 1 – z). The water molecule is disordered with respect to one of the disordered cations that lie on an inversion site; the symmetry-related equivalent is shown (and labeled with an ii superscript).

Tetraimidazolium bis(imidazole-κN)di-µ₄-oxido-tetra-µ₃-oxido-hexa-µ₂-oxido-τetradecaoxido-octamolybdate(VI) monohydrate

Crystal data

(C3H5N2)4[Mo8O26(C3H4N2)2]·H2O	Z = 1
Mr = 1614.06	F(000) = 774
Triclinic, P1	Dx = 2.631 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 9.9723 (6) Å	Cell parameters from 6997 reflections
b = 10.9891 (7) Å	θ = 2.6–26.1°
c = 11.0273 (7) Å	µ = 2.49 mm^−1
α = 73.411 (1)°	T = 295 K
β = 68.510 (1)°	Block, yellow
γ = 66.702 (1)°	0.32 × 0.20 × 0.18 mm
V = 1018.7 (1) Å^3

Data collection

Bruker APEXII area-detector diffractometer	4001 independent reflections
Radiation source: fine-focus sealed tube	3818 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.019
φ and ω scans	θmax = 26.1°, θmin = 2.6°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −12→12
Tmin = 0.509, Tmax = 0.663	k = −13→13
8712 measured reflections	l = −13→13

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)] = 0.019	H-atom parameters constrained
wR(F^2) = 0.050	w = 1/[σ^2(Fo^2) + (0.0244P)^2 + 1.3243P] where P = (Fo^2 + 2Fc^2)/3
S = 1.03	(Δ/σ)max = 0.001
4001 reflections	Δρmax = 0.56 e Å^−3
335 parameters	Δρmin = −0.53 e Å^−3
84 restraints	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0115 (4)

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

	x	y	z	Uiso*/Ueq	Occ. (<1)
Mo1	0.66852 (3)	0.39691 (3)	0.78701 (2)	0.02253 (8)
Mo2	0.68776 (3)	0.69805 (2)	0.70065 (2)	0.02160 (8)
Mo3	0.90982 (3)	0.78651 (2)	0.41399 (2)	0.02006 (7)
Mo4	0.85357 (2)	0.48189 (2)	0.46941 (2)	0.01675 (7)
O1	0.7212 (3)	0.2601 (2)	0.9016 (2)	0.0378 (5)
O2	0.4752 (2)	0.4615 (3)	0.8447 (2)	0.0391 (5)
O3	0.7318 (2)	0.5242 (2)	0.81780 (19)	0.0260 (4)
O4	0.6743 (2)	0.54871 (19)	0.60330 (18)	0.0202 (4)
O5	0.4939 (2)	0.7582 (2)	0.7651 (2)	0.0347 (5)
O6	0.7564 (3)	0.7744 (2)	0.7672 (2)	0.0344 (5)
O7	0.7015 (2)	0.80454 (19)	0.52633 (19)	0.0226 (4)
O8	0.9465 (2)	0.8797 (2)	0.4910 (2)	0.0306 (5)
O9	0.8773 (3)	0.8888 (2)	0.2709 (2)	0.0339 (5)
O10	0.8527 (2)	0.62994 (19)	0.35338 (19)	0.0229 (4)
O11	1.1133 (2)	0.66457 (19)	0.35825 (18)	0.0213 (4)
O12	1.0724 (2)	0.39639 (18)	0.43058 (18)	0.0195 (4)
O13	0.8008 (2)	0.3943 (2)	0.4009 (2)	0.0262 (4)
O1w	0.3555 (4)	1.0254 (4)	0.8580 (3)	0.0679 (9)	0.50
H1w1	0.3986	0.9668	0.8068	0.102*	0.50
H1w2	0.2719	1.0777	0.8417	0.102*	0.50
N1	0.6259 (3)	0.2831 (2)	0.6778 (2)	0.0260 (5)
N2	0.5113 (3)	0.2301 (3)	0.5761 (3)	0.0368 (6)
H2n	0.4468	0.2366	0.5392	0.044*
N3	0.1740 (3)	0.7977 (3)	0.8697 (3)	0.0374 (6)
H3n	0.2508	0.7723	0.8983	0.045*
N4	0.0393 (3)	0.8412 (3)	0.7417 (3)	0.0415 (7)
H4n	0.0137	0.8491	0.6736	0.050*
C1	0.7039 (3)	0.1532 (3)	0.6544 (3)	0.0318 (7)
H1	0.7924	0.0974	0.6771	0.038*
C2	0.6319 (4)	0.1197 (3)	0.5934 (3)	0.0348 (7)
H2	0.6593	0.0372	0.5682	0.042*
C3	0.5111 (4)	0.3266 (3)	0.6266 (4)	0.0359 (7)
H3	0.4401	0.4126	0.6260	0.043*
C4	0.0271 (4)	0.8470 (4)	0.9408 (3)	0.0416 (8)
H4	−0.0082	0.8596	1.0284	0.050*
C5	−0.0579 (4)	0.8742 (4)	0.8598 (4)	0.0424 (8)
H5	−0.1636	0.9091	0.8810	0.051*
C6	0.1799 (4)	0.7951 (4)	0.7497 (4)	0.0424 (8)
H6	0.2679	0.7657	0.6821	0.051*
N5	0.3555 (4)	1.0254 (4)	0.8580 (3)	0.0679 (9)	0.50
H5n	0.3196	0.9993	0.8148	0.081*	0.50
N6	0.4811 (8)	1.0259 (7)	0.9896 (8)	0.041 (2)	0.50
H6n	0.5364	0.9982	1.0414	0.049*	0.50
C7	0.3365 (6)	1.1560 (6)	0.8651 (5)	0.0470 (18)	0.50
H7	0.2792	1.2331	0.8211	0.056*	0.50
C8	0.4124 (7)	1.1557 (6)	0.9444 (6)	0.0411 (16)	0.50
H8	0.4167	1.2306	0.9642	0.049*	0.50
C9	0.4474 (7)	0.9492 (6)	0.9394 (6)	0.0488 (18)	0.50
H9	0.4814	0.8558	0.9567	0.059*	0.50
N7	0.9672 (17)	0.4876 (9)	0.9137 (14)	0.050 (3)	0.50
H7n	0.9340	0.4812	0.8557	0.060*	0.50
N8	1.1196 (12)	0.4892 (9)	1.0082 (13)	0.039 (2)	0.50
H8n	1.2000	0.4842	1.0223	0.047*	0.50
C10	0.8828 (10)	0.5156 (13)	1.0355 (17)	0.056 (4)	0.50
H10	0.7784	0.5313	1.0716	0.067*	0.50
C11	0.978 (2)	0.5166 (13)	1.0951 (8)	0.056 (4)	0.50
H11	0.9520	0.5331	1.1804	0.067*	0.50
C12	1.1117 (12)	0.4716 (7)	0.8992 (9)	0.053 (2)	0.50
H12	1.1931	0.4514	0.8240	0.064*	0.50

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Mo1	0.01925 (13)	0.03160 (14)	0.02000 (13)	−0.01112 (10)	−0.00580 (9)	−0.00471 (10)
Mo2	0.01642 (12)	0.02691 (14)	0.02408 (13)	−0.00400 (9)	−0.00577 (9)	−0.01252 (10)
Mo3	0.01810 (12)	0.01817 (13)	0.02476 (13)	−0.00365 (9)	−0.00905 (9)	−0.00422 (9)
Mo4	0.01450 (12)	0.01969 (12)	0.01785 (12)	−0.00303 (9)	−0.00688 (9)	−0.00644 (9)
O1	0.0425 (13)	0.0477 (14)	0.0291 (11)	−0.0227 (11)	−0.0158 (10)	0.0037 (10)
O2	0.0244 (11)	0.0538 (15)	0.0419 (13)	−0.0139 (10)	−0.0021 (10)	−0.0201 (11)
O3	0.0255 (10)	0.0355 (11)	0.0226 (10)	−0.0108 (9)	−0.0097 (8)	−0.0082 (8)
O4	0.0154 (9)	0.0242 (10)	0.0222 (9)	−0.0034 (7)	−0.0066 (7)	−0.0083 (8)
O5	0.0207 (10)	0.0409 (13)	0.0418 (13)	−0.0046 (9)	−0.0047 (9)	−0.0190 (10)
O6	0.0366 (12)	0.0411 (13)	0.0371 (12)	−0.0132 (10)	−0.0143 (10)	−0.0175 (10)
O7	0.0172 (9)	0.0214 (10)	0.0291 (10)	−0.0010 (7)	−0.0102 (8)	−0.0069 (8)
O8	0.0271 (11)	0.0294 (11)	0.0406 (12)	−0.0084 (9)	−0.0106 (9)	−0.0133 (9)
O9	0.0367 (12)	0.0287 (11)	0.0356 (12)	−0.0091 (9)	−0.0180 (10)	0.0035 (9)
O10	0.0234 (10)	0.0236 (10)	0.0233 (10)	−0.0050 (8)	−0.0100 (8)	−0.0055 (8)
O11	0.0181 (9)	0.0243 (10)	0.0214 (9)	−0.0056 (8)	−0.0069 (7)	−0.0038 (8)
O12	0.0157 (9)	0.0218 (9)	0.0208 (9)	−0.0029 (7)	−0.0061 (7)	−0.0070 (7)
O13	0.0267 (10)	0.0281 (11)	0.0299 (11)	−0.0073 (8)	−0.0120 (8)	−0.0110 (8)
O1w	0.0488 (19)	0.081 (3)	0.068 (2)	−0.0181 (17)	−0.0152 (16)	−0.0111 (19)
N1	0.0218 (12)	0.0279 (13)	0.0307 (13)	−0.0075 (10)	−0.0113 (10)	−0.0047 (10)
N2	0.0321 (14)	0.0407 (16)	0.0495 (17)	−0.0065 (12)	−0.0253 (13)	−0.0146 (13)
N3	0.0322 (14)	0.0409 (16)	0.0471 (17)	−0.0132 (12)	−0.0201 (13)	−0.0052 (13)
N4	0.0448 (17)	0.0482 (17)	0.0431 (17)	−0.0137 (14)	−0.0205 (14)	−0.0161 (14)
C1	0.0243 (15)	0.0256 (15)	0.0468 (19)	−0.0036 (12)	−0.0169 (14)	−0.0055 (13)
C2	0.0321 (16)	0.0300 (16)	0.0441 (19)	−0.0080 (13)	−0.0101 (14)	−0.0132 (14)
C3	0.0298 (16)	0.0322 (17)	0.052 (2)	−0.0018 (13)	−0.0240 (15)	−0.0125 (15)
C4	0.045 (2)	0.053 (2)	0.0300 (17)	−0.0220 (17)	−0.0085 (15)	−0.0072 (15)
C5	0.0315 (17)	0.050 (2)	0.050 (2)	−0.0112 (15)	−0.0137 (15)	−0.0144 (17)
C6	0.0357 (18)	0.048 (2)	0.048 (2)	−0.0140 (16)	−0.0065 (16)	−0.0211 (17)
N5	0.0488 (19)	0.081 (3)	0.068 (2)	−0.0181 (17)	−0.0152 (16)	−0.0111 (19)
N6	0.031 (4)	0.061 (6)	0.031 (3)	−0.016 (4)	−0.014 (3)	0.000 (4)
C7	0.034 (3)	0.058 (4)	0.036 (4)	−0.013 (3)	−0.004 (3)	0.001 (3)
C8	0.042 (4)	0.043 (4)	0.037 (3)	−0.020 (3)	0.000 (3)	−0.009 (3)
C9	0.050 (4)	0.043 (4)	0.049 (4)	−0.023 (3)	0.005 (3)	−0.017 (3)
N7	0.044 (5)	0.071 (5)	0.055 (6)	−0.024 (5)	−0.033 (5)	−0.006 (4)
N8	0.046 (5)	0.050 (4)	0.037 (5)	−0.021 (3)	−0.025 (4)	−0.006 (4)
C10	0.047 (5)	0.073 (6)	0.050 (8)	−0.030 (5)	0.004 (5)	−0.021 (6)
C11	0.051 (8)	0.092 (7)	0.030 (4)	−0.025 (6)	−0.010 (5)	−0.016 (4)
C12	0.045 (5)	0.087 (6)	0.034 (5)	−0.025 (4)	−0.014 (4)	−0.012 (4)

Geometric parameters (Å, º)

Mo1—O1	1.706 (2)	N3—C4	1.352 (5)
Mo1—O2	1.704 (2)	N3—H3n	0.8500
Mo1—O3	1.896 (2)	N4—C6	1.317 (5)
Mo1—O4	2.225 (2)	N4—C5	1.355 (5)
Mo1—O11^i	2.158 (2)	N4—H4n	0.8500
Mo1—N1	2.203 (2)	C1—C2	1.344 (4)
Mo2—O3	1.964 (2)	C1—H1	0.9300
Mo2—O4	2.269 (2)	C2—H2	0.9300
Mo2—O5	1.711 (2)	C3—H3	0.9300
Mo2—O6	1.699 (2)	C4—C5	1.344 (5)
Mo2—O7	1.932 (2)	C4—H4	0.9300
Mo2—O12^i	2.292 (2)	C5—H5	0.9300
Mo3—O7	1.954 (2)	C6—H6	0.9300
Mo3—O8	1.710 (2)	N6—C9	1.326 (8)
Mo3—O9	1.713 (2)	N6—C8	1.350 (7)
Mo3—O10	2.333 (2)	N6—H6n	0.8500
Mo3—O11	1.923 (2)	C7—C8	1.348 (7)
Mo3—O12^i	2.232 (2)	C7—H1w2	1.383 (7)
Mo4—O4	1.887 (2)	C7—H7	0.9300
Mo4—O10	1.759 (2)	C8—H8	0.9300
Mo4—O13	1.697 (2)	C9—H9	0.9300
Mo4—O11^i	2.146 (2)	N7—C12	1.334 (8)
Mo4—O12	1.937 (2)	N7—C10	1.346 (8)
Mo4—O12^i	2.402 (2)	N7—H7n	0.8500
O1w—H1w1	0.85	N8—C12	1.304 (10)
O1w—H1w2	0.85	N8—C11	1.355 (7)
N1—C3	1.320 (4)	N8—H8n	0.8500
N1—C1	1.377 (4)	C10—C11	1.345 (8)
N2—C3	1.331 (4)	C10—H10	0.9300
N2—C2	1.355 (4)	C11—H11	0.9300
N2—H2n	0.8500	C12—H12	0.9300
N3—C6	1.311 (4)
O2—Mo1—O1	105.35 (12)	Mo3—O11—Mo4^i	105.25 (8)
O2—Mo1—O3	101.92 (10)	Mo3—O11—Mo1^i	151.90 (10)
O1—Mo1—O3	102.68 (10)	Mo4^i—O11—Mo1^i	102.74 (8)
O2—Mo1—O11^i	156.67 (10)	Mo4—O12—Mo3^i	101.61 (8)
O1—Mo1—O11^i	92.44 (10)	Mo4—O12—Mo2^i	154.72 (10)
O3—Mo1—O11^i	88.40 (8)	Mo3^i—O12—Mo2^i	92.40 (7)
O2—Mo1—N1	85.71 (10)	Mo4—O12—Mo4^i	103.28 (8)
O1—Mo1—N1	93.59 (10)	Mo3^i—O12—Mo4^i	96.46 (7)
O3—Mo1—N1	159.31 (9)	Mo2^i—O12—Mo4^i	95.84 (6)
O11^i—Mo1—N1	78.10 (8)	H1w1—O1w—H1w2	108.5
O2—Mo1—O4	92.04 (10)	C3—N1—C1	105.7 (3)
O1—Mo1—O4	162.36 (9)	C3—N1—Mo1	125.4 (2)
O3—Mo1—O4	75.99 (8)	C1—N1—Mo1	128.82 (19)
O11^i—Mo1—O4	69.99 (7)	C3—N2—C2	108.3 (3)
N1—Mo1—O4	84.62 (8)	C3—N2—H2n	125.8
O6—Mo2—O5	104.82 (11)	C2—N2—H2n	125.8
O6—Mo2—O7	101.14 (10)	C6—N3—C4	109.6 (3)
O5—Mo2—O7	97.72 (10)	C6—N3—H3n	125.2
O6—Mo2—O3	96.44 (10)	C4—N3—H3n	125.2
O5—Mo2—O3	99.64 (10)	C6—N4—C5	108.7 (3)
O7—Mo2—O3	151.18 (8)	C6—N4—H4n	125.6
O6—Mo2—O4	161.32 (9)	C5—N4—H4n	125.6
O5—Mo2—O4	92.62 (9)	C2—C1—N1	109.3 (3)
O7—Mo2—O4	82.71 (7)	C2—C1—H1	125.4
O3—Mo2—O4	73.70 (7)	N1—C1—H1	125.4
O6—Mo2—O12^i	90.97 (9)	C1—C2—N2	106.2 (3)
O5—Mo2—O12^i	163.23 (9)	C1—C2—H2	126.9
O7—Mo2—O12^i	73.26 (7)	N2—C2—H2	126.9
O3—Mo2—O12^i	83.85 (8)	N1—C3—N2	110.4 (3)
O4—Mo2—O12^i	72.49 (6)	N1—C3—H3	124.8
O8—Mo3—O9	105.42 (11)	N2—C3—H3	124.8
O8—Mo3—O11	98.40 (9)	C5—C4—N3	106.4 (3)
O9—Mo3—O11	104.31 (10)	C5—C4—H4	126.8
O8—Mo3—O7	96.66 (9)	N3—C4—H4	126.8
O9—Mo3—O7	101.11 (10)	C4—C5—N4	107.2 (3)
O11—Mo3—O7	145.67 (8)	C4—C5—H5	126.4
O8—Mo3—O12^i	96.90 (9)	N4—C5—H5	126.4
O9—Mo3—O12^i	157.63 (9)	N3—C6—N4	108.0 (3)
O11—Mo3—O12^i	73.43 (7)	N3—C6—H6	126.0
O7—Mo3—O12^i	74.25 (7)	N4—C6—H6	126.0
O8—Mo3—O10	167.65 (9)	C9—N6—C8	108.3 (5)
O9—Mo3—O10	86.49 (9)	C9—N6—H6n	125.8
O11—Mo3—O10	81.41 (7)	C8—N6—H6n	125.8
O7—Mo3—O10	77.49 (7)	C8—C7—H1w2	141.5 (5)
O12^i—Mo3—O10	71.14 (7)	C8—C7—H7	124.6
O13—Mo4—O10	103.16 (9)	H1w2—C7—H7	91.4
O13—Mo4—O4	102.77 (9)	C7—C8—N6	107.0 (5)
O10—Mo4—O4	100.08 (9)	C7—C8—H8	126.5
O13—Mo4—O12	103.31 (9)	N6—C8—H8	126.5
O10—Mo4—O12	97.93 (8)	N6—C9—H9	124.3
O4—Mo4—O12	143.81 (8)	C12—N7—C10	108.6 (6)
O13—Mo4—O11^i	97.64 (9)	C12—N7—H7n	125.7
O10—Mo4—O11^i	159.11 (8)	C10—N7—H7n	125.7
O4—Mo4—O11^i	76.84 (8)	C12—N8—C11	108.6 (5)
O12—Mo4—O11^i	75.20 (8)	C12—N8—H8n	125.7
O13—Mo4—O12^i	179.16 (8)	C11—N8—H8n	125.7
O10—Mo4—O12^i	77.66 (7)	C11—C10—N7	106.9 (5)
O4—Mo4—O12^i	76.85 (7)	C11—C10—H10	126.6
O12—Mo4—O12^i	76.72 (8)	N7—C10—H10	126.6
O11^i—Mo4—O12^i	81.54 (7)	C10—C11—N8	107.5 (5)
Mo1—O3—Mo2	113.87 (9)	C10—C11—H11	126.3
Mo4—O4—Mo1	109.41 (8)	N8—C11—H11	126.3
Mo4—O4—Mo2	113.61 (8)	N8—C12—N7	108.5 (6)
Mo1—O4—Mo2	92.07 (7)	N8—C12—H12	125.8
Mo2—O7—Mo3	114.32 (9)	N7—C12—H12	125.8
Mo4—O10—Mo3	114.67 (9)
O2—Mo1—O3—Mo2	−70.97 (13)	O11—Mo3—O10—Mo4	77.92 (10)
O1—Mo1—O3—Mo2	−179.92 (11)	O7—Mo3—O10—Mo4	−74.82 (10)
O11^i—Mo1—O3—Mo2	87.93 (10)	O12^i—Mo3—O10—Mo4	2.59 (9)
N1—Mo1—O3—Mo2	39.0 (3)	O8—Mo3—O11—Mo4^i	79.29 (10)
O4—Mo1—O3—Mo2	18.16 (9)	O9—Mo3—O11—Mo4^i	−172.35 (9)
O6—Mo2—O3—Mo1	178.21 (11)	O7—Mo3—O11—Mo4^i	−35.79 (17)
O5—Mo2—O3—Mo1	71.93 (12)	O12^i—Mo3—O11—Mo4^i	−15.45 (7)
O7—Mo2—O3—Mo1	−54.3 (2)	O10—Mo3—O11—Mo4^i	−88.22 (8)
O4—Mo2—O3—Mo1	−18.00 (9)	O8—Mo3—O11—Mo1^i	−95.6 (2)
O12^i—Mo2—O3—Mo1	−91.51 (10)	O9—Mo3—O11—Mo1^i	12.7 (2)
O13—Mo4—O4—Mo1	87.02 (10)	O7—Mo3—O11—Mo1^i	149.31 (18)
O10—Mo4—O4—Mo1	−166.87 (8)	O12^i—Mo3—O11—Mo1^i	169.6 (2)
O12—Mo4—O4—Mo1	−48.16 (17)	O10—Mo3—O11—Mo1^i	96.9 (2)
O11^i—Mo4—O4—Mo1	−7.97 (7)	O13—Mo4—O12—Mo3^i	−79.55 (10)
O12^i—Mo4—O4—Mo1	−92.20 (8)	O10—Mo4—O12—Mo3^i	174.83 (8)
O13—Mo4—O4—Mo2	−171.69 (9)	O4—Mo4—O12—Mo3^i	55.51 (16)
O10—Mo4—O4—Mo2	−65.58 (10)	O11^i—Mo4—O12—Mo3^i	14.97 (7)
O12—Mo4—O4—Mo2	53.13 (17)	O12^i—Mo4—O12—Mo3^i	99.58 (9)
O11^i—Mo4—O4—Mo2	93.32 (9)	O13—Mo4—O12—Mo2^i	42.8 (2)
O12^i—Mo4—O4—Mo2	9.08 (8)	O10—Mo4—O12—Mo2^i	−62.8 (2)
O2—Mo1—O4—Mo4	−156.55 (11)	O4—Mo4—O12—Mo2^i	177.84 (17)
O1—Mo1—O4—Mo4	13.9 (3)	O11^i—Mo4—O12—Mo2^i	137.3 (2)
O3—Mo1—O4—Mo4	101.67 (10)	O12^i—Mo4—O12—Mo2^i	−138.1 (3)
O11^i—Mo1—O4—Mo4	8.21 (8)	O13—Mo4—O12—Mo4^i	−179.13 (9)
N1—Mo1—O4—Mo4	−71.06 (10)	O10—Mo4—O12—Mo4^i	75.25 (9)
O2—Mo1—O4—Mo2	87.49 (9)	O4—Mo4—O12—Mo4^i	−44.07 (16)
O1—Mo1—O4—Mo2	−102.1 (3)	O11^i—Mo4—O12—Mo4^i	−84.61 (8)
O3—Mo1—O4—Mo2	−14.29 (7)	O12^i—Mo4—O12—Mo4^i	0.0
O11^i—Mo1—O4—Mo2	−107.74 (8)	O2—Mo1—N1—C3	34.4 (3)
N1—Mo1—O4—Mo2	172.98 (8)	O1—Mo1—N1—C3	139.6 (3)
O6—Mo2—O4—Mo4	−38.3 (3)	O3—Mo1—N1—C3	−78.3 (4)
O5—Mo2—O4—Mo4	162.41 (11)	O11^i—Mo1—N1—C3	−128.7 (3)
O7—Mo2—O4—Mo4	64.96 (10)	O4—Mo1—N1—C3	−58.0 (3)
O3—Mo2—O4—Mo4	−98.31 (10)	O2—Mo1—N1—C1	−141.6 (3)
O12^i—Mo2—O4—Mo4	−9.73 (8)	O1—Mo1—N1—C1	−36.5 (3)
O6—Mo2—O4—Mo1	73.9 (3)	O3—Mo1—N1—C1	105.6 (3)
O5—Mo2—O4—Mo1	−85.34 (9)	O11^i—Mo1—N1—C1	55.3 (3)
O7—Mo2—O4—Mo1	177.21 (7)	O4—Mo1—N1—C1	125.9 (3)
O3—Mo2—O4—Mo1	13.94 (7)	C3—N1—C1—C2	−1.9 (4)
O12^i—Mo2—O4—Mo1	102.52 (7)	Mo1—N1—C1—C2	174.7 (2)
O6—Mo2—O7—Mo3	67.07 (12)	N1—C1—C2—N2	1.5 (4)
O5—Mo2—O7—Mo3	173.91 (11)	C3—N2—C2—C1	−0.5 (4)
O3—Mo2—O7—Mo3	−59.4 (2)	C1—N1—C3—N2	1.6 (4)
O4—Mo2—O7—Mo3	−94.41 (10)	Mo1—N1—C3—N2	−175.2 (2)
O12^i—Mo2—O7—Mo3	−20.57 (9)	C2—N2—C3—N1	−0.7 (4)
O8—Mo3—O7—Mo2	−74.29 (12)	C6—N3—C4—C5	0.3 (4)
O9—Mo3—O7—Mo2	178.51 (11)	N3—C4—C5—N4	−0.2 (4)
O11—Mo3—O7—Mo2	41.28 (19)	C6—N4—C5—C4	0.1 (4)
O12^i—Mo3—O7—Mo2	21.03 (9)	C4—N3—C6—N4	−0.3 (4)
O10—Mo3—O7—Mo2	94.68 (10)	C5—N4—C6—N3	0.1 (4)
O13—Mo4—O10—Mo3	177.47 (9)	C9—N6—C8—C7	−0.2 (5)
O4—Mo4—O10—Mo3	71.68 (10)	C12—N7—C10—C11	0.1 (3)
O12—Mo4—O10—Mo3	−76.79 (10)	N7—C10—C11—N8	0.0 (3)
O11^i—Mo4—O10—Mo3	−7.8 (3)	C12—N8—C11—C10	−0.1 (5)
O12^i—Mo4—O10—Mo3	−2.33 (8)	C11—N8—C12—N7	0.2 (6)
O8—Mo3—O10—Mo4	−12.1 (4)	C10—N7—C12—N8	−0.2 (5)
O9—Mo3—O10—Mo4	−177.03 (12)

Symmetry code: (i) −x+2, −y+1, −z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2n···O7^ii	0.85	2.10	2.926 (3)	164
N3—H3n···O1^iii	0.85	2.24	2.889 (4)	134
N4—H4n···O8^iv	0.85	2.25	3.094 (4)	178
N5—H5n···O9^v	0.85	2.25	2.866 (4)	130
N6—H6n···O1w^vi	0.85	1.72	2.556 (7)	169
N7—H7n···O3	0.85	2.05	2.760 (9)	140
N8—H8n···O3^vii	0.85	2.08	2.766 (9)	138
O1w—H1w1···O5	0.85	2.22	3.010 (4)	154
O1w—H1w2···O9^v	0.85	2.13	2.866 (4)	144

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