Dianilinium tetradeca­chloro­hexamolybdate dihydrate, (PhNH3)2[(Mo6Cl8)Cl6]·2H2O

Flemström, A.

doi:10.1107/S1600536803004884

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Dianilinium tetradecachlorohexamolybdate dihydrate, (PhNH₃)₂[(Mo₆Cl₈)Cl₆]·2H₂O

A. Flemström

The title compound, (C₆H₈N)₂[(Mo₆Cl₈)Cl₆]·2H₂O, the anilinium salt of an Mo^II chloride cluster, shows a rigid and stable hydrogen-bonded network. The chloromolybdate cluster dianion occupies a special position on a twofold axis.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803004884/ya6150sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536803004884/ya6150Isup2.hkl Contains datablock I

CCDC reference: 209886

checkCIF report

Key indicators

Single-crystal X-ray study
T = 293 K
Mean (C-C) = 0.011 Å
R factor = 0.029
wR factor = 0.062
Data-to-parameter ratio = 13.9

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


 Alert Level B:



THETM_01  Alert B The value of sine(theta_max)/wavelength is less than 0.575
          Calculated sin(theta_max)/wavelength =    0.5700

Author response: Larger sample to detector required for resolution of reflection

PLAT_731  Alert B Bond    Calc     0.90(9), Rep     0.90(2) ....       4.50 su-Ratio
                     O1   -HW1     1.555   1.555


 Alert Level C:



CRYSC_01  Alert C The word below has not been recognised as a standard
          identifier.
          Cognac

REFLT_03
         From the CIF: _diffrn_reflns_theta_max           23.90
         From the CIF: _reflns_number_total               2368
         TEST2: Reflns within _diffrn_reflns_theta_max
         Count of symmetry unique reflns         2548
         Completeness (_total/calc)             92.94%
          Alert C: < 95% complete

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    183
                   CL4 -MO3 -CL1 -MO1   -38.50  0.50   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    190
                   CL4 -MO3 -CL1 -MO2    33.60  0.50   1.555   1.555   1.555   2.655

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    196
                   CL3 -MO1 -CL1 -MO3    35.00  0.50   2.655   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    203
                   CL3 -MO1 -CL1 -MO2   -37.10  0.50   2.655   1.555   1.555   2.655

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    212
                   CL4 -MO3 -CL2 -MO1    43.10  0.50   2.655   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    219
                   CL4 -MO3 -CL2 -MO2   -29.00  0.50   2.655   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    226
                   CL3 -MO1 -CL2 -MO3   -36.50  0.40   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    233
                   CL3 -MO1 -CL2 -MO2    35.80  0.40   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    240
                   CL1 -MO2 -CL2 -MO3    35.60  0.50   2.655   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    247
                   CL1 -MO2 -CL2 -MO1   -36.40  0.50   2.655   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    254
                   CL2 -MO1 -CL3 -MO1   -35.70  0.40   1.555   1.555   1.555   2.655

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    261
                   CL2 -MO1 -CL3 -MO2    36.40  0.40   1.555   1.555   1.555   2.655

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    266
                   CL3 -MO2 -CL4 -MO3   -31.80  0.40   2.655   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    273
                   CL3 -MO2 -CL4 -MO3    40.70  0.40   2.655   1.555   1.555   2.655

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    281
                   CL1 -MO3 -CL4 -MO2    38.50  0.50   1.555   1.555   1.555   1.555

PLAT_710  Alert C Delete 1-2-3 or 2-3-4 (CIF) Linear Torsion Angle #    288
                   CL1 -MO3 -CL4 -MO3   -33.40  0.50   1.555   1.555   1.555   2.655

PLAT_732  Alert C Angle   Calc    60.14(5), Rep    60.14(2) ....       2.63 su-Ratio
                     MO3  -MO1  -MO2     1.555   1.555   1.555

PLAT_732  Alert C Angle   Calc    60.10(5), Rep    60.10(2) ....       2.63 su-Ratio
                     MO1  -MO3  -MO2     1.555   1.555   1.555

PLAT_732  Alert C Angle   Calc     107(12), Rep      107(3) ....       4.00 su-Ratio
                     HW1  -O1   -HW2     1.555   1.555   1.555

PLAT_733  Alert C Torsion Calc   178.76(7), Rep   178.76(3) ....       2.33 su-Ratio
                     MO3 -MO1 -MO2 -CL3    1.555   1.555   1.555   2.655

PLAT_733  Alert C Torsion Calc  -177.26(7), Rep  -177.26(3) ....       2.33 su-Ratio
                     CL3 -MO1 -MO2 -CL4    2.655   1.555   1.555   1.555

PLAT_733  Alert C Torsion Calc     0.18(5), Rep     0.18(1) ....       3.33 su-Ratio
                     MO2 -MO1 -MO2 -MO3    2.655   1.555   1.555   2.655

PLAT_733  Alert C Torsion Calc  -178.76(7), Rep  -178.76(3) ....       2.33 su-Ratio
                     CL3 -MO1 -MO2 -MO3    2.655   1.555   1.555   1.555

PLAT_733  Alert C Torsion Calc    -1.54(6), Rep    -1.54(2) ....       3.00 su-Ratio
                     CL1 -MO1 -MO2 -MO3    1.555   1.555   1.555   1.555

PLAT_733  Alert C Torsion Calc     0.12(5), Rep     0.11(2) ....       2.50 su-Ratio
                     MO1 -MO1 -MO3 -MO3    2.655   1.555   1.555   2.655

PLAT_733  Alert C Torsion Calc     1.54(6), Rep     1.55(2) ....       3.00 su-Ratio
                     MO1 -MO2 -MO3 -CL1    1.555   1.555   1.555   1.555

PLAT_733  Alert C Torsion Calc   177.25(7), Rep   177.25(3) ....       2.33 su-Ratio
                     CL3 -MO2 -MO3 -CL4    2.655   1.555   1.555   1.555

PLAT_733  Alert C Torsion Calc     0.18(5), Rep     0.18(1) ....       3.33 su-Ratio
                     MO1 -MO2 -MO3 -MO2    2.655   1.555   1.555   2.655

PLAT_733  Alert C Torsion Calc    -1.57(6), Rep    -1.57(2) ....       3.00 su-Ratio
                     MO2 -MO3 -CL1 -MO1    1.555   1.555   1.555   1.555

PLAT_733  Alert C Torsion Calc     1.57(6), Rep     1.57(2) ....       3.00 su-Ratio
                     MO2 -MO1 -CL1 -MO3    1.555   1.555   1.555   1.555

PLAT_745  Alert C D-H     Calc     0.90(9), Rep     0.90000 ....    Missing su
                     O1   -HW1     1.555   1.555

PLAT_745  Alert C D-H     Calc     0.90(8), Rep     0.90000 ....    Missing su
                     O1   -HW2     1.555   1.555

PLAT_746  Alert C H...A   Calc     2.56(9), Rep     2.56000 ....    Missing su
                     HW1  -CL6     1.555   6.565

PLAT_746  Alert C H...A   Calc    2.32(10), Rep     2.32000 ....    Missing su
                     HW2  -CL7     1.555   6.555

General Notes



ABSTM_02  The ratio of expected to reported Tmax/Tmin(RR) is > 1.10
          Tmin and Tmax reported:      0.463     0.634
          Tmin and Tmax expected:      0.454     0.713
          RR =      1.146
          Please check that your absorption correction is appropriate.


 0 Alert Level A = Potentially serious problem

 2 Alert Level B = Potential problem

 36 Alert Level C = Please check

Comment top

The title compound, (I), represents the dihydrate of the anilinium salt of the tetradecachloromolybdate dianion, (PhNH₃)₂[(Mo₆Cl₈)Cl₆]·2H₂O (Figs. 1 and 2). It has been investigated as part of a project aimed at the synthesis of extended molecular assemblies based on the [(Mo₆Cl₈)Cl₆]^-2 clusters.

On crystallization of the title compound, the pH of mother liquor was < 0.3, which implies that equilibrium should be shifted towards protonation of aniline rather than water molecules. In order to confirm this, fluorescence emission spectra were obtained. The neutral aniline species is known to exhibit pronounced emission at 310–400 nm. However, the emission spectrum of the title compound, recorded in the aniline wavelength, shows only the water Raman peak.

The fluorescence emission spectrum of the title compound shows the only peak, its position coinciding with the position of the peak observed in the spectrum of pure (H₃O)₂[(Mo₆Cl₈)Cl₆]·7H₂O. In compounds, containing the central (Mo₆Cl₈)⁺⁴ cluster unit, it is the Mo core which is responsible for the emission (Maverick & Gray, 1981) and this does not change when different counter-ions are introduced into the crystal structures. This confirms that aniline exists in this structure as the protonated anilinium cation.

The negatively charged clusters are linked together along the b direction of the crystal through hydrogen bonds involving the water molecules. Hydrogen bonds involving the anilinium cations link the clusters along the a direction. The –NH₃···H₂O hydrogen bonding completes the three-dimensional hydrogen-bonding framework [Fig. 3(a)-(c)]. Similar hydrogen-bonding systems involving [(Mo₆Cl₈)Cl₆]^-2 clusters (Fig. 3 d) have been observed earlier (Flemström et al., 2002).

Experimental top

The title compound was synthesized by dripping 2 ml of commercial aniline into 20 ml of hot (360 K) saturated solution of (H₃O)₂[(Mo₆Cl₈)Cl₆]·7H₂O (Flemström et al., 2002) in 1 M HCl. After 24 h at 280 K, cognac-colored parallelepiped-shaped crystals precipitated. A well shaped crystal was chosen and glued on a glass fibre.

Computing details top

Data collection: IPDS Software (Stoe & Cie, 1997); cell refinement: IPDS Software; data reduction: IPDS Software; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997) and JANA2000 (Petricek & Dusek, 2000); program(s) used to refine structure: SHELXL97 and JANA2000; software used to prepare material for publication: SHELXL97 and JANA2000.

Figures top

	Fig. 1. The structure of (PhNH₃)₂[(Mo₆Cl₈)Cl₆]·2H₂O, viewed along the [010] direction. Red atoms: water oxygen, blue: nitrogen, black: carbon and grey: molybdenum.
	Fig. 2. The cation, anion and hydrate molecule in the crystal structure of the title compound. Displacement ellipsoids are drawn at the 50% probability level.
	Fig. 3. (a) Infinite chains along the b direction involving hydrogen-bonded water molecules and anionic clusters. (b) Infinite chains along the a direction involving hydrogen-bonded anilinium cations and anionic clusters. (c) NH₃···H₂O hydrogen bonding viewed down the a direction, with the anionic clusters omitted. (d) The hydrogen-bond arrangement around the anionic clusters.

(I) top

Crystal data top

2C₆H₈N⁺·Mo₆Cl₁₄²⁻·2H₂O	F(000) = 2448
M_r = 1296.24	D_x = 2.626 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 20.665 (8) Å	Cell parameters from 5000 reflections
b = 11.335 (3) Å	θ = 4.1–28.3°
c = 17.347 (6) Å	µ = 3.38 mm⁻¹
β = 126.21 (5)°	T = 293 K
V = 3279 (3) Å³	Parallelepiped, cognac brown
Z = 4	0.3 × 0.2 × 0.1 mm

Data collection top

Stoe IPDS diffractometer	2368 independent reflections
Radiation source: X-ray fine-focus sealed tube	1908 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.049
Detector resolution: 6.0 pixels mm^-1	θ_max = 23.9°, θ_min = 3.5°
Area–detector ϕ scans	h = −23→23
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 1996)	k = −12→12
T_min = 0.463, T_max = 0.634	l = −18→18
8558 measured reflections

Refinement top

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)] = 0.029	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.062	H-atom parameters constrained
S = 1.37	w = 1/[σ²(F_o²) + (0.02P)²] where P = (F_o² + 2F_c²)/3
2368 reflections	(Δ/σ)_max < 0.001
170 parameters	Δρ_max = 0.58 e Å⁻³
3 restraints	Δρ_min = −0.57 e Å⁻³

Crystal data top

2C₆H₈N⁺·Mo₆Cl₁₄²⁻·2H₂O	V = 3279 (3) Å³
M_r = 1296.24	Z = 4
Monoclinic, C2/c	Mo Kα radiation
a = 20.665 (8) Å	µ = 3.38 mm⁻¹
b = 11.335 (3) Å	T = 293 K
c = 17.347 (6) Å	0.3 × 0.2 × 0.1 mm
β = 126.21 (5)°

Data collection top

Stoe IPDS diffractometer	2368 independent reflections
Absorption correction: numerical (X-SHAPE; Stoe & Cie, 1996)	1908 reflections with I > 2σ(I)
T_min = 0.463, T_max = 0.634	R_int = 0.049
8558 measured reflections	θ_max = 23.9°

Refinement top

R[F² > 2σ(F²)] = 0.029	3 restraints
wR(F²) = 0.062	H-atom parameters constrained
S = 1.37	Δρ_max = 0.58 e Å⁻³
2368 reflections	Δρ_min = −0.57 e Å⁻³
170 parameters

Special details top

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 (Å²) top

	x	y	z	U_iso*/U_eq
Mo1	0.425215 (18)	0.48452 (3)	0.17398 (2)	0.02159 (12)
Mo2	0.465522 (17)	0.36924 (3)	0.32710 (2)	0.02036 (11)
Mo3	0.424981 (18)	0.25454 (3)	0.17358 (2)	0.01952 (12)
Cl1	0.39093 (5)	0.36952 (9)	0.03281 (6)	0.0284 (2)
Cl2	0.32587 (5)	0.36887 (9)	0.17906 (7)	0.0268 (2)
Cl3	0.53322 (6)	0.58768 (9)	0.17742 (7)	0.0303 (3)
Cl4	0.46711 (5)	0.15080 (9)	0.32243 (7)	0.0269 (2)
Cl5	0.42060 (6)	0.36609 (11)	0.42975 (8)	0.0408 (3)
Cl6	0.32670 (6)	0.64103 (9)	0.07510 (8)	0.0404 (3)
Cl7	0.32621 (6)	0.10384 (10)	0.07325 (8)	0.0396 (3)
N1	0.3396 (3)	0.1392 (4)	−0.5535 (4)	0.0649 (13)
HN1	0.3771	0.1192	−0.4930	0.097*
HN2	0.2920	0.1415	−0.5638	0.097*
HN3	0.3508	0.2099	−0.5651	0.097*
C1	0.3376 (3)	0.0514 (4)	−0.6174 (4)	0.0452 (13)
C2	0.2847 (3)	0.0670 (6)	−0.7141 (5)	0.0632 (17)
H2	0.2508	0.1322	−0.7391	0.095*
C3	0.2825 (4)	−0.0176 (8)	−0.7747 (5)	0.083 (2)
H3	0.2468	−0.0095	−0.8407	0.125*
C4	0.3337 (5)	−0.1123 (7)	−0.7357 (7)	0.086 (2)
H4	0.3326	−0.1683	−0.7757	0.129*
C5	0.3858 (5)	−0.1254 (6)	−0.6398 (6)	0.080 (2)
H5	0.4203	−0.1899	−0.6147	0.120*
C6	0.3883 (3)	−0.0435 (5)	−0.5786 (5)	0.0560 (15)
H6	0.4236	−0.0529	−0.5127	0.084*
O1	0.4405 (4)	0.1188 (5)	−0.3535 (5)	0.1147 (18)
HW1	0.416 (5)	0.177 (5)	−0.345 (8)	0.172*
HW2	0.417 (6)	0.051 (4)	−0.355 (9)	0.172*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Mo1	0.01705 (19)	0.0265 (2)	0.0198 (2)	0.00297 (13)	0.01005 (17)	0.00258 (13)
Mo2	0.01682 (18)	0.0287 (2)	0.01668 (19)	−0.00060 (13)	0.01050 (15)	−0.00134 (14)
Mo3	0.01425 (19)	0.0266 (2)	0.0154 (2)	−0.00133 (12)	0.00749 (16)	−0.00139 (12)
Cl1	0.0223 (5)	0.0419 (5)	0.0155 (5)	0.0024 (4)	0.0081 (4)	0.0031 (4)
Cl2	0.0153 (4)	0.0383 (5)	0.0254 (5)	0.0013 (4)	0.0112 (4)	−0.0004 (4)
Cl3	0.0303 (5)	0.0312 (5)	0.0322 (6)	−0.0007 (4)	0.0199 (5)	0.0072 (4)
Cl4	0.0248 (5)	0.0316 (5)	0.0254 (5)	−0.0023 (4)	0.0154 (4)	0.0039 (4)
Cl5	0.0422 (6)	0.0602 (7)	0.0350 (6)	−0.0088 (5)	0.0311 (5)	−0.0093 (5)
Cl6	0.0311 (5)	0.0401 (6)	0.0478 (7)	0.0137 (5)	0.0220 (5)	0.0169 (6)
Cl7	0.0306 (5)	0.0476 (6)	0.0334 (6)	−0.0150 (5)	0.0149 (5)	−0.0119 (5)
N1	0.058 (3)	0.069 (3)	0.091 (4)	−0.008 (2)	0.057 (3)	−0.003 (3)
C1	0.036 (3)	0.053 (3)	0.055 (4)	−0.008 (2)	0.031 (3)	0.002 (3)
C2	0.039 (3)	0.079 (4)	0.066 (5)	−0.006 (3)	0.028 (3)	0.024 (3)
C3	0.065 (4)	0.131 (7)	0.050 (5)	−0.049 (5)	0.032 (4)	−0.005 (4)
C4	0.102 (6)	0.101 (6)	0.094 (6)	−0.048 (5)	0.079 (5)	−0.033 (5)
C5	0.101 (5)	0.071 (4)	0.110 (7)	0.005 (4)	0.086 (5)	0.001 (4)
C6	0.050 (3)	0.068 (4)	0.054 (4)	0.010 (3)	0.034 (3)	0.022 (3)
O1	0.115 (5)	0.088 (3)	0.127 (5)	0.008 (3)	0.064 (4)	0.002 (4)

Geometric parameters (Å, º) top

Mo1—Cl6	2.4714 (15)	Mo3—Mo3ⁱ	2.633 (2)
Mo1—Cl3ⁱ	2.4767 (14)	Cl1—Mo2ⁱ	2.488 (2)
Mo1—Cl1	2.4795 (13)	Cl3—Mo1ⁱ	2.4767 (14)
Mo1—Cl2	2.4809 (11)	Cl3—Mo2ⁱ	2.4779 (12)
Mo1—Cl3	2.4889 (12)	Cl4—Mo3ⁱ	2.4856 (12)
Mo1—Mo3	2.6069 (8)	N1—C1	1.472 (7)
Mo1—Mo2	2.6158 (11)	N1—HN1	0.89
Mo1—Mo2ⁱ	2.6184 (9)	N1—HN2	0.89
Mo1—Mo1ⁱ	2.623 (2)	N1—HN3	0.89
Mo2—Cl5	2.4467 (13)	C1—C2	1.368 (8)
Mo2—Cl3ⁱ	2.4779 (12)	C1—C6	1.370 (7)
Mo2—Cl4	2.4782 (12)	C2—C3	1.405 (10)
Mo2—Cl2	2.483 (2)	C2—H2	0.93
Mo2—Cl1ⁱ	2.488 (2)	C3—C4	1.373 (11)
Mo2—Mo3ⁱ	2.6157 (9)	C3—H3	0.93
Mo2—Mo3	2.6168 (11)	C4—C5	1.354 (11)
Mo2—Mo1ⁱ	2.6184 (9)	C4—H4	0.93
Mo3—Cl7	2.4323 (15)	C5—C6	1.388 (9)
Mo3—Cl2	2.4725 (11)	C5—H5	0.93
Mo3—Cl1	2.4753 (13)	C6—H6	0.93
Mo3—Cl4	2.4803 (14)	O1—HW1	0.90 (2)
Mo3—Cl4ⁱ	2.4856 (12)	O1—HW2	0.90 (2)
Mo3—Mo2ⁱ	2.6157 (9)

Cl6—Mo1—Cl3ⁱ	91.17 (6)	Cl7—Mo3—Cl1	91.98 (6)
Cl6—Mo1—Cl1	93.11 (6)	Cl2—Mo3—Cl1	90.16 (5)
Cl3ⁱ—Mo1—Cl1	175.71 (3)	Cl7—Mo3—Cl4	92.41 (6)
Cl6—Mo1—Cl2	92.54 (5)	Cl2—Mo3—Cl4	89.87 (5)
Cl3ⁱ—Mo1—Cl2	89.88 (5)	Cl1—Mo3—Cl4	175.61 (3)
Cl1—Mo1—Cl2	89.87 (5)	Cl7—Mo3—Cl4ⁱ	92.72 (5)
Cl6—Mo1—Cl3	92.22 (5)	Cl2—Mo3—Cl4ⁱ	175.43 (3)
Cl3ⁱ—Mo1—Cl3	89.91 (6)	Cl1—Mo3—Cl4ⁱ	90.23 (5)
Cl1—Mo1—Cl3	89.98 (5)	Cl4—Mo3—Cl4ⁱ	89.39 (6)
Cl2—Mo1—Cl3	175.24 (3)	Cl7—Mo3—Mo1	134.72 (4)
Cl6—Mo1—Mo3	135.77 (4)	Cl2—Mo3—Mo1	58.40 (3)
Cl3ⁱ—Mo1—Mo3	118.28 (3)	Cl1—Mo3—Mo1	58.33 (3)
Cl1—Mo1—Mo3	58.18 (3)	Cl4—Mo3—Mo1	118.19 (3)
Cl2—Mo1—Mo3	58.09 (3)	Cl4ⁱ—Mo3—Mo1	118.21 (3)
Cl3—Mo1—Mo3	118.04 (3)	Cl7—Mo3—Mo2ⁱ	135.10 (4)
Cl6—Mo1—Mo2	134.50 (4)	Cl2—Mo3—Mo2ⁱ	118.56 (4)
Cl3ⁱ—Mo1—Mo2	58.16 (4)	Cl1—Mo3—Mo2ⁱ	58.42 (5)
Cl1—Mo1—Mo2	118.30 (4)	Cl4—Mo3—Mo2ⁱ	117.89 (6)
Cl2—Mo1—Mo2	58.25 (5)	Cl4ⁱ—Mo3—Mo2ⁱ	58.06 (3)
Cl3—Mo1—Mo2	117.85 (6)	Mo1—Mo3—Mo2ⁱ	60.178 (17)
Mo3—Mo1—Mo2	60.138 (19)	Cl7—Mo3—Mo2	134.91 (4)
Cl6—Mo1—Mo2ⁱ	135.52 (4)	Cl2—Mo3—Mo2	58.33 (5)
Cl3ⁱ—Mo1—Mo2ⁱ	118.21 (6)	Cl1—Mo3—Mo2	118.42 (4)
Cl1—Mo1—Mo2ⁱ	58.34 (5)	Cl4—Mo3—Mo2	58.11 (4)
Cl2—Mo1—Mo2ⁱ	118.15 (4)	Cl4ⁱ—Mo3—Mo2	117.65 (6)
Cl3—Mo1—Mo2ⁱ	57.98 (3)	Mo1—Mo3—Mo2	60.100 (19)
Mo3—Mo1—Mo2ⁱ	60.078 (17)	Mo2ⁱ—Mo3—Mo2	89.99 (4)
Mo2—Mo1—Mo2ⁱ	89.96 (4)	Cl7—Mo3—Mo3ⁱ	135.39 (4)
Cl6—Mo1—Mo1ⁱ	134.12 (4)	Cl2—Mo3—Mo3ⁱ	118.09 (4)
Cl3ⁱ—Mo1—Mo1ⁱ	58.35 (5)	Cl1—Mo3—Mo3ⁱ	118.22 (5)
Cl1—Mo1—Mo1ⁱ	118.20 (5)	Cl4—Mo3—Mo3ⁱ	58.08 (5)
Cl2—Mo1—Mo1ⁱ	118.20 (4)	Cl4ⁱ—Mo3—Mo3ⁱ	57.89 (4)
Cl3—Mo1—Mo1ⁱ	57.89 (4)	Mo1—Mo3—Mo3ⁱ	89.892 (11)
Mo3—Mo1—Mo1ⁱ	90.108 (11)	Mo2ⁱ—Mo3—Mo3ⁱ	59.82 (3)
Mo2—Mo1—Mo1ⁱ	59.98 (4)	Mo2—Mo3—Mo3ⁱ	59.77 (4)
Mo2ⁱ—Mo1—Mo1ⁱ	59.88 (3)	Mo3—Cl1—Mo1	63.49 (4)
Cl5—Mo2—Cl3ⁱ	93.05 (4)	Mo3—Cl1—Mo2ⁱ	63.61 (5)
Cl5—Mo2—Cl4	91.56 (4)	Mo1—Cl1—Mo2ⁱ	63.62 (5)
Cl3ⁱ—Mo2—Cl4	175.38 (3)	Mo3—Cl2—Mo1	63.51 (3)
Cl5—Mo2—Cl2	92.51 (5)	Mo3—Cl2—Mo2	63.74 (4)
Cl3ⁱ—Mo2—Cl2	89.80 (3)	Mo1—Cl2—Mo2	63.60 (4)
Cl4—Mo2—Cl2	89.67 (3)	Mo1ⁱ—Cl3—Mo2ⁱ	63.74 (3)
Cl5—Mo2—Cl1ⁱ	92.01 (5)	Mo1ⁱ—Cl3—Mo1	63.76 (6)
Cl3ⁱ—Mo2—Cl1ⁱ	90.05 (3)	Mo2ⁱ—Cl3—Mo1	63.63 (3)
Cl4—Mo2—Cl1ⁱ	90.12 (3)	Mo2—Cl4—Mo3	63.71 (3)
Cl2—Mo2—Cl1ⁱ	175.47 (3)	Mo2—Cl4—Mo3ⁱ	63.60 (3)
Cl5—Mo2—Mo3ⁱ	134.20 (4)	Mo3—Cl4—Mo3ⁱ	64.03 (6)
Cl3ⁱ—Mo2—Mo3ⁱ	118.12 (3)	C1—N1—HN1	109.5
Cl4—Mo2—Mo3ⁱ	58.34 (2)	C1—N1—HN2	109.5
Cl2—Mo2—Mo3ⁱ	118.32 (4)	HN1—N1—HN2	109.5
Cl1ⁱ—Mo2—Mo3ⁱ	57.97 (4)	C1—N1—HN3	109.5
Cl5—Mo2—Mo1	135.74 (4)	HN1—N1—HN3	109.5
Cl3ⁱ—Mo2—Mo1	58.11 (3)	HN2—N1—HN3	109.5
Cl4—Mo2—Mo1	117.93 (3)	C2—C1—C6	122.0 (6)
Cl2—Mo2—Mo1	58.16 (4)	C2—C1—N1	118.8 (5)
Cl1ⁱ—Mo2—Mo1	118.16 (5)	C6—C1—N1	119.2 (5)
Mo3ⁱ—Mo2—Mo1	90.06 (4)	C1—C2—C3	118.5 (6)
Cl5—Mo2—Mo3	134.62 (4)	C1—C2—H2	120.7
Cl3ⁱ—Mo2—Mo3	117.86 (3)	C3—C2—H2	120.7
Cl4—Mo2—Mo3	58.19 (3)	C4—C3—C2	119.4 (7)
Cl2—Mo2—Mo3	57.93 (4)	C4—C3—H3	120.3
Cl1ⁱ—Mo2—Mo3	118.36 (5)	C2—C3—H3	120.3
Mo3ⁱ—Mo2—Mo3	60.41 (5)	C5—C4—C3	120.9 (7)
Mo1—Mo2—Mo3	59.76 (3)	C5—C4—H4	119.5
Cl5—Mo2—Mo1ⁱ	135.39 (4)	C3—C4—H4	119.5
Cl3ⁱ—Mo2—Mo1ⁱ	58.39 (3)	C4—C5—C6	120.7 (7)
Cl4—Mo2—Mo1ⁱ	118.05 (3)	C4—C5—H5	119.7
Cl2—Mo2—Mo1ⁱ	118.28 (4)	C6—C5—H5	119.7
Cl1ⁱ—Mo2—Mo1ⁱ	58.04 (4)	C1—C6—C5	118.5 (6)
Mo3ⁱ—Mo2—Mo1ⁱ	59.74 (3)	C1—C6—H6	120.7
Mo1—Mo2—Mo1ⁱ	60.14 (5)	C5—C6—H6	120.7
Mo3—Mo2—Mo1ⁱ	89.99 (4)	HW1—O1—HW2	107 (3)
Cl7—Mo3—Cl2	91.81 (5)

Cl6—Mo1—Mo2—Cl5	1.93 (6)	Cl5—Mo2—Mo3—Cl4ⁱ	−125.57 (6)
Cl3ⁱ—Mo1—Mo2—Cl5	56.72 (6)	Cl3ⁱ—Mo2—Mo3—Cl4ⁱ	107.14 (5)
Cl1—Mo1—Mo2—Cl5	−126.06 (6)	Cl4—Mo2—Mo3—Cl4ⁱ	−70.11 (5)
Cl2—Mo1—Mo2—Cl5	−55.71 (6)	Cl2—Mo2—Mo3—Cl4ⁱ	177.50 (4)
Cl3—Mo1—Mo2—Cl5	127.44 (6)	Cl1ⁱ—Mo2—Mo3—Cl4ⁱ	0.49 (4)
Mo3—Mo1—Mo2—Cl5	−124.52 (5)	Mo3ⁱ—Mo2—Mo3—Cl4ⁱ	−1.10 (3)
Mo2ⁱ—Mo1—Mo2—Cl5	−179.44 (4)	Mo1—Mo2—Mo3—Cl4ⁱ	108.32 (4)
Mo1ⁱ—Mo1—Mo2—Cl5	125.95 (5)	Mo1ⁱ—Mo2—Mo3—Cl4ⁱ	53.50 (4)
Cl6—Mo1—Mo2—Cl3ⁱ	−54.79 (6)	Cl5—Mo2—Mo3—Mo1	126.11 (6)
Cl1—Mo1—Mo2—Cl3ⁱ	177.22 (4)	Cl3ⁱ—Mo2—Mo3—Mo1	−1.19 (3)
Cl2—Mo1—Mo2—Cl3ⁱ	−112.43 (4)	Cl4—Mo2—Mo3—Mo1	−178.44 (3)
Cl3—Mo1—Mo2—Cl3ⁱ	70.72 (5)	Cl2—Mo2—Mo3—Mo1	69.18 (4)
Mo3—Mo1—Mo2—Cl3ⁱ	178.76 (3)	Cl1ⁱ—Mo2—Mo3—Mo1	−107.83 (4)
Mo2ⁱ—Mo1—Mo2—Cl3ⁱ	123.85 (4)	Mo3ⁱ—Mo2—Mo3—Mo1	−109.42 (3)
Mo1ⁱ—Mo1—Mo2—Cl3ⁱ	69.23 (4)	Mo1ⁱ—Mo2—Mo3—Mo1	−54.82 (3)
Cl6—Mo1—Mo2—Cl4	127.96 (6)	Cl5—Mo2—Mo3—Mo2ⁱ	−178.89 (4)
Cl3ⁱ—Mo1—Mo2—Cl4	−177.26 (3)	Cl3ⁱ—Mo2—Mo3—Mo2ⁱ	53.81 (4)
Cl1—Mo1—Mo2—Cl4	−0.04 (4)	Cl4—Mo2—Mo3—Mo2ⁱ	−123.44 (4)
Cl2—Mo1—Mo2—Cl4	70.31 (4)	Cl2—Mo2—Mo3—Mo2ⁱ	124.18 (4)
Cl3—Mo1—Mo2—Cl4	−106.54 (5)	Cl1ⁱ—Mo2—Mo3—Mo2ⁱ	−52.83 (4)
Mo3—Mo1—Mo2—Cl4	1.50 (3)	Mo3ⁱ—Mo2—Mo3—Mo2ⁱ	−54.42 (3)
Mo2ⁱ—Mo1—Mo2—Cl4	−53.41 (4)	Mo1—Mo2—Mo3—Mo2ⁱ	55.00 (3)
Mo1ⁱ—Mo1—Mo2—Cl4	−108.03 (4)	Mo1ⁱ—Mo2—Mo3—Mo2ⁱ	0.179 (15)
Cl6—Mo1—Mo2—Cl2	57.64 (5)	Cl5—Mo2—Mo3—Mo3ⁱ	−124.47 (5)
Cl3ⁱ—Mo1—Mo2—Cl2	112.43 (4)	Cl3ⁱ—Mo2—Mo3—Mo3ⁱ	108.23 (4)
Cl1—Mo1—Mo2—Cl2	−70.35 (4)	Cl4—Mo2—Mo3—Mo3ⁱ	−69.02 (3)
Cl3—Mo1—Mo2—Cl2	−176.85 (4)	Cl2—Mo2—Mo3—Mo3ⁱ	178.60 (3)
Mo3—Mo1—Mo2—Cl2	−68.81 (4)	Cl1ⁱ—Mo2—Mo3—Mo3ⁱ	1.59 (3)
Mo2ⁱ—Mo1—Mo2—Cl2	−123.73 (4)	Mo1—Mo2—Mo3—Mo3ⁱ	109.42 (3)
Mo1ⁱ—Mo1—Mo2—Cl2	−178.34 (3)	Mo1ⁱ—Mo2—Mo3—Mo3ⁱ	54.60 (3)
Cl6—Mo1—Mo2—Cl1ⁱ	−125.40 (5)	Cl7—Mo3—Cl1—Mo1	143.70 (4)
Cl3ⁱ—Mo1—Mo2—Cl1ⁱ	−70.61 (5)	Cl2—Mo3—Cl1—Mo1	51.88 (4)
Cl1—Mo1—Mo2—Cl1ⁱ	106.61 (4)	Cl4—Mo3—Cl1—Mo1	−38.5 (5)
Cl2—Mo1—Mo2—Cl1ⁱ	176.96 (4)	Cl4ⁱ—Mo3—Cl1—Mo1	−123.57 (4)
Cl3—Mo1—Mo2—Cl1ⁱ	0.11 (4)	Mo2ⁱ—Mo3—Cl1—Mo1	−72.14 (3)
Mo3—Mo1—Mo2—Cl1ⁱ	108.15 (4)	Mo2—Mo3—Cl1—Mo1	−1.57 (2)
Mo2ⁱ—Mo1—Mo2—Cl1ⁱ	53.23 (4)	Mo3ⁱ—Mo3—Cl1—Mo1	−70.52 (4)
Mo1ⁱ—Mo1—Mo2—Cl1ⁱ	−1.38 (3)	Cl7—Mo3—Cl1—Mo2ⁱ	−144.16 (4)
Cl6—Mo1—Mo2—Mo3ⁱ	−178.45 (4)	Cl2—Mo3—Cl1—Mo2ⁱ	124.02 (4)
Cl3ⁱ—Mo1—Mo2—Mo3ⁱ	−123.67 (4)	Cl4—Mo3—Cl1—Mo2ⁱ	33.6 (5)
Cl1—Mo1—Mo2—Mo3ⁱ	53.56 (4)	Cl4ⁱ—Mo3—Cl1—Mo2ⁱ	−51.43 (4)
Cl2—Mo1—Mo2—Mo3ⁱ	123.90 (4)	Mo1—Mo3—Cl1—Mo2ⁱ	72.14 (3)
Cl3—Mo1—Mo2—Mo3ⁱ	−52.95 (4)	Mo2—Mo3—Cl1—Mo2ⁱ	70.56 (4)
Mo3—Mo1—Mo2—Mo3ⁱ	55.10 (3)	Mo3ⁱ—Mo3—Cl1—Mo2ⁱ	1.62 (3)
Mo2ⁱ—Mo1—Mo2—Mo3ⁱ	0.179 (15)	Cl6—Mo1—Cl1—Mo3	−144.17 (3)
Mo1ⁱ—Mo1—Mo2—Mo3ⁱ	−54.43 (3)	Cl3ⁱ—Mo1—Cl1—Mo3	35.0 (5)
Cl6—Mo1—Mo2—Mo3	126.45 (5)	Cl2—Mo1—Cl1—Mo3	−51.63 (4)
Cl3ⁱ—Mo1—Mo2—Mo3	−178.76 (3)	Cl3—Mo1—Cl1—Mo3	123.61 (4)
Cl1—Mo1—Mo2—Mo3	−1.54 (2)	Mo2—Mo1—Cl1—Mo3	1.57 (2)
Cl2—Mo1—Mo2—Mo3	68.81 (4)	Mo2ⁱ—Mo1—Cl1—Mo3	72.12 (3)
Cl3—Mo1—Mo2—Mo3	−108.04 (4)	Mo1ⁱ—Mo1—Cl1—Mo3	70.71 (4)
Mo2ⁱ—Mo1—Mo2—Mo3	−54.92 (3)	Cl6—Mo1—Cl1—Mo2ⁱ	143.71 (4)
Mo1ⁱ—Mo1—Mo2—Mo3	−109.53 (3)	Cl3ⁱ—Mo1—Cl1—Mo2ⁱ	−37.1 (5)
Cl6—Mo1—Mo2—Mo1ⁱ	−124.02 (5)	Cl2—Mo1—Cl1—Mo2ⁱ	−123.75 (4)
Cl3ⁱ—Mo1—Mo2—Mo1ⁱ	−69.23 (4)	Cl3—Mo1—Cl1—Mo2ⁱ	51.49 (4)
Cl1—Mo1—Mo2—Mo1ⁱ	107.99 (4)	Mo3—Mo1—Cl1—Mo2ⁱ	−72.12 (3)
Cl2—Mo1—Mo2—Mo1ⁱ	178.34 (3)	Mo2—Mo1—Cl1—Mo2ⁱ	−70.55 (4)
Cl3—Mo1—Mo2—Mo1ⁱ	1.49 (3)	Mo1ⁱ—Mo1—Cl1—Mo2ⁱ	−1.41 (3)
Mo3—Mo1—Mo2—Mo1ⁱ	109.53 (3)	Cl7—Mo3—Cl2—Mo1	−143.81 (4)
Mo2ⁱ—Mo1—Mo2—Mo1ⁱ	54.61 (3)	Cl1—Mo3—Cl2—Mo1	−51.83 (4)
Cl6—Mo1—Mo3—Cl7	0.54 (7)	Cl4—Mo3—Cl2—Mo1	123.78 (5)
Cl3ⁱ—Mo1—Mo3—Cl7	126.41 (7)	Cl4ⁱ—Mo3—Cl2—Mo1	43.1 (5)
Cl1—Mo1—Mo3—Cl7	−56.38 (7)	Mo2ⁱ—Mo3—Cl2—Mo1	1.68 (3)
Cl2—Mo1—Mo3—Cl7	56.16 (6)	Mo2—Mo3—Cl2—Mo1	72.05 (3)
Cl3—Mo1—Mo3—Cl7	−127.05 (6)	Mo3ⁱ—Mo3—Cl2—Mo1	70.68 (3)
Mo2—Mo1—Mo3—Cl7	125.22 (6)	Cl7—Mo3—Cl2—Mo2	144.14 (4)
Mo2ⁱ—Mo1—Mo3—Cl7	−125.55 (6)	Cl1—Mo3—Cl2—Mo2	−123.88 (4)
Mo1ⁱ—Mo1—Mo3—Cl7	179.91 (4)	Cl4—Mo3—Cl2—Mo2	51.73 (4)
Cl6—Mo1—Mo3—Cl2	−55.62 (6)	Cl4ⁱ—Mo3—Cl2—Mo2	−29.0 (5)
Cl3ⁱ—Mo1—Mo3—Cl2	70.26 (7)	Mo1—Mo3—Cl2—Mo2	−72.05 (3)
Cl1—Mo1—Mo3—Cl2	−112.54 (7)	Mo2ⁱ—Mo3—Cl2—Mo2	−70.37 (3)
Cl3—Mo1—Mo3—Cl2	176.79 (4)	Mo3ⁱ—Mo3—Cl2—Mo2	−1.37 (3)
Mo2—Mo1—Mo3—Cl2	69.06 (6)	Cl6—Mo1—Cl2—Mo3	144.81 (4)
Mo2ⁱ—Mo1—Mo3—Cl2	178.30 (3)	Cl3ⁱ—Mo1—Cl2—Mo3	−124.02 (5)
Mo1ⁱ—Mo1—Mo3—Cl2	123.75 (4)	Cl1—Mo1—Cl2—Mo3	51.70 (4)
Cl6—Mo1—Mo3—Cl1	56.92 (7)	Cl3—Mo1—Cl2—Mo3	−36.5 (4)
Cl3ⁱ—Mo1—Mo3—Cl1	−177.21 (4)	Mo2—Mo1—Cl2—Mo3	−72.28 (3)
Cl2—Mo1—Mo3—Cl1	112.54 (7)	Mo2ⁱ—Mo1—Cl2—Mo3	−1.67 (3)
Cl3—Mo1—Mo3—Cl1	−70.67 (7)	Mo1ⁱ—Mo1—Cl2—Mo3	−70.65 (3)
Mo2—Mo1—Mo3—Cl1	−178.40 (3)	Cl6—Mo1—Cl2—Mo2	−142.91 (4)
Mo2ⁱ—Mo1—Mo3—Cl1	−69.17 (6)	Cl3ⁱ—Mo1—Cl2—Mo2	−51.74 (4)
Mo1ⁱ—Mo1—Mo3—Cl1	−123.72 (5)	Cl1—Mo1—Cl2—Mo2	123.98 (4)
Cl6—Mo1—Mo3—Cl4	−126.18 (7)	Cl3—Mo1—Cl2—Mo2	35.8 (4)
Cl3ⁱ—Mo1—Mo3—Cl4	−0.31 (4)	Mo3—Mo1—Cl2—Mo2	72.28 (3)
Cl1—Mo1—Mo3—Cl4	176.90 (4)	Mo2ⁱ—Mo1—Cl2—Mo2	70.60 (3)
Cl2—Mo1—Mo3—Cl4	−70.57 (7)	Mo1ⁱ—Mo1—Cl2—Mo2	1.63 (3)
Cl3—Mo1—Mo3—Cl4	106.22 (7)	Cl5—Mo2—Cl2—Mo3	−143.34 (4)
Mo2—Mo1—Mo3—Cl4	−1.51 (3)	Cl3ⁱ—Mo2—Cl2—Mo3	123.62 (3)
Mo2ⁱ—Mo1—Mo3—Cl4	107.73 (6)	Cl4—Mo2—Cl2—Mo3	−51.79 (3)
Mo1ⁱ—Mo1—Mo3—Cl4	53.18 (5)	Cl1ⁱ—Mo2—Cl2—Mo3	35.6 (5)
Cl6—Mo1—Mo3—Cl4ⁱ	127.92 (6)	Mo3ⁱ—Mo2—Cl2—Mo3	1.38 (3)
Cl3ⁱ—Mo1—Mo3—Cl4ⁱ	−106.21 (7)	Mo1—Mo2—Cl2—Mo3	71.92 (3)
Cl1—Mo1—Mo3—Cl4ⁱ	71.00 (7)	Mo1ⁱ—Mo2—Cl2—Mo3	70.28 (4)
Cl2—Mo1—Mo3—Cl4ⁱ	−176.46 (4)	Cl5—Mo2—Cl2—Mo1	144.75 (4)
Cl3—Mo1—Mo3—Cl4ⁱ	0.33 (5)	Cl3ⁱ—Mo2—Cl2—Mo1	51.70 (3)
Mo2—Mo1—Mo3—Cl4ⁱ	−107.40 (7)	Cl4—Mo2—Cl2—Mo1	−123.71 (3)
Mo2ⁱ—Mo1—Mo3—Cl4ⁱ	1.83 (3)	Cl1ⁱ—Mo2—Cl2—Mo1	−36.4 (5)
Mo1ⁱ—Mo1—Mo3—Cl4ⁱ	−52.71 (5)	Mo3ⁱ—Mo2—Cl2—Mo1	−70.53 (4)
Cl6—Mo1—Mo3—Mo2ⁱ	126.09 (6)	Mo3—Mo2—Cl2—Mo1	−71.92 (3)
Cl3ⁱ—Mo1—Mo3—Mo2ⁱ	−108.04 (6)	Mo1ⁱ—Mo2—Cl2—Mo1	−1.64 (3)
Cl1—Mo1—Mo3—Mo2ⁱ	69.17 (6)	Cl6—Mo1—Cl3—Mo1ⁱ	142.96 (4)
Cl2—Mo1—Mo3—Mo2ⁱ	−178.30 (3)	Cl3ⁱ—Mo1—Cl3—Mo1ⁱ	51.79 (5)
Cl3—Mo1—Mo3—Mo2ⁱ	−1.50 (3)	Cl1—Mo1—Cl3—Mo1ⁱ	−123.93 (4)
Mo2—Mo1—Mo3—Mo2ⁱ	−109.23 (6)	Cl2—Mo1—Cl3—Mo1ⁱ	−35.7 (4)
Mo1ⁱ—Mo1—Mo3—Mo2ⁱ	−54.55 (4)	Mo3—Mo1—Cl3—Mo1ⁱ	−70.63 (3)
Cl6—Mo1—Mo3—Mo2	−124.68 (6)	Mo2—Mo1—Cl3—Mo1ⁱ	−1.52 (3)
Cl3ⁱ—Mo1—Mo3—Mo2	1.19 (3)	Mo2ⁱ—Mo1—Cl3—Mo1ⁱ	−72.17 (3)
Cl1—Mo1—Mo3—Mo2	178.40 (3)	Cl6—Mo1—Cl3—Mo2ⁱ	−144.88 (4)
Cl2—Mo1—Mo3—Mo2	−69.06 (6)	Cl3ⁱ—Mo1—Cl3—Mo2ⁱ	123.95 (5)
Cl3—Mo1—Mo3—Mo2	107.73 (7)	Cl1—Mo1—Cl3—Mo2ⁱ	−51.76 (4)
Mo2ⁱ—Mo1—Mo3—Mo2	109.23 (6)	Cl2—Mo1—Cl3—Mo2ⁱ	36.4 (4)
Mo1ⁱ—Mo1—Mo3—Mo2	54.69 (5)	Mo3—Mo1—Cl3—Mo2ⁱ	1.54 (3)
Cl6—Mo1—Mo3—Mo3ⁱ	−179.25 (4)	Mo2—Mo1—Cl3—Mo2ⁱ	70.64 (3)
Cl3ⁱ—Mo1—Mo3—Mo3ⁱ	−53.38 (5)	Mo1ⁱ—Mo1—Cl3—Mo2ⁱ	72.17 (3)
Cl1—Mo1—Mo3—Mo3ⁱ	123.83 (5)	Cl5—Mo2—Cl4—Mo3	144.09 (4)
Cl2—Mo1—Mo3—Mo3ⁱ	−123.64 (4)	Cl3ⁱ—Mo2—Cl4—Mo3	−31.8 (4)
Cl3—Mo1—Mo3—Mo3ⁱ	53.15 (5)	Cl2—Mo2—Cl4—Mo3	51.59 (5)
Mo2—Mo1—Mo3—Mo3ⁱ	−54.58 (5)	Cl1ⁱ—Mo2—Cl4—Mo3	−123.89 (5)
Mo2ⁱ—Mo1—Mo3—Mo3ⁱ	54.66 (4)	Mo3ⁱ—Mo2—Cl4—Mo3	−72.54 (6)
Mo1ⁱ—Mo1—Mo3—Mo3ⁱ	0.11 (2)	Mo1—Mo2—Cl4—Mo3	−1.53 (3)
Cl5—Mo2—Mo3—Cl7	1.16 (7)	Mo1ⁱ—Mo2—Cl4—Mo3	−70.67 (6)
Cl3ⁱ—Mo2—Mo3—Cl7	−126.14 (6)	Cl5—Mo2—Cl4—Mo3ⁱ	−143.38 (5)
Cl4—Mo2—Mo3—Cl7	56.62 (6)	Cl3ⁱ—Mo2—Cl4—Mo3ⁱ	40.7 (4)
Cl2—Mo2—Mo3—Cl7	−55.77 (6)	Cl2—Mo2—Cl4—Mo3ⁱ	124.12 (4)
Cl1ⁱ—Mo2—Mo3—Cl7	127.22 (5)	Cl1ⁱ—Mo2—Cl4—Mo3ⁱ	−51.36 (4)
Mo3ⁱ—Mo2—Mo3—Cl7	125.63 (5)	Mo1—Mo2—Cl4—Mo3ⁱ	71.01 (6)
Mo1—Mo2—Mo3—Cl7	−124.95 (5)	Mo3—Mo2—Cl4—Mo3ⁱ	72.54 (6)
Mo1ⁱ—Mo2—Mo3—Cl7	−179.77 (4)	Mo1ⁱ—Mo2—Cl4—Mo3ⁱ	1.86 (3)
Cl5—Mo2—Mo3—Cl2	56.93 (6)	Cl7—Mo3—Cl4—Mo2	−143.71 (3)
Cl3ⁱ—Mo2—Mo3—Cl2	−70.37 (4)	Cl2—Mo3—Cl4—Mo2	−51.90 (4)
Cl4—Mo2—Mo3—Cl2	112.38 (4)	Cl1—Mo3—Cl4—Mo2	38.5 (5)
Cl1ⁱ—Mo2—Mo3—Cl2	−177.01 (4)	Cl4ⁱ—Mo3—Cl4—Mo2	123.59 (4)
Mo3ⁱ—Mo2—Mo3—Cl2	−178.60 (3)	Mo1—Mo3—Cl4—Mo2	1.54 (3)
Mo1—Mo2—Mo3—Cl2	−69.18 (4)	Mo2ⁱ—Mo3—Cl4—Mo2	70.76 (3)
Mo1ⁱ—Mo2—Mo3—Cl2	−124.00 (4)	Mo3ⁱ—Mo3—Cl4—Mo2	71.88 (3)
Cl5—Mo2—Mo3—Cl1	127.66 (6)	Cl7—Mo3—Cl4—Mo3ⁱ	144.41 (4)
Cl3ⁱ—Mo2—Mo3—Cl1	0.36 (4)	Cl2—Mo3—Cl4—Mo3ⁱ	−123.78 (4)
Cl4—Mo2—Mo3—Cl1	−176.89 (4)	Cl1—Mo3—Cl4—Mo3ⁱ	−33.4 (5)
Cl2—Mo2—Mo3—Cl1	70.72 (4)	Cl4ⁱ—Mo3—Cl4—Mo3ⁱ	51.71 (4)
Cl1ⁱ—Mo2—Mo3—Cl1	−106.29 (4)	Mo1—Mo3—Cl4—Mo3ⁱ	−70.34 (3)
Mo3ⁱ—Mo2—Mo3—Cl1	−107.87 (4)	Mo2ⁱ—Mo3—Cl4—Mo3ⁱ	−1.12 (3)
Mo1—Mo2—Mo3—Cl1	1.55 (2)	Mo2—Mo3—Cl4—Mo3ⁱ	−71.88 (3)
Mo1ⁱ—Mo2—Mo3—Cl1	−53.27 (4)	C6—C1—C2—C3	0.2 (8)
Cl5—Mo2—Mo3—Cl4	−55.45 (6)	N1—C1—C2—C3	−179.4 (4)
Cl3ⁱ—Mo2—Mo3—Cl4	177.25 (3)	C1—C2—C3—C4	−0.6 (8)
Cl2—Mo2—Mo3—Cl4	−112.38 (4)	C2—C3—C4—C5	0.3 (9)
Cl1ⁱ—Mo2—Mo3—Cl4	70.60 (5)	C3—C4—C5—C6	0.4 (10)
Mo3ⁱ—Mo2—Mo3—Cl4	69.02 (3)	C2—C1—C6—C5	0.5 (7)
Mo1—Mo2—Mo3—Cl4	178.44 (3)	N1—C1—C6—C5	−179.9 (5)
Mo1ⁱ—Mo2—Mo3—Cl4	123.62 (4)	C4—C5—C6—C1	−0.8 (9)

Symmetry code: (i) −x+1, y, −z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N1—HN1···O1	0.89	1.96	2.810 (13)	160
N1—HN2···Cl6ⁱⁱ	0.89	2.34	3.229 (6)	174
N1—HN3···Cl5ⁱⁱⁱ	0.89	2.32	3.174 (6)	161
O1—HW1···Cl6^iv	0.90	2.56	3.321 (8)	143
O1—HW2···Cl7^v	0.90	2.32	3.165 (8)	155

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

Experimental details

Crystal data
Chemical formula	2C₆H₈N⁺·Mo₆Cl₁₄²⁻·2H₂O
M_r	1296.24
Crystal system, space group	Monoclinic, C2/c
Temperature (K)	293
a, b, c (Å)	20.665 (8), 11.335 (3), 17.347 (6)
β (°)	126.21 (5)
V (Å³)	3279 (3)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	3.38
Crystal size (mm)	0.3 × 0.2 × 0.1

Data collection
Diffractometer	Stoe IPDS diffractometer
Absorption correction	Numerical (X-SHAPE; Stoe & Cie, 1996)
T_min, T_max	0.463, 0.634
No. of measured, independent and observed [I > 2σ(I)] reflections	8558, 2368, 1908
R_int	0.049
θ_max (°)	23.9
(sin θ/λ)_max (Å⁻¹)	0.570

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.029, 0.062, 1.37
No. of reflections	2368
No. of parameters	170
No. of restraints	3
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.58, −0.57

Computer programs: IPDS Software (Stoe & Cie, 1997), IPDS Software, SHELXS97 (Sheldrick, 1997) and JANA2000 (Petricek & Dusek, 2000), SHELXL97 and JANA2000.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N1—HN1···O1	0.89	1.96	2.810 (13)	160
N1—HN2···Cl6ⁱ	0.89	2.34	3.229 (6)	174
N1—HN3···Cl5ⁱⁱ	0.89	2.32	3.174 (6)	161
O1—HW1···Cl6ⁱⁱⁱ	0.90	2.56	3.321 (8)	143
O1—HW2···Cl7^iv	0.90	2.32	3.165 (8)	155

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

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