Hexakis(dimethyl­ammonium) di-μ6-oxido-tetra-μ3-oxido-tetra­deca-μ2-oxido-octa­oxidodeca­vanadate(V) monohydrate

Wang, S.; Lu, L.; Feng, S.; Zhu, M.

doi:10.1107/S1600536810016442

metal-organic compounds

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ISSN: 2056-9890

Volume 66| Part 6| June 2010| Page m632

https://doi.org/10.1107/S1600536810016442

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Hexakis(dimethylammonium) di-μ₆-oxido-tetra-μ₃-oxido-tetradeca-μ₂-oxido-octaoxidodecavanadate(V) monohydrate

Sulian Wang,^a Liping Lu,^a ^* Sisi Feng ^a and Miaoli Zhu ^a ^*

^aInstitute of Molecular Science, Key Laboratory of Chemical Biology and Molecular Engineering of the Education Ministry, Shanxi University, Taiyuan, Shanxi 030006, People's Republic of China
^*Correspondence e-mail: luliping@sxu.edu.cn, miaoli@sxu.edu.cn

(Received 27 April 2010; accepted 5 May 2010; online 8 May 2010)

In the title compound, (C₂H₈N)₆[V₁₀O₂₈]·H₂O, the [V₁₀O₂₈]⁶⁻ polymetalate anion has crystallographic mirror symmetry with six V atoms and 12 O atoms lying on the mirror plane. Each of the V^V atoms adopts a distorted octahedral geometry. Eight terminal O atoms are bonded to V^V atoms with double bonds and the others act as bridging atoms. In the crystal structure, a network of N—H⋯O and O—H⋯O hydrogen bonds helps to establish the packing.

Related literature

For the biological activity of oxovanadates and vanadium complexes, see: Pacigová et al. (2007 ); Yuan, Lu, Gao et al. (2009 ). For a related structure, see: Yuan, Lu, Zhu et al. (2009 ).

Experimental

Crystal data

(C₂H₈N)₆[V₁₀O₂₈]·H₂O
M_r = 1251.98
Orthorhombic, C m c a
a = 13.6149 (18) Å
b = 18.629 (3) Å
c = 30.235 (2) Å
V = 7668.5 (16) Å³
Z = 8
Mo Kα radiation
μ = 2.42 mm⁻¹
T = 203 K
0.35 × 0.11 × 0.05 mm

Data collection

Bruker SMART 1K CCD diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ) T_min = 0.484, T_max = 0.888
18064 measured reflections
3464 independent reflections
2951 reflections with I > 2σ(I)
R_int = 0.078

Refinement

R[F² > 2σ(F²)] = 0.096
wR(F²) = 0.177
S = 1.26
3464 reflections
296 parameters
6 restraints
H-atom parameters constrained
Δρ_max = 1.70 e Å⁻³
Δρ_min = −0.83 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O21—H21B⋯O10ⁱ	0.85	2.30	2.950 (19)	133
O21—H21A⋯O16	0.85	2.26	3.101 (18)	171
N4—H4D⋯O5ⁱⁱ	0.91	1.77	2.673 (8)	170
N4—H4E⋯O5	0.91	1.77	2.673 (8)	170
N2—H2D⋯O6	0.91	1.88	2.759 (10)	162
N2—H2E⋯O6ⁱⁱⁱ	0.91	2.22	2.986 (10)	141
N2—H2E⋯O7ⁱⁱⁱ	0.91	2.05	2.812 (9)	140
N1—H1A⋯O8^iv	0.91	1.86	2.732 (10)	161
N1—H1B⋯O3	0.91	1.79	2.674 (10)	164
Symmetry codes: (i) $[x, y-{\script{1\over 2}}, -z+{\script{3\over 2}}]$ ; (ii) $[-x+{\script{3\over 2}}, y, -z+{\script{3\over 2}}]$ ; (iii) $[-x+{\script{3\over 2}}, -y+{\script{3\over 2}}, -z+2]$ ; (iv) $[-x+{\script{3\over 2}}, y+{\script{1\over 2}}, z]$ .

Data collection: SMART (Bruker, 2007 ); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT (Bruker, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536810016442/hy2304sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536810016442/hy2304Isup2.hkl

checkCIF report

Comment top

Oxovanadates(V) and peroxovanadium compounds are of great interest in biochemistry and medicine because of their diverse biological activites (Pacigová et al., 2007). Of them, decavanadates have shown high affinity for selected kinases and phosphorylase and have been used to facilitate crystallization of proteins. Vanadium complexes can inhibit effectively activity of protein tyrosine phosphatase (Yuan, Lu, Gao et al., 2009). In our previous work, (C₅H₇N₂)₆[V₁₀O₂₈].2H₂O was reported (Yuan, Lu, Zhu et al., 2009). Herein, we report the structure of the title compound.

The title compound consists of a [V₁₀O₂₈]^6- polyanion, six dimethylaminium cations and one water molecule (Fig. 1). The polyanion is constructed by ten edge-sharing VO₆ octahedra. Six V atoms and twelve O atoms lie on the mirror plane at x = 1/2. Different coordination O atoms existing in the anion result in differnet V—O bond distances. The V—O(terminal) double bond distances range from 1.551 (10) to 1.576 (6) Å, shorter than those in (C₅H₇N₂)₆[V₁₀O₂₈].2H₂O (Yuan, Lu, Zhu et al., 2009). The V—O(µ₃) single bond distances range from 1.638 (10) to 2.066 (10) Å. The V—O (µ₂) single bond distances range from 1.897 (6) to 1.991 (6)Å. The V—O (µ₆) single bond distances are more longer [2.137 (8) to 2.275 (9)Å].

A three-dimensional supramolecular hydrogen-bonding network is observed in the crystal structure and details are given in Table 1 and Fig. 2.

Related literature top

For the biological activity of oxovanadates and vanadium complexes, see: Pacigová et al. (2007); Yuan, Lu, Gao et al. (2009). For a related structure, see: Yuan, Lu, Zhu et al. (2009).

Experimental top

A mixture containing 1.5 mmol each of VO(acac)₂ (acac = acetylacetone), 1,10-phenanthroline and 2-(2-hydroxylphenyl)benzimidazole in methanol (24 ml) was refluxed for 30 min. Light green precipitate was filtrated and collected. The solid was dissolved in dimethylformamide. The solvent was slowly evaporated for one month and yellow crystals of the title compound were obtained.

Structure description top

A three-dimensional supramolecular hydrogen-bonding network is observed in the crystal structure and details are given in Table 1 and Fig. 2.

For the biological activity of oxovanadates and vanadium complexes, see: Pacigová et al. (2007); Yuan, Lu, Gao et al. (2009). For a related structure, see: Yuan, Lu, Zhu et al. (2009).

Computing details top

Data collection: SMART (Bruker, 2007); cell refinement: SAINT (Bruker, 2007); data reduction: SAINT (Bruker, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top

	Fig. 1. The structure of the title compound. Displacement ellipsoids are drawn at the 30% probability level. [Symmetry codes: (i) 3/2-x, y, 3/2-z; (ii) 1-x, y, z.]
	Fig. 2. The crystal packing in the title compound. Hydrogen bonds are indicated by dashed lines. [Red, O; green, V; blue, N; gray, C and green open circle, H.]

Hexakis(dimethylammonium) di-µ₆-oxido-tetra-µ₃-oxido- tetradeca-µ₂-oxido-octaoxidodecavanadate(V) monohydrate top

Crystal data top

(C₂H₈N)₆[V₁₀O₂₈]·H₂O	F(000) = 5008
M_r = 1251.98	D_x = 2.169 Mg m⁻³
Orthorhombic, Cmca	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2bc 2	Cell parameters from 1649 reflections
a = 13.6149 (18) Å	θ = 2.3–22.0°
b = 18.629 (3) Å	µ = 2.42 mm⁻¹
c = 30.235 (2) Å	T = 203 K
V = 7668.5 (16) Å³	Needle, yellow
Z = 8	0.35 × 0.11 × 0.05 mm

Data collection top

Bruker SMART 1K CCD diffractometer	3464 independent reflections
Radiation source: fine-focus sealed tube	2951 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.078
φ and ω scans	θ_max = 25.0°, θ_min = 2.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −15→16
T_min = 0.484, T_max = 0.888	k = −22→22
18064 measured reflections	l = −35→28

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)] = 0.096	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.177	H-atom parameters constrained
S = 1.26	w = 1/[σ²(F_o²) + (0.0331P)² + 151.3848P] where P = (F_o² + 2F_c²)/3
3464 reflections	(Δ/σ)_max = 0.001
296 parameters	Δρ_max = 1.70 e Å⁻³
6 restraints	Δρ_min = −0.83 e Å⁻³

Crystal data top

(C₂H₈N)₆[V₁₀O₂₈]·H₂O	V = 7668.5 (16) Å³
M_r = 1251.98	Z = 8
Orthorhombic, Cmca	Mo Kα radiation
a = 13.6149 (18) Å	µ = 2.42 mm⁻¹
b = 18.629 (3) Å	T = 203 K
c = 30.235 (2) Å	0.35 × 0.11 × 0.05 mm

Data collection top

Bruker SMART 1K CCD diffractometer	3464 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	2951 reflections with I > 2σ(I)
T_min = 0.484, T_max = 0.888	R_int = 0.078
18064 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.096	6 restraints
wR(F²) = 0.177	H-atom parameters constrained
S = 1.26	w = 1/[σ²(F_o²) + (0.0331P)² + 151.3848P] where P = (F_o² + 2F_c²)/3
3464 reflections	Δρ_max = 1.70 e Å⁻³
296 parameters	Δρ_min = −0.83 e Å⁻³

Special details top

Refinement. The structure was phased by direct methods. The space group choice was confirmed by successful convergence of the full-matrix least-squares refinement on F². The Ueq of N3 is large. It is resulted from the severe systematic disorder of N3 atom, which is located at crystallographic mirror symmetry. ISOR instruction was employed to have ellipsoids of site N3 be restraint to more appropriate values. So, 6 restraints were used for anisotropic refinement.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
V1	0.66109 (11)	0.75463 (8)	0.90694 (5)	0.0247 (4)
V2	0.66020 (10)	0.61321 (8)	0.86058 (5)	0.0238 (4)
V3	0.5000	0.86507 (12)	0.89222 (8)	0.0312 (6)
V4	0.5000	0.72904 (12)	0.83754 (7)	0.0236 (5)
V5	0.5000	0.58253 (13)	0.79179 (7)	0.0263 (5)
V6	0.5000	0.78222 (13)	0.97603 (8)	0.0290 (6)
V7	0.5000	0.63836 (11)	0.92977 (7)	0.0197 (5)
V8	0.5000	0.50136 (12)	0.87744 (8)	0.0295 (6)
O1	0.7763 (4)	0.7541 (4)	0.9081 (2)	0.0376 (17)
O2	0.7759 (4)	0.6129 (4)	0.8602 (2)	0.0385 (17)
O3	0.6330 (5)	0.8441 (3)	0.8900 (2)	0.0338 (17)
O4	0.6366 (4)	0.7163 (3)	0.8497 (2)	0.0245 (14)
O5	0.6308 (4)	0.5943 (3)	0.8034 (2)	0.0266 (14)
O6	0.6325 (4)	0.7704 (3)	0.9642 (2)	0.0269 (15)
O7	0.6361 (4)	0.6511 (3)	0.91878 (19)	0.0218 (13)
O8	0.6329 (4)	0.5241 (3)	0.8785 (2)	0.0273 (14)
O9	0.5000	0.9456 (5)	0.8775 (4)	0.047 (3)
O10	0.5000	0.8170 (5)	0.8307 (3)	0.035 (2)
O11	0.5000	0.6906 (5)	0.7888 (3)	0.031 (2)
O12	0.5000	0.5657 (6)	0.7412 (3)	0.049 (3)
O13	0.5000	0.8687 (5)	0.9508 (3)	0.034 (2)
O14	0.5000	0.7460 (4)	0.9052 (3)	0.0171 (17)
O15	0.5000	0.6211 (4)	0.8632 (3)	0.0229 (19)
O16	0.5000	0.4958 (5)	0.8191 (3)	0.031 (2)
O17	0.5000	0.8004 (5)	1.0263 (3)	0.041 (3)
O18	0.5000	0.6771 (5)	0.9790 (3)	0.027 (2)
O19	0.5000	0.5509 (5)	0.9370 (3)	0.030 (2)
O20	0.5000	0.4213 (5)	0.8915 (4)	0.048 (3)
O21	0.5000	0.3555 (9)	0.7640 (5)	0.119 (6)
H21A	0.5000	0.3911	0.7816	0.119*
H21B	0.5000	0.3717	0.7377	0.119*
N1	0.7294 (6)	0.9384 (4)	0.8394 (3)	0.037 (2)
H1A	0.7635	0.9719	0.8551	0.044*
H1B	0.6913	0.9134	0.8588	0.044*
C1	0.6667 (9)	0.9744 (7)	0.8076 (4)	0.058 (3)
H1C	0.7061	1.0065	0.7895	0.087*
H1D	0.6170	1.0019	0.8231	0.087*
H1E	0.6353	0.9390	0.7888	0.087*
C2	0.7972 (10)	0.8902 (7)	0.8190 (5)	0.066 (4)
H2A	0.7615	0.8509	0.8054	0.099*
H2B	0.8419	0.8714	0.8411	0.099*
H2C	0.8343	0.9156	0.7965	0.099*
N2	0.7745 (6)	0.8610 (4)	0.9977 (3)	0.040 (2)
H2D	0.7384	0.8266	0.9839	0.048*
H2E	0.8145	0.8386	1.0175	0.048*
C3	0.8341 (10)	0.8966 (7)	0.9655 (4)	0.063 (4)
H3A	0.7924	0.9230	0.9452	0.094*
H3B	0.8720	0.8613	0.9492	0.094*
H3C	0.8784	0.9296	0.9803	0.094*
C4	0.7104 (10)	0.9067 (7)	1.0209 (4)	0.061 (4)
H4A	0.7484	0.9405	1.0383	0.092*
H4B	0.6691	0.8784	1.0403	0.092*
H4C	0.6697	0.9327	1.0000	0.092*
N3	0.0000	0.6868 (16)	0.8841 (10)	0.177 (12)
H3D	−0.0530	0.6904	0.9023	0.177*	0.50
H3E	0.0530	0.6904	0.9023	0.177*	0.50
C5	0.0000	0.7485 (9)	0.8640 (6)	0.052 (4)
H5A	0.0665	0.7669	0.8626	0.052*	0.50
H5B	−0.0412	0.7821	0.8800	0.052*	0.50
H5C	−0.0254	0.7422	0.8343	0.052*	0.50
C6	0.0000	0.6194 (9)	0.8737 (6)	0.060 (5)
H6A	−0.0588	0.5967	0.8852	0.060*	0.50
H6B	0.0576	0.5963	0.8861	0.060*	0.50
H6C	0.0000	0.6147	0.8417	0.060*
N4	0.7500	0.6685 (6)	0.7500	0.040 (3)
H4D	0.7849	0.6396	0.7315	0.047*	0.50
H4E	0.7151	0.6396	0.7685	0.047*	0.50
C7	0.8174 (10)	0.7099 (7)	0.7757 (4)	0.066 (4)
H7A	0.8489	0.7453	0.7569	0.099*
H7B	0.8668	0.6785	0.7883	0.099*
H7C	0.7822	0.7341	0.7993	0.099*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
V1	0.0161 (8)	0.0257 (8)	0.0322 (9)	−0.0038 (7)	−0.0006 (7)	−0.0023 (7)
V2	0.0152 (7)	0.0285 (8)	0.0277 (9)	0.0032 (6)	−0.0005 (7)	−0.0034 (7)
V3	0.0291 (13)	0.0183 (12)	0.0462 (16)	0.000	0.000	0.0019 (11)
V4	0.0233 (12)	0.0268 (12)	0.0207 (12)	0.000	0.000	0.0065 (10)
V5	0.0235 (12)	0.0358 (13)	0.0198 (12)	0.000	0.000	−0.0055 (10)
V6	0.0265 (12)	0.0349 (13)	0.0255 (13)	0.000	0.000	−0.0098 (11)
V7	0.0175 (10)	0.0250 (11)	0.0167 (11)	0.000	0.000	0.0037 (9)
V8	0.0340 (13)	0.0195 (11)	0.0351 (14)	0.000	0.000	0.0020 (10)
O1	0.018 (3)	0.044 (4)	0.051 (5)	−0.008 (3)	0.001 (3)	−0.006 (4)
O2	0.017 (3)	0.057 (5)	0.041 (4)	0.006 (3)	−0.003 (3)	−0.002 (4)
O3	0.031 (4)	0.027 (3)	0.044 (4)	−0.014 (3)	−0.001 (3)	0.004 (3)
O4	0.020 (3)	0.026 (3)	0.027 (3)	0.000 (3)	−0.001 (3)	0.003 (3)
O5	0.025 (3)	0.025 (3)	0.030 (4)	−0.003 (3)	0.007 (3)	−0.006 (3)
O6	0.020 (3)	0.033 (4)	0.028 (3)	−0.006 (3)	−0.003 (3)	−0.009 (3)
O7	0.020 (3)	0.024 (3)	0.021 (3)	0.000 (3)	−0.008 (3)	−0.004 (3)
O8	0.023 (3)	0.023 (3)	0.035 (4)	0.011 (3)	−0.002 (3)	0.000 (3)
O9	0.042 (6)	0.035 (6)	0.063 (8)	0.000	0.000	0.001 (5)
O10	0.037 (6)	0.032 (5)	0.035 (6)	0.000	0.000	0.009 (4)
O11	0.021 (5)	0.035 (5)	0.035 (6)	0.000	0.000	0.010 (4)
O12	0.052 (7)	0.071 (8)	0.023 (6)	0.000	0.000	−0.014 (5)
O13	0.036 (5)	0.030 (5)	0.038 (6)	0.000	0.000	−0.012 (5)
O14	0.016 (4)	0.012 (4)	0.023 (5)	0.000	0.000	0.004 (4)
O15	0.019 (4)	0.028 (5)	0.022 (5)	0.000	0.000	0.006 (4)
O16	0.035 (5)	0.034 (5)	0.024 (5)	0.000	0.000	−0.003 (4)
O17	0.039 (6)	0.050 (6)	0.034 (6)	0.000	0.000	−0.018 (5)
O18	0.023 (5)	0.041 (5)	0.017 (5)	0.000	0.000	−0.004 (4)
O19	0.033 (5)	0.025 (5)	0.033 (6)	0.000	0.000	0.008 (4)
O20	0.053 (7)	0.029 (6)	0.062 (8)	0.000	0.000	−0.004 (5)
O21	0.172 (18)	0.101 (13)	0.084 (13)	0.000	0.000	−0.009 (10)
N1	0.045 (5)	0.030 (4)	0.036 (5)	−0.017 (4)	−0.001 (4)	−0.004 (4)
C1	0.066 (8)	0.060 (8)	0.048 (7)	−0.017 (7)	−0.014 (7)	−0.009 (6)
C2	0.069 (9)	0.055 (8)	0.074 (10)	0.017 (7)	0.000 (7)	−0.015 (7)
N2	0.047 (5)	0.035 (5)	0.039 (5)	−0.013 (4)	−0.029 (5)	0.011 (4)
C3	0.080 (10)	0.059 (8)	0.049 (8)	−0.018 (7)	−0.014 (7)	0.017 (6)
C4	0.064 (9)	0.052 (7)	0.068 (9)	−0.013 (7)	−0.022 (7)	−0.008 (7)
N3	0.207 (15)	0.163 (14)	0.160 (15)	0.000	0.000	−0.003 (10)
C5	0.036 (9)	0.045 (10)	0.075 (13)	0.000	0.000	0.003 (10)
C6	0.057 (11)	0.045 (10)	0.078 (14)	0.000	0.000	−0.042 (10)
N4	0.044 (7)	0.035 (7)	0.040 (7)	0.000	0.019 (6)	0.000
C7	0.068 (9)	0.065 (8)	0.064 (9)	−0.013 (7)	0.032 (7)	−0.031 (7)

Geometric parameters (Å, º) top

V1—O1	1.569 (6)	V8—O15	2.272 (9)
V1—O3	1.784 (7)	O21—H21A	0.8500
V1—O6	1.799 (6)	O21—H21B	0.8500
V1—O4	1.902 (6)	N1—C2	1.428 (13)
V1—O7	1.991 (6)	N1—C1	1.452 (14)
V1—O14	2.200 (2)	N1—H1A	0.9100
V2—O2	1.576 (6)	N1—H1B	0.9100
V2—O8	1.785 (6)	C1—H1C	0.9700
V2—O5	1.810 (6)	C1—H1D	0.9700
V2—O7	1.924 (6)	C1—H1E	0.9700
V2—O4	1.975 (6)	C2—H2A	0.9700
V2—O15	2.188 (2)	C2—H2B	0.9700
V3—O9	1.565 (10)	C2—H2C	0.9700
V3—O13	1.771 (10)	N2—C4	1.406 (14)
V3—O3	1.854 (7)	N2—C3	1.431 (14)
V3—O10	2.066 (10)	N2—H2D	0.9100
V3—O14	2.254 (8)	N2—H2E	0.9100
V4—O11	1.638 (10)	C3—H3A	0.9700
V4—O10	1.651 (9)	C3—H3B	0.9700
V4—O4	1.910 (6)	C3—H3C	0.9700
V4—O14	2.071 (8)	C4—H4A	0.9700
V4—O15	2.155 (8)	C4—H4B	0.9700
V5—O12	1.561 (10)	C4—H4C	0.9700
V5—O16	1.814 (9)	N3—C6	1.29 (3)
V5—O5	1.829 (6)	N3—C5	1.30 (3)
V5—O11	2.015 (9)	N3—H3D	0.9100
V5—O15	2.275 (9)	N3—H3E	0.9100
V6—O17	1.556 (10)	C5—H5A	0.9700
V6—O13	1.782 (10)	C5—H5B	0.9700
V6—O6	1.852 (6)	C5—H5C	0.9700
V6—O18	1.961 (9)	C6—H6A	0.9700
V6—O14	2.244 (8)	C6—H6B	0.9700
V7—O19	1.643 (9)	C6—H6C	0.9700
V7—O18	1.655 (8)	N4—C7ⁱ	1.428 (13)
V7—O7	1.897 (6)	N4—C7	1.428 (13)
V7—O15	2.039 (9)	N4—H4D	0.9100
V7—O14	2.137 (8)	N4—H4E	0.9100
V8—O20	1.551 (10)	C7—H7A	0.9700
V8—O16	1.766 (9)	C7—H7B	0.9700
V8—O8	1.858 (6)	C7—H7C	0.9700
V8—O19	2.025 (10)

O1—V1—O3	103.1 (3)	O20—V8—O16	102.6 (5)
O1—V1—O6	101.3 (3)	O20—V8—O8	102.41 (19)
O3—V1—O6	94.4 (3)	O16—V8—O8	91.8 (2)
O1—V1—O4	101.1 (3)	O20—V8—O8ⁱⁱ	102.41 (19)
O3—V1—O4	93.0 (3)	O16—V8—O8ⁱⁱ	91.8 (2)
O6—V1—O4	154.0 (3)	O8—V8—O8ⁱⁱ	153.5 (4)
O1—V1—O7	99.3 (3)	O20—V8—O19	101.2 (5)
O3—V1—O7	156.8 (3)	O16—V8—O19	156.2 (4)
O6—V1—O7	87.0 (3)	O8—V8—O19	83.1 (2)
O4—V1—O7	76.7 (2)	O8ⁱⁱ—V8—O19	83.1 (2)
O1—V1—O14	175.5 (3)	O20—V8—O15	175.0 (5)
O3—V1—O14	81.3 (3)	O16—V8—O15	82.4 (4)
O6—V1—O14	79.5 (3)	O8—V8—O15	77.24 (19)
O4—V1—O14	77.1 (3)	O8ⁱⁱ—V8—O15	77.24 (19)
O7—V1—O14	76.3 (3)	O19—V8—O15	73.8 (3)
O2—V2—O8	102.0 (3)	O20—V8—V2ⁱⁱ	134.48 (5)
O2—V2—O5	102.3 (3)	O16—V8—V2ⁱⁱ	82.7 (2)
O8—V2—O5	93.6 (3)	O8—V8—V2ⁱⁱ	122.8 (2)
O2—V2—O7	100.3 (3)	O8ⁱⁱ—V8—V2ⁱⁱ	32.15 (18)
O8—V2—O7	91.6 (3)	O19—V8—V2ⁱⁱ	80.65 (18)
O5—V2—O7	155.2 (3)	O15—V8—V2ⁱⁱ	45.55 (4)
O2—V2—O4	99.5 (3)	V1—O3—V3	113.4 (3)
O8—V2—O4	157.0 (3)	V1—O4—V4	107.4 (3)
O5—V2—O4	89.7 (3)	V1—O4—V2	100.6 (3)
O7—V2—O4	76.6 (2)	V4—O4—V2	108.1 (3)
O2—V2—O15	176.0 (4)	V2—O5—V5	114.9 (3)
O8—V2—O15	81.0 (3)	V1—O6—V6	114.6 (3)
O5—V2—O15	80.1 (3)	V7—O7—V2	106.3 (3)
O7—V2—O15	76.8 (3)	V7—O7—V1	108.7 (3)
O4—V2—O15	77.2 (3)	V2—O7—V1	99.3 (3)
O9—V3—O13	104.4 (5)	V2—O8—V8	114.2 (3)
O9—V3—O3ⁱⁱ	101.1 (2)	V4—O10—V3	108.5 (5)
O13—V3—O3ⁱⁱ	92.5 (2)	V4—O11—V5	113.3 (5)
O9—V3—O3	101.1 (2)	V3—O13—V6	113.2 (5)
O13—V3—O3	92.5 (2)	V4—O14—V7	101.6 (3)
O3ⁱⁱ—V3—O3	155.3 (4)	V4—O14—V1	92.0 (2)
O9—V3—O10	99.1 (5)	V7—O14—V1	93.49 (19)
O13—V3—O10	156.5 (4)	V4—O14—V1ⁱⁱ	92.0 (2)
O3ⁱⁱ—V3—O10	82.9 (2)	V7—O14—V1ⁱⁱ	93.49 (19)
O3—V3—O10	82.9 (2)	V1—O14—V1ⁱⁱ	171.2 (4)
O9—V3—O14	173.5 (5)	V4—O14—V6	171.2 (4)
O13—V3—O14	82.1 (4)	V7—O14—V6	87.2 (3)
O3ⁱⁱ—V3—O14	78.4 (2)	V1—O14—V6	87.5 (2)
O3—V3—O14	78.4 (2)	V1ⁱⁱ—O14—V6	87.5 (2)
O10—V3—O14	74.4 (3)	V4—O14—V3	88.7 (3)
O9—V3—V1ⁱⁱ	133.66 (5)	V7—O14—V3	169.8 (4)
O13—V3—V1ⁱⁱ	83.1 (2)	V1—O14—V3	86.08 (19)
O3ⁱⁱ—V3—V1ⁱⁱ	32.60 (19)	V1ⁱⁱ—O14—V3	86.08 (19)
O3—V3—V1ⁱⁱ	124.5 (2)	V6—O14—V3	82.5 (3)
O10—V3—V1ⁱⁱ	80.70 (18)	V7—O15—V4	102.0 (4)
O14—V3—V1ⁱⁱ	46.22 (4)	V7—O15—V2ⁱⁱ	92.6 (2)
O11—V4—O10	108.7 (5)	V4—O15—V2ⁱⁱ	92.9 (2)
O11—V4—O4	96.8 (2)	V7—O15—V2	92.6 (2)
O10—V4—O4	98.5 (2)	V4—O15—V2	92.9 (2)
O11—V4—O4ⁱⁱ	96.8 (2)	V2ⁱⁱ—O15—V2	171.3 (5)
O10—V4—O4ⁱⁱ	98.5 (2)	V7—O15—V8	88.1 (3)
O4—V4—O4ⁱⁱ	153.5 (4)	V4—O15—V8	169.8 (4)
O11—V4—O14	162.8 (4)	V2ⁱⁱ—O15—V8	86.6 (2)
O10—V4—O14	88.5 (4)	V2—O15—V8	86.6 (2)
O4—V4—O14	80.13 (19)	V7—O15—V5	170.7 (4)
O4ⁱⁱ—V4—O14	80.13 (19)	V4—O15—V5	87.3 (3)
O11—V4—O15	85.2 (4)	V2ⁱⁱ—O15—V5	86.8 (2)
O10—V4—O15	166.1 (4)	V2—O15—V5	86.8 (2)
O4—V4—O15	79.34 (19)	V8—O15—V5	82.5 (3)
O4ⁱⁱ—V4—O15	79.34 (19)	V8—O16—V5	113.7 (5)
O14—V4—O15	77.7 (3)	V7—O18—V6	113.2 (5)
O11—V4—V1ⁱⁱ	133.00 (8)	V7—O19—V8	109.4 (5)
O10—V4—V1ⁱⁱ	86.1 (2)	H21A—O21—H21B	108.0
O4—V4—V1ⁱⁱ	125.6 (2)	C2—N1—C1	112.5 (9)
O4ⁱⁱ—V4—V1ⁱⁱ	36.19 (19)	C2—N1—H1A	109.1
O14—V4—V1ⁱⁱ	45.69 (4)	C1—N1—H1A	109.1
O15—V4—V1ⁱⁱ	84.21 (17)	C2—N1—H1B	109.1
O12—V5—O16	105.5 (5)	C1—N1—H1B	109.1
O12—V5—O5ⁱⁱ	102.2 (2)	H1A—N1—H1B	107.8
O16—V5—O5ⁱⁱ	91.1 (2)	N1—C1—H1C	109.5
O12—V5—O5	102.2 (2)	N1—C1—H1D	109.5
O16—V5—O5	91.1 (2)	H1C—C1—H1D	109.5
O5ⁱⁱ—V5—O5	153.9 (4)	N1—C1—H1E	109.5
O12—V5—O11	99.0 (5)	H1C—C1—H1E	109.5
O16—V5—O11	155.5 (4)	H1D—C1—H1E	109.5
O5ⁱⁱ—V5—O11	83.6 (2)	N1—C2—H2A	109.5
O5—V5—O11	83.6 (2)	N1—C2—H2B	109.5
O12—V5—O15	173.2 (5)	H2A—C2—H2B	109.5
O16—V5—O15	81.3 (3)	N1—C2—H2C	109.5
O5ⁱⁱ—V5—O15	77.3 (2)	H2A—C2—H2C	109.5
O5—V5—O15	77.3 (2)	H2B—C2—H2C	109.5
O11—V5—O15	74.2 (3)	C4—N2—C3	114.2 (10)
O12—V5—V2ⁱⁱ	134.56 (5)	C4—N2—H2D	108.7
O16—V5—V2ⁱⁱ	81.8 (2)	C3—N2—H2D	108.7
O5ⁱⁱ—V5—V2ⁱⁱ	32.34 (19)	C4—N2—H2E	108.7
O5—V5—V2ⁱⁱ	122.7 (2)	C3—N2—H2E	108.7
O11—V5—V2ⁱⁱ	81.0 (2)	H2D—N2—H2E	107.6
O15—V5—V2ⁱⁱ	45.40 (4)	N2—C3—H3A	109.5
O17—V6—O13	102.8 (5)	N2—C3—H3B	109.5
O17—V6—O6ⁱⁱ	102.4 (2)	H3A—C3—H3B	109.5
O13—V6—O6ⁱⁱ	91.4 (2)	N2—C3—H3C	109.5
O17—V6—O6	102.4 (2)	H3A—C3—H3C	109.5
O13—V6—O6	91.4 (2)	H3B—C3—H3C	109.5
O6ⁱⁱ—V6—O6	153.8 (4)	N2—C4—H4A	109.5
O17—V6—O18	99.9 (5)	N2—C4—H4B	109.5
O13—V6—O18	157.3 (4)	H4A—C4—H4B	109.5
O6ⁱⁱ—V6—O18	83.7 (2)	N2—C4—H4C	109.5
O6—V6—O18	83.7 (2)	H4A—C4—H4C	109.5
O17—V6—O14	175.1 (5)	H4B—C4—H4C	109.5
O13—V6—O14	82.1 (4)	C6—N3—C5	138 (3)
O6ⁱⁱ—V6—O14	77.30 (19)	C6—N3—H3D	102.6
O6—V6—O14	77.30 (19)	C5—N3—H3D	102.5
O18—V6—O14	75.1 (3)	C6—N3—H3E	102.6
O17—V6—V1ⁱⁱ	134.43 (4)	C5—N3—H3E	102.5
O13—V6—V1ⁱⁱ	81.9 (2)	H3D—N3—H3E	105.0
O6ⁱⁱ—V6—V1ⁱⁱ	32.18 (19)	N3—C5—H5A	109.5
O6—V6—V1ⁱⁱ	123.0 (2)	N3—C5—H5B	109.8
O18—V6—V1ⁱⁱ	82.20 (18)	H5A—C5—H5B	109.5
O14—V6—V1ⁱⁱ	45.67 (4)	N3—C5—H5C	109.1
O19—V7—O18	108.1 (5)	H5A—C5—H5C	109.5
O19—V7—O7ⁱⁱ	98.49 (19)	H5B—C5—H5C	109.5
O18—V7—O7ⁱⁱ	95.91 (19)	N3—C6—H6A	109.6
O19—V7—O7	98.49 (19)	N3—C6—H6B	109.6
O18—V7—O7	95.91 (19)	H6A—C6—H6B	109.5
O7ⁱⁱ—V7—O7	155.1 (4)	N3—C6—H6C	109.3
O19—V7—O15	88.6 (4)	H6A—C6—H6C	108.6
O18—V7—O15	163.2 (4)	H6B—C6—H6C	110.3
O7ⁱⁱ—V7—O15	81.19 (18)	C7ⁱ—N4—C7	114.6 (14)
O7—V7—O15	81.19 (18)	C7ⁱ—N4—H4D	108.6
O19—V7—O14	167.4 (4)	C7—N4—H4D	108.6
O18—V7—O14	84.5 (4)	C7ⁱ—N4—H4E	108.6
O7ⁱⁱ—V7—O14	79.73 (18)	C7—N4—H4E	108.6
O7—V7—O14	79.73 (18)	H4D—N4—H4E	107.6
O15—V7—O14	78.8 (3)	N4—C7—H7A	109.5
O19—V7—V2ⁱⁱ	86.5 (2)	N4—C7—H7B	109.5
O18—V7—V2ⁱⁱ	133.03 (8)	H7A—C7—H7B	109.5
O7ⁱⁱ—V7—V2ⁱⁱ	37.15 (17)	N4—C7—H7C	109.5
O7—V7—V2ⁱⁱ	126.58 (19)	H7A—C7—H7C	109.5
O15—V7—V2ⁱⁱ	45.60 (4)	H7B—C7—H7C	109.5
O14—V7—V2ⁱⁱ	84.63 (16)

O1—V1—O3—V3	−172.9 (4)	O3—V3—O13—V6	−77.9 (2)
O6—V1—O3—V3	−70.1 (4)	O11—V4—O14—V1	94.0 (2)
O4—V1—O3—V3	85.0 (4)	O10—V4—O14—V1	−86.0 (2)
O7—V1—O3—V3	22.6 (9)	O4—V4—O14—V1	12.8 (2)
O14—V1—O3—V3	8.6 (4)	O15—V4—O14—V1	94.0 (2)
O9—V3—O3—V1	178.2 (5)	O11—V4—O14—V1ⁱⁱ	−94.0 (2)
O13—V3—O3—V1	73.0 (4)	O10—V4—O14—V1ⁱⁱ	86.0 (2)
O3ⁱⁱ—V3—O3—V1	−28.6 (13)	O4—V4—O14—V1ⁱⁱ	−175.1 (3)
O10—V3—O3—V1	−83.9 (4)	O15—V4—O14—V1ⁱⁱ	−94.0 (2)
O14—V3—O3—V1	−8.4 (4)	O19—V7—O14—V1	−92.7 (2)
V1ⁱⁱ—V3—O3—V1	−10.4 (5)	O18—V7—O14—V1	87.3 (2)
O1—V1—O4—V4	−169.4 (3)	O7ⁱⁱ—V7—O14—V1	−175.7 (3)
O3—V1—O4—V4	−65.5 (3)	O7—V7—O14—V1	−9.8 (3)
O6—V1—O4—V4	41.0 (7)	O15—V7—O14—V1	−92.7 (2)
O7—V1—O4—V4	93.5 (3)	O19—V7—O14—V1ⁱⁱ	92.7 (2)
O14—V1—O4—V4	14.8 (3)	O18—V7—O14—V1ⁱⁱ	−87.3 (2)
O1—V1—O4—V2	77.6 (3)	O7ⁱⁱ—V7—O14—V1ⁱⁱ	9.8 (3)
O3—V1—O4—V2	−178.5 (3)	O7—V7—O14—V1ⁱⁱ	175.7 (3)
O6—V1—O4—V2	−72.1 (7)	O15—V7—O14—V1ⁱⁱ	92.7 (2)
O7—V1—O4—V2	−19.5 (2)	O3—V1—O14—V4	82.1 (3)
O14—V1—O4—V2	−98.2 (3)	O6—V1—O14—V4	178.3 (3)
O11—V4—O4—V1	−178.5 (4)	O4—V1—O14—V4	−13.0 (3)
O10—V4—O4—V1	71.3 (4)	O7—V1—O14—V4	−92.3 (3)
O4ⁱⁱ—V4—O4—V1	−57.9 (9)	O3—V1—O14—V7	−176.2 (3)
O14—V4—O4—V1	−15.6 (3)	O6—V1—O14—V7	−80.0 (3)
O15—V4—O4—V1	−94.8 (3)	O4—V1—O14—V7	88.7 (3)
V1ⁱⁱ—V4—O4—V1	−19.9 (4)	O7—V1—O14—V7	9.4 (3)
O11—V4—O4—V2	−70.7 (4)	O6—V1—O14—V6	7.0 (3)
O10—V4—O4—V2	179.2 (4)	O4—V1—O14—V6	175.7 (3)
O4ⁱⁱ—V4—O4—V2	49.9 (10)	O7—V1—O14—V6	96.5 (3)
O14—V4—O4—V2	92.2 (3)	O3—V1—O14—V3	−6.5 (3)
O15—V4—O4—V2	13.1 (3)	O6—V1—O14—V3	89.7 (3)
V1ⁱⁱ—V4—O4—V2	87.9 (3)	O4—V1—O14—V3	−101.6 (3)
O2—V2—O4—V1	−78.2 (3)	O7—V1—O14—V3	179.2 (3)
O8—V2—O4—V1	80.9 (7)	O6—V6—O14—V7	86.7 (2)
O5—V2—O4—V1	179.4 (3)	O6—V6—O14—V1	−6.9 (2)
O7—V2—O4—V1	20.2 (2)	O6ⁱⁱ—V6—O14—V1ⁱⁱ	6.9 (2)
O15—V2—O4—V1	99.5 (3)	O6—V6—O14—V1ⁱⁱ	−179.6 (3)
O2—V2—O4—V4	169.3 (3)	O3—V3—O14—V4	−85.8 (2)
O8—V2—O4—V4	−31.6 (9)	O3—V3—O14—V7	94.2 (2)
O5—V2—O4—V4	66.9 (3)	O13—V3—O14—V1	−87.9 (2)
O7—V2—O4—V4	−92.3 (3)	O3ⁱⁱ—V3—O14—V1	177.8 (3)
O15—V2—O4—V4	−13.0 (3)	O3—V3—O14—V1	6.3 (3)
O2—V2—O5—V5	174.9 (4)	O10—V3—O14—V1	92.1 (2)
O8—V2—O5—V5	71.8 (4)	O13—V3—O14—V1ⁱⁱ	87.9 (2)
O7—V2—O5—V5	−30.0 (8)	O3ⁱⁱ—V3—O14—V1ⁱⁱ	−6.3 (3)
O4—V2—O5—V5	−85.5 (3)	O3—V3—O14—V1ⁱⁱ	−177.8 (3)
O15—V2—O5—V5	−8.4 (4)	O10—V3—O14—V1ⁱⁱ	−92.1 (2)
O12—V5—O5—V2	−178.8 (5)	O3—V3—O14—V6	94.2 (2)
O16—V5—O5—V2	−72.7 (4)	O7—V7—O15—V2ⁱⁱ	−174.7 (3)
O5ⁱⁱ—V5—O5—V2	22.2 (11)	O14—V7—O15—V2ⁱⁱ	−93.5 (2)
O11—V5—O5—V2	83.3 (4)	O19—V7—O15—V2	−86.5 (2)
O15—V5—O5—V2	8.2 (3)	O18—V7—O15—V2	93.5 (2)
V2ⁱⁱ—V5—O5—V2	8.3 (4)	O7ⁱⁱ—V7—O15—V2	174.7 (3)
O1—V1—O6—V6	175.2 (4)	O7—V7—O15—V2	12.3 (3)
O3—V1—O6—V6	70.9 (4)	O14—V7—O15—V2	93.5 (2)
O4—V1—O6—V6	−35.3 (8)	O4—V4—O15—V7	82.1 (2)
O7—V1—O6—V6	−85.9 (3)	O14—V4—O15—V7	0.0
O14—V1—O6—V6	−9.4 (3)	O11—V4—O15—V2ⁱⁱ	−86.7 (2)
O17—V6—O6—V1	−175.8 (5)	O10—V4—O15—V2ⁱⁱ	93.3 (2)
O13—V6—O6—V1	−72.4 (4)	O4—V4—O15—V2ⁱⁱ	175.4 (3)
O6ⁱⁱ—V6—O6—V1	23.8 (12)	O4ⁱⁱ—V4—O15—V2ⁱⁱ	11.2 (3)
O18—V6—O6—V1	85.4 (4)	O14—V4—O15—V2ⁱⁱ	93.3 (2)
O14—V6—O6—V1	9.3 (3)	V1ⁱⁱ—V4—O15—V2ⁱⁱ	47.5 (2)
O19—V7—O7—V2	72.7 (4)	O11—V4—O15—V2	86.7 (2)
O18—V7—O7—V2	−177.9 (4)	O10—V4—O15—V2	−93.3 (2)
O7ⁱⁱ—V7—O7—V2	−59.9 (9)	O4—V4—O15—V2	−11.2 (3)
O15—V7—O7—V2	−14.6 (3)	O4ⁱⁱ—V4—O15—V2	−175.4 (3)
O14—V7—O7—V2	−94.7 (3)	O14—V4—O15—V2	−93.3 (2)
O19—V7—O7—V1	178.7 (4)	O4—V4—O15—V8	−97.9 (2)
O18—V7—O7—V1	−71.9 (4)	O4—V4—O15—V5	−97.9 (2)
O7ⁱⁱ—V7—O7—V1	46.1 (10)	O8—V2—O15—V7	81.5 (3)
O15—V7—O7—V1	91.5 (3)	O5—V2—O15—V7	176.8 (3)
O14—V7—O7—V1	11.4 (3)	O7—V2—O15—V7	−12.3 (3)
O2—V2—O7—V7	−169.1 (3)	O4—V2—O15—V7	−91.3 (3)
O8—V2—O7—V7	−66.6 (3)	O8—V2—O15—V4	−176.3 (3)
O5—V2—O7—V7	35.6 (7)	O5—V2—O15—V4	−81.0 (3)
O4—V2—O7—V7	93.5 (3)	O7—V2—O15—V4	89.9 (3)
O15—V2—O7—V7	13.8 (3)	O4—V2—O15—V4	10.9 (3)
O2—V2—O7—V1	78.2 (3)	O8—V2—O15—V8	−6.5 (3)
O8—V2—O7—V1	−179.3 (3)	O5—V2—O15—V8	88.8 (3)
O5—V2—O7—V1	−77.1 (7)	O7—V2—O15—V8	−100.3 (3)
O4—V2—O7—V1	−19.2 (2)	O4—V2—O15—V8	−179.2 (3)
O15—V2—O7—V1	−98.9 (3)	O8—V2—O15—V5	−89.2 (3)
O1—V1—O7—V7	169.8 (3)	O5—V2—O15—V5	6.2 (3)
O3—V1—O7—V7	−25.5 (9)	O7—V2—O15—V5	177.0 (3)
O6—V1—O7—V7	68.7 (3)	O4—V2—O15—V5	98.1 (3)
O4—V1—O7—V7	−90.9 (3)	O8—V8—O15—V7	−86.5 (2)
O14—V1—O7—V7	−11.2 (3)	O8ⁱⁱ—V8—O15—V7	86.5 (2)
O1—V1—O7—V2	−79.4 (3)	O8—V8—O15—V4	93.5 (2)
O3—V1—O7—V2	85.3 (7)	O8ⁱⁱ—V8—O15—V4	−93.5 (2)
O6—V1—O7—V2	179.6 (3)	O16—V8—O15—V2ⁱⁱ	87.2 (2)
O4—V1—O7—V2	19.9 (2)	O8—V8—O15—V2ⁱⁱ	−179.2 (3)
O14—V1—O7—V2	99.6 (3)	O8ⁱⁱ—V8—O15—V2ⁱⁱ	−6.3 (3)
O2—V2—O8—V8	−174.0 (4)	O19—V8—O15—V2ⁱⁱ	−92.8 (2)
O5—V2—O8—V8	−70.6 (4)	O16—V8—O15—V2	−87.2 (2)
O7—V2—O8—V8	85.1 (4)	O8—V8—O15—V2	6.3 (3)
O4—V2—O8—V8	27.1 (9)	O8ⁱⁱ—V8—O15—V2	179.2 (3)
O15—V2—O8—V8	8.7 (4)	O19—V8—O15—V2	92.8 (2)
O20—V8—O8—V2	176.6 (5)	O8—V8—O15—V5	93.5 (2)
O16—V8—O8—V2	73.4 (4)	O5—V5—O15—V4	86.9 (2)
O8ⁱⁱ—V8—O8—V2	−24.1 (12)	O16—V5—O15—V2ⁱⁱ	−87.0 (2)
O19—V8—O8—V2	−83.3 (4)	O5—V5—O15—V2ⁱⁱ	179.9 (3)
O15—V8—O8—V2	−8.5 (3)	O16—V5—O15—V2	87.0 (2)
O4—V4—O10—V3	−79.8 (2)	O5—V5—O15—V2	−6.1 (3)
O3ⁱⁱ—V3—O10—V4	−79.9 (2)	O11—V5—O15—V2	−93.0 (2)
O3—V3—O10—V4	79.9 (2)	O5—V5—O15—V8	−93.1 (2)
O5—V5—O11—V4	−78.6 (2)	O6—V6—O18—V7	−78.5 (2)
O15—V5—O11—V4	0.0	V1ⁱⁱ—V6—O18—V7	46.10 (4)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O21—H21B···O10ⁱⁱⁱ	0.85	2.30	2.950 (19)	133
O21—H21A···O16	0.85	2.26	3.101 (18)	171
N4—H4D···O5ⁱ	0.91	1.77	2.673 (8)	170
N4—H4E···O5	0.91	1.77	2.673 (8)	170
N2—H2D···O6	0.91	1.88	2.759 (10)	162
N2—H2E···O6^iv	0.91	2.22	2.986 (10)	141
N2—H2E···O7^iv	0.91	2.05	2.812 (9)	140
N1—H1A···O8^v	0.91	1.86	2.732 (10)	161
N1—H1B···O3	0.91	1.79	2.674 (10)	164

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

Experimental details

Crystal data
Chemical formula	(C₂H₈N)₆[V₁₀O₂₈]·H₂O
M_r	1251.98
Crystal system, space group	Orthorhombic, Cmca
Temperature (K)	203
a, b, c (Å)	13.6149 (18), 18.629 (3), 30.235 (2)
V (Å³)	7668.5 (16)
Z	8
Radiation type	Mo Kα
µ (mm⁻¹)	2.42
Crystal size (mm)	0.35 × 0.11 × 0.05

Data collection
Diffractometer	Bruker SMART 1K CCD
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.484, 0.888
No. of measured, independent and observed [I > 2σ(I)] reflections	18064, 3464, 2951
R_int	0.078
(sin θ/λ)_max (Å⁻¹)	0.595

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.096, 0.177, 1.26
No. of reflections	3464
No. of parameters	296
No. of restraints	6
H-atom treatment	H-atom parameters constrained
	w = 1/[σ²(F_o²) + (0.0331P)² + 151.3848P] where P = (F_o² + 2F_c²)/3
Δρ_max, Δρ_min (e Å⁻³)	1.70, −0.83

Computer programs: SMART (Bruker, 2007), SAINT (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O21—H21B···O10ⁱ	0.85	2.30	2.950 (19)	133
O21—H21A···O16	0.85	2.26	3.101 (18)	171
N4—H4D···O5ⁱⁱ	0.91	1.77	2.673 (8)	170
N4—H4E···O5	0.91	1.77	2.673 (8)	170
N2—H2D···O6	0.91	1.88	2.759 (10)	162
N2—H2E···O6ⁱⁱⁱ	0.91	2.22	2.986 (10)	141
N2—H2E···O7ⁱⁱⁱ	0.91	2.05	2.812 (9)	140
N1—H1A···O8^iv	0.91	1.86	2.732 (10)	161
N1—H1B···O3	0.91	1.79	2.674 (10)	164

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

Acknowledgements

MZ acknowledges the National Natural Science Foundation of China (No. 20471033) and the Natural Science Foundation of Shanxi Province (No. 2010011011-2), LL thanks the Overseas Returned Scholar Foundation of Shanxi Province in 2008 and SF thanks the Natural Science Foundation for Young Scientists of Shanxi Province (No. 2010021010-1) and the Doctoral Startup Foundation of Shanxi University for financial support.

References

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