The new heteropolyoxometalate compound (C₆H₈N)₅[HAs₂Mo₆O₂₆(H₂O)]·3H₂O: crystal structure and Hirshfeld surface analysis

A detailed description of the crystal structure and a Hirshfeld surface analysis of the new heteropolyoxometalate compound (C₆H₈N)₅[HAs₂Mo₆O₂₆(H₂O)]·3H₂O are reported. The title compound was synthesized using solution methods and its structure was characterized by single-crystal X-ray diffraction. The investigated compound contains a new [HAs₂Mo₆O₂₆(H₂O)]⁵⁻ polyanion and crystallizes in the monoclinic space group P2₁/c. The crystallographic analysis provided an understanding of the architecture and structural features of the complex crystal lattice and the Hirshfeld surface analysis shed more light on the inter­molecular inter­actions occurring in the crystal.

Computing details

Data collection: CrysAlis PRO (Rigaku OD, 2015); cell refinement: CrysAlis PRO (Rigaku OD, 2015); data reduction: CrysAlis PRO (Rigaku OD, 2015); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: OLEX2 (Dolomanov et al., 2009), DIAMOND (Brandenburg & Putz, 2005) and Mercury (Macrae et al., 2008); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009).

(I)

Crystal data

(C6H8N)5[HAs2Mo6O26(H2O)]·3H2O	F(000) = 3288
Mr = 1685.22	Dx = 2.243 Mg m^−3
Monoclinic, P21/c	Ag Kα radiation, λ = 0.56087 Å
a = 14.1301 (2) Å	Cell parameters from 13108 reflections
b = 15.4385 (2) Å	θ = 1.9–29.1°
c = 23.1563 (4) Å	µ = 6.29 mm^−1
β = 98.9698 (15)°	T = 100 K
V = 4989.72 (14) Å^3	Prism, light yellow
Z = 4	0.22 × 0.17 × 0.07 mm

Data collection

Rigaku SuperNova Eos diffractometer	24193 independent reflections
Radiation source: micro-focus sealed X-ray tube, SuperNova (Ag) X-ray Source	17848 reflections with I > 2σ(I)
Mirror monochromator	Rint = 0.037
Detector resolution: 16.0128 pixels mm^-1	θmax = 27.9°, θmin = 2.0°
ω scans	h = −23→14
Absorption correction: gaussian (CrysAlis PRO; Rigaku OD, 2015)	k = −25→20
Tmin = 0.460, Tmax = 1.000	l = −38→37
47915 measured reflections

Refinement

Refinement on F^2	7 restraints
Least-squares matrix: full	Hydrogen site location: mixed
R[F^2 > 2σ(F^2)] = 0.044	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.080	w = 1/[σ^2(Fo^2) + (0.022P)^2 + 5.4855P] where P = (Fo^2 + 2Fc^2)/3
S = 1.03	(Δ/σ)max = 0.003
24193 reflections	Δρmax = 2.71 e Å^−3
714 parameters	Δρmin = −1.77 e Å^−3

Special details

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. A good-quality single crystal of 1 was selected for diffraction experiment at 100 K. Diffraction data were collected on the Agilent Technologies SuperNova Single source diffractometer with Ag Kα radiation (λ = 0.56087 Å) using CrysAlis RED software (CrysAlis, 2008). The numerical absorption correction using a Gaussian integration over a multifaceted crystal model and empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm, was applied (CrysAlis, 2008).

The structural determination procedure was carried out using the SHELX package (Sheldrick, 2008). The structure was solved with direct methods and then successive least-square refinement was carried out based on the full-matrix least-squares method on F² using the SHELXL program (Sheldrick, 2008). The figures for this publication were prepared using Olex2, Diamond 3 and Mercury programs (Dolomanov et al., 2009; Brandenburg & Putz, 2005; Macrae et al., 2008). The molecular interactions in crystal were identified using PLATON (Spek, 2009).

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

	x	y	z	Uiso*/Ueq
Mo1	0.46052 (2)	0.43535 (2)	0.90587 (2)	0.00798 (4)
Mo2	0.59031 (2)	0.34986 (2)	0.78937 (2)	0.00845 (4)
Mo3	0.49430 (2)	0.36165 (2)	0.64936 (2)	0.00874 (4)
Mo4	0.25864 (2)	0.32363 (2)	0.62170 (2)	0.00821 (4)
Mo5	0.16350 (2)	0.26173 (2)	0.73644 (2)	0.00888 (4)
Mo6	0.23816 (2)	0.37357 (2)	0.87687 (2)	0.00830 (4)
As1	0.34908 (2)	0.43638 (2)	0.75026 (2)	0.00629 (5)
As2	0.40155 (2)	0.19749 (2)	0.73624 (2)	0.00781 (5)
O1	0.53726 (15)	0.38171 (13)	0.85631 (9)	0.0109 (4)
O1W	0.38938 (15)	0.29479 (13)	0.89024 (9)	0.0102 (4)
H1WA	0.394 (4)	0.259 (3)	0.918 (2)	0.051*
H1WB	0.406 (4)	0.272 (3)	0.859 (2)	0.051*
O2	0.58084 (15)	0.30579 (13)	0.70944 (9)	0.0112 (4)
O3	0.36757 (14)	0.40199 (12)	0.62702 (9)	0.0097 (4)
O4	0.18959 (15)	0.24133 (13)	0.65734 (9)	0.0117 (4)
O5	0.20994 (15)	0.29517 (13)	0.81537 (9)	0.0114 (4)
O6	0.33634 (15)	0.44171 (12)	0.92851 (8)	0.0098 (4)
O7	0.46053 (14)	0.41137 (12)	0.73800 (8)	0.0080 (3)
O8	0.27085 (14)	0.36262 (12)	0.71614 (9)	0.0092 (4)
O9	0.34516 (14)	0.43228 (12)	0.82315 (8)	0.0093 (4)
O10	0.47421 (15)	0.24444 (13)	0.79224 (9)	0.0113 (4)
O11	0.39476 (15)	0.25059 (12)	0.67230 (8)	0.0096 (4)
O12	0.29538 (15)	0.17668 (13)	0.75542 (9)	0.0118 (4)
O13	0.45896 (16)	0.09961 (13)	0.72919 (10)	0.0134 (4)
H13	0.427 (4)	0.059 (3)	0.720 (2)	0.056*
O14	0.31694 (15)	0.53532 (12)	0.72493 (9)	0.0101 (4)
O15	0.52436 (16)	0.40780 (13)	0.97150 (9)	0.0141 (4)
O16	0.48933 (15)	0.54269 (13)	0.89678 (9)	0.0118 (4)
O17	0.67562 (16)	0.27736 (14)	0.81788 (9)	0.0147 (4)
O18	0.65200 (16)	0.44449 (14)	0.78179 (10)	0.0151 (4)
O19	0.51255 (16)	0.29835 (13)	0.59181 (9)	0.0138 (4)
O20	0.55584 (15)	0.45710 (13)	0.64145 (9)	0.0126 (4)
O21	0.27579 (16)	0.26952 (13)	0.55889 (9)	0.0125 (4)
O22	0.17076 (15)	0.39777 (13)	0.59915 (9)	0.0137 (4)
O23	0.09920 (16)	0.16990 (14)	0.74488 (9)	0.0146 (4)
O24	0.07784 (15)	0.33936 (14)	0.72010 (10)	0.0152 (4)
O25	0.20632 (16)	0.31536 (14)	0.93326 (10)	0.0158 (4)
O26	0.14963 (16)	0.44861 (14)	0.86073 (10)	0.0151 (4)
O2W	0.40475 (18)	0.19056 (16)	0.97818 (10)	0.0184 (5)
H2WA	0.451 (3)	0.193 (3)	1.0064 (17)	0.056*
H2WB	0.358 (3)	0.199 (3)	0.997 (2)	0.056*
O3W	0.01755 (18)	0.52286 (15)	0.77340 (11)	0.0183 (5)
H3WA	0.056 (4)	0.511 (3)	0.803 (2)	0.056*
H3WB	−0.004 (4)	0.5717 (19)	0.782 (2)	0.056*
O4W	0.8612 (2)	0.4095 (2)	0.77036 (13)	0.0340 (7)
H4WA	0.9161 (18)	0.436 (3)	0.772 (2)	0.051*
H4WB	0.832 (3)	0.407 (3)	0.8034 (14)	0.051*
N1A	0.32753 (19)	0.09688 (16)	0.54219 (11)	0.0116 (4)
H1AA	0.383 (3)	0.081 (3)	0.563 (2)	0.045*
H1AB	0.338 (3)	0.088 (3)	0.5061 (11)	0.045*
H1AC	0.324 (3)	0.1522 (13)	0.547 (2)	0.045*
C1A	0.2453 (2)	0.04776 (19)	0.55697 (13)	0.0129 (5)
C2A	0.1588 (3)	0.0884 (2)	0.55512 (19)	0.0260 (8)
H2A	0.1521	0.1467	0.5451	0.031*
C3A	0.0811 (3)	0.0416 (2)	0.5685 (2)	0.0336 (10)
H3A	0.0222	0.0688	0.5676	0.040*
C4A	0.0906 (3)	−0.0448 (3)	0.58299 (17)	0.0294 (8)
H4A	0.0387	−0.0756	0.5926	0.035*
C5A	0.1782 (3)	−0.0857 (3)	0.5832 (2)	0.0373 (11)
H5A	0.1846	−0.1443	0.5924	0.045*
C6A	0.2565 (3)	−0.0395 (2)	0.56976 (19)	0.0298 (9)
H6A	0.3151	−0.0667	0.5694	0.036*
N1B	0.2494 (2)	0.02014 (18)	0.80618 (14)	0.0236 (6)
H1BA	0.3009	−0.0126	0.8172	0.028*
H1BB	0.2676	0.0725	0.7961	0.028*
H1BC	0.2129	−0.0043	0.7757	0.028*
C1B	0.1949 (3)	0.0281 (2)	0.85451 (15)	0.0188 (6)
C2B	0.1324 (2)	−0.0378 (2)	0.86481 (15)	0.0192 (6)
H2B	0.1205	−0.0843	0.8391	0.023*
C3B	0.0888 (2)	−0.0327 (2)	0.91368 (15)	0.0192 (6)
H3B	0.0462	−0.0757	0.9211	0.023*
C4B	0.1079 (2)	0.0363 (2)	0.95201 (14)	0.0203 (7)
H4B	0.0802	0.0381	0.9859	0.024*
C5B	0.1682 (2)	0.1028 (2)	0.94003 (16)	0.0208 (7)
H5B	0.1792	0.1499	0.9653	0.025*
C6B	0.2116 (2)	0.0991 (2)	0.89110 (16)	0.0206 (7)
H6B	0.2516	0.1436	0.8826	0.025*
N1C	0.5731 (2)	0.10115 (17)	0.85860 (11)	0.0123 (5)
H1CA	0.617 (4)	0.077 (3)	0.837 (2)	0.045*
H1CB	0.530 (4)	0.063 (3)	0.858 (2)	0.045*
H1CC	0.544 (3)	0.146 (3)	0.836 (2)	0.045*
C1C	0.6097 (2)	0.12234 (18)	0.92012 (12)	0.0109 (5)
C2C	0.6240 (2)	0.20819 (19)	0.93577 (13)	0.0141 (6)
H2C	0.6102	0.2521	0.9082	0.017*
C3C	0.6593 (2)	0.2274 (2)	0.99372 (14)	0.0164 (6)
H3C	0.6686	0.2850	1.0050	0.020*
C4C	0.6809 (2)	0.1628 (2)	1.03491 (13)	0.0145 (6)
H4C	0.7066	0.1764	1.0733	0.017*
C5C	0.6638 (2)	0.0772 (2)	1.01823 (14)	0.0185 (6)
H5C	0.6761	0.0333	1.0459	0.022*
C6C	0.6285 (2)	0.05650 (19)	0.96057 (13)	0.0166 (6)
H6C	0.6176	−0.0009	0.9494	0.020*
N1D	0.12574 (19)	0.52960 (16)	0.67883 (11)	0.0137 (5)
H1DA	0.1197	0.4800	0.6591	0.016*
H1DB	0.0873	0.5290	0.7058	0.016*
H1DC	0.1862	0.5359	0.6961	0.016*
C1D	0.0995 (2)	0.60201 (19)	0.63842 (13)	0.0129 (5)
C2D	0.1344 (2)	0.6036 (2)	0.58568 (15)	0.0186 (6)
H2D	0.1762	0.5609	0.5767	0.022*
C3D	0.1058 (3)	0.6702 (2)	0.54647 (15)	0.0222 (7)
H3D	0.1284	0.6722	0.5109	0.027*
C4D	0.0438 (3)	0.7335 (2)	0.56023 (16)	0.0237 (7)
H4D	0.0234	0.7770	0.5334	0.028*
C5D	0.0120 (3)	0.7324 (2)	0.61380 (16)	0.0212 (7)
H5D	−0.0282	0.7761	0.6232	0.025*
C6D	0.0396 (2)	0.66654 (19)	0.65362 (14)	0.0151 (6)
H6D	0.0185	0.6657	0.6897	0.018*
N1E	0.35884 (19)	0.64701 (16)	0.81868 (12)	0.0109 (4)
H1EA	0.351 (3)	0.618 (3)	0.787 (2)	0.045*
H1EB	0.403 (3)	0.624 (3)	0.849 (2)	0.045*
H1EC	0.383 (3)	0.695 (3)	0.809 (2)	0.045*
C1E	0.2670 (2)	0.66505 (18)	0.83821 (13)	0.0109 (5)
C2E	0.2009 (2)	0.71497 (19)	0.80198 (14)	0.0153 (6)
H2E	0.2148	0.7360	0.7666	0.018*
C3E	0.1137 (2)	0.7328 (2)	0.81975 (16)	0.0192 (6)
H3E	0.0682	0.7657	0.7959	0.023*
C4E	0.0937 (2)	0.7020 (2)	0.87280 (15)	0.0190 (6)
H4E	0.0353	0.7149	0.8847	0.023*
C5E	0.1606 (2)	0.6520 (2)	0.90804 (14)	0.0172 (6)
H5E	0.1467	0.6310	0.9434	0.021*
C6E	0.2485 (2)	0.63290 (19)	0.89100 (13)	0.0142 (5)
H6E	0.2936	0.5993	0.9146	0.017*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Mo1	0.00897 (10)	0.00774 (9)	0.00689 (9)	−0.00051 (8)	0.00017 (7)	−0.00024 (7)
Mo2	0.00748 (9)	0.00854 (9)	0.00935 (10)	0.00073 (7)	0.00140 (7)	0.00167 (8)
Mo3	0.00951 (10)	0.00882 (9)	0.00847 (9)	0.00101 (8)	0.00318 (8)	0.00182 (8)
Mo4	0.01006 (10)	0.00772 (9)	0.00686 (9)	−0.00051 (8)	0.00141 (7)	−0.00080 (7)
Mo5	0.00843 (10)	0.00991 (9)	0.00848 (10)	−0.00301 (8)	0.00191 (7)	−0.00182 (8)
Mo6	0.00895 (10)	0.00890 (9)	0.00711 (9)	−0.00096 (8)	0.00141 (7)	−0.00058 (7)
As1	0.00710 (11)	0.00564 (11)	0.00605 (11)	−0.00023 (9)	0.00074 (9)	0.00006 (9)
As2	0.01015 (12)	0.00577 (11)	0.00784 (12)	0.00039 (9)	0.00247 (9)	0.00067 (9)
O1	0.0106 (9)	0.0104 (9)	0.0116 (9)	0.0000 (7)	0.0013 (7)	0.0005 (7)
O1W	0.0136 (10)	0.0083 (9)	0.0087 (9)	0.0003 (7)	0.0018 (7)	0.0007 (7)
O2	0.0114 (9)	0.0124 (9)	0.0102 (9)	0.0044 (8)	0.0030 (7)	0.0018 (7)
O3	0.0117 (9)	0.0077 (8)	0.0099 (9)	−0.0006 (7)	0.0023 (7)	0.0026 (7)
O4	0.0164 (10)	0.0100 (9)	0.0089 (9)	−0.0036 (8)	0.0024 (8)	−0.0020 (7)
O5	0.0136 (10)	0.0123 (9)	0.0084 (9)	−0.0036 (8)	0.0017 (7)	−0.0019 (7)
O6	0.0119 (9)	0.0099 (9)	0.0076 (9)	−0.0006 (7)	0.0019 (7)	−0.0008 (7)
O7	0.0065 (8)	0.0087 (8)	0.0090 (9)	0.0010 (7)	0.0022 (7)	0.0000 (7)
O8	0.0098 (9)	0.0098 (9)	0.0080 (9)	−0.0020 (7)	0.0009 (7)	−0.0008 (7)
O9	0.0100 (9)	0.0108 (9)	0.0064 (8)	−0.0005 (7)	−0.0009 (7)	0.0003 (7)
O10	0.0166 (10)	0.0095 (9)	0.0074 (9)	−0.0023 (8)	0.0009 (7)	0.0006 (7)
O11	0.0130 (10)	0.0082 (8)	0.0081 (9)	0.0010 (7)	0.0031 (7)	0.0019 (7)
O12	0.0105 (9)	0.0107 (9)	0.0152 (10)	−0.0001 (7)	0.0052 (8)	0.0025 (8)
O13	0.0127 (10)	0.0079 (9)	0.0199 (11)	0.0024 (8)	0.0034 (8)	0.0008 (8)
O14	0.0120 (10)	0.0062 (8)	0.0119 (9)	0.0007 (7)	0.0007 (7)	0.0003 (7)
O15	0.0160 (10)	0.0152 (10)	0.0100 (10)	0.0028 (8)	−0.0016 (8)	−0.0008 (8)
O16	0.0142 (10)	0.0087 (9)	0.0123 (10)	−0.0014 (7)	0.0017 (8)	−0.0005 (7)
O17	0.0144 (10)	0.0175 (10)	0.0123 (10)	0.0057 (8)	0.0025 (8)	0.0033 (8)
O18	0.0124 (10)	0.0152 (10)	0.0170 (11)	−0.0038 (8)	0.0000 (8)	0.0031 (8)
O19	0.0159 (11)	0.0130 (9)	0.0136 (10)	0.0013 (8)	0.0056 (8)	0.0012 (8)
O20	0.0120 (10)	0.0122 (9)	0.0142 (10)	0.0003 (8)	0.0038 (8)	0.0036 (8)
O21	0.0176 (11)	0.0115 (9)	0.0090 (9)	−0.0011 (8)	0.0040 (8)	−0.0009 (7)
O22	0.0135 (10)	0.0141 (10)	0.0130 (10)	0.0005 (8)	0.0004 (8)	−0.0003 (8)
O23	0.0157 (11)	0.0153 (10)	0.0134 (10)	−0.0058 (8)	0.0042 (8)	−0.0020 (8)
O24	0.0106 (10)	0.0186 (10)	0.0162 (11)	−0.0015 (8)	0.0014 (8)	−0.0043 (8)
O25	0.0178 (11)	0.0171 (10)	0.0128 (10)	−0.0057 (9)	0.0035 (8)	−0.0001 (8)
O26	0.0136 (10)	0.0150 (10)	0.0165 (11)	0.0022 (8)	0.0015 (8)	−0.0020 (8)
O2W	0.0189 (12)	0.0246 (12)	0.0122 (11)	0.0023 (10)	0.0041 (9)	0.0051 (9)
O3W	0.0209 (12)	0.0142 (10)	0.0193 (12)	0.0046 (9)	0.0010 (9)	0.0003 (9)
O4W	0.0333 (17)	0.0420 (17)	0.0279 (15)	−0.0015 (13)	0.0083 (13)	0.0024 (13)
N1A	0.0125 (11)	0.0113 (11)	0.0110 (11)	0.0020 (9)	0.0021 (9)	0.0009 (9)
C1A	0.0124 (13)	0.0141 (13)	0.0116 (13)	−0.0033 (10)	−0.0002 (10)	0.0012 (10)
C2A	0.0195 (17)	0.0126 (14)	0.049 (2)	−0.0004 (12)	0.0135 (16)	−0.0048 (15)
C3A	0.0217 (19)	0.0227 (17)	0.060 (3)	−0.0024 (15)	0.0189 (19)	−0.0123 (18)
C4A	0.0248 (19)	0.035 (2)	0.029 (2)	−0.0117 (16)	0.0055 (15)	0.0035 (16)
C5A	0.026 (2)	0.028 (2)	0.054 (3)	−0.0064 (16)	−0.0061 (19)	0.0235 (19)
C6A	0.0175 (17)	0.0228 (17)	0.046 (2)	0.0010 (14)	−0.0038 (16)	0.0154 (16)
N1B	0.0320 (17)	0.0160 (13)	0.0261 (16)	−0.0009 (12)	0.0149 (13)	0.0012 (11)
C1B	0.0238 (17)	0.0124 (13)	0.0237 (17)	0.0026 (12)	0.0143 (13)	0.0038 (12)
C2B	0.0239 (17)	0.0132 (13)	0.0227 (16)	0.0000 (12)	0.0103 (13)	0.0024 (12)
C3B	0.0179 (15)	0.0208 (15)	0.0197 (16)	−0.0019 (12)	0.0051 (12)	0.0063 (12)
C4B	0.0204 (16)	0.0272 (17)	0.0124 (14)	−0.0005 (13)	−0.0006 (12)	0.0064 (12)
C5B	0.0183 (16)	0.0183 (15)	0.0240 (17)	0.0014 (12)	−0.0026 (13)	0.0018 (13)
C6B	0.0198 (16)	0.0128 (14)	0.0305 (19)	0.0018 (12)	0.0078 (14)	0.0054 (13)
N1C	0.0164 (12)	0.0117 (11)	0.0083 (11)	0.0020 (9)	0.0000 (9)	−0.0009 (9)
C1C	0.0130 (13)	0.0113 (12)	0.0081 (12)	0.0031 (10)	0.0007 (10)	−0.0005 (10)
C2C	0.0185 (15)	0.0131 (13)	0.0102 (13)	0.0000 (11)	0.0002 (11)	0.0009 (10)
C3C	0.0198 (15)	0.0148 (13)	0.0144 (14)	0.0009 (11)	0.0017 (12)	−0.0035 (11)
C4C	0.0152 (14)	0.0205 (14)	0.0073 (12)	0.0038 (11)	−0.0003 (10)	−0.0017 (11)
C5C	0.0258 (17)	0.0162 (14)	0.0129 (14)	0.0083 (12)	0.0013 (12)	0.0004 (11)
C6C	0.0283 (17)	0.0104 (12)	0.0107 (13)	0.0037 (12)	0.0014 (12)	0.0001 (10)
N1D	0.0126 (12)	0.0125 (11)	0.0152 (12)	0.0030 (9)	−0.0003 (9)	−0.0016 (9)
C1D	0.0101 (12)	0.0147 (13)	0.0135 (13)	0.0002 (10)	0.0002 (10)	0.0005 (10)
C2D	0.0183 (15)	0.0194 (15)	0.0198 (16)	−0.0011 (12)	0.0081 (12)	−0.0039 (12)
C3D	0.0266 (18)	0.0235 (16)	0.0175 (16)	−0.0066 (14)	0.0067 (13)	−0.0011 (13)
C4D	0.0257 (18)	0.0204 (16)	0.0238 (18)	−0.0014 (14)	0.0002 (14)	0.0067 (14)
C5D	0.0205 (16)	0.0167 (14)	0.0266 (18)	0.0051 (12)	0.0046 (13)	0.0011 (13)
C6D	0.0125 (13)	0.0165 (13)	0.0166 (14)	0.0037 (11)	0.0032 (11)	0.0003 (11)
N1E	0.0113 (11)	0.0087 (10)	0.0128 (11)	0.0004 (9)	0.0023 (9)	−0.0019 (9)
C1E	0.0106 (12)	0.0093 (11)	0.0122 (12)	−0.0020 (9)	0.0000 (10)	−0.0023 (10)
C2E	0.0150 (14)	0.0143 (13)	0.0165 (14)	−0.0004 (11)	0.0018 (11)	0.0020 (11)
C3E	0.0103 (13)	0.0162 (14)	0.0299 (18)	0.0005 (11)	−0.0001 (12)	−0.0007 (13)
C4E	0.0128 (14)	0.0185 (14)	0.0266 (17)	−0.0016 (12)	0.0059 (12)	−0.0062 (13)
C5E	0.0184 (15)	0.0173 (14)	0.0174 (15)	−0.0026 (12)	0.0076 (12)	−0.0018 (12)
C6E	0.0162 (14)	0.0105 (12)	0.0149 (14)	−0.0010 (10)	−0.0001 (11)	−0.0007 (10)

Geometric parameters (Å, º)

Mo1—O1	1.889 (2)	C4A—C5A	1.389 (6)
Mo1—O1W	2.395 (2)	C5A—H5A	0.9300
Mo1—O6	1.910 (2)	C5A—C6A	1.392 (5)
Mo1—O9	2.3140 (19)	C6A—H6A	0.9300
Mo1—O15	1.696 (2)	N1B—H1BA	0.8900
Mo1—O16	1.727 (2)	N1B—H1BB	0.8900
Mo2—O1	1.889 (2)	N1B—H1BC	0.8900
Mo2—O2	1.957 (2)	C1B—N1B	1.459 (4)
Mo2—O7	2.2358 (19)	C1B—C2B	1.392 (5)
Mo2—O10	2.319 (2)	C1B—C6B	1.383 (5)
Mo2—O17	1.701 (2)	C2B—H2B	0.9300
Mo2—O18	1.724 (2)	C2B—C3B	1.373 (5)
Mo3—O2	1.909 (2)	C3B—H3B	0.9300
Mo3—O3	1.890 (2)	C3B—C4B	1.386 (5)
Mo3—O7	2.3099 (19)	C4B—H4B	0.9300
Mo3—O11	2.331 (2)	C4B—C5B	1.390 (5)
Mo3—O19	1.704 (2)	C5B—H5B	0.9300
Mo3—O20	1.735 (2)	C5B—C6B	1.370 (5)
Mo4—O3	1.946 (2)	C6B—H6B	0.9300
Mo4—O4	1.870 (2)	N1C—H1CA	0.93 (5)
Mo4—O8	2.249 (2)	N1C—H1CB	0.85 (5)
Mo4—O11	2.375 (2)	N1C—H1CC	0.92 (5)
Mo4—O21	1.727 (2)	C1C—N1C	1.474 (4)
Mo4—O22	1.709 (2)	C1C—C2C	1.381 (4)
Mo5—O4	1.950 (2)	C1C—C6C	1.380 (4)
Mo5—O5	1.914 (2)	C2C—H2C	0.9300
Mo5—O8	2.274 (2)	C2C—C3C	1.389 (4)
Mo5—O12	2.266 (2)	C3C—H3C	0.9300
Mo5—O23	1.711 (2)	C3C—C4C	1.381 (4)
Mo5—O24	1.703 (2)	C4C—H4C	0.9300
Mo6—O1W	2.436 (2)	C4C—C5C	1.387 (4)
Mo6—O5	1.864 (2)	C5C—H5C	0.9300
Mo6—O6	1.986 (2)	C5C—C6C	1.388 (4)
Mo6—O9	2.289 (2)	C6C—H6C	0.9300
Mo6—O25	1.702 (2)	N1D—H1DA	0.8900
Mo6—O26	1.703 (2)	N1D—H1DB	0.8900
As1—O7	1.6880 (19)	N1D—H1DC	0.8900
As1—O8	1.6943 (19)	C1D—N1D	1.468 (4)
As1—O9	1.698 (2)	C1D—C2D	1.387 (4)
As1—O14	1.6734 (19)	C1D—C6D	1.387 (4)
As2—O10	1.687 (2)	C2D—H2D	0.9300
As2—O11	1.6819 (19)	C2D—C3D	1.390 (5)
As2—O12	1.661 (2)	C3D—H3D	0.9300
As2—O13	1.735 (2)	C3D—C4D	1.382 (5)
O1W—H1WA	0.85 (5)	C4D—H4D	0.9300
O1W—H1WB	0.86 (5)	C4D—C5D	1.383 (5)
O13—H13	0.79 (5)	C5D—H5D	0.9300
O2W—H2WA	0.853 (19)	C5D—C6D	1.387 (4)
O2W—H2WB	0.850 (19)	C6D—H6D	0.9300
O3W—H3WA	0.82 (5)	N1E—H1EA	0.84 (5)
O3W—H3WB	0.849 (19)	N1E—H1EB	0.94 (5)
O4W—H4WA	0.875 (10)	N1E—H1EC	0.86 (5)
O4W—H4WB	0.926 (19)	C1E—N1E	1.466 (4)
N1A—H1AA	0.89 (5)	C1E—C2E	1.388 (4)
N1A—H1AB	0.879 (19)	C1E—C6E	1.382 (4)
N1A—H1AC	0.865 (19)	C2E—H2E	0.9300
C1A—N1A	1.472 (4)	C2E—C3E	1.386 (5)
C1A—C2A	1.369 (5)	C3E—H3E	0.9300
C1A—C6A	1.383 (4)	C3E—C4E	1.387 (5)
C2A—H2A	0.9300	C4E—H4E	0.9300
C2A—C3A	1.388 (5)	C4E—C5E	1.384 (5)
C3A—H3A	0.9300	C5E—H5E	0.9300
C3A—C4A	1.377 (5)	C5E—C6E	1.392 (4)
C4A—H4A	0.9300	C6E—H6E	0.9300
O1—Mo1—O1W	77.18 (8)	As2—O11—Mo4	126.61 (11)
O1—Mo1—O6	145.91 (9)	As2—O12—Mo5	125.86 (11)
O1—Mo1—O9	83.40 (8)	As2—O13—H13	118 (4)
O6—Mo1—O1W	72.92 (8)	H2WA—O2W—H2WB	100 (5)
O6—Mo1—O9	70.71 (8)	H3WA—O3W—H3WB	102 (5)
O9—Mo1—O1W	68.37 (7)	H4WA—O4W—H4WB	119 (4)
O15—Mo1—O1	99.15 (10)	H1AA—N1A—H1AB	103 (4)
O15—Mo1—O1W	93.46 (9)	H1AA—N1A—H1AC	105 (4)
O15—Mo1—O6	98.63 (10)	H1AB—N1A—H1AC	107 (4)
O15—Mo1—O9	160.76 (9)	C1A—N1A—H1AA	113 (3)
O15—Mo1—O16	104.31 (10)	C1A—N1A—H1AB	113 (3)
O16—Mo1—O1	100.25 (9)	C1A—N1A—H1AC	115 (3)
O16—Mo1—O1W	162.21 (9)	C2A—C1A—N1A	119.3 (3)
O16—Mo1—O6	103.19 (9)	C2A—C1A—C6A	121.7 (3)
O16—Mo1—O9	93.89 (8)	C6A—C1A—N1A	118.9 (3)
O1—Mo2—O2	152.78 (9)	C1A—C2A—H2A	120.4
O1—Mo2—O7	85.90 (8)	C1A—C2A—C3A	119.1 (3)
O1—Mo2—O10	77.66 (8)	C3A—C2A—H2A	120.4
O2—Mo2—O7	73.44 (8)	C2A—C3A—H3A	119.7
O2—Mo2—O10	80.72 (8)	C4A—C3A—C2A	120.6 (4)
O7—Mo2—O10	77.77 (7)	C4A—C3A—H3A	119.7
O17—Mo2—O1	101.57 (10)	C3A—C4A—H4A	120.2
O17—Mo2—O2	94.48 (9)	C3A—C4A—C5A	119.6 (4)
O17—Mo2—O7	163.48 (9)	C5A—C4A—H4A	120.2
O17—Mo2—O10	89.35 (9)	C4A—C5A—H5A	119.8
O17—Mo2—O18	104.96 (11)	C4A—C5A—C6A	120.3 (4)
O18—Mo2—O1	97.73 (10)	C6A—C5A—H5A	119.8
O18—Mo2—O2	99.18 (10)	C1A—C6A—C5A	118.6 (4)
O18—Mo2—O7	88.38 (9)	C1A—C6A—H6A	120.7
O18—Mo2—O10	165.62 (9)	C5A—C6A—H6A	120.7
O2—Mo3—O7	72.54 (8)	H1BA—N1B—H1BB	109.5
O2—Mo3—O11	80.93 (8)	H1BA—N1B—H1BC	109.5
O3—Mo3—O2	145.09 (9)	H1BB—N1B—H1BC	109.5
O3—Mo3—O7	79.37 (8)	C1B—N1B—H1BA	109.5
O3—Mo3—O11	74.05 (8)	C1B—N1B—H1BB	109.5
O7—Mo3—O11	79.99 (7)	C1B—N1B—H1BC	109.5
O19—Mo3—O2	98.80 (9)	C2B—C1B—N1B	119.6 (3)
O19—Mo3—O3	103.14 (10)	C6B—C1B—N1B	118.5 (3)
O19—Mo3—O7	164.32 (8)	C6B—C1B—C2B	121.8 (3)
O19—Mo3—O11	85.80 (9)	C1B—C2B—H2B	120.7
O19—Mo3—O20	105.37 (10)	C3B—C2B—C1B	118.5 (3)
O20—Mo3—O2	100.71 (9)	C3B—C2B—H2B	120.7
O20—Mo3—O3	99.23 (9)	C2B—C3B—H3B	119.9
O20—Mo3—O7	89.31 (9)	C2B—C3B—C4B	120.3 (3)
O20—Mo3—O11	168.20 (9)	C4B—C3B—H3B	119.9
O3—Mo4—O8	80.33 (8)	C3B—C4B—H4B	119.9
O3—Mo4—O11	72.08 (7)	C3B—C4B—C5B	120.3 (3)
O4—Mo4—O3	148.87 (9)	C5B—C4B—H4B	119.9
O4—Mo4—O8	73.68 (8)	C4B—C5B—H5B	120.0
O4—Mo4—O11	84.13 (8)	C6B—C5B—C4B	120.0 (3)
O8—Mo4—O11	73.37 (7)	C6B—C5B—H5B	120.0
O21—Mo4—O3	98.08 (9)	C1B—C6B—H6B	120.5
O21—Mo4—O4	101.20 (9)	C5B—C6B—C1B	119.0 (3)
O21—Mo4—O8	161.63 (9)	C5B—C6B—H6B	120.5
O21—Mo4—O11	88.67 (9)	H1CA—N1C—H1CB	105 (4)
O22—Mo4—O3	97.63 (9)	H1CA—N1C—H1CC	106 (4)
O22—Mo4—O4	100.70 (10)	H1CB—N1C—H1CC	105 (4)
O22—Mo4—O8	93.43 (9)	C1C—N1C—H1CA	117 (3)
O22—Mo4—O11	164.23 (9)	C1C—N1C—H1CB	108 (3)
O22—Mo4—O21	104.91 (10)	C1C—N1C—H1CC	116 (3)
O4—Mo5—O8	71.73 (8)	C2C—C1C—N1C	118.8 (3)
O4—Mo5—O12	79.53 (8)	C6C—C1C—N1C	119.6 (3)
O5—Mo5—O4	148.63 (9)	C6C—C1C—C2C	121.6 (3)
O5—Mo5—O8	82.66 (8)	C1C—C2C—H2C	120.8
O5—Mo5—O12	79.74 (8)	C1C—C2C—C3C	118.3 (3)
O12—Mo5—O8	83.23 (7)	C3C—C2C—H2C	120.8
O23—Mo5—O4	98.91 (9)	C2C—C3C—H3C	119.3
O23—Mo5—O5	102.92 (10)	C4C—C3C—C2C	121.4 (3)
O23—Mo5—O8	166.95 (9)	C4C—C3C—H3C	119.3
O23—Mo5—O12	86.16 (9)	C3C—C4C—H4C	120.5
O24—Mo5—O4	97.86 (10)	C3C—C4C—C5C	119.1 (3)
O24—Mo5—O5	98.53 (10)	C5C—C4C—H4C	120.5
O24—Mo5—O8	86.90 (9)	C4C—C5C—H5C	119.7
O24—Mo5—O12	170.11 (9)	C4C—C5C—C6C	120.5 (3)
O24—Mo5—O23	103.70 (11)	C6C—C5C—H5C	119.7
O5—Mo6—O1W	81.47 (8)	C1C—C6C—C5C	119.1 (3)
O5—Mo6—O6	148.22 (9)	C1C—C6C—H6C	120.5
O5—Mo6—O9	85.56 (8)	C5C—C6C—H6C	120.5
O6—Mo6—O1W	70.82 (8)	H1DA—N1D—H1DB	109.5
O6—Mo6—O9	70.06 (8)	H1DA—N1D—H1DC	109.5
O9—Mo6—O1W	68.05 (7)	H1DB—N1D—H1DC	109.5
O25—Mo6—O1W	88.31 (9)	C1D—N1D—H1DA	109.5
O25—Mo6—O5	101.10 (10)	C1D—N1D—H1DB	109.5
O25—Mo6—O6	93.51 (9)	C1D—N1D—H1DC	109.5
O25—Mo6—O9	154.37 (9)	C2D—C1D—N1D	119.0 (3)
O25—Mo6—O26	104.75 (11)	C6D—C1D—N1D	119.3 (3)
O26—Mo6—O1W	165.27 (9)	C6D—C1D—C2D	121.7 (3)
O26—Mo6—O5	102.22 (10)	C1D—C2D—H2D	120.6
O26—Mo6—O6	101.07 (9)	C1D—C2D—C3D	118.7 (3)
O26—Mo6—O9	97.82 (9)	C3D—C2D—H2D	120.6
O7—As1—O8	109.01 (10)	C2D—C3D—H3D	119.9
O7—As1—O9	109.54 (10)	C4D—C3D—C2D	120.2 (3)
O8—As1—O9	108.57 (10)	C4D—C3D—H3D	119.9
O14—As1—O7	111.05 (10)	C3D—C4D—H4D	119.9
O14—As1—O8	109.17 (10)	C3D—C4D—C5D	120.2 (3)
O14—As1—O9	109.47 (10)	C5D—C4D—H4D	119.9
O10—As2—O13	102.07 (10)	C4D—C5D—H5D	119.7
O11—As2—O10	114.30 (10)	C4D—C5D—C6D	120.6 (3)
O11—As2—O13	107.76 (10)	C6D—C5D—H5D	119.7
O12—As2—O10	110.14 (10)	C1D—C6D—C5D	118.5 (3)
O12—As2—O11	113.56 (10)	C1D—C6D—H6D	120.8
O12—As2—O13	108.16 (10)	C5D—C6D—H6D	120.8
Mo1—O1—Mo2	162.11 (12)	H1EA—N1E—H1EB	116 (4)
Mo1—O1W—Mo6	84.60 (6)	H1EA—N1E—H1EC	104 (4)
Mo1—O1W—H1WA	120 (3)	H1EB—N1E—H1EC	106 (4)
Mo1—O1W—H1WB	110 (3)	C1E—N1E—H1EA	111 (3)
Mo6—O1W—H1WA	112 (3)	C1E—N1E—H1EB	111 (3)
Mo6—O1W—H1WB	116 (3)	C1E—N1E—H1EC	109 (3)
H1WA—O1W—H1WB	112 (4)	C2E—C1E—N1E	117.6 (3)
Mo3—O2—Mo2	118.28 (10)	C6E—C1E—N1E	120.2 (3)
Mo3—O3—Mo4	121.24 (10)	C6E—C1E—C2E	122.1 (3)
Mo4—O4—Mo5	119.53 (10)	C1E—C2E—H2E	120.8
Mo6—O5—Mo5	154.86 (12)	C3E—C2E—C1E	118.5 (3)
Mo1—O6—Mo6	113.13 (10)	C3E—C2E—H2E	120.8
Mo2—O7—Mo3	93.77 (7)	C2E—C3E—H3E	119.7
As1—O7—Mo2	135.81 (11)	C2E—C3E—C4E	120.6 (3)
As1—O7—Mo3	123.56 (10)	C4E—C3E—H3E	119.7
Mo4—O8—Mo5	93.74 (7)	C3E—C4E—H4E	120.1
As1—O8—Mo4	125.38 (11)	C5E—C4E—C3E	119.9 (3)
As1—O8—Mo5	140.51 (11)	C5E—C4E—H4E	120.1
Mo6—O9—Mo1	89.88 (7)	C4E—C5E—H5E	119.7
As1—O9—Mo1	133.94 (11)	C4E—C5E—C6E	120.6 (3)
As1—O9—Mo6	132.95 (10)	C6E—C5E—H5E	119.7
As2—O10—Mo2	128.90 (11)	C1E—C6E—C5E	118.4 (3)
Mo3—O11—Mo4	90.53 (7)	C1E—C6E—H6E	120.8
As2—O11—Mo3	127.27 (11)	C5E—C6E—H6E	120.8
O1W—Mo1—O1—Mo2	102.0 (4)	O18—Mo2—O1—Mo1	72.7 (4)
O1W—Mo6—O5—Mo5	−132.6 (3)	O19—Mo3—O3—Mo4	68.20 (13)
O2—Mo2—O1—Mo1	−55.3 (5)	O20—Mo3—O3—Mo4	176.48 (12)
O2—Mo3—O3—Mo4	−59.3 (2)	O21—Mo4—O4—Mo5	172.21 (12)
O3—Mo4—O4—Mo5	45.0 (2)	O22—Mo4—O4—Mo5	−80.07 (13)
O6—Mo1—O1—Mo2	72.9 (4)	O25—Mo6—O5—Mo5	140.9 (3)
O6—Mo6—O5—Mo5	−103.3 (3)	O26—Mo6—O5—Mo5	32.9 (3)
O7—Mo2—O1—Mo1	−15.1 (4)	N1A—C1A—C2A—C3A	179.3 (3)
O7—Mo3—O3—Mo4	−95.98 (12)	N1A—C1A—C6A—C5A	−179.5 (4)
O7—As1—O8—Mo4	−51.37 (14)	C1A—C2A—C3A—C4A	−0.4 (7)
O7—As1—O8—Mo5	119.56 (16)	C2A—C1A—C6A—C5A	−2.5 (6)
O7—As1—O9—Mo1	18.54 (17)	C2A—C3A—C4A—C5A	−1.2 (7)
O7—As1—O9—Mo6	−134.73 (13)	C3A—C4A—C5A—C6A	1.0 (7)
O8—Mo4—O4—Mo5	10.39 (11)	C4A—C5A—C6A—C1A	0.8 (7)
O8—As1—O7—Mo2	−103.20 (15)	C6A—C1A—C2A—C3A	2.3 (6)
O8—As1—O7—Mo3	39.52 (14)	N1B—C1B—C2B—C3B	174.0 (3)
O8—As1—O9—Mo1	137.47 (13)	N1B—C1B—C6B—C5B	−173.4 (3)
O8—As1—O9—Mo6	−15.80 (17)	C1B—C2B—C3B—C4B	−0.8 (5)
O9—Mo1—O1—Mo2	32.7 (4)	C2B—C1B—C6B—C5B	2.6 (5)
O9—Mo6—O5—Mo5	−64.1 (3)	C2B—C3B—C4B—C5B	2.8 (5)
O9—As1—O7—Mo2	15.46 (17)	C3B—C4B—C5B—C6B	−2.1 (5)
O9—As1—O7—Mo3	158.18 (10)	C4B—C5B—C6B—C1B	−0.6 (5)
O9—As1—O8—Mo4	−170.63 (11)	C6B—C1B—C2B—C3B	−1.9 (5)
O9—As1—O8—Mo5	0.30 (19)	N1C—C1C—C2C—C3C	−179.4 (3)
O10—Mo2—O1—Mo1	−93.4 (4)	N1C—C1C—C6C—C5C	179.4 (3)
O10—As2—O11—Mo3	13.04 (16)	C1C—C2C—C3C—C4C	0.7 (5)
O10—As2—O11—Mo4	−112.40 (13)	C2C—C1C—C6C—C5C	−0.9 (5)
O10—As2—O12—Mo5	96.18 (14)	C2C—C3C—C4C—C5C	−2.2 (5)
O11—Mo3—O3—Mo4	−13.46 (10)	C3C—C4C—C5C—C6C	2.1 (5)
O11—Mo4—O4—Mo5	84.75 (12)	C4C—C5C—C6C—C1C	−0.6 (5)
O11—As2—O10—Mo2	−15.89 (17)	C6C—C1C—C2C—C3C	0.9 (5)
O11—As2—O12—Mo5	−33.48 (16)	N1D—C1D—C2D—C3D	177.1 (3)
O12—As2—O10—Mo2	−145.15 (13)	N1D—C1D—C6D—C5D	−177.1 (3)
O12—As2—O11—Mo3	140.57 (12)	C1D—C2D—C3D—C4D	0.1 (5)
O12—As2—O11—Mo4	15.13 (16)	C2D—C1D—C6D—C5D	2.2 (5)
O13—As2—O10—Mo2	100.14 (14)	C2D—C3D—C4D—C5D	1.9 (5)
O13—As2—O11—Mo3	−99.64 (13)	C3D—C4D—C5D—C6D	−1.9 (5)
O13—As2—O11—Mo4	134.92 (12)	C4D—C5D—C6D—C1D	−0.2 (5)
O13—As2—O12—Mo5	−153.04 (13)	C6D—C1D—C2D—C3D	−2.2 (5)
O14—As1—O7—Mo2	136.49 (14)	N1E—C1E—C2E—C3E	−179.9 (3)
O14—As1—O7—Mo3	−80.79 (13)	N1E—C1E—C6E—C5E	179.6 (3)
O14—As1—O8—Mo4	70.10 (14)	C1E—C2E—C3E—C4E	0.6 (5)
O14—As1—O8—Mo5	−118.98 (17)	C2E—C1E—C6E—C5E	−0.3 (4)
O14—As1—O9—Mo1	−103.44 (15)	C2E—C3E—C4E—C5E	−0.9 (5)
O14—As1—O9—Mo6	103.29 (15)	C3E—C4E—C5E—C6E	0.6 (5)
O15—Mo1—O1—Mo2	−166.5 (4)	C4E—C5E—C6E—C1E	0.0 (5)
O16—Mo1—O1—Mo2	−60.1 (4)	C6E—C1E—C2E—C3E	0.0 (4)
O17—Mo2—O1—Mo1	179.8 (4)