Effect of the ammonium ion on proton conduction in porous ionic crystals based on Keggin-type silicododeca­tungstate

Proton conduction in crystalline porous materials has received much attention from basic scientific research through to practical applications. Polyoxometalates (POMs) can efficiently transport protons because of their small superficial negative charge density. A simple method for enhancing proton conductivity is to introduce NH₄⁺ into the crystal structure, because NH₄⁺ can form hydrogen bonds and function as a proton carrier. According to these considerations, NH₄⁺ was introduced into the porous structure of A₂[Cr₃O(OOCH)₆(etpy)₃]₂[α-SiW₁₂O₄₀]·nH₂O (A = Li, Na, K and Cs; etpy = 4-ethyl­pyridine) (I-A⁺) via topotactic cation exchange. The resulting compound, di­ammonium tris­(4-ethyl­pyridine)­hexa­formatooxidotrichromium α-silicododecatungstate hexahydrate, (NH₄)₂[Cr₃(CHO₂)₆O(C₇H₉N)₃]₂[α-SiW₁₂O₄₀]·6H₂O, showed high pro­ton conductivity and low activation energy under high relative humidity (RH), suggesting that protons migrate efficiently via rearrangement of the hydrogen-bonding network formed by the NH₄⁺ cations and the waters of crystallization (Grotthuss mechanism). The proton conductivity and activation energy greatly decreased and increased, respectively, with the decrease in RH, suggesting that protons migrate as NH₄⁺ and/or H₃O⁺ under low RH (vehicle mechanism).

Computing details

Data collection: CrystalClear (Rigaku, 2007); cell refinement: CrystalClear (Rigaku, 2007); data reduction: CrystalClear (Rigaku, 2007); program(s) used to solve structure: SHELXL97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: CrystalStructure (Rigaku, 2015); software used to prepare material for publication: CrystalStructure (Rigaku, 2015).

Diammonium tris(4-ethylpyridine)hexaformatooxidotrichromium α-silicododecatungstate

Crystal data

(NH4)2[Cr3(CHO2)6O(C7H9N)3]2[SiW12O40]·8H2O	F(000) = 8232.00
Mr = 4491.50	Dx = 2.853 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71075 Å
a = 32.303 (4) Å	Cell parameters from 15010 reflections
b = 25.546 (3) Å	θ = 1.0–25.4°
c = 13.561 (2) Å	µ = 13.87 mm^−1
β = 110.885 (6)°	T = 93 K
V = 10456 (2) Å^3	Block, brown
Z = 4	0.20 × 0.20 × 0.20 mm

Data collection

Rigaku Saturn70 diffractometer	7855 reflections with F^2 > 2.0σ(F^2)
Detector resolution: 7.314 pixels mm^-1	Rint = 0.056
ω scans	θmax = 25.3°, θmin = 1.0°
Absorption correction: multi-scan (REQAB; Rigaku, 1998)	h = −38→38
Tmin = 0.009, Tmax = 0.062	k = −30→28
35536 measured reflections	l = −14→16
9475 independent reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
R[F^2 > 2σ(F^2)] = 0.058	Secondary atom site location: difference Fourier map
wR(F^2) = 0.175	H-atom parameters not defined
S = 1.11	w = 1/[σ^2(Fo^2) + (0.0924P)^2 + 183.152P] where P = (Fo^2 + 2Fc^2)/3
9475 reflections	(Δ/σ)max < 0.001
662 parameters	Δρmax = 3.11 e Å^−3
0 restraints	Δρmin = −3.90 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. Oxygen atoms of the [SiO4] unit of polyoxometalate were disorderd between two positions. Tungsten, chromium, and carbon atoms refined anisotropically. Oxygen atoms of the chromium cation and polyoxometalate were refined anisotropically, while those of the disordered [SiO4] unit of polyoxometalate were refined isotropically. Oxygen atoms of the water of crystallization were refined isotropically. Nitrogen atoms of the chromium cation were refined anisotropically, while that of the ammonium ion was refined isotropically. Silicon atom of the polyoxometalate was refined isotropically. Otherwise, non-positive definite anisotropic displacement parameters were observed. Hydrogen atoms were not included in the calculation. TG and elemental analysis showed that 6 water of crystallization and 2 ammonium ion existed per formula. 3 out of the 6 water of crystallization per formula could be located.

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

	x	y	z	Uiso*/Ueq	Occ. (<1)
W1	0.08250 (2)	0.22238 (2)	0.45055 (4)	0.02356 (16)
W2	0.08301 (2)	0.36076 (2)	0.45091 (4)	0.02339 (16)
W3	−0.00012 (2)	0.29122 (2)	0.50938 (4)	0.02474 (16)
W4	0.08314 (2)	0.36002 (2)	0.19168 (5)	0.02883 (17)
W5	0.0000	0.15333 (3)	0.2500	0.0382 (2)
W6	0.0000	0.42973 (3)	0.2500	0.0330 (2)
W7	0.08256 (2)	0.22207 (3)	0.19064 (6)	0.0415 (2)
Cr1	0.34683 (6)	0.52309 (7)	0.52795 (15)	0.0187 (4)
Cr2	0.24018 (6)	0.55105 (8)	0.46334 (15)	0.0209 (4)
Cr3	0.27545 (6)	0.43017 (8)	0.52804 (16)	0.0216 (4)
Si1	0.0000	0.29143 (15)	0.2500	0.0102 (9)*
O1	0.0330 (5)	0.3426 (6)	0.2808 (12)	0.015 (3)*	0.5
O2	0.0294 (5)	0.2917 (6)	0.3661 (13)	0.017 (3)*	0.5
O3	0.0314 (5)	0.2395 (6)	0.2824 (12)	0.016 (3)*	0.5
O4	0.0290 (5)	0.2929 (6)	0.1733 (13)	0.016 (3)*	0.5
O5	0.0435 (4)	0.2405 (4)	0.5211 (11)	0.050 (3)
O6	0.0432 (4)	0.3430 (4)	0.5201 (12)	0.056 (3)
O7	0.0436 (6)	0.1669 (7)	0.3857 (13)	0.100 (7)
O8	0.1048 (6)	0.2185 (7)	0.3406 (12)	0.097 (7)
O9	0.1215 (3)	0.1885 (4)	0.1630 (8)	0.038 (2)
O10	0.1046 (4)	0.2919 (4)	0.4768 (11)	0.047 (3)
O11	0.0429 (5)	0.4156 (7)	0.3831 (9)	0.100 (7)
O12	0.0423 (6)	0.4141 (7)	0.1891 (11)	0.096 (7)
O13	0.1054 (4)	0.2930 (5)	0.2051 (14)	0.093 (7)
O14	0.0000	0.4958 (5)	0.2500	0.039 (4)
O15	0.1210 (3)	0.3943 (6)	0.1594 (8)	0.057 (4)
O16	0.1068 (6)	0.3658 (7)	0.3421 (10)	0.092 (6)
O17	0.0419 (5)	0.2425 (5)	0.0495 (13)	0.095 (6)
O18	0.0000	0.0887 (5)	0.2500	0.060 (5)
O19	0.1219 (3)	0.3939 (4)	0.5478 (9)	0.047 (3)
O20	0.0435 (5)	0.1677 (7)	0.1940 (11)	0.098 (7)
O21	0.1219 (4)	0.1906 (5)	0.5453 (12)	0.069 (4)
O22	0.0437 (4)	0.3434 (4)	0.0507 (12)	0.082 (5)
O23	0.0004 (5)	0.2928 (5)	0.6340 (10)	0.066 (4)
O24	0.2877 (3)	0.5013 (3)	0.5074 (6)	0.0173 (17)
O25	0.2705 (3)	0.5978 (4)	0.5828 (7)	0.033 (2)
O26	0.3425 (3)	0.5884 (4)	0.6030 (7)	0.029 (2)
O27	0.2634 (3)	0.5910 (3)	0.3706 (7)	0.026 (2)
O28	0.3310 (3)	0.5608 (4)	0.3935 (6)	0.0261 (19)
O29	0.3292 (3)	0.4201 (4)	0.6547 (7)	0.031 (2)
O30	0.3729 (3)	0.4901 (4)	0.6696 (7)	0.029 (2)
O31	0.3052 (3)	0.4019 (3)	0.4360 (7)	0.030 (2)
O32	0.3597 (3)	0.4611 (3)	0.4576 (7)	0.028 (2)
O33	0.2062 (3)	0.5206 (4)	0.5480 (7)	0.033 (2)
O34	0.2432 (3)	0.4487 (4)	0.6222 (7)	0.032 (2)
O35	0.2039 (3)	0.5089 (4)	0.3421 (7)	0.031 (2)
O36	0.2193 (3)	0.4274 (4)	0.4046 (7)	0.030 (2)
O100	−0.0246 (11)	0.3907 (14)	0.716 (3)	0.100 (11)*	0.5
O101	0.0005 (11)	0.4441 (13)	−0.053 (3)	0.091 (10)*	0.5
O102	0.0857 (12)	0.5487 (14)	0.193 (3)	0.098 (11)*	0.5
N1	0.4126 (3)	0.5440 (4)	0.5507 (8)	0.024 (2)
N2	0.2612 (4)	0.3526 (5)	0.5604 (9)	0.031 (3)
N3	0.1891 (4)	0.6077 (4)	0.4155 (8)	0.024 (2)
N4	0.1116 (10)	0.5104 (11)	0.385 (2)	0.135 (10)*
C1	0.3111 (5)	0.6074 (6)	0.6232 (10)	0.030 (3)
C2	0.2976 (4)	0.5894 (5)	0.3479 (10)	0.023 (3)
C3	0.3613 (4)	0.4485 (6)	0.6989 (10)	0.030 (3)
C4	0.3386 (4)	0.4198 (5)	0.4200 (10)	0.026 (3)
C5	0.2142 (5)	0.4830 (6)	0.6106 (11)	0.034 (3)
C6	0.1992 (5)	0.4607 (6)	0.3377 (11)	0.032 (3)
C7	0.4226 (4)	0.5923 (5)	0.5198 (9)	0.026 (3)
C8	0.4656 (4)	0.6057 (5)	0.5336 (10)	0.028 (3)
C9	0.5009 (4)	0.5710 (5)	0.5820 (11)	0.030 (3)
C10	0.4901 (4)	0.5227 (5)	0.6123 (10)	0.026 (3)
C11	0.4465 (5)	0.5116 (5)	0.5967 (12)	0.031 (3)
C12	0.5477 (4)	0.5855 (6)	0.6015 (13)	0.040 (4)
C13	0.5635 (5)	0.6284 (7)	0.6905 (14)	0.049 (4)
C14	0.2946 (5)	0.3172 (5)	0.5903 (11)	0.030 (3)
C15	0.2888 (4)	0.2687 (5)	0.6338 (13)	0.037 (4)
C16	0.2480 (5)	0.2569 (6)	0.6420 (11)	0.034 (3)
C17	0.2140 (5)	0.2925 (6)	0.6017 (13)	0.038 (4)
C18	0.2211 (4)	0.3398 (5)	0.5617 (11)	0.030 (3)
C19	0.2426 (7)	0.2070 (6)	0.6967 (16)	0.059 (6)
C20	0.2542 (13)	0.2216 (15)	0.818 (3)	0.139 (13)*
C21	0.1725 (4)	0.6287 (6)	0.4852 (12)	0.034 (3)
C22	0.1432 (5)	0.6701 (6)	0.4588 (12)	0.041 (4)
C23	0.1286 (5)	0.6916 (6)	0.3589 (12)	0.036 (3)
C24	0.1449 (5)	0.6678 (6)	0.2844 (12)	0.041 (4)
C25	0.1742 (5)	0.6273 (6)	0.3163 (10)	0.035 (3)
C26	0.0973 (6)	0.7382 (7)	0.3252 (15)	0.054 (5)
C27	0.1151 (12)	0.7828 (9)	0.399 (2)	0.109 (11)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
W1	0.0170 (3)	0.0282 (3)	0.0223 (3)	0.0051 (2)	0.0032 (2)	0.0032 (2)
W2	0.0180 (3)	0.0304 (3)	0.0167 (3)	0.0043 (2)	0.0000 (2)	−0.00719 (19)
W3	0.0253 (3)	0.0291 (3)	0.0165 (3)	0.0026 (2)	0.0034 (2)	0.00589 (19)
W4	0.0205 (3)	0.0255 (3)	0.0461 (4)	−0.0057 (2)	0.0187 (3)	0.0013 (2)
W5	0.0455 (5)	0.0107 (4)	0.0682 (6)	0.000	0.0323 (5)	0.000
W6	0.0635 (6)	0.0106 (4)	0.0284 (4)	0.000	0.0204 (4)	0.000
W7	0.0173 (3)	0.0444 (4)	0.0612 (5)	−0.0005 (2)	0.0121 (3)	−0.0357 (3)
Cr1	0.0154 (9)	0.0199 (10)	0.0192 (10)	0.0006 (7)	0.0042 (7)	0.0021 (7)
Cr2	0.0188 (10)	0.0258 (11)	0.0179 (10)	0.0047 (8)	0.0062 (8)	0.0005 (8)
Cr3	0.0150 (9)	0.0221 (10)	0.0273 (11)	0.0019 (8)	0.0068 (8)	0.0072 (8)
O5	0.043 (6)	0.021 (5)	0.102 (10)	−0.001 (5)	0.046 (7)	−0.007 (6)
O6	0.037 (6)	0.022 (6)	0.128 (11)	−0.001 (5)	0.051 (7)	−0.006 (6)
O7	0.106 (13)	0.132 (15)	0.097 (12)	−0.082 (12)	0.080 (11)	−0.082 (11)
O8	0.105 (12)	0.135 (14)	0.080 (10)	−0.103 (11)	0.069 (10)	−0.079 (10)
O9	0.024 (5)	0.050 (6)	0.035 (6)	0.013 (5)	0.006 (4)	−0.009 (5)
O10	0.041 (6)	0.033 (6)	0.088 (9)	0.005 (4)	0.050 (7)	−0.003 (5)
O11	0.119 (12)	0.161 (16)	0.036 (7)	0.122 (12)	0.048 (8)	0.035 (8)
O12	0.127 (13)	0.129 (14)	0.059 (8)	0.103 (12)	0.067 (9)	0.056 (9)
O13	0.038 (7)	0.047 (8)	0.122 (13)	0.008 (6)	−0.060 (8)	−0.018 (7)
O14	0.059 (10)	0.010 (6)	0.043 (9)	0.000	0.015 (7)	0.000
O15	0.031 (6)	0.107 (10)	0.032 (6)	−0.041 (6)	0.009 (5)	−0.005 (6)
O16	0.116 (13)	0.137 (14)	0.044 (8)	0.102 (11)	0.053 (8)	0.041 (8)
O17	0.067 (9)	0.029 (7)	0.125 (13)	−0.018 (6)	−0.045 (9)	−0.030 (7)
O18	0.086 (13)	0.014 (7)	0.053 (10)	0.000	−0.010 (9)	0.000
O19	0.030 (5)	0.046 (7)	0.064 (7)	−0.018 (5)	0.016 (5)	−0.043 (6)
O20	0.087 (11)	0.159 (16)	0.065 (9)	−0.101 (11)	0.047 (8)	−0.078 (10)
O21	0.037 (7)	0.063 (8)	0.105 (11)	0.027 (6)	0.022 (7)	0.071 (8)
O22	0.048 (7)	0.017 (6)	0.118 (12)	0.004 (5)	−0.047 (8)	−0.012 (6)
O23	0.108 (12)	0.057 (9)	0.056 (8)	0.036 (7)	0.058 (9)	0.021 (6)
O24	0.014 (4)	0.019 (4)	0.016 (4)	0.002 (3)	0.003 (3)	0.001 (3)
O25	0.025 (5)	0.038 (6)	0.033 (5)	0.003 (4)	0.008 (4)	−0.016 (4)
O26	0.023 (5)	0.033 (5)	0.027 (5)	−0.001 (4)	0.005 (4)	−0.007 (4)
O27	0.029 (5)	0.024 (5)	0.031 (5)	0.007 (4)	0.018 (4)	0.009 (4)
O28	0.019 (4)	0.033 (5)	0.021 (5)	0.003 (4)	0.002 (4)	0.007 (4)
O29	0.020 (5)	0.035 (5)	0.034 (5)	0.002 (4)	0.007 (4)	0.012 (4)
O30	0.022 (5)	0.040 (6)	0.020 (5)	−0.006 (4)	0.000 (4)	0.010 (4)
O31	0.031 (5)	0.016 (5)	0.043 (6)	−0.005 (4)	0.015 (4)	−0.004 (4)
O32	0.016 (4)	0.028 (5)	0.041 (5)	−0.002 (4)	0.012 (4)	−0.006 (4)
O33	0.026 (5)	0.041 (6)	0.038 (6)	0.019 (4)	0.020 (4)	0.014 (4)
O34	0.028 (5)	0.029 (5)	0.040 (6)	0.007 (4)	0.015 (4)	0.009 (4)
O35	0.029 (5)	0.028 (5)	0.031 (5)	0.008 (4)	0.007 (4)	−0.003 (4)
O36	0.025 (5)	0.021 (5)	0.041 (6)	−0.001 (4)	0.009 (4)	0.003 (4)
N1	0.022 (5)	0.020 (5)	0.029 (6)	−0.003 (4)	0.008 (5)	−0.005 (4)
N2	0.021 (6)	0.034 (7)	0.032 (6)	−0.006 (5)	0.003 (5)	−0.001 (5)
N3	0.030 (6)	0.024 (6)	0.021 (6)	0.008 (5)	0.011 (5)	−0.003 (4)
C1	0.031 (7)	0.034 (8)	0.023 (7)	0.001 (6)	0.009 (6)	−0.001 (5)
C2	0.026 (6)	0.018 (6)	0.025 (7)	0.009 (5)	0.008 (5)	0.000 (5)
C3	0.016 (6)	0.049 (9)	0.023 (7)	−0.004 (6)	0.003 (5)	0.006 (6)
C4	0.015 (6)	0.023 (7)	0.037 (8)	−0.006 (5)	0.006 (5)	0.007 (5)
C5	0.029 (7)	0.043 (9)	0.035 (8)	0.005 (7)	0.017 (6)	0.007 (7)
C6	0.032 (7)	0.036 (9)	0.028 (7)	0.002 (6)	0.009 (6)	−0.009 (6)
C7	0.022 (6)	0.036 (8)	0.014 (6)	−0.004 (5)	−0.003 (5)	0.005 (5)
C8	0.023 (6)	0.031 (7)	0.028 (7)	0.001 (6)	0.009 (5)	0.006 (6)
C9	0.014 (6)	0.031 (7)	0.041 (8)	−0.006 (5)	0.007 (5)	0.003 (6)
C10	0.017 (6)	0.028 (7)	0.032 (7)	0.001 (5)	0.006 (5)	0.004 (5)
C11	0.034 (8)	0.018 (7)	0.044 (9)	0.005 (6)	0.016 (6)	−0.001 (6)
C12	0.015 (6)	0.036 (8)	0.066 (11)	−0.005 (6)	0.011 (7)	0.006 (7)
C13	0.038 (9)	0.054 (11)	0.053 (10)	−0.016 (8)	0.011 (8)	−0.013 (8)
C14	0.029 (7)	0.024 (7)	0.033 (8)	0.007 (6)	0.006 (6)	0.008 (6)
C15	0.021 (7)	0.018 (7)	0.061 (10)	−0.006 (5)	0.000 (6)	0.005 (6)
C16	0.029 (7)	0.033 (8)	0.037 (8)	−0.016 (6)	0.010 (6)	0.012 (6)
C17	0.020 (7)	0.044 (10)	0.049 (10)	−0.005 (6)	0.011 (7)	0.017 (7)
C18	0.022 (7)	0.029 (7)	0.038 (8)	−0.014 (6)	0.009 (6)	−0.002 (6)
C19	0.062 (12)	0.035 (10)	0.064 (12)	−0.025 (8)	0.003 (10)	0.020 (8)
C21	0.023 (7)	0.037 (8)	0.041 (8)	0.010 (6)	0.009 (6)	−0.005 (6)
C22	0.046 (9)	0.035 (8)	0.046 (9)	0.018 (7)	0.022 (7)	−0.007 (7)
C23	0.027 (7)	0.034 (8)	0.050 (10)	0.008 (6)	0.016 (7)	0.008 (7)
C24	0.039 (9)	0.046 (9)	0.032 (8)	0.004 (7)	0.007 (7)	−0.001 (7)
C25	0.035 (8)	0.040 (8)	0.017 (7)	0.016 (6)	−0.007 (6)	−0.004 (6)
C26	0.038 (9)	0.040 (10)	0.084 (13)	0.022 (8)	0.022 (9)	0.001 (9)
C27	0.17 (3)	0.048 (13)	0.080 (18)	0.018 (16)	0.013 (19)	−0.011 (12)

Geometric parameters (Å, º)

W1—O21	1.663 (10)	Cr2—N3	2.116 (10)
W1—O8	1.875 (13)	Cr3—O24	1.901 (8)
W1—O7	1.891 (13)	Cr3—O31	1.964 (9)
W1—O5	1.891 (10)	Cr3—O34	1.973 (9)
W1—O10	1.900 (10)	Cr3—O29	1.975 (9)
W1—O3	2.331 (15)	Cr3—O36	1.983 (9)
W1—O2	2.447 (15)	Cr3—N2	2.114 (12)
W2—O19	1.687 (9)	Si1—O2	1.521 (16)
W2—O10	1.878 (10)	Si1—O2^i	1.521 (16)
W2—O16	1.896 (12)	Si1—O4^i	1.630 (16)
W2—O6	1.898 (11)	Si1—O4	1.630 (16)
W2—O11	1.908 (12)	Si1—O3^i	1.633 (15)
W2—O1	2.342 (15)	Si1—O3	1.633 (15)
W2—O2	2.454 (15)	Si1—O1^i	1.645 (15)
W3—O23	1.685 (12)	Si1—O1	1.645 (15)
W3—O17^i	1.799 (14)	O1—O2	1.77 (2)
W3—O5	1.879 (10)	O2—O4^i	1.77 (2)
W3—O6	1.893 (10)	O2—O3	1.77 (2)
W3—O22^i	1.899 (11)	O4—O2^i	1.77 (2)
W3—O4^i	2.315 (16)	O4—W3^i	2.315 (16)
W3—O2	2.450 (16)	O17—W3^i	1.800 (14)
W4—O15	1.685 (10)	O22—W3^i	1.898 (11)
W4—O13	1.841 (12)	O25—C1	1.250 (16)
W4—O12	1.903 (12)	O26—C1	1.241 (16)
W4—O16	1.911 (13)	O27—C2	1.251 (15)
W4—O22	1.929 (12)	O28—C2	1.266 (14)
W4—O1	2.383 (15)	O29—C3	1.233 (16)
W4—O4	2.398 (15)	O30—C3	1.239 (16)
W5—O18	1.652 (14)	O31—C4	1.258 (15)
W5—O20^i	1.856 (13)	O32—C4	1.263 (15)
W5—O20	1.856 (13)	O33—C5	1.246 (17)
W5—O7^i	1.908 (16)	O34—C5	1.250 (17)
W5—O7	1.908 (16)	O35—C6	1.239 (17)
W5—O3	2.397 (15)	O36—C6	1.243 (17)
W5—O3^i	2.397 (15)	O100—O100^ii	1.53 (7)
W6—O14	1.687 (12)	N1—C11	1.336 (17)
W6—O12	1.874 (12)	N1—C7	1.378 (16)
W6—O12^i	1.874 (12)	N2—C18	1.345 (17)
W6—O11^i	1.877 (13)	N2—C14	1.352 (17)
W6—O11	1.877 (13)	N3—C21	1.351 (17)
W6—O1	2.438 (15)	N3—C25	1.353 (17)
W6—O1^i	2.438 (15)	C7—C8	1.375 (18)
W7—O9	1.671 (9)	C8—C9	1.411 (18)
W7—O20	1.889 (13)	C9—C10	1.382 (18)
W7—O8	1.902 (16)	C9—C12	1.485 (17)
W7—O13	1.938 (13)	C10—C11	1.379 (18)
W7—O17	1.967 (14)	C12—C13	1.57 (2)
W7—O3	2.438 (15)	C14—C15	1.41 (2)
W7—O4	2.456 (15)	C15—C16	1.396 (19)
Cr1—O24	1.913 (8)	C16—C17	1.38 (2)
Cr1—O28	1.963 (8)	C16—C19	1.516 (19)
Cr1—O32	1.968 (9)	C17—C18	1.376 (19)
Cr1—O26	1.985 (9)	C19—C20	1.59 (4)
Cr1—O30	1.989 (8)	C21—C22	1.378 (19)
Cr1—N1	2.105 (10)	C22—C23	1.38 (2)
Cr2—O24	1.917 (8)	C23—C24	1.43 (2)
Cr2—O27	1.964 (8)	C23—C26	1.52 (2)
Cr2—O35	1.966 (9)	C24—C25	1.36 (2)
Cr2—O25	1.970 (9)	C26—C27	1.49 (3)
Cr2—O33	2.008 (9)
O21—W1—O8	100.6 (8)	O27—Cr2—O33	168.3 (4)
O21—W1—O7	101.1 (8)	O35—Cr2—O33	88.9 (4)
O8—W1—O7	88.3 (5)	O25—Cr2—O33	88.8 (4)
O21—W1—O5	101.2 (6)	O24—Cr2—N3	178.4 (4)
O8—W1—O5	158.3 (8)	O27—Cr2—N3	83.3 (4)
O7—W1—O5	88.1 (5)	O35—Cr2—N3	87.2 (4)
O21—W1—O10	100.3 (7)	O25—Cr2—N3	86.7 (4)
O8—W1—O10	88.4 (5)	O33—Cr2—N3	85.1 (4)
O7—W1—O10	158.6 (8)	O24—Cr3—O31	94.8 (4)
O5—W1—O10	87.1 (4)	O24—Cr3—O34	92.9 (4)
O21—W1—O3	158.1 (7)	O31—Cr3—O34	172.2 (4)
O8—W1—O3	64.5 (7)	O24—Cr3—O29	95.0 (4)
O7—W1—O3	64.1 (7)	O31—Cr3—O29	91.5 (4)
O5—W1—O3	94.7 (5)	O34—Cr3—O29	88.4 (4)
O10—W1—O3	95.5 (6)	O24—Cr3—O36	94.9 (4)
O21—W1—O2	158.6 (7)	O31—Cr3—O36	87.6 (4)
O8—W1—O2	94.0 (8)	O34—Cr3—O36	91.1 (4)
O7—W1—O2	94.9 (8)	O29—Cr3—O36	170.1 (4)
O5—W1—O2	65.0 (5)	O24—Cr3—N2	176.2 (4)
O10—W1—O2	64.2 (5)	O31—Cr3—N2	88.8 (4)
O3—W1—O2	43.3 (5)	O34—Cr3—N2	83.5 (4)
O19—W2—O10	101.6 (6)	O29—Cr3—N2	83.5 (4)
O19—W2—O16	100.1 (7)	O36—Cr3—N2	86.6 (4)
O10—W2—O16	89.0 (5)	O2—Si1—O2^i	179.6 (12)
O19—W2—O6	100.5 (6)	O2—Si1—O4^i	68.1 (8)
O10—W2—O6	87.5 (4)	O2^i—Si1—O4^i	111.9 (8)
O16—W2—O6	159.3 (7)	O2—Si1—O4	111.9 (8)
O19—W2—O11	101.3 (7)	O2^i—Si1—O4	68.1 (8)
O10—W2—O11	157.1 (7)	O4^i—Si1—O4	177.4 (10)
O16—W2—O11	88.3 (5)	O2—Si1—O3^i	112.3 (8)
O6—W2—O11	87.1 (6)	O2^i—Si1—O3^i	68.0 (8)
O19—W2—O1	157.9 (6)	O4^i—Si1—O3^i	75.4 (7)
O10—W2—O1	94.5 (6)	O4—Si1—O3^i	106.8 (8)
O16—W2—O1	64.9 (7)	O2—Si1—O3	68.0 (8)
O6—W2—O1	95.1 (6)	O2^i—Si1—O3	112.3 (8)
O11—W2—O1	63.8 (6)	O4^i—Si1—O3	106.8 (8)
O19—W2—O2	158.7 (6)	O4—Si1—O3	75.3 (7)
O10—W2—O2	64.3 (5)	O3^i—Si1—O3	71.2 (11)
O16—W2—O2	95.7 (7)	O2—Si1—O1^i	111.6 (8)
O6—W2—O2	64.5 (5)	O2^i—Si1—O1^i	68.0 (8)
O11—W2—O2	93.3 (7)	O4^i—Si1—O1^i	71.1 (7)
O1—W2—O2	43.3 (5)	O4—Si1—O1^i	106.7 (8)
O23—W3—O17^i	101.5 (8)	O3^i—Si1—O1^i	107.1 (8)
O23—W3—O5	101.1 (6)	O3—Si1—O1^i	177.7 (7)
O17^i—W3—O5	89.0 (6)	O2—Si1—O1	68.0 (8)
O23—W3—O6	99.4 (7)	O2^i—Si1—O1	111.6 (8)
O17^i—W3—O6	159.1 (8)	O4^i—Si1—O1	106.7 (8)
O5—W3—O6	87.9 (5)	O4—Si1—O1	71.1 (7)
O23—W3—O22^i	98.9 (7)	O3^i—Si1—O1	177.7 (7)
O17^i—W3—O22^i	88.3 (5)	O3—Si1—O1	107.1 (8)
O5—W3—O22^i	160.0 (7)	O1^i—Si1—O1	74.6 (11)
O6—W3—O22^i	87.5 (5)	Si1—O1—O2	52.7 (7)
O23—W3—O4^i	158.3 (7)	Si1—O1—W2	124.4 (8)
O17^i—W3—O4^i	65.5 (7)	O2—O1—W2	71.7 (7)
O5—W3—O4^i	96.2 (6)	Si1—O1—W4	121.0 (8)
O6—W3—O4^i	94.2 (6)	O2—O1—W4	133.1 (9)
O22^i—W3—O4^i	64.8 (6)	W2—O1—W4	96.2 (5)
O23—W3—O2	158.1 (7)	Si1—O1—W6	118.6 (8)
O17^i—W3—O2	95.4 (7)	O2—O1—W6	131.0 (9)
O5—W3—O2	65.1 (5)	W2—O1—W6	95.4 (5)
O6—W3—O2	64.7 (5)	W4—O1—W6	94.5 (5)
O22^i—W3—O2	95.4 (7)	Si1—O2—O4^i	58.8 (8)
O4^i—W3—O2	43.4 (5)	Si1—O2—O3	59.0 (7)
O15—W4—O13	102.4 (8)	O4^i—O2—O3	95.7 (10)
O15—W4—O12	100.4 (7)	Si1—O2—O1	59.3 (7)
O13—W4—O12	157.1 (8)	O4^i—O2—O1	95.8 (10)
O15—W4—O16	100.7 (7)	O3—O2—O1	96.3 (11)
O13—W4—O16	88.4 (7)	Si1—O2—W1	123.8 (8)
O12—W4—O16	88.6 (6)	O4^i—O2—W1	130.5 (9)
O15—W4—O22	98.1 (6)	O3—O2—W1	64.8 (7)
O13—W4—O22	89.4 (5)	O1—O2—W1	129.6 (10)
O12—W4—O22	86.1 (6)	Si1—O2—W3	123.1 (9)
O16—W4—O22	161.1 (8)	O4^i—O2—W3	64.2 (7)
O15—W4—O1	156.5 (6)	O3—O2—W3	128.3 (9)
O13—W4—O1	95.0 (8)	O1—O2—W3	130.9 (9)
O12—W4—O1	63.4 (6)	W1—O2—W3	91.8 (5)
O16—W4—O1	63.8 (6)	Si1—O2—W2	124.3 (8)
O22—W4—O1	97.7 (6)	O4^i—O2—W2	128.9 (9)
O15—W4—O4	156.2 (6)	O3—O2—W2	131.5 (10)
O13—W4—O4	65.7 (6)	O1—O2—W2	65.0 (7)
O12—W4—O4	92.4 (7)	W1—O2—W2	92.3 (6)
O16—W4—O4	99.5 (7)	W3—O2—W2	92.3 (5)
O22—W4—O4	62.6 (6)	Si1—O3—O2	53.0 (7)
O1—W4—O4	46.9 (5)	Si1—O3—W1	124.8 (8)
O18—W5—O20^i	101.4 (6)	O2—O3—W1	71.8 (7)
O18—W5—O20	101.4 (6)	Si1—O3—W5	121.0 (8)
O20^i—W5—O20	157.3 (12)	O2—O3—W5	134.4 (9)
O18—W5—O7^i	100.4 (6)	W1—O3—W5	96.5 (6)
O20^i—W5—O7^i	87.3 (6)	Si1—O3—W7	118.7 (8)
O20—W5—O7^i	88.6 (7)	O2—O3—W7	130.7 (9)
O18—W5—O7	100.4 (6)	W1—O3—W7	95.3 (5)
O20^i—W5—O7	88.6 (7)	W5—O3—W7	93.4 (5)
O20—W5—O7	87.3 (6)	Si1—O4—O2^i	53.0 (7)
O7^i—W5—O7	159.1 (12)	Si1—O4—W3^i	125.3 (9)
O18—W5—O3	156.6 (4)	O2^i—O4—W3^i	72.4 (7)
O20^i—W5—O3	94.4 (7)	Si1—O4—W4	120.9 (8)
O20—W5—O3	64.0 (6)	O2^i—O4—W4	134.7 (9)
O7^i—W5—O3	97.4 (7)	W3^i—O4—W4	97.2 (6)
O7—W5—O3	62.5 (7)	Si1—O4—W7	117.9 (8)
O18—W5—O3^i	156.6 (4)	O2^i—O4—W7	130.9 (9)
O20^i—W5—O3^i	64.0 (6)	W3^i—O4—W7	95.2 (5)
O20—W5—O3^i	94.4 (7)	W4—O4—W7	93.1 (6)
O7^i—W5—O3^i	62.5 (7)	W3—O5—W1	137.8 (7)
O7—W5—O3^i	97.4 (7)	W3—O6—W2	137.9 (7)
O3—W5—O3^i	46.7 (7)	W1—O7—W5	136.4 (11)
O14—W6—O12	102.3 (5)	W1—O8—W7	138.0 (11)
O14—W6—O12^i	102.3 (5)	W2—O10—W1	138.7 (7)
O12—W6—O12^i	155.5 (11)	W6—O11—W2	138.3 (9)
O14—W6—O11^i	101.1 (6)	W6—O12—W4	139.1 (8)
O12—W6—O11^i	86.5 (7)	W4—O13—W7	137.6 (8)
O12^i—W6—O11^i	88.8 (6)	W2—O16—W4	134.9 (10)
O14—W6—O11	101.1 (6)	W3^i—O17—W7	138.6 (9)
O12—W6—O11	88.8 (6)	W5—O20—W7	139.9 (9)
O12^i—W6—O11	86.5 (7)	W3^i—O22—W4	135.0 (9)
O11^i—W6—O11	157.8 (12)	Cr3—O24—Cr1	120.4 (4)
O14—W6—O1	155.9 (4)	Cr3—O24—Cr2	119.6 (4)
O12—W6—O1	62.5 (6)	Cr1—O24—Cr2	120.0 (4)
O12^i—W6—O1	94.2 (7)	C1—O25—Cr2	128.0 (9)
O11^i—W6—O1	96.7 (7)	C1—O26—Cr1	130.8 (9)
O11—W6—O1	62.1 (6)	C2—O27—Cr2	135.5 (8)
O14—W6—O1^i	155.9 (4)	C2—O28—Cr1	129.1 (8)
O12—W6—O1^i	94.2 (7)	C3—O29—Cr3	132.3 (9)
O12^i—W6—O1^i	62.5 (6)	C3—O30—Cr1	126.9 (8)
O11^i—W6—O1^i	62.1 (6)	C4—O31—Cr3	128.3 (9)
O11—W6—O1^i	96.7 (7)	C4—O32—Cr1	133.7 (8)
O1—W6—O1^i	48.3 (7)	C5—O33—Cr2	131.7 (9)
O9—W7—O20	101.0 (7)	C5—O34—Cr3	129.2 (9)
O9—W7—O8	100.9 (7)	C6—O35—Cr2	127.6 (9)
O20—W7—O8	86.5 (6)	C6—O36—Cr3	132.4 (9)
O9—W7—O13	102.3 (7)	C11—N1—C7	117.1 (11)
O20—W7—O13	156.6 (8)	C11—N1—Cr1	121.8 (9)
O8—W7—O13	87.2 (7)	C7—N1—Cr1	121.1 (8)
O9—W7—O17	102.3 (6)	C18—N2—C14	120.1 (12)
O20—W7—O17	89.9 (7)	C18—N2—Cr3	120.9 (10)
O8—W7—O17	156.8 (8)	C14—N2—Cr3	118.7 (9)
O13—W7—O17	87.0 (5)	C21—N3—C25	117.4 (11)
O9—W7—O3	155.4 (5)	C21—N3—Cr2	121.2 (9)
O20—W7—O3	62.7 (6)	C25—N3—Cr2	121.3 (8)
O8—W7—O3	61.9 (6)	O26—C1—O25	129.7 (13)
O13—W7—O3	94.6 (7)	O27—C2—O28	124.9 (12)
O17—W7—O3	96.3 (7)	O29—C3—O30	130.3 (12)
O9—W7—O4	156.5 (5)	O31—C4—O32	127.4 (13)
O20—W7—O4	95.2 (7)	O33—C5—O34	126.1 (13)
O8—W7—O4	97.0 (7)	O35—C6—O36	128.4 (13)
O13—W7—O4	63.3 (6)	C8—C7—N1	121.1 (12)
O17—W7—O4	60.5 (6)	C7—C8—C9	121.1 (12)
O3—W7—O4	48.1 (5)	C10—C9—C8	116.8 (11)
O24—Cr1—O28	95.3 (3)	C10—C9—C12	121.2 (12)
O24—Cr1—O32	93.9 (3)	C8—C9—C12	122.0 (12)
O28—Cr1—O32	88.5 (4)	C11—C10—C9	119.5 (12)
O24—Cr1—O26	94.1 (4)	N1—C11—C10	124.4 (13)
O28—Cr1—O26	91.2 (4)	C9—C12—C13	109.9 (13)
O32—Cr1—O26	172.0 (4)	N2—C14—C15	120.2 (13)
O24—Cr1—O30	94.3 (4)	C16—C15—C14	119.3 (13)
O28—Cr1—O30	170.3 (4)	C17—C16—C15	117.9 (12)
O32—Cr1—O30	92.1 (4)	C17—C16—C19	122.4 (14)
O26—Cr1—O30	86.8 (4)	C15—C16—C19	119.7 (15)
O24—Cr1—N1	177.8 (4)	C18—C17—C16	121.1 (13)
O28—Cr1—N1	85.8 (4)	N2—C18—C17	121.0 (13)
O32—Cr1—N1	84.1 (4)	C16—C19—C20	106.4 (19)
O26—Cr1—N1	87.9 (4)	N3—C21—C22	122.0 (13)
O30—Cr1—N1	84.7 (4)	C21—C22—C23	121.6 (14)
O24—Cr2—O27	95.7 (4)	C22—C23—C24	116.0 (13)
O24—Cr2—O35	94.0 (4)	C22—C23—C26	124.4 (14)
O27—Cr2—O35	90.0 (4)	C24—C23—C26	119.6 (14)
O24—Cr2—O25	92.1 (4)	C25—C24—C23	119.2 (14)
O27—Cr2—O25	91.1 (4)	N3—C25—C24	123.7 (13)
O35—Cr2—O25	173.6 (4)	C27—C26—C23	109.9 (17)
O24—Cr2—O33	96.0 (3)
O2^i—Si1—O1—O2	179.8 (6)	O1—Si1—O4—W4	1.3 (8)
O4^i—Si1—O1—O2	57.3 (9)	O2—Si1—O4—W7	58.5 (10)
O4—Si1—O1—O2	−124.2 (9)	O2^i—Si1—O4—W7	−122.0 (10)
O3—Si1—O1—O2	−56.9 (9)	O3^i—Si1—O4—W7	−64.8 (10)
O1^i—Si1—O1—O2	121.6 (10)	O3—Si1—O4—W7	−0.1 (8)
O2—Si1—O1—W2	−1.4 (9)	O1^i—Si1—O4—W7	−179.1 (8)
O2^i—Si1—O1—W2	178.4 (9)	O1—Si1—O4—W7	114.2 (10)
O4^i—Si1—O1—W2	55.9 (11)	O23—W3—O5—W1	−155.7 (10)
O4—Si1—O1—W2	−125.6 (11)	O17^i—W3—O5—W1	102.8 (11)
O3—Si1—O1—W2	−58.3 (11)	O6—W3—O5—W1	−56.5 (10)
O1^i—Si1—O1—W2	120.2 (13)	O22^i—W3—O5—W1	20 (2)
O2—Si1—O1—W4	122.9 (11)	O4^i—W3—O5—W1	37.5 (10)
O2^i—Si1—O1—W4	−57.3 (11)	O2—W3—O5—W1	6.4 (9)
O4^i—Si1—O1—W4	−179.8 (8)	O21—W1—O5—W3	156.3 (10)
O4—Si1—O1—W4	−1.3 (8)	O8—W1—O5—W3	−22 (2)
O3—Si1—O1—W4	66.0 (10)	O7—W1—O5—W3	−102.7 (11)
O1^i—Si1—O1—W4	−115.5 (12)	O10—W1—O5—W3	56.4 (10)
O2—Si1—O1—W6	−121.6 (10)	O3—W1—O5—W3	−38.9 (10)
O2^i—Si1—O1—W6	58.2 (10)	O2—W1—O5—W3	−6.4 (9)
O4^i—Si1—O1—W6	−64.3 (10)	O23—W3—O6—W2	155.6 (10)
O4—Si1—O1—W6	114.2 (10)	O17^i—W3—O6—W2	−27 (2)
O3—Si1—O1—W6	−178.5 (7)	O5—W3—O6—W2	54.8 (11)
O1^i—Si1—O1—W6	0.000 (1)	O22^i—W3—O6—W2	−105.7 (11)
O4—Si1—O2—O4^i	177.2 (11)	O4^i—W3—O6—W2	−41.3 (11)
O3^i—Si1—O2—O4^i	−62.7 (9)	O2—W3—O6—W2	−8.5 (9)
O3—Si1—O2—O4^i	−119.9 (9)	O19—W2—O6—W3	−155.5 (10)
O1^i—Si1—O2—O4^i	57.7 (9)	O10—W2—O6—W3	−54.1 (11)
O1—Si1—O2—O4^i	119.8 (9)	O16—W2—O6—W3	26 (2)
O4^i—Si1—O2—O3	119.9 (9)	O11—W2—O6—W3	103.6 (11)
O4—Si1—O2—O3	−62.9 (9)	O1—W2—O6—W3	40.2 (11)
O3^i—Si1—O2—O3	57.2 (12)	O2—W2—O6—W3	8.5 (9)
O1^i—Si1—O2—O3	177.6 (8)	O21—W1—O7—W5	−155.5 (12)
O1—Si1—O2—O3	−120.3 (10)	O8—W1—O7—W5	−55.1 (13)
O4^i—Si1—O2—O1	−119.8 (9)	O5—W1—O7—W5	103.5 (12)
O4—Si1—O2—O1	57.4 (9)	O10—W1—O7—W5	26 (2)
O3^i—Si1—O2—O1	177.6 (8)	O3—W1—O7—W5	7.3 (10)
O3—Si1—O2—O1	120.3 (10)	O2—W1—O7—W5	38.8 (12)
O1^i—Si1—O2—O1	−62.1 (12)	O21—W1—O8—W7	157.0 (13)
O4^i—Si1—O2—W1	120.5 (11)	O7—W1—O8—W7	56.0 (14)
O4—Si1—O2—W1	−62.3 (11)	O5—W1—O8—W7	−25 (2)
O3^i—Si1—O2—W1	57.9 (12)	O10—W1—O8—W7	−102.9 (13)
O3—Si1—O2—W1	0.6 (8)	O3—W1—O8—W7	−6.0 (11)
O1^i—Si1—O2—W1	178.2 (8)	O2—W1—O8—W7	−38.8 (13)
O1—Si1—O2—W1	−119.7 (12)	O19—W2—O10—W1	155.8 (10)
O4^i—Si1—O2—W3	1.8 (8)	O16—W2—O10—W1	−104.1 (11)
O4—Si1—O2—W3	179.0 (8)	O6—W2—O10—W1	55.6 (10)
O3^i—Si1—O2—W3	−60.9 (11)	O11—W2—O10—W1	−20.9 (19)
O3—Si1—O2—W3	−118.1 (11)	O1—W2—O10—W1	−39.3 (10)
O1^i—Si1—O2—W3	59.5 (11)	O2—W2—O10—W1	−7.3 (9)
O1—Si1—O2—W3	121.5 (11)	O21—W1—O10—W2	−157.1 (10)
O4^i—Si1—O2—W2	−118.4 (11)	O8—W1—O10—W2	102.5 (12)
O4—Si1—O2—W2	58.8 (12)	O7—W1—O10—W2	21 (2)
O3^i—Si1—O2—W2	178.9 (8)	O5—W1—O10—W2	−56.2 (10)
O3—Si1—O2—W2	121.7 (12)	O3—W1—O10—W2	38.3 (10)
O1^i—Si1—O2—W2	−60.7 (12)	O2—W1—O10—W2	7.3 (9)
O1—Si1—O2—W2	1.3 (8)	O14—W6—O11—W2	−154.8 (13)
W2—O1—O2—Si1	178.8 (8)	O12—W6—O11—W2	−52.5 (15)
W4—O1—O2—Si1	−100.1 (12)	O12^i—W6—O11—W2	103.4 (15)
W6—O1—O2—Si1	97.7 (11)	O11^i—W6—O11—W2	25.2 (13)
Si1—O1—O2—O4^i	−48.3 (7)	O1—W6—O11—W2	6.8 (12)
W2—O1—O2—O4^i	130.5 (8)	O1^i—W6—O11—W2	41.6 (15)
W4—O1—O2—O4^i	−148.4 (11)	O14—W6—O12—W4	152.2 (15)
W6—O1—O2—O4^i	49.4 (14)	O12^i—W6—O12—W4	−27.8 (15)
Si1—O1—O2—O3	48.1 (8)	O11^i—W6—O12—W4	−107.2 (17)
W2—O1—O2—O3	−133.1 (9)	O11—W6—O12—W4	51.1 (17)
W4—O1—O2—O3	−52.0 (15)	O1—W6—O12—W4	−7.8 (13)
W6—O1—O2—O3	145.8 (10)	O1^i—W6—O12—W4	−45.6 (17)
Si1—O1—O2—W1	110.4 (12)	O15—W4—O13—W7	−152.7 (15)
W2—O1—O2—W1	−70.8 (10)	O12—W4—O13—W7	24 (3)
W4—O1—O2—W1	10.3 (19)	O16—W4—O13—W7	106.7 (17)
W6—O1—O2—W1	−151.9 (8)	O22—W4—O13—W7	−54.5 (17)
Si1—O1—O2—W3	−109.0 (12)	O1—W4—O13—W7	43.1 (16)
W2—O1—O2—W3	69.8 (11)	O4—W4—O13—W7	5.5 (14)
W4—O1—O2—W3	151.0 (9)	O19—W2—O16—W4	−158.6 (11)
W6—O1—O2—W3	−11.2 (19)	O10—W2—O16—W4	99.8 (12)
Si1—O1—O2—W2	−178.8 (8)	O6—W2—O16—W4	20 (2)
W4—O1—O2—W2	81.2 (11)	O11—W2—O16—W4	−57.5 (13)
W6—O1—O2—W2	−81.1 (10)	O1—W2—O16—W4	4.3 (10)
O2^i—Si1—O3—O2	179.8 (6)	O2—W2—O16—W4	35.7 (12)
O4^i—Si1—O3—O2	−57.2 (9)	O18—W5—O20—W7	−157.9 (15)
O4—Si1—O3—O2	121.3 (9)	O20^i—W5—O20—W7	22.1 (15)
O3^i—Si1—O3—O2	−124.7 (11)	O7^i—W5—O20—W7	101.8 (17)
O1—Si1—O3—O2	56.9 (9)	O7—W5—O20—W7	−57.7 (17)
O2—Si1—O3—W1	−0.7 (9)	O3—W5—O20—W7	2.8 (14)
O2^i—Si1—O3—W1	179.1 (9)	O3^i—W5—O20—W7	39.5 (17)
O4^i—Si1—O3—W1	−57.9 (11)	O9—W7—O20—W5	157.6 (15)
O4—Si1—O3—W1	120.7 (11)	O8—W7—O20—W5	57.2 (17)
O3^i—Si1—O3—W1	−125.4 (14)	O13—W7—O20—W5	−18 (3)
O1—Si1—O3—W1	56.2 (11)	O17—W7—O20—W5	−99.9 (17)
O2—Si1—O3—W5	124.7 (11)	O3—W7—O20—W5	−2.8 (13)
O2^i—Si1—O3—W5	−55.5 (11)	O4—W7—O20—W5	−39.5 (17)
O4^i—Si1—O3—W5	67.5 (10)	Cr1—O26—C1—O25	−18 (2)
O4—Si1—O3—W5	−113.9 (10)	Cr2—O25—C1—O26	−4 (2)
O3^i—Si1—O3—W5	−0.001 (1)	Cr2—O27—C2—O28	−8 (2)
O1—Si1—O3—W5	−178.4 (7)	Cr1—O28—C2—O27	−14.9 (19)
O2—Si1—O3—W7	−121.3 (11)	Cr3—O29—C3—O30	−11 (2)
O2^i—Si1—O3—W7	58.5 (11)	Cr1—O30—C3—O29	−8 (2)
O4^i—Si1—O3—W7	−178.5 (8)	Cr3—O31—C4—O32	−2 (2)
O4—Si1—O3—W7	0.1 (8)	Cr1—O32—C4—O31	−15 (2)
O3^i—Si1—O3—W7	114.0 (12)	Cr2—O33—C5—O34	−13 (2)
O1—Si1—O3—W7	−64.4 (10)	Cr3—O34—C5—O33	−17 (2)
O4^i—O2—O3—Si1	48.2 (7)	Cr2—O35—C6—O36	−7 (2)
O1—O2—O3—Si1	−48.3 (8)	Cr3—O36—C6—O35	−17 (2)
W1—O2—O3—Si1	−179.4 (8)	C11—N1—C7—C8	1.5 (19)
W3—O2—O3—Si1	109.6 (12)	Cr1—N1—C7—C8	−179.3 (10)
W2—O2—O3—Si1	−110.2 (12)	N1—C7—C8—C9	−1 (2)
Si1—O2—O3—W1	179.4 (8)	C7—C8—C9—C10	1 (2)
O4^i—O2—O3—W1	−132.4 (8)	C7—C8—C9—C12	−177.6 (14)
O1—O2—O3—W1	131.1 (9)	C8—C9—C10—C11	−2 (2)
W3—O2—O3—W1	−70.9 (10)	C12—C9—C10—C11	177.4 (14)
W2—O2—O3—W1	69.2 (11)	C7—N1—C11—C10	−2 (2)
Si1—O2—O3—W5	−99.5 (12)	Cr1—N1—C11—C10	179.0 (11)
O4^i—O2—O3—W5	−51.3 (15)	C9—C10—C11—N1	2 (2)
O1—O2—O3—W5	−147.8 (11)	C10—C9—C12—C13	−109.1 (16)
W1—O2—O3—W5	81.1 (11)	C8—C9—C12—C13	69.8 (18)
W3—O2—O3—W5	10 (2)	C18—N2—C14—C15	−7 (2)
W2—O2—O3—W5	150.3 (9)	Cr3—N2—C14—C15	166.6 (11)
Si1—O2—O3—W7	98.3 (11)	N2—C14—C15—C16	2 (2)
O4^i—O2—O3—W7	146.5 (10)	C14—C15—C16—C17	3 (2)
O1—O2—O3—W7	50.0 (14)	C14—C15—C16—C19	−175.0 (15)
W1—O2—O3—W7	−81.2 (10)	C15—C16—C17—C18	−5 (2)
W3—O2—O3—W7	−152.1 (8)	C19—C16—C17—C18	173.6 (16)
W2—O2—O3—W7	−12.0 (19)	C14—N2—C18—C17	6 (2)
O2—Si1—O4—O2^i	−179.5 (12)	Cr3—N2—C18—C17	−167.7 (12)
O3^i—Si1—O4—O2^i	57.1 (9)	C16—C17—C18—N2	0 (2)
O3—Si1—O4—O2^i	121.9 (9)	C17—C16—C19—C20	−87 (2)
O1^i—Si1—O4—O2^i	−57.2 (9)	C15—C16—C19—C20	91 (2)
O1—Si1—O4—O2^i	−123.9 (9)	C25—N3—C21—C22	−3 (2)
O2—Si1—O4—W3^i	178.5 (8)	Cr2—N3—C21—C22	171.9 (12)
O2^i—Si1—O4—W3^i	−1.9 (9)	N3—C21—C22—C23	1 (2)
O3^i—Si1—O4—W3^i	55.2 (11)	C21—C22—C23—C24	1 (2)
O3—Si1—O4—W3^i	120.0 (10)	C21—C22—C23—C26	−178.2 (16)
O1^i—Si1—O4—W3^i	−59.1 (11)	C22—C23—C24—C25	−2 (2)
O1—Si1—O4—W3^i	−125.8 (11)	C26—C23—C24—C25	177.6 (15)
O2—Si1—O4—W4	−54.4 (11)	C21—N3—C25—C24	2 (2)
O2^i—Si1—O4—W4	125.2 (11)	Cr2—N3—C25—C24	−172.6 (12)
O3^i—Si1—O4—W4	−177.7 (8)	C23—C24—C25—N3	0 (2)
O3—Si1—O4—W4	−112.9 (10)	C22—C23—C26—C27	53 (3)
O1^i—Si1—O4—W4	68.0 (10)	C24—C23—C26—C27	−126 (2)

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