Tris(N,N-dimethyl­ethane-1,2-diammonium) deca­vanadate(V) penta­hydrate

Zhu, C.-Y.; Li, Y.-T.; Wu, Z.-Y.; Xiao, N.-Y.

doi:10.1107/S1600536807002267

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Tris(N,N-dimethylethane-1,2-diammonium) decavanadate(V) pentahydrate

C.-Y. Zhu, Y.-T. Li, Z.-Y. Wu and N.-Y. Xiao

The asymmetric unit of the title compound, (C₄H₁₄N₂)₃[V₁₀O₂₈]·5H₂O, is composed of half of a centrosymmetric [V₁₀O₂₈]^6- polyanion, one and a half doubly protonated N,N-dimethylethane-1,2-diammonium cations (H₂dmen²⁺) and two and a half solvent water molecules. Disorder is observed in one of the H₂dmen²⁺ cations and also in the water solvent molecules. Hydrogen bonds assemble the compound to form a three-dimensional supramolecular structure.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807002267/ww2073sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536807002267/ww2073Isup2.hkl Contains datablock I

CCDC reference: 636833

checkCIF report

Key indicators

Single-crystal X-ray study
T = 298 K
Mean (C-C) = 0.009 Å
H-atom completeness 89%
Disorder in solvent or counterion
R factor = 0.039
wR factor = 0.117
Data-to-parameter ratio = 11.5

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings    Differ ....          ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT153_ALERT_1_C The su's on the Cell Axes are Equal (x 100000) .        700 Ang.
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for         C6
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for         C7
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor ....       2.32
PLAT302_ALERT_4_C Anion/Solvent Disorder .........................      29.00 Perc.
PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........        O4W
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...          9
PLAT430_ALERT_2_C Short Inter D...A Contact  O2W    ..  O6      ..       2.89 Ang.
PLAT432_ALERT_2_C Short Inter X...Y Contact  O3     ..  C7      ..       2.99 Ang.
PLAT716_ALERT_1_C H...A   Unknown or Inconsistent Label ..........          ?
PLAT716_ALERT_1_C H...A   Unknown or Inconsistent Label ..........          ?

Alert level G
FORMU01_ALERT_2_G  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and the formula from the _atom_site* data.
            Atom count from _chemical_formula_sum:C12 H52 N6 O33 V10
            Atom count from the _atom_site data:  C12 H46 N6 O33 V10
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional?
           From the CIF: _cell_formula_units_Z    1
           From the CIF: _chemical_formula_sum  C12 H52 N6 O33 V10
           TEST: Compare cell contents of formula and atom_site data

           atom    Z*formula  cif sites diff
           C         12.00     12.00    0.00
           H         52.00     46.00    6.00
           N          6.00      6.00    0.00
           O         33.00     33.00    0.00
           V         10.00     10.00    0.00

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

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

Computing details top

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP (Siemens, 1994); software used to prepare material for publication: WinGX (Farrugia, 1999).

Tris(N,N-dimethylethane-1,2-diammonium) decavanadate pentahydrate top

Crystal data top

(C₄H₁₄N₂)₃[V₁₀O₂₈]·5H₂O	Z = 1
M_r = 1317.99	F(000) = 654
Triclinic, P1	D_x = 2.215 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 10.362 (7) Å	Cell parameters from 1650 reflections
b = 10.469 (7) Å	θ = 3.2–25.0°
c = 10.935 (7) Å	µ = 2.37 mm⁻¹
α = 96.827 (11)°	T = 298 K
β = 106.257 (10)°	Cube, orange
γ = 115.898 (10)°	0.35 × 0.33 × 0.26 mm
V = 983.7 (11) Å³

Data collection top

Bruker APEX area-detector diffractometer	3474 independent reflections
Radiation source: fine-focus sealed tube	2590 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.019
φ and ω scans	θ_max = 25.0°, θ_min = 2.0°
Absorption correction: multi-scan (SADABS; Bruker, 2002)	h = −10→12
T_min = 0.461, T_max = 0.543	k = −12→8
5074 measured reflections	l = −12→13

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)] = 0.039	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.117	H-atom parameters constrained
S = 1.04	w = 1/[σ²(F_o²) + (0.0687P)²] where P = (F_o² + 2F_c²)/3
3474 reflections	(Δ/σ)_max < 0.001
301 parameters	Δρ_max = 0.61 e Å⁻³
3 restraints	Δρ_min = −0.56 e Å⁻³

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	Occ. (<1)
V1	0.15687 (8)	0.17498 (8)	0.39834 (7)	0.0208 (2)
V2	0.37897 (8)	0.49503 (7)	0.57341 (7)	0.01636 (19)
V3	0.49158 (8)	0.25681 (8)	0.56608 (7)	0.0181 (2)
V4	0.37947 (9)	0.18342 (8)	0.25983 (7)	0.0229 (2)
V5	0.27638 (8)	0.42111 (8)	0.25945 (7)	0.0199 (2)
O1	−0.0123 (3)	0.0580 (3)	0.3858 (3)	0.0286 (7)
O2	0.4056 (3)	0.6313 (3)	0.6942 (3)	0.0233 (7)
O3	0.5715 (3)	0.1993 (3)	0.6789 (3)	0.0272 (7)
O4	0.3849 (4)	0.0742 (4)	0.1463 (3)	0.0356 (8)
O5	0.2009 (3)	0.4841 (3)	0.1491 (3)	0.0278 (7)
O6	0.1934 (3)	0.0763 (3)	0.2729 (3)	0.0220 (7)
O7	0.2045 (3)	0.3484 (3)	0.5441 (3)	0.0215 (6)
O8	0.2888 (3)	0.1454 (3)	0.5370 (3)	0.0201 (6)
O9	0.1100 (3)	0.2822 (3)	0.2837 (3)	0.0231 (7)
O10	0.4842 (3)	0.1545 (3)	0.4145 (3)	0.0198 (6)
O11	0.3067 (3)	0.2913 (3)	0.1636 (3)	0.0233 (7)
O12	0.3168 (3)	0.5651 (3)	0.4243 (3)	0.0183 (6)
O13	0.5003 (3)	0.4255 (3)	0.6862 (3)	0.0182 (6)
O14	0.4010 (3)	0.3611 (3)	0.4256 (2)	0.0158 (6)
C1	−0.0413 (6)	0.5335 (6)	0.2768 (6)	0.0524 (16)
H1A	−0.0139	0.4973	0.3510	0.079*
H1B	−0.0790	0.4590	0.1958	0.079*
H1C	−0.1203	0.5572	0.2796	0.079*
N1	0.0960 (4)	0.6675 (4)	0.2831 (4)	0.0332 (10)
H1	0.1749	0.6469	0.2988	0.040*
C2	0.0748 (7)	0.7099 (7)	0.1531 (5)	0.0532 (15)
H2D	0.0490	0.6284	0.0826	0.080*
H2E	0.1691	0.7941	0.1610	0.080*
H2F	−0.0069	0.7338	0.1338	0.080*
C3	0.1457 (6)	0.7972 (5)	0.3934 (5)	0.0326 (11)
H3A	0.0676	0.8273	0.3757	0.039*
H3B	0.2410	0.8791	0.3970	0.039*
C4	0.1711 (5)	0.7635 (5)	0.5270 (5)	0.0288 (11)
H4A	0.0745	0.7209	0.5415	0.035*
H4B	0.2083	0.6931	0.5289	0.035*
N2	0.2872 (4)	0.9045 (4)	0.6327 (4)	0.0291 (9)
H2A	0.3819	0.9230	0.6404	0.044*
H2B	0.2754	0.8963	0.7095	0.044*
H2C	0.2734	0.9782	0.6112	0.044*
O1W	0.2024 (4)	0.8571 (5)	0.8577 (4)	0.0517 (10)
C5	0.4584 (7)	0.5420 (6)	−0.0134 (5)	0.0477 (15)
H5A	0.4608	0.5693	−0.0947	0.057*
H5B	0.3512	0.4800	−0.0253	0.057*
C6	0.6971 (9)	0.7720 (11)	0.1397 (10)	0.056 (3)	0.50
H6A	0.7310	0.8570	0.2102	0.084*	0.50
H6B	0.7219	0.8035	0.0663	0.084*	0.50
H6C	0.7480	0.7179	0.1705	0.084*	0.50
N3	0.5286 (7)	0.6764 (5)	0.0965 (5)	0.0621 (15)	0.50
H3	0.5085	0.6476	0.1675	0.075*	0.50
C7	0.4385 (11)	0.7554 (12)	0.0497 (12)	0.052 (3)	0.50
H7A	0.3298	0.6881	0.0224	0.078*	0.50
H7B	0.4599	0.7895	−0.0238	0.078*	0.50
H7C	0.4689	0.8382	0.1210	0.078*	0.50
N4	0.5286 (7)	0.6764 (5)	0.0965 (5)	0.0621 (15)	0.50
H4C	0.4804	0.7279	0.0762	0.093*	0.50
H4D	0.6281	0.7313	0.1100	0.093*	0.50
H4E	0.5199	0.6511	0.1699	0.093*	0.50
O3W	0.8520 (11)	0.8600 (12)	0.1128 (11)	0.097 (4)	0.50
O4W	0.433 (2)	0.850 (2)	0.0421 (13)	0.166 (8)	0.50
O2W	0.965 (2)	1.015 (3)	0.0180 (19)	0.150 (7)	0.50
H1W	0.1156	0.8366	0.8655	0.080*
H2W	0.2680	0.8844	0.9374	0.080*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
V1	0.0163 (4)	0.0172 (4)	0.0268 (4)	0.0063 (3)	0.0081 (3)	0.0064 (3)
V2	0.0168 (4)	0.0165 (4)	0.0182 (4)	0.0084 (3)	0.0092 (3)	0.0058 (3)
V3	0.0173 (4)	0.0150 (4)	0.0215 (4)	0.0075 (3)	0.0065 (3)	0.0070 (3)
V4	0.0249 (4)	0.0199 (4)	0.0223 (4)	0.0105 (3)	0.0092 (3)	0.0019 (3)
V5	0.0206 (4)	0.0172 (4)	0.0174 (4)	0.0078 (3)	0.0032 (3)	0.0051 (3)
O1	0.0175 (16)	0.0229 (17)	0.0370 (19)	0.0041 (14)	0.0080 (14)	0.0093 (15)
O2	0.0254 (16)	0.0226 (16)	0.0227 (16)	0.0110 (14)	0.0118 (13)	0.0058 (14)
O3	0.0260 (17)	0.0245 (17)	0.0285 (17)	0.0124 (15)	0.0049 (14)	0.0120 (14)
O4	0.041 (2)	0.0303 (18)	0.034 (2)	0.0173 (17)	0.0163 (16)	0.0017 (16)
O5	0.0282 (17)	0.0292 (18)	0.0226 (17)	0.0143 (15)	0.0040 (14)	0.0085 (14)
O6	0.0207 (16)	0.0149 (15)	0.0239 (16)	0.0068 (13)	0.0049 (13)	0.0005 (13)
O7	0.0206 (16)	0.0205 (16)	0.0260 (16)	0.0095 (14)	0.0129 (13)	0.0074 (14)
O8	0.0196 (15)	0.0175 (15)	0.0243 (16)	0.0082 (13)	0.0103 (13)	0.0082 (13)
O9	0.0164 (15)	0.0189 (15)	0.0270 (17)	0.0057 (13)	0.0034 (13)	0.0068 (13)
O10	0.0201 (15)	0.0187 (15)	0.0253 (16)	0.0124 (13)	0.0105 (13)	0.0049 (13)
O11	0.0262 (16)	0.0212 (16)	0.0188 (15)	0.0095 (14)	0.0077 (13)	0.0037 (13)
O12	0.0187 (15)	0.0151 (15)	0.0219 (15)	0.0092 (13)	0.0072 (12)	0.0049 (13)
O13	0.0184 (15)	0.0191 (15)	0.0195 (15)	0.0102 (13)	0.0078 (12)	0.0080 (13)
O14	0.0175 (15)	0.0145 (14)	0.0163 (14)	0.0082 (13)	0.0071 (12)	0.0042 (12)
C1	0.031 (3)	0.029 (3)	0.076 (4)	0.005 (3)	0.018 (3)	−0.008 (3)
N1	0.025 (2)	0.028 (2)	0.044 (3)	0.0136 (19)	0.0104 (19)	0.002 (2)
C2	0.058 (4)	0.054 (4)	0.038 (3)	0.030 (3)	0.006 (3)	0.000 (3)
C3	0.034 (3)	0.021 (2)	0.041 (3)	0.013 (2)	0.013 (2)	0.006 (2)
C4	0.026 (2)	0.025 (3)	0.043 (3)	0.015 (2)	0.019 (2)	0.010 (2)
N2	0.024 (2)	0.027 (2)	0.037 (2)	0.0126 (18)	0.0111 (18)	0.0140 (19)
O1W	0.032 (2)	0.065 (3)	0.049 (2)	0.018 (2)	0.0120 (18)	0.013 (2)
C5	0.069 (4)	0.053 (4)	0.041 (3)	0.033 (3)	0.039 (3)	0.023 (3)
C6	0.074 (9)	0.056 (8)	0.035 (7)	0.029 (8)	0.026 (6)	0.004 (6)
N3	0.110 (5)	0.054 (3)	0.052 (3)	0.048 (4)	0.054 (3)	0.026 (3)
C7	0.073 (9)	0.056 (8)	0.045 (7)	0.037 (7)	0.032 (7)	0.029 (7)
N4	0.110 (5)	0.054 (3)	0.052 (3)	0.048 (4)	0.054 (3)	0.026 (3)
O3W	0.054 (6)	0.098 (8)	0.093 (8)	0.042 (6)	−0.017 (6)	−0.039 (7)
O4W	0.244 (18)	0.27 (2)	0.081 (9)	0.215 (19)	0.042 (10)	0.048 (12)
O2W	0.135 (17)	0.177 (15)	0.107 (12)	0.099 (13)	−0.008 (10)	−0.031 (11)

Geometric parameters (Å, º) top

V1—O1	1.595 (3)	C1—H1A	0.9600
V1—O6	1.840 (3)	C1—H1B	0.9600
V1—O9	1.881 (3)	C1—H1C	0.9600
V1—O8	1.893 (3)	N1—C3	1.489 (6)
V1—O7	2.042 (3)	N1—C2	1.525 (6)
V1—O14	2.328 (3)	N1—H1	0.9100
V2—O2	1.691 (3)	C2—H2D	0.9600
V2—O7	1.691 (3)	C2—H2E	0.9600
V2—O12	1.929 (3)	C2—H2F	0.9600
V2—O13	1.943 (3)	C3—C4	1.522 (6)
V2—O14ⁱ	2.109 (3)	C3—H3A	0.9700
V2—O14	2.140 (3)	C3—H3B	0.9700
V3—O3	1.616 (3)	C4—N2	1.492 (6)
V3—O8	1.810 (3)	C4—H4A	0.9700
V3—O10	1.826 (3)	C4—H4B	0.9700
V3—O12ⁱ	2.008 (3)	N2—H2A	0.8900
V3—O13	2.024 (3)	N2—H2B	0.8900
V3—O14	2.218 (3)	N2—H2C	0.8900
V4—O4	1.615 (3)	O1W—H1W	0.8600
V4—O6	1.816 (3)	O1W—H2W	0.8600
V4—O10	1.873 (3)	C5—N3	1.472 (7)
V4—O11	1.881 (3)	C5—C5ⁱⁱ	1.479 (10)
V4—O2ⁱ	2.084 (3)	C5—H5A	0.9700
V4—O14	2.324 (3)	C5—H5B	0.9700
V5—O5	1.617 (3)	C6—N3	1.474 (6)
V5—O11	1.806 (3)	C6—H6A	0.9600
V5—O9	1.821 (3)	C6—H6B	0.9600
V5—O13ⁱ	2.011 (3)	C6—H6C	0.9600
V5—O12	2.020 (3)	N3—C7	1.526 (6)
V5—O14	2.243 (3)	N3—H3	0.9100
O2—V4ⁱ	2.084 (3)	C7—H7A	0.9600
O12—V3ⁱ	2.008 (3)	C7—H7B	0.9600
O13—V5ⁱ	2.011 (3)	C7—H7C	0.9600
O14—V2ⁱ	2.109 (3)	O2W—O2Wⁱⁱⁱ	1.05 (2)
C1—N1	1.475 (6)

O1—V1—O6	103.30 (15)	V2—O12—V3ⁱ	106.23 (13)
O1—V1—O9	100.57 (14)	V2—O12—V5	107.35 (13)
O6—V1—O9	90.89 (14)	V3ⁱ—O12—V5	100.65 (12)
O1—V1—O8	103.75 (14)	V2—O13—V5ⁱ	106.91 (13)
O6—V1—O8	91.23 (13)	V2—O13—V3	106.73 (14)
O9—V1—O8	154.39 (13)	V5ⁱ—O13—V3	100.42 (12)
O1—V1—O7	100.45 (15)	V2ⁱ—O14—V2	102.26 (12)
O6—V1—O7	156.24 (12)	V2ⁱ—O14—V3	93.38 (10)
O9—V1—O7	84.13 (13)	V2—O14—V3	93.85 (11)
O8—V1—O7	83.71 (13)	V2ⁱ—O14—V5	93.70 (10)
O1—V1—O14	175.19 (14)	V2—O14—V5	93.05 (11)
O6—V1—O14	81.26 (12)	V3—O14—V5	168.85 (14)
O9—V1—O14	77.65 (11)	V2ⁱ—O14—V4	88.22 (10)
O8—V1—O14	77.46 (11)	V2—O14—V4	169.51 (13)
O7—V1—O14	74.98 (11)	V3—O14—V4	85.91 (10)
O2—V2—O7	106.49 (15)	V5—O14—V4	85.72 (10)
O2—V2—O12	97.84 (14)	V2ⁱ—O14—V1	170.84 (14)
O7—V2—O12	97.81 (13)	V2—O14—V1	86.90 (10)
O2—V2—O13	97.23 (14)	V3—O14—V1	85.89 (10)
O7—V2—O13	96.10 (13)	V5—O14—V1	85.75 (10)
O12—V2—O13	155.66 (12)	V4—O14—V1	82.62 (10)
O2—V2—O14ⁱ	88.25 (13)	N1—C1—H1A	109.5
O7—V2—O14ⁱ	165.22 (13)	N1—C1—H1B	109.5
O12—V2—O14ⁱ	80.88 (11)	H1A—C1—H1B	109.5
O13—V2—O14ⁱ	80.59 (11)	N1—C1—H1C	109.5
O2—V2—O14	165.99 (13)	H1A—C1—H1C	109.5
O7—V2—O14	87.50 (13)	H1B—C1—H1C	109.5
O12—V2—O14	80.62 (12)	C1—N1—C3	113.0 (4)
O13—V2—O14	80.13 (12)	C1—N1—C2	112.9 (4)
O14ⁱ—V2—O14	77.74 (12)	C3—N1—C2	109.3 (4)
O3—V3—O8	102.11 (14)	C1—N1—H1	107.1
O3—V3—O10	102.66 (15)	C3—N1—H1	107.1
O8—V3—O10	95.86 (13)	C2—N1—H1	107.1
O3—V3—O12ⁱ	98.44 (14)	N1—C2—H2D	109.5
O8—V3—O12ⁱ	156.59 (12)	N1—C2—H2E	109.5
O10—V3—O12ⁱ	90.42 (13)	H2D—C2—H2E	109.5
O3—V3—O13	98.54 (15)	N1—C2—H2F	109.5
O8—V3—O13	89.54 (13)	H2D—C2—H2F	109.5
O10—V3—O13	156.46 (11)	H2E—C2—H2F	109.5
O12ⁱ—V3—O13	76.36 (12)	N1—C3—C4	112.2 (4)
O3—V3—O14	173.63 (14)	N1—C3—H3A	109.2
O8—V3—O14	82.10 (11)	C4—C3—H3A	109.2
O10—V3—O14	81.49 (12)	N1—C3—H3B	109.2
O12ⁱ—V3—O14	76.55 (11)	C4—C3—H3B	109.2
O13—V3—O14	76.57 (11)	H3A—C3—H3B	107.9
O4—V4—O6	104.96 (16)	N2—C4—C3	108.4 (4)
O4—V4—O10	101.60 (15)	N2—C4—H4A	110.0
O6—V4—O10	92.26 (13)	C3—C4—H4A	110.0
O4—V4—O11	102.42 (16)	N2—C4—H4B	110.0
O6—V4—O11	91.32 (13)	C3—C4—H4B	110.0
O10—V4—O11	153.89 (13)	H4A—C4—H4B	108.4
O4—V4—O2ⁱ	99.08 (15)	C4—N2—H2A	109.5
O6—V4—O2ⁱ	155.95 (13)	C4—N2—H2B	109.5
O10—V4—O2ⁱ	82.99 (12)	H2A—N2—H2B	109.5
O11—V4—O2ⁱ	83.27 (13)	C4—N2—H2C	109.5
O4—V4—O14	173.18 (14)	H2A—N2—H2C	109.5
O6—V4—O14	81.85 (12)	H2B—N2—H2C	109.5
O10—V4—O14	77.69 (11)	H1W—O1W—H2W	106.00
O11—V4—O14	77.24 (12)	N3—C5—C5ⁱⁱ	111.0 (6)
O2ⁱ—V4—O14	74.10 (11)	N3—C5—H5A	109.4
O5—V5—O11	103.20 (15)	C5ⁱⁱ—C5—H5A	109.4
O5—V5—O9	103.45 (15)	N3—C5—H5B	109.4
O11—V5—O9	95.86 (14)	C5ⁱⁱ—C5—H5B	109.4
O5—V5—O13ⁱ	98.67 (14)	H5A—C5—H5B	108.0
O11—V5—O13ⁱ	90.03 (13)	N3—C6—H6A	109.5
O9—V5—O13ⁱ	155.10 (12)	N3—C6—H6B	109.5
O5—V5—O12	98.87 (14)	H6A—C6—H6B	109.5
O11—V5—O12	155.61 (12)	N3—C6—H6C	109.5
O9—V5—O12	88.93 (13)	H6A—C6—H6C	109.5
O13ⁱ—V5—O12	76.39 (12)	H6B—C6—H6C	109.5
O5—V5—O14	173.37 (14)	C5—N3—C6	116.0 (6)
O11—V5—O14	80.88 (12)	C5—N3—C7	104.6 (6)
O9—V5—O14	81.12 (12)	C6—N3—C7	113.0 (4)
O13ⁱ—V5—O14	75.95 (11)	C5—N3—H3	107.6
O12—V5—O14	76.24 (11)	C6—N3—H3	107.6
V2—O2—V4ⁱ	109.43 (15)	C7—N3—H3	107.6
V4—O6—V1	114.26 (15)	N3—C7—H7A	109.5
V2—O7—V1	110.60 (14)	N3—C7—H7B	109.5
V3—O8—V1	113.54 (14)	H7A—C7—H7B	109.5
V5—O9—V1	114.33 (15)	N3—C7—H7C	109.5
V3—O10—V4	113.62 (14)	H7A—C7—H7C	109.5
V5—O11—V4	114.88 (15)	H7B—C7—H7C	109.5

O7—V2—O2—V4ⁱ	178.94 (12)	O7—V2—O14—V2ⁱ	−179.05 (12)
O12—V2—O2—V4ⁱ	−80.47 (15)	O12—V2—O14—V2ⁱ	82.61 (12)
O13—V2—O2—V4ⁱ	80.36 (15)	O13—V2—O14—V2ⁱ	−82.41 (12)
O14ⁱ—V2—O2—V4ⁱ	0.07 (13)	O14ⁱ—V2—O14—V2ⁱ	0.0
O14—V2—O2—V4ⁱ	2.2 (6)	O2—V2—O14—V3	92.1 (5)
O4—V4—O6—V1	179.45 (16)	O7—V2—O14—V3	−84.75 (12)
O10—V4—O6—V1	76.80 (16)	O12—V2—O14—V3	176.92 (11)
O11—V4—O6—V1	−77.33 (16)	O13—V2—O14—V3	11.89 (10)
O2ⁱ—V4—O6—V1	−1.0 (4)	O14ⁱ—V2—O14—V3	94.30 (12)
O14—V4—O6—V1	−0.41 (14)	O2—V2—O14—V5	−96.7 (5)
O1—V1—O6—V4	178.86 (15)	O7—V2—O14—V5	86.49 (12)
O9—V1—O6—V4	77.78 (16)	O12—V2—O14—V5	−11.85 (10)
O8—V1—O6—V4	−76.70 (16)	O13—V2—O14—V5	−176.87 (11)
O7—V1—O6—V4	0.4 (4)	O14ⁱ—V2—O14—V5	−94.46 (12)
O14—V1—O6—V4	0.41 (14)	O2—V2—O14—V4	−179.6 (6)
O2—V2—O7—V1	179.68 (13)	O7—V2—O14—V4	3.5 (7)
O12—V2—O7—V1	79.06 (15)	O12—V2—O14—V4	−94.8 (7)
O13—V2—O7—V1	−80.91 (15)	O13—V2—O14—V4	100.2 (7)
O14ⁱ—V2—O7—V1	−4.8 (5)	O14ⁱ—V2—O14—V4	−177.4 (7)
O14—V2—O7—V1	−1.12 (13)	O2—V2—O14—V1	177.8 (4)
O1—V1—O7—V2	−177.40 (15)	O7—V2—O14—V1	0.92 (11)
O6—V1—O7—V2	1.1 (4)	O12—V2—O14—V1	−97.42 (11)
O9—V1—O7—V2	−77.69 (16)	O13—V2—O14—V1	97.55 (11)
O8—V1—O7—V2	79.72 (16)	O14ⁱ—V2—O14—V1	179.97 (13)
O14—V1—O7—V2	1.06 (12)	O8—V3—O14—V2ⁱ	−177.59 (12)
O3—V3—O8—V1	−175.82 (16)	O10—V3—O14—V2ⁱ	−80.42 (12)
O10—V3—O8—V1	−71.50 (17)	O12ⁱ—V3—O14—V2ⁱ	12.06 (10)
O12ⁱ—V3—O8—V1	33.3 (4)	O13—V3—O14—V2ⁱ	90.98 (11)
O13—V3—O8—V1	85.54 (16)	O8—V3—O14—V2	79.87 (12)
O14—V3—O8—V1	9.04 (15)	O10—V3—O14—V2	177.04 (12)
O1—V1—O8—V3	176.05 (16)	O12ⁱ—V3—O14—V2	−90.47 (12)
O6—V1—O8—V3	72.03 (17)	O13—V3—O14—V2	−11.56 (10)
O9—V1—O8—V3	−22.6 (4)	O8—V3—O14—V5	−48.2 (7)
O7—V1—O8—V3	−84.69 (16)	O10—V3—O14—V5	48.9 (7)
O14—V1—O8—V3	−8.73 (14)	O12ⁱ—V3—O14—V5	141.4 (7)
O5—V5—O9—V1	175.29 (17)	O13—V3—O14—V5	−139.6 (7)
O11—V5—O9—V1	70.19 (18)	O8—V3—O14—V4	−89.62 (12)
O13ⁱ—V5—O9—V1	−32.7 (4)	O10—V3—O14—V4	7.55 (10)
O12—V5—O9—V1	−85.85 (17)	O12ⁱ—V3—O14—V4	100.04 (11)
O14—V5—O9—V1	−9.60 (15)	O13—V3—O14—V4	178.95 (11)
O1—V1—O9—V5	−175.21 (17)	O8—V3—O14—V1	−6.74 (11)
O6—V1—O9—V5	−71.50 (18)	O10—V3—O14—V1	90.43 (11)
O8—V1—O9—V5	23.2 (4)	O12ⁱ—V3—O14—V1	−177.08 (11)
O7—V1—O9—V5	85.22 (17)	O13—V3—O14—V1	−98.17 (11)
O14—V1—O9—V5	9.36 (15)	O11—V5—O14—V2ⁱ	80.46 (13)
O3—V3—O10—V4	174.69 (15)	O9—V5—O14—V2ⁱ	177.91 (13)
O8—V3—O10—V4	70.86 (16)	O13ⁱ—V5—O14—V2ⁱ	−11.88 (10)
O12ⁱ—V3—O10—V4	−86.56 (16)	O12—V5—O14—V2ⁱ	−91.02 (12)
O13—V3—O10—V4	−31.6 (4)	O11—V5—O14—V2	−177.04 (12)
O14—V3—O10—V4	−10.23 (14)	O9—V5—O14—V2	−79.58 (13)
O4—V4—O10—V3	−177.06 (16)	O13ⁱ—V5—O14—V2	90.63 (12)
O6—V4—O10—V3	−71.28 (17)	O12—V5—O14—V2	11.49 (10)
O11—V4—O10—V3	26.3 (4)	O11—V5—O14—V3	−48.9 (7)
O2ⁱ—V4—O10—V3	85.06 (16)	O9—V5—O14—V3	48.6 (7)
O14—V4—O10—V3	9.87 (13)	O13ⁱ—V5—O14—V3	−141.2 (7)
O5—V5—O11—V4	−175.14 (16)	O12—V5—O14—V3	139.6 (7)
O9—V5—O11—V4	−69.82 (17)	O11—V5—O14—V4	−7.47 (11)
O13ⁱ—V5—O11—V4	85.94 (16)	O9—V5—O14—V4	89.98 (12)
O12—V5—O11—V4	30.6 (4)	O13ⁱ—V5—O14—V4	−99.81 (11)
O14—V5—O11—V4	10.18 (15)	O12—V5—O14—V4	−178.95 (11)
O4—V4—O11—V5	177.04 (17)	O11—V5—O14—V1	−90.38 (12)
O6—V4—O11—V5	71.40 (17)	O9—V5—O14—V1	7.08 (11)
O10—V4—O11—V5	−26.4 (4)	O13ⁱ—V5—O14—V1	177.29 (11)
O2ⁱ—V4—O11—V5	−85.10 (17)	O12—V5—O14—V1	98.15 (11)
O14—V4—O11—V5	−9.94 (14)	O6—V4—O14—V2ⁱ	−179.81 (11)
O2—V2—O12—V3ⁱ	72.70 (15)	O10—V4—O14—V2ⁱ	86.07 (12)
O7—V2—O12—V3ⁱ	−179.36 (13)	O11—V4—O14—V2ⁱ	−86.58 (12)
O13—V2—O12—V3ⁱ	−55.1 (3)	O2ⁱ—V4—O14—V2ⁱ	−0.05 (9)
O14ⁱ—V2—O12—V3ⁱ	−14.25 (12)	O6—V4—O14—V2	−2.3 (7)
O14—V2—O12—V3ⁱ	−93.21 (13)	O10—V4—O14—V2	−96.5 (7)
O2—V2—O12—V5	179.71 (13)	O11—V4—O14—V2	90.9 (7)
O7—V2—O12—V5	−72.35 (15)	O2ⁱ—V4—O14—V2	177.4 (7)
O13—V2—O12—V5	51.9 (3)	O6—V4—O14—V3	86.68 (11)
O14ⁱ—V2—O12—V5	92.76 (13)	O10—V4—O14—V3	−7.45 (10)
O14—V2—O12—V5	13.80 (12)	O11—V4—O14—V3	179.90 (11)
O5—V5—O12—V2	171.20 (14)	O2ⁱ—V4—O14—V3	−93.57 (11)
O11—V5—O12—V2	−34.1 (4)	O6—V4—O14—V5	−85.96 (11)
O9—V5—O12—V2	67.75 (14)	O10—V4—O14—V5	179.91 (11)
O13ⁱ—V5—O12—V2	−91.95 (13)	O11—V4—O14—V5	7.26 (10)
O14—V5—O12—V2	−13.37 (11)	O2ⁱ—V4—O14—V5	93.80 (11)
O5—V5—O12—V3ⁱ	−77.90 (15)	O6—V4—O14—V1	0.30 (10)
O11—V5—O12—V3ⁱ	76.8 (3)	O10—V4—O14—V1	−93.83 (11)
O9—V5—O12—V3ⁱ	178.65 (12)	O11—V4—O14—V1	93.52 (11)
O13ⁱ—V5—O12—V3ⁱ	18.95 (11)	O2ⁱ—V4—O14—V1	−179.94 (10)
O14—V5—O12—V3ⁱ	97.53 (12)	O6—V1—O14—V2	179.22 (11)
O2—V2—O13—V5ⁱ	−72.91 (15)	O9—V1—O14—V2	86.37 (12)
O7—V2—O13—V5ⁱ	179.56 (13)	O8—V1—O14—V2	−87.55 (12)
O12—V2—O13—V5ⁱ	55.0 (3)	O7—V1—O14—V2	−0.79 (9)
O14ⁱ—V2—O13—V5ⁱ	14.10 (12)	O6—V1—O14—V3	−86.70 (12)
O14—V2—O13—V5ⁱ	93.17 (14)	O9—V1—O14—V3	−179.55 (12)
O2—V2—O13—V3	−179.69 (13)	O8—V1—O14—V3	6.54 (10)
O7—V2—O13—V3	72.78 (15)	O7—V1—O14—V3	93.30 (11)
O12—V2—O13—V3	−51.8 (3)	O6—V1—O14—V5	85.93 (12)
O14ⁱ—V2—O13—V3	−92.68 (13)	O9—V1—O14—V5	−6.93 (11)
O14—V2—O13—V3	−13.61 (12)	O8—V1—O14—V5	179.16 (12)
O3—V3—O13—V2	−170.87 (14)	O7—V1—O14—V5	−94.08 (11)
O8—V3—O13—V2	−68.69 (14)	O6—V1—O14—V4	−0.30 (10)
O10—V3—O13—V2	35.0 (4)	O9—V1—O14—V4	−93.15 (12)
O12ⁱ—V3—O13—V2	92.45 (14)	O8—V1—O14—V4	92.94 (11)
O14—V3—O13—V2	13.29 (11)	O7—V1—O14—V4	179.70 (10)
O3—V3—O13—V5ⁱ	77.78 (15)	C1—N1—C3—C4	54.1 (5)
O8—V3—O13—V5ⁱ	179.96 (11)	C2—N1—C3—C4	−179.3 (4)
O10—V3—O13—V5ⁱ	−76.3 (3)	N1—C3—C4—N2	152.9 (4)
O12ⁱ—V3—O13—V5ⁱ	−18.90 (11)	C5ⁱⁱ—C5—N3—C6	50.7 (8)
O14—V3—O13—V5ⁱ	−98.05 (12)	C5ⁱⁱ—C5—N3—C7	175.9 (6)
O2—V2—O14—V2ⁱ	−2.2 (5)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1···O5	0.91	2.38	3.010 (5)	127
N1—H1···O12	0.91	2.24	3.054 (5)	148
N1—H1···O3ⁱ	0.91	2.33	2.975 (5)	128
N2—H2B···O1W	0.89	1.99	2.862 (5)	168
N2—H2C···O1^iv	0.89	2.57	2.997 (5)	110
N2—H2C···O8^v	0.89	1.98	2.838 (5)	162
N2—H2A···O10ⁱ	0.89	2.07	2.855 (5)	147
N2—H2A···O3^v	0.89	2.59	3.052 (5)	114
N3—H3···O13ⁱ	0.91	1.86	2.756 (5)	167
N4—H4E···O13ⁱ	0.89	1.87	2.756 (5)	172
O1W—H1W···O9^iv	0.86	2.13	2.74 (1)	128.5
O1W—H2W···O4W^vi	0.86	1.97	2.69 (1)	140.6
O1W—H1W···O2W^vii	0.86	2.44	3.09 (1)	132.2
O1W—H2W···O4^viii	0.86	2.43	3.15 (1)	141.0
O2W···O6ⁱⁱ	?	?	3.02 (2)	?
O2W···O3Wⁱⁱⁱ	?	?	2.78 (4)	?

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

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