metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 67| Part 6| June 2011| Pages m811-m812

Triclinic modification of tetra­kis­(tri­ethyl­ammonium) di­hydrogeno­deca­vanadate(V)

aDepartment of Chemistry, University of Malaya, 50603 Kuala Lumpur, Malaysia
*Correspondence e-mail: seikweng@um.edu.my

(Received 12 May 2011; accepted 24 May 2011; online 28 May 2011)

In the title ammonium polyoxometallate salt, (C6H16N)4[H2V10O28], the anion features O atoms engaged in μ6-, μ3- and μ2-bridging of adjacent VV atoms, confering an octa­hedral coordination at each of the twenty unique metal atoms. Two anions are linked by μ3- and μ2-bridged OH units across a center of inversion, forming a dimer which is linked to the cations by N—H⋯O hydrogen bonds. The cation is disordered over two positions in a 0.776 (4):0.224 (4) ratio in one of the two independent ion pairs in the asymmetric unit, and 0.627 (10):0.373 (10) in the other.

Related literature

For the monoclinic modification, see: Correia et al. (2004[Correia, I., Avecilla, F., Marcão, S. & Pessoa, J. C. (2004). Inorg. Chim. Acta, 357, 4476-4487.]); Sarkar & Pal (2008[Sarkar, A. & Pal, S. (2008). Polyhedron, 27, 3472-3476.]).

[Scheme 1]

Experimental

Crystal data
  • (C6H16N)4[H2V10O28]

  • Mr = 1368.21

  • Triclinic, [P \overline 1]

  • a = 13.1735 (4) Å

  • b = 20.0061 (7) Å

  • c = 20.2427 (7) Å

  • α = 62.669 (3)°

  • β = 86.263 (3)°

  • γ = 76.979 (3)°

  • V = 4613.0 (3) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 2.02 mm−1

  • T = 100 K

  • 0.20 × 0.15 × 0.10 mm

Data collection
  • Agilent SuperNova Dual diffractometer with an Atlas detector

  • Absorption correction: multi-scan (CrysAlis PRO; Agilent, 2010[Agilent (2010). CrysAlis PRO. Agilent Technologies, Yarnton, England.]) Tmin = 0.688, Tmax = 0.824

  • 38533 measured reflections

  • 20465 independent reflections

  • 13087 reflections with I > 2σ(I)

  • Rint = 0.041

Refinement
  • R[F2 > 2σ(F2)] = 0.049

  • wR(F2) = 0.133

  • S = 1.04

  • 20465 reflections

  • 1230 parameters

  • 132 restraints

  • H-atom parameters constrained

  • Δρmax = 1.47 e Å−3

  • Δρmin = −0.79 e Å−3

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
N1—H1⋯O3 0.88 2.06 2.937 (4) 175
N2—H2⋯O14 0.88 1.89 2.765 (4) 176
N3—H3⋯O41 0.88 1.82 2.699 (4) 175
N4—H4⋯O9 0.88 2.13 2.968 (9) 160
N4′—H4′⋯O9 0.88 1.99 2.830 (16) 158
N5—H5⋯O26 0.88 2.39 2.981 (5) 125
N5—H5⋯O28 0.88 2.38 3.187 (5) 153
N6—H6⋯O51 0.88 1.96 2.823 (4) 167
N7—H7⋯O34 0.88 2.33 3.061 (4) 141
N7—H7⋯O45 0.88 2.44 3.156 (5) 139
N7—H7⋯O46 0.88 2.40 3.139 (4) 142
N8—H8⋯O52 0.88 1.91 2.766 (4) 162
O15—H15⋯O18i 0.84 1.99 2.819 (4) 171
O17—H17⋯O16i 0.84 1.90 2.715 (4) 162
O54—H54⋯O55ii 0.84 1.88 2.686 (4) 159
O56—H56⋯O53ii 0.84 1.94 2.775 (4) 177
Symmetry codes: (i) -x+1, -y+1, -z; (ii) -x+2, -y, -z+2.

Data collection: CrysAlis PRO (Agilent, 2010[Agilent (2010). CrysAlis PRO. Agilent Technologies, Yarnton, England.]); cell refinement: CrysAlis PRO; data reduction: CrysAlis PRO; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: X-SEED (Barbour, 2001[Barbour, L. J. (2001). J. Supramol. Chem. 1, 189-191.]); software used to prepare material for publication: publCIF (Westrip, 2010[Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.]).

Supporting information


Comment top

The polyoxometallate, 4(C2H5)3NH+ [H2O28V10]4-, tetrakis(triethylammonium) bis(µ6-oxo)-(µ3-hydroxo)-tris(µ3-oxo)-(µ2-hydroxo)-trideca(µ2-oxo)-octaoxo-decavanadate(V) (Scheme I) was the product obtained by reacting triethylammonium D,L-aminopropionate, salicylaldehyde and vanadyl(IV) sulfate in methanol (Correia et al., 2004). The POM can also be synthesized from the reaction of triethylamine and vanadium(V) oxide in water (Sarkar & Pal, 2008). The compound, which belongs to the monoclinic P21/c space group, features the dihydrogenodecavanadate tetraanion surrounded by the cations; two tetraanions are linked by a pair of O–H···O hydrogen bonds to generate a dimer. In the present triclinic modification, the ion similarly features oxygen atoms engaged in µ6–, µ3– and µ2-bridging of adjacent vanadium(V) atoms to confer octahedral coordination at the metal centers (Figs. 1 & 2). Two ions are linked by µ3-bridged and µ2-bridged OH units across a center-of-inversion to form a dimer (Fig. 3). The dimers are linked to the cations by N–H···O hydrogen bonds (Table 1).

Related literature top

For the monoclinic modification, see: Correia et al. (2004); Sarkar & Pal (2008).

Experimental top

Vanadyl(IV) sulfate (0.25 g, 1 mmol), 4-oxo-1,4-pyran-2,6-dicarboxylic acid (chelidonic acid) (0.18 g, 1 mmol) and triethylamine (0.4 ml, 3 mmol) were heated in water (100 ml) for an hour. The solution was filtered and upon slow evaporation of the filtrate afforded orange prisms of the title compound as a side product in low yield.

Refinement top

Carbon-bound H-atoms were placed in calculated positions [C—H = 0.95–0.98 Å, N—H = 0.88 Å; Uiso(H) 1.2 to 1.5Ueq(C)] and were included in the refinement in the riding model approximation. For each tetraanion, only two of the twenty-eight O atoms were within the range for hydrogen-bonding interaction with the O atom of an adjacent anion. Of the two, one is connected to two V atoms and the other to three V atoms. Hydrogen atoms were placed in calculated positions for these two and their displacement parameters were tied by a factor of 1.5. Two of the eight cations are disordered. The occupancies refined to 0.627 (1) and 0.776 (1) under these conditions: the carbon–carbon and carbon–nitrogen distances were restrained to 1.50±0.01 Å; the distances of the 1,3-related atoms were restrained to 2.35±0.01 Å. The atoms of the minor components were refined isotropically with the thermal parameters of the primed atoms set to those of the unprimed ones. The displacement parameters of the unprimed (major component) atoms were refined anisotropically but they were tightly restrained. The final difference Fourier map had a peak in the vicinity of the cation with the N4/N4' atoms. The (4 8 4) reflection was omitted owing to bad disagreement between observed and calculated structure factors.

Computing details top

Data collection: CrysAlis PRO (Agilent, 2010); cell refinement: CrysAlis PRO (Agilent, 2010); data reduction: CrysAlis PRO (Agilent, 2010); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2010).

Figures top
[Figure 1] Fig. 1. Thermal ellipsoid plot (Barbour, 2001) of one independent 4(C2H5)3NH+ [H2O28V10]4- ion-pair at the 70% probability level. Hydrogen atoms are drawn as spheres of arbitrary radius. The disorder is not shown and O atoms other than those involved in hydrogen bonding are not labeled.
[Figure 2] Fig. 2. Thermal ellipsoid plot (Barbour, 2001) of the second independent 4(C2H5)3NH+ [H2O28V10]4- ion-pair at the 70% probability level. Hydrogen atoms are drawn as spheres of arbitrary radius. The disorder is not shown and O atoms other than those involved in hydrogen bonding are not labeled.
[Figure 3] Fig. 3. Hydrogen bonding linking the two independent [H2O28V10]4- anions into a centrosymmetric dimer.
tetrakis(triethylammonium) dihydrogenodecavanadate(V) top
Crystal data top
(C6H16N)4[H2V10O28]Z = 4
Mr = 1368.21F(000) = 2768
Triclinic, P1Dx = 1.970 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 13.1735 (4) ÅCell parameters from 9283 reflections
b = 20.0061 (7) Åθ = 2.3–29.4°
c = 20.2427 (7) ŵ = 2.02 mm1
α = 62.669 (3)°T = 100 K
β = 86.263 (3)°Block, orange
γ = 76.979 (3)°0.20 × 0.15 × 0.10 mm
V = 4613.0 (3) Å3
Data collection top
Agilent SuperNova Dual
diffractometer with an Atlas detector
20465 independent reflections
Radiation source: SuperNova (Mo) X-ray Source13087 reflections with I > 2σ(I)
Mirror monochromatorRint = 0.041
Detector resolution: 10.4041 pixels mm-1θmax = 27.5°, θmin = 2.3°
ω scansh = 1715
Absorption correction: multi-scan
(CrysAlis PRO; Agilent, 2010)
k = 2525
Tmin = 0.688, Tmax = 0.824l = 2520
38533 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.049Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.133H-atom parameters constrained
S = 1.04 w = 1/[σ2(Fo2) + (0.0374P)2 + 4.321P]
where P = (Fo2 + 2Fc2)/3
20465 reflections(Δ/σ)max = 0.001
1230 parametersΔρmax = 1.47 e Å3
132 restraintsΔρmin = 0.79 e Å3
Crystal data top
(C6H16N)4[H2V10O28]γ = 76.979 (3)°
Mr = 1368.21V = 4613.0 (3) Å3
Triclinic, P1Z = 4
a = 13.1735 (4) ÅMo Kα radiation
b = 20.0061 (7) ŵ = 2.02 mm1
c = 20.2427 (7) ÅT = 100 K
α = 62.669 (3)°0.20 × 0.15 × 0.10 mm
β = 86.263 (3)°
Data collection top
Agilent SuperNova Dual
diffractometer with an Atlas detector
20465 independent reflections
Absorption correction: multi-scan
(CrysAlis PRO; Agilent, 2010)
13087 reflections with I > 2σ(I)
Tmin = 0.688, Tmax = 0.824Rint = 0.041
38533 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.049132 restraints
wR(F2) = 0.133H-atom parameters constrained
S = 1.04Δρmax = 1.47 e Å3
20465 reflectionsΔρmin = 0.79 e Å3
1230 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
V10.77694 (5)0.48056 (4)0.19071 (4)0.01186 (15)
V20.64243 (5)0.35842 (4)0.26737 (4)0.00949 (15)
V30.49939 (5)0.24453 (4)0.34541 (4)0.01232 (15)
V40.30463 (5)0.37271 (4)0.26944 (4)0.01214 (15)
V50.43466 (5)0.49681 (4)0.19648 (4)0.00913 (15)
V60.57976 (5)0.60703 (4)0.12594 (4)0.01115 (15)
V70.62844 (5)0.45585 (4)0.09648 (4)0.00919 (15)
V80.48033 (5)0.33937 (4)0.17231 (4)0.00959 (15)
V90.60521 (5)0.50398 (4)0.29472 (4)0.01161 (15)
V100.45934 (5)0.39236 (4)0.36584 (4)0.01140 (15)
V110.71402 (5)0.02601 (4)0.81411 (4)0.01270 (15)
V120.84886 (5)0.14660 (4)0.73596 (4)0.00935 (15)
V130.99257 (5)0.25928 (4)0.65730 (4)0.01173 (15)
V141.18718 (5)0.12853 (4)0.72405 (4)0.01212 (15)
V151.05599 (5)0.00684 (4)0.79868 (4)0.00968 (15)
V160.91101 (5)0.10410 (4)0.87182 (4)0.01230 (15)
V170.87818 (5)0.00486 (4)0.70336 (4)0.01267 (15)
V181.02116 (5)0.11650 (4)0.62872 (4)0.01241 (15)
V190.87140 (5)0.04489 (4)0.90605 (4)0.00972 (15)
V201.02180 (5)0.15933 (4)0.82893 (4)0.00976 (15)
O10.9002 (2)0.47302 (16)0.19015 (15)0.0167 (6)
O20.7239 (2)0.58138 (15)0.13065 (14)0.0134 (6)
O30.5482 (2)0.69759 (15)0.06765 (14)0.0145 (6)
O40.4329 (2)0.59004 (15)0.13614 (14)0.0124 (6)
O50.3104 (2)0.48724 (15)0.20236 (14)0.0130 (6)
O60.1800 (2)0.38170 (17)0.26912 (15)0.0169 (6)
O70.3571 (2)0.27151 (16)0.33046 (14)0.0139 (6)
O80.5246 (2)0.15373 (16)0.40010 (15)0.0182 (7)
O90.6476 (2)0.26382 (15)0.32380 (14)0.0121 (6)
O100.7667 (2)0.36935 (15)0.25483 (14)0.0121 (6)
O110.5996 (2)0.47965 (15)0.19271 (14)0.0101 (6)
O120.4799 (2)0.37827 (15)0.25905 (14)0.0095 (6)
O130.7568 (2)0.45384 (15)0.11218 (14)0.0110 (6)
O140.3377 (2)0.36151 (15)0.18450 (14)0.0117 (6)
O150.5855 (2)0.56775 (15)0.05089 (14)0.0112 (6)
H150.57120.59610.00520.017*
O160.6266 (2)0.44679 (15)0.02124 (14)0.0125 (6)
O170.4674 (2)0.46055 (15)0.11595 (14)0.0093 (6)
H170.42720.48470.07780.014*
O180.4837 (2)0.32842 (15)0.09755 (14)0.0135 (6)
O190.5097 (2)0.24799 (15)0.24725 (14)0.0115 (6)
O200.6233 (2)0.35625 (15)0.17384 (14)0.0106 (6)
O210.7416 (2)0.49103 (16)0.27595 (14)0.0140 (6)
O220.5725 (2)0.60376 (15)0.21513 (14)0.0123 (6)
O230.4558 (2)0.49871 (15)0.28460 (14)0.0115 (6)
O240.3275 (2)0.39811 (16)0.34592 (14)0.0142 (6)
O250.4972 (2)0.28613 (15)0.40824 (14)0.0140 (6)
O260.4561 (2)0.40915 (16)0.43642 (14)0.0158 (6)
O270.6107 (2)0.39441 (15)0.33944 (14)0.0119 (6)
O280.6005 (2)0.51805 (16)0.36690 (15)0.0165 (6)
O290.7669 (2)0.07452 (15)0.86913 (15)0.0137 (6)
O300.5907 (2)0.03358 (16)0.81715 (15)0.0178 (6)
O310.7244 (2)0.13831 (15)0.75029 (14)0.0131 (6)
O320.9684 (2)0.35063 (16)0.60587 (15)0.0166 (6)
O330.8472 (2)0.24138 (15)0.68300 (14)0.0120 (6)
O341.1353 (2)0.23117 (15)0.66626 (14)0.0127 (6)
O351.3102 (2)0.12123 (16)0.71899 (15)0.0164 (6)
O361.1812 (2)0.01466 (15)0.78935 (15)0.0130 (6)
O371.0575 (2)0.08693 (15)0.85708 (14)0.0121 (6)
O380.9343 (2)0.19435 (16)0.92642 (16)0.0185 (7)
O390.8912 (2)0.02654 (15)0.80575 (14)0.0107 (6)
O401.0128 (2)0.12615 (15)0.73946 (14)0.0110 (6)
O410.7417 (2)0.01906 (16)0.72553 (15)0.0139 (6)
O420.8759 (2)0.00794 (17)0.63138 (15)0.0191 (7)
O430.8729 (2)0.11523 (15)0.65973 (14)0.0124 (6)
O441.0201 (2)0.10541 (16)0.55509 (15)0.0176 (6)
O450.9883 (2)0.22217 (16)0.59116 (14)0.0138 (6)
O461.1563 (2)0.10872 (16)0.64621 (14)0.0138 (6)
O471.0280 (2)0.00889 (15)0.70875 (14)0.0115 (6)
O480.9115 (2)0.09615 (16)0.77991 (15)0.0142 (6)
O490.7417 (2)0.04857 (15)0.89374 (14)0.0131 (6)
O500.8769 (2)0.14513 (15)0.83057 (14)0.0097 (6)
O510.9921 (2)0.25453 (15)0.75635 (14)0.0120 (6)
O521.1606 (2)0.13761 (15)0.81181 (14)0.0119 (6)
O531.0255 (2)0.16673 (15)0.90495 (14)0.0133 (6)
O541.0318 (2)0.03896 (15)0.88213 (14)0.0098 (6)
H541.07390.01320.91910.015*
O550.8771 (2)0.05317 (15)0.98159 (14)0.0127 (6)
O560.9129 (2)0.06647 (15)0.94731 (14)0.0128 (6)
H560.92990.09590.99250.019*
N10.3270 (3)0.7559 (2)0.01839 (19)0.0174 (8)
H10.39350.73660.03180.021*
N20.1601 (3)0.3797 (2)0.10687 (18)0.0172 (8)
H20.21820.37340.13020.021*
N30.5922 (3)0.01294 (19)0.66663 (19)0.0173 (8)
H30.63840.00250.68790.021*
N40.8593 (7)0.1626 (4)0.3509 (4)0.041 (2)0.627 (10)
H40.79480.18490.35450.050*0.627 (10)
N4'0.8484 (12)0.1702 (7)0.3354 (6)0.041*0.373 (10)
H4'0.78370.18890.34230.050*0.373 (10)
N50.6502 (3)0.3714 (3)0.5262 (3)0.0225 (12)0.776 (4)
H50.62430.40140.48040.027*0.776 (4)
N5'0.6922 (10)0.3397 (7)0.5707 (7)0.022*0.224 (4)
H5'0.74450.31640.60410.027*0.224 (4)
N60.9823 (3)0.4006 (2)0.74805 (18)0.0172 (8)
H60.99580.35470.74980.021*
N71.1956 (3)0.2586 (2)0.5087 (2)0.0247 (9)
H71.16410.23500.55000.030*
N81.3126 (2)0.16130 (15)0.88166 (15)0.0182 (8)
H81.25560.16170.86100.022*
C10.2940 (2)0.70526 (15)0.00914 (15)0.0241 (11)
H1A0.33350.70860.05350.029*
H1B0.31190.65100.03000.029*
C20.1789 (4)0.7274 (3)0.0292 (3)0.0345 (13)
H2A0.16170.69300.04680.052*
H2B0.16090.78080.06860.052*
H2C0.13930.72300.01480.052*
C30.3195 (4)0.8377 (3)0.0415 (2)0.0246 (11)
H3A0.24790.85890.06440.029*
H3B0.33190.86950.01830.029*
C40.3959 (4)0.8441 (3)0.1014 (3)0.0301 (12)
H4A0.38700.89820.13870.045*
H4B0.38330.81350.12520.045*
H4C0.46710.82460.07940.045*
C50.2721 (4)0.7530 (3)0.0870 (2)0.0255 (11)
H5A0.25450.70190.11580.031*
H5B0.20620.79270.07200.031*
C60.3388 (4)0.7666 (3)0.1360 (3)0.0313 (12)
H6A0.30040.76460.17980.047*
H6B0.35560.81740.10790.047*
H6C0.40340.72670.15200.047*
C70.0947 (3)0.4578 (2)0.0931 (2)0.0198 (10)
H7A0.03230.46970.06160.024*
H7B0.07050.45560.14130.024*
C80.1528 (3)0.5219 (2)0.0556 (2)0.0207 (10)
H8A0.10670.57090.04820.031*
H8B0.17550.52530.00730.031*
H8C0.21380.51110.08710.031*
C90.1908 (3)0.3753 (3)0.0361 (2)0.0190 (10)
H9A0.23100.41510.00700.023*
H9B0.12700.38690.00600.023*
C100.2556 (3)0.2969 (2)0.0498 (2)0.0224 (10)
H10A0.27270.29680.00200.034*
H10B0.21600.25730.07830.034*
H10C0.32020.28600.07800.034*
C110.1067 (3)0.3176 (3)0.1589 (2)0.0201 (10)
H11A0.09750.32060.20650.024*
H11B0.15230.26680.16960.024*
C120.0020 (3)0.3225 (3)0.1292 (3)0.0255 (11)
H12A0.02850.28050.16600.038*
H12B0.01050.31810.08280.038*
H12C0.04430.37220.11960.038*
C130.5780 (4)0.0479 (3)0.5879 (3)0.0344 (13)
H13A0.51460.04660.56520.041*
H13B0.63840.03700.55990.041*
C140.5679 (6)0.1267 (3)0.5816 (3)0.065 (2)
H14A0.55760.16500.52900.098*
H14B0.63150.12880.60240.098*
H14C0.50790.13780.60900.098*
C150.6393 (4)0.0902 (3)0.6706 (3)0.0300 (12)
H15A0.70410.08720.64270.036*
H15B0.59010.10410.64660.036*
C160.6642 (4)0.1526 (3)0.7503 (3)0.0517 (17)
H16A0.69400.20220.75060.078*
H16B0.60020.15590.77800.078*
H16C0.71460.13980.77380.078*
C170.4948 (4)0.0111 (3)0.7089 (3)0.0249 (11)
H17A0.46800.04210.70230.030*
H17B0.51260.04510.76250.030*
C180.4092 (4)0.0359 (3)0.6859 (3)0.0282 (11)
H18A0.34840.03270.71580.042*
H18B0.43390.08910.69390.042*
H18C0.38970.00190.63310.042*
C190.8857 (6)0.0872 (4)0.4179 (5)0.038 (3)0.627 (10)
H19A0.92800.09110.45410.046*0.627 (10)
H19B0.92760.04820.40390.046*0.627 (10)
C19'0.8708 (12)0.0864 (6)0.3795 (7)0.038*0.373 (10)
H19C0.94620.06410.38080.046*0.373 (10)
H19D0.83150.06300.35870.046*0.373 (10)
C200.7888 (7)0.0626 (5)0.4525 (5)0.044 (3)0.627 (10)
H20A0.80660.01780.50150.066*0.627 (10)
H20B0.75420.04870.42070.066*0.627 (10)
H20C0.74190.10500.45830.066*0.627 (10)
C20'0.8358 (15)0.0724 (9)0.4570 (6)0.044*0.373 (10)
H20D0.85110.01680.49040.066*0.373 (10)
H20E0.76070.09340.45480.066*0.373 (10)
H20F0.87320.09800.47560.066*0.373 (10)
C210.8633 (9)0.1551 (7)0.2837 (5)0.075 (4)0.627 (10)
H21A0.88680.20030.24440.090*0.627 (10)
H21B0.91830.10900.29170.090*0.627 (10)
C21'0.8587 (15)0.1918 (11)0.2574 (7)0.075*0.373 (10)
H21C0.86050.24720.23060.090*0.373 (10)
H21D0.92630.16230.25080.090*0.373 (10)
C220.7735 (9)0.1488 (8)0.2552 (7)0.080 (4)0.627 (10)
H22A0.79380.12110.22550.120*0.627 (10)
H22B0.73180.20050.22390.120*0.627 (10)
H22C0.73210.12050.29650.120*0.627 (10)
C22'0.7774 (17)0.1792 (15)0.2239 (11)0.080*0.373 (10)
H22D0.78180.20490.16960.120*0.373 (10)
H22E0.70950.20040.23760.120*0.373 (10)
H22F0.78510.12370.24140.120*0.373 (10)
C230.9264 (8)0.2132 (5)0.3466 (6)0.049 (3)0.627 (10)
H23A0.91020.22710.38780.059*0.627 (10)
H23B0.90830.26140.29940.059*0.627 (10)
C23'0.9174 (15)0.2034 (10)0.3591 (11)0.049*0.373 (10)
H23D0.91250.18640.41320.059*0.373 (10)
H23C0.89590.26030.33290.059*0.373 (10)
C241.0387 (8)0.1828 (8)0.3501 (8)0.035 (2)0.627 (10)
H24A1.07510.22500.33430.053*0.627 (10)
H24B1.05470.15860.31710.053*0.627 (10)
H24C1.06160.14440.40130.053*0.627 (10)
C24'1.0264 (13)0.1785 (15)0.3423 (15)0.035*0.373 (10)
H24D1.07180.20300.35620.053*0.373 (10)
H24E1.03050.19380.28890.053*0.373 (10)
H24F1.04880.12230.37050.053*0.373 (10)
C250.6693 (4)0.2917 (3)0.5363 (3)0.0262 (14)0.776 (4)
H25A0.60300.28180.52640.031*0.776 (4)
H25B0.69200.25560.58880.031*0.776 (4)
C25'0.7244 (14)0.3481 (9)0.4959 (7)0.026*0.224 (4)
H25C0.78240.37550.47930.031*0.224 (4)
H25D0.66520.37770.45890.031*0.224 (4)
C260.7509 (6)0.2749 (4)0.4863 (3)0.0245 (17)0.776 (4)
H26A0.75960.22130.49580.037*0.776 (4)
H26B0.81740.28320.49660.037*0.776 (4)
H26C0.72830.30950.43410.037*0.776 (4)
C26'0.759 (3)0.2677 (11)0.5042 (13)0.024*0.224 (4)
H26D0.78240.27000.45650.037*0.224 (4)
H26E0.70030.24190.51980.037*0.224 (4)
H26F0.81630.23890.54180.037*0.224 (4)
C270.5682 (4)0.3843 (3)0.5754 (3)0.0229 (14)0.776 (4)
H27A0.55210.43960.56340.028*0.776 (4)
H27B0.50410.37240.56470.028*0.776 (4)
C27'0.6069 (12)0.2985 (9)0.5915 (8)0.023*0.224 (4)
H27C0.63250.24560.59730.028*0.224 (4)
H27D0.55030.32570.55220.028*0.224 (4)
C280.5969 (5)0.3376 (3)0.6557 (3)0.0261 (14)0.776 (4)
H28A0.53910.34900.68460.039*0.776 (4)
H28B0.65920.35000.66720.039*0.776 (4)
H28C0.61130.28270.66850.039*0.776 (4)
C28'0.5672 (14)0.2959 (12)0.6631 (9)0.026*0.224 (4)
H28D0.50790.27070.67700.039*0.224 (4)
H28E0.54470.34850.65720.039*0.224 (4)
H28F0.62280.26660.70210.039*0.224 (4)
C290.7450 (4)0.3949 (3)0.5310 (3)0.0282 (15)0.776 (4)
H29A0.79300.38870.49350.034*0.776 (4)
H29B0.77960.36010.58070.034*0.776 (4)
C29'0.6463 (13)0.4197 (7)0.5591 (10)0.028*0.224 (4)
H29C0.61880.41930.60600.034*0.224 (4)
H29D0.58880.44480.52060.034*0.224 (4)
C300.7270 (6)0.4775 (3)0.5186 (4)0.0205 (17)0.776 (4)
H30A0.79380.48900.52340.031*0.776 (4)
H30B0.68000.48420.55570.031*0.776 (4)
H30C0.69550.51260.46860.031*0.776 (4)
C30'0.734 (2)0.4615 (11)0.5342 (18)0.020*0.224 (4)
H30D0.70790.51540.52400.031*0.224 (4)
H30E0.76200.45960.48890.031*0.224 (4)
H30F0.78930.43680.57350.031*0.224 (4)
C311.1202 (4)0.2836 (3)0.4447 (3)0.0368 (13)
H31A1.08910.23970.45330.044*
H31B1.15940.29620.39860.044*
C321.0330 (4)0.3525 (3)0.4327 (3)0.0363 (13)
H32A0.98730.36500.39040.054*
H32B1.06270.39690.42240.054*
H32C0.99250.34020.47760.054*
C331.2265 (4)0.3257 (3)0.5115 (3)0.0358 (13)
H33A1.24510.36070.46110.043*
H33B1.16550.35500.52560.043*
C341.3170 (4)0.3020 (3)0.5656 (3)0.0322 (12)
H34A1.33270.34810.56460.048*
H34B1.37830.27410.55140.048*
H34C1.29860.26850.61600.048*
C351.2915 (4)0.2011 (3)0.5072 (3)0.0377 (13)
H35A1.32930.17540.55630.045*
H35B1.33820.22950.46960.045*
C361.2687 (4)0.1394 (3)0.4894 (3)0.0302 (12)
H36A1.33440.10480.48920.045*
H36B1.23260.16410.44040.045*
H36C1.22440.10970.52730.045*
C370.8857 (3)0.4478 (3)0.6989 (2)0.0215 (10)
H37A0.90220.46000.64670.026*
H37B0.86390.49720.70160.026*
C380.7960 (3)0.4071 (3)0.7203 (2)0.0210 (10)
H38A0.73520.44040.68680.032*
H38B0.77830.39570.77160.032*
H38C0.81630.35890.71630.032*
C391.0752 (3)0.4353 (3)0.7183 (2)0.0218 (10)
H39A1.13350.40610.75610.026*
H39B1.05800.48890.71160.026*
C401.1123 (4)0.4367 (3)0.6452 (2)0.0275 (11)
H40A1.17310.46010.63040.041*
H40B1.05630.46690.60670.041*
H40C1.13160.38380.65130.041*
C410.9646 (3)0.3902 (3)0.8260 (2)0.0214 (10)
H41A0.90140.36910.84370.026*
H41B0.95100.44140.82500.026*
C421.0544 (4)0.3377 (3)0.8808 (2)0.0237 (10)
H42A1.03760.33440.92990.035*
H42B1.11730.35830.86410.035*
H42C1.06660.28610.88390.035*
C431.3975 (3)0.0997 (3)0.8767 (2)0.0229 (10)
H43A1.40860.11300.82370.027*
H43B1.46320.09820.89900.027*
C441.3723 (4)0.0214 (3)0.9158 (3)0.0293 (12)
H44A1.42980.01670.91110.044*
H44B1.30810.02220.89330.044*
H44C1.36270.00740.96860.044*
C451.3358 (4)0.2403 (3)0.8381 (2)0.0264 (11)
H45A1.28830.27650.85310.032*
H45B1.40810.23800.85110.032*
C461.3238 (5)0.2706 (3)0.7561 (3)0.0462 (16)
H46A1.33870.32230.73100.069*
H46B1.25230.27340.74280.069*
H46C1.37270.23620.74060.069*
C471.2892 (3)0.1450 (3)0.9610 (2)0.0221 (10)
H47A1.23470.18820.96070.027*
H47B1.26120.09770.98530.027*
C481.3837 (3)0.1345 (3)1.0059 (2)0.0229 (10)
H48A1.36390.12441.05660.034*
H48B1.41120.18140.98270.034*
H48C1.43730.09081.00770.034*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
V10.0087 (4)0.0141 (4)0.0140 (3)0.0032 (3)0.0005 (3)0.0071 (3)
V20.0081 (3)0.0105 (4)0.0087 (3)0.0013 (3)0.0000 (3)0.0036 (3)
V30.0122 (4)0.0115 (4)0.0105 (3)0.0032 (3)0.0004 (3)0.0025 (3)
V40.0090 (4)0.0154 (4)0.0115 (3)0.0037 (3)0.0019 (3)0.0054 (3)
V50.0085 (3)0.0097 (3)0.0082 (3)0.0014 (3)0.0002 (3)0.0036 (3)
V60.0117 (4)0.0100 (4)0.0119 (3)0.0028 (3)0.0003 (3)0.0048 (3)
V70.0083 (3)0.0103 (3)0.0087 (3)0.0025 (3)0.0008 (3)0.0039 (3)
V80.0094 (3)0.0104 (4)0.0093 (3)0.0032 (3)0.0013 (3)0.0045 (3)
V90.0117 (4)0.0146 (4)0.0100 (3)0.0037 (3)0.0003 (3)0.0065 (3)
V100.0107 (4)0.0140 (4)0.0091 (3)0.0031 (3)0.0020 (3)0.0050 (3)
V110.0086 (4)0.0145 (4)0.0154 (4)0.0034 (3)0.0008 (3)0.0068 (3)
V120.0075 (3)0.0091 (3)0.0101 (3)0.0008 (3)0.0004 (3)0.0037 (3)
V130.0120 (4)0.0098 (4)0.0112 (3)0.0026 (3)0.0016 (3)0.0030 (3)
V140.0097 (4)0.0122 (4)0.0140 (4)0.0035 (3)0.0018 (3)0.0053 (3)
V150.0075 (3)0.0097 (4)0.0120 (3)0.0023 (3)0.0013 (3)0.0051 (3)
V160.0115 (4)0.0103 (4)0.0153 (4)0.0037 (3)0.0014 (3)0.0056 (3)
V170.0111 (4)0.0154 (4)0.0147 (4)0.0050 (3)0.0015 (3)0.0088 (3)
V180.0126 (4)0.0142 (4)0.0117 (3)0.0050 (3)0.0029 (3)0.0064 (3)
V190.0088 (3)0.0095 (3)0.0097 (3)0.0017 (3)0.0012 (3)0.0036 (3)
V200.0097 (3)0.0090 (3)0.0101 (3)0.0020 (3)0.0002 (3)0.0040 (3)
O10.0113 (15)0.0226 (17)0.0195 (15)0.0052 (13)0.0014 (12)0.0117 (14)
O20.0139 (15)0.0157 (15)0.0138 (14)0.0070 (12)0.0037 (12)0.0081 (13)
O30.0166 (16)0.0113 (15)0.0135 (14)0.0017 (12)0.0011 (12)0.0045 (12)
O40.0130 (15)0.0115 (15)0.0126 (14)0.0014 (12)0.0004 (11)0.0058 (12)
O50.0116 (15)0.0160 (15)0.0131 (14)0.0017 (12)0.0002 (11)0.0085 (13)
O60.0126 (15)0.0227 (17)0.0168 (15)0.0061 (13)0.0041 (12)0.0096 (14)
O70.0123 (15)0.0164 (16)0.0117 (14)0.0049 (12)0.0004 (11)0.0046 (13)
O80.0208 (17)0.0158 (16)0.0158 (15)0.0063 (13)0.0010 (12)0.0043 (13)
O90.0095 (14)0.0117 (15)0.0143 (14)0.0012 (12)0.0000 (11)0.0058 (12)
O100.0111 (15)0.0109 (14)0.0132 (14)0.0003 (12)0.0001 (11)0.0054 (12)
O110.0096 (14)0.0101 (14)0.0097 (13)0.0036 (11)0.0002 (11)0.0030 (12)
O120.0084 (14)0.0105 (14)0.0085 (13)0.0030 (11)0.0007 (11)0.0031 (12)
O130.0108 (14)0.0119 (15)0.0094 (13)0.0020 (11)0.0006 (11)0.0042 (12)
O140.0110 (15)0.0143 (15)0.0104 (14)0.0039 (12)0.0029 (11)0.0059 (12)
O150.0137 (15)0.0115 (15)0.0072 (13)0.0033 (12)0.0014 (11)0.0032 (12)
O160.0121 (15)0.0137 (15)0.0120 (14)0.0015 (12)0.0019 (11)0.0068 (12)
O170.0074 (14)0.0118 (14)0.0073 (13)0.0031 (11)0.0011 (10)0.0024 (12)
O180.0135 (15)0.0153 (15)0.0142 (14)0.0036 (12)0.0003 (12)0.0088 (13)
O190.0118 (15)0.0096 (14)0.0120 (14)0.0025 (11)0.0002 (11)0.0037 (12)
O200.0087 (14)0.0118 (15)0.0123 (14)0.0017 (11)0.0007 (11)0.0065 (12)
O210.0119 (15)0.0170 (16)0.0148 (14)0.0037 (12)0.0005 (12)0.0082 (13)
O220.0097 (14)0.0136 (15)0.0153 (14)0.0022 (12)0.0022 (11)0.0083 (13)
O230.0112 (15)0.0135 (15)0.0123 (14)0.0032 (12)0.0013 (11)0.0079 (12)
O240.0152 (15)0.0162 (16)0.0122 (14)0.0048 (12)0.0039 (12)0.0070 (13)
O250.0156 (16)0.0133 (15)0.0101 (14)0.0058 (12)0.0027 (11)0.0020 (12)
O260.0162 (16)0.0207 (16)0.0103 (14)0.0051 (13)0.0025 (12)0.0067 (13)
O270.0102 (14)0.0145 (15)0.0097 (13)0.0036 (12)0.0006 (11)0.0039 (12)
O280.0153 (16)0.0216 (17)0.0131 (14)0.0018 (13)0.0033 (12)0.0089 (13)
O290.0121 (15)0.0151 (15)0.0161 (15)0.0056 (12)0.0041 (12)0.0081 (13)
O300.0118 (15)0.0196 (16)0.0212 (16)0.0058 (13)0.0013 (12)0.0075 (14)
O310.0125 (15)0.0147 (15)0.0120 (14)0.0018 (12)0.0005 (11)0.0066 (13)
O320.0167 (16)0.0135 (15)0.0166 (15)0.0032 (12)0.0019 (12)0.0046 (13)
O330.0100 (14)0.0118 (15)0.0115 (14)0.0019 (12)0.0012 (11)0.0034 (12)
O340.0112 (15)0.0131 (15)0.0131 (14)0.0037 (12)0.0021 (11)0.0052 (12)
O350.0126 (15)0.0163 (16)0.0228 (16)0.0066 (12)0.0036 (12)0.0099 (14)
O360.0121 (15)0.0112 (15)0.0176 (15)0.0024 (12)0.0000 (12)0.0082 (13)
O370.0101 (14)0.0100 (14)0.0158 (14)0.0015 (11)0.0003 (11)0.0057 (12)
O380.0156 (16)0.0144 (16)0.0254 (16)0.0056 (13)0.0044 (13)0.0084 (14)
O390.0073 (14)0.0111 (15)0.0138 (14)0.0024 (11)0.0015 (11)0.0058 (12)
O400.0069 (14)0.0124 (15)0.0142 (14)0.0027 (11)0.0022 (11)0.0064 (12)
O410.0116 (15)0.0160 (16)0.0150 (14)0.0049 (12)0.0011 (12)0.0072 (13)
O420.0222 (17)0.0225 (17)0.0185 (15)0.0071 (14)0.0032 (13)0.0136 (14)
O430.0106 (15)0.0154 (15)0.0116 (14)0.0030 (12)0.0001 (11)0.0065 (12)
O440.0205 (17)0.0201 (16)0.0169 (15)0.0069 (13)0.0042 (13)0.0117 (14)
O450.0134 (15)0.0171 (16)0.0094 (14)0.0049 (12)0.0032 (11)0.0043 (12)
O460.0135 (15)0.0156 (15)0.0129 (14)0.0061 (12)0.0043 (12)0.0063 (13)
O470.0123 (15)0.0118 (15)0.0130 (14)0.0045 (12)0.0034 (11)0.0074 (12)
O480.0115 (15)0.0148 (15)0.0200 (15)0.0049 (12)0.0023 (12)0.0104 (13)
O490.0109 (15)0.0114 (15)0.0133 (14)0.0002 (12)0.0011 (11)0.0035 (12)
O500.0086 (14)0.0088 (14)0.0104 (13)0.0003 (11)0.0011 (11)0.0038 (12)
O510.0131 (15)0.0105 (14)0.0125 (14)0.0037 (12)0.0029 (11)0.0050 (12)
O520.0096 (14)0.0127 (15)0.0148 (14)0.0048 (12)0.0015 (11)0.0066 (12)
O530.0136 (15)0.0140 (15)0.0136 (14)0.0026 (12)0.0013 (11)0.0075 (13)
O540.0085 (14)0.0094 (14)0.0110 (13)0.0004 (11)0.0022 (11)0.0048 (12)
O550.0113 (15)0.0135 (15)0.0118 (14)0.0012 (12)0.0003 (11)0.0050 (12)
O560.0158 (15)0.0087 (14)0.0098 (14)0.0009 (12)0.0013 (11)0.0015 (12)
N10.0117 (18)0.019 (2)0.0218 (19)0.0027 (15)0.0009 (15)0.0101 (17)
N20.0140 (19)0.024 (2)0.0158 (18)0.0059 (16)0.0002 (15)0.0098 (17)
N30.019 (2)0.017 (2)0.0195 (19)0.0023 (16)0.0029 (15)0.0111 (17)
N40.031 (4)0.048 (4)0.030 (4)0.010 (3)0.012 (3)0.012 (3)
N50.021 (2)0.025 (3)0.024 (2)0.005 (2)0.003 (2)0.014 (2)
N60.022 (2)0.0135 (19)0.0182 (19)0.0040 (16)0.0012 (15)0.0089 (16)
N70.030 (2)0.028 (2)0.0151 (19)0.0117 (19)0.0109 (17)0.0086 (18)
N80.0159 (19)0.0147 (19)0.0193 (19)0.0046 (15)0.0026 (15)0.0029 (16)
C10.025 (3)0.016 (2)0.031 (3)0.000 (2)0.010 (2)0.011 (2)
C20.029 (3)0.025 (3)0.040 (3)0.013 (2)0.013 (2)0.003 (2)
C30.027 (3)0.018 (2)0.029 (3)0.010 (2)0.002 (2)0.009 (2)
C40.039 (3)0.030 (3)0.025 (3)0.013 (2)0.005 (2)0.015 (2)
C50.024 (3)0.022 (3)0.025 (3)0.000 (2)0.007 (2)0.009 (2)
C60.032 (3)0.037 (3)0.027 (3)0.005 (2)0.007 (2)0.022 (2)
C70.017 (2)0.022 (2)0.018 (2)0.0051 (19)0.0010 (18)0.012 (2)
C80.019 (2)0.022 (2)0.019 (2)0.0033 (19)0.0032 (18)0.008 (2)
C90.018 (2)0.025 (3)0.014 (2)0.0072 (19)0.0040 (18)0.009 (2)
C100.021 (3)0.024 (3)0.027 (3)0.009 (2)0.008 (2)0.015 (2)
C110.017 (2)0.028 (3)0.016 (2)0.010 (2)0.0028 (18)0.009 (2)
C120.017 (2)0.028 (3)0.036 (3)0.005 (2)0.003 (2)0.018 (2)
C130.039 (3)0.041 (3)0.021 (3)0.014 (3)0.007 (2)0.009 (2)
C140.102 (6)0.026 (3)0.051 (4)0.025 (3)0.049 (4)0.008 (3)
C150.017 (3)0.029 (3)0.054 (3)0.003 (2)0.001 (2)0.029 (3)
C160.040 (4)0.024 (3)0.086 (5)0.002 (3)0.036 (3)0.020 (3)
C170.024 (3)0.028 (3)0.026 (3)0.002 (2)0.001 (2)0.016 (2)
C180.020 (3)0.036 (3)0.037 (3)0.006 (2)0.005 (2)0.023 (3)
C190.024 (4)0.047 (4)0.030 (4)0.012 (3)0.007 (3)0.005 (3)
C200.030 (4)0.049 (4)0.036 (4)0.016 (3)0.010 (3)0.004 (3)
C210.074 (6)0.096 (6)0.079 (5)0.012 (4)0.012 (4)0.063 (5)
C220.073 (6)0.077 (6)0.110 (6)0.010 (4)0.013 (4)0.063 (5)
C230.050 (5)0.040 (4)0.040 (5)0.008 (3)0.020 (4)0.013 (4)
C240.045 (4)0.037 (4)0.036 (4)0.017 (3)0.017 (3)0.022 (3)
C250.028 (3)0.024 (3)0.026 (3)0.000 (2)0.006 (2)0.012 (2)
C260.029 (3)0.032 (3)0.015 (3)0.001 (2)0.010 (3)0.015 (3)
C270.019 (3)0.025 (3)0.024 (3)0.002 (2)0.002 (2)0.012 (2)
C280.026 (3)0.028 (3)0.025 (3)0.003 (2)0.000 (2)0.014 (2)
C290.025 (3)0.028 (3)0.030 (3)0.001 (2)0.002 (2)0.013 (3)
C300.021 (3)0.015 (3)0.020 (4)0.001 (2)0.002 (2)0.006 (3)
C310.040 (3)0.044 (3)0.024 (3)0.015 (3)0.005 (2)0.012 (3)
C320.045 (3)0.028 (3)0.025 (3)0.008 (3)0.005 (2)0.002 (2)
C330.045 (4)0.038 (3)0.031 (3)0.021 (3)0.019 (3)0.019 (3)
C340.035 (3)0.038 (3)0.032 (3)0.025 (3)0.012 (2)0.017 (3)
C350.025 (3)0.059 (4)0.031 (3)0.009 (3)0.007 (2)0.023 (3)
C360.032 (3)0.036 (3)0.028 (3)0.009 (2)0.008 (2)0.019 (2)
C370.026 (3)0.018 (2)0.018 (2)0.001 (2)0.0023 (19)0.009 (2)
C380.018 (2)0.023 (3)0.024 (2)0.0036 (19)0.0025 (19)0.015 (2)
C390.021 (2)0.025 (3)0.022 (2)0.012 (2)0.0060 (19)0.011 (2)
C400.024 (3)0.035 (3)0.028 (3)0.011 (2)0.009 (2)0.017 (2)
C410.022 (2)0.024 (3)0.018 (2)0.003 (2)0.0024 (19)0.010 (2)
C420.024 (3)0.025 (3)0.019 (2)0.008 (2)0.0024 (19)0.007 (2)
C430.016 (2)0.031 (3)0.025 (2)0.002 (2)0.0003 (19)0.016 (2)
C440.024 (3)0.024 (3)0.045 (3)0.004 (2)0.008 (2)0.023 (3)
C450.031 (3)0.021 (3)0.027 (3)0.008 (2)0.004 (2)0.009 (2)
C460.075 (5)0.031 (3)0.034 (3)0.025 (3)0.014 (3)0.008 (3)
C470.020 (2)0.023 (3)0.024 (2)0.005 (2)0.0017 (19)0.012 (2)
C480.023 (3)0.028 (3)0.017 (2)0.009 (2)0.0019 (19)0.008 (2)
Geometric parameters (Å, º) top
V1—O11.596 (3)C3—H3B0.9900
V1—O21.805 (3)C4—H4A0.9800
V1—O211.850 (3)C4—H4B0.9800
V1—O131.945 (3)C4—H4C0.9800
V1—O102.028 (3)C5—C61.516 (6)
V1—O112.338 (3)C5—H5A0.9900
V2—O101.688 (3)C5—H5B0.9900
V2—O91.691 (3)C6—H6A0.9800
V2—O271.890 (3)C6—H6B0.9800
V2—O201.948 (3)C6—H6C0.9800
V2—O122.091 (3)C7—C81.510 (6)
V2—O112.148 (3)C7—H7A0.9900
V3—O81.602 (3)C7—H7B0.9900
V3—O251.807 (3)C8—H8A0.9800
V3—O71.834 (3)C8—H8B0.9800
V3—O191.953 (3)C8—H8C0.9800
V3—O92.055 (3)C9—C101.514 (6)
V3—O122.395 (3)C9—H9A0.9900
V4—O61.611 (3)C9—H9B0.9900
V4—O71.813 (3)C10—H10A0.9800
V4—O141.846 (3)C10—H10B0.9800
V4—O241.897 (3)C10—H10C0.9800
V4—O52.076 (3)C11—C121.506 (6)
V4—O122.328 (3)C11—H11A0.9900
V5—O51.680 (3)C11—H11B0.9900
V5—O41.692 (3)C12—H12A0.9800
V5—O231.842 (3)C12—H12B0.9800
V5—O172.055 (3)C12—H12C0.9800
V5—O122.070 (3)C13—C141.496 (7)
V5—O112.124 (3)C13—H13A0.9900
V6—O31.615 (3)C13—H13B0.9900
V6—O221.773 (3)C14—H14A0.9800
V6—O21.849 (3)C14—H14B0.9800
V6—O151.997 (3)C14—H14C0.9800
V6—O42.021 (3)C15—C161.518 (7)
V6—O112.230 (3)C15—H15A0.9900
V7—O161.617 (3)C15—H15B0.9900
V7—O131.728 (3)C16—H16A0.9800
V7—O201.900 (3)C16—H16B0.9800
V7—O151.945 (3)C16—H16C0.9800
V7—O172.122 (3)C17—C181.504 (6)
V7—O112.200 (3)C17—H17A0.9900
V8—O181.622 (3)C17—H17B0.9900
V8—O191.733 (3)C18—H18A0.9800
V8—O141.859 (3)C18—H18B0.9800
V8—O201.991 (3)C18—H18C0.9800
V8—O172.123 (3)C19—C201.488 (8)
V8—O122.223 (3)C19—H19A0.9900
V9—O281.605 (3)C19—H19B0.9900
V9—O211.797 (3)C19'—C20'1.519 (9)
V9—O221.875 (3)C19'—H19C0.9900
V9—O271.935 (3)C19'—H19D0.9900
V9—O232.024 (3)C20—H20A0.9800
V9—O112.338 (3)C20—H20B0.9800
V10—O261.607 (3)C20—H20C0.9800
V10—O241.776 (3)C20'—H20D0.9800
V10—O251.845 (3)C20'—H20E0.9800
V10—O231.996 (3)C20'—H20F0.9800
V10—O272.035 (3)C21—C221.404 (8)
V10—O122.297 (3)C21—H21A0.9900
V11—O301.597 (3)C21—H21B0.9900
V11—O291.784 (3)C21'—C22'1.430 (10)
V11—O411.868 (3)C21'—H21C0.9900
V11—O491.938 (3)C21'—H21D0.9900
V11—O312.046 (3)C22—H22A0.9800
V11—O392.332 (3)C22—H22B0.9800
V12—O311.678 (3)C22—H22C0.9800
V12—O331.692 (3)C22'—H22D0.9800
V12—O431.900 (3)C22'—H22E0.9800
V12—O501.960 (3)C22'—H22F0.9800
V12—O402.106 (3)C23—C241.460 (8)
V12—O392.112 (3)C23—H23A0.9900
V13—O321.600 (3)C23—H23B0.9900
V13—O451.813 (3)C23'—C24'1.481 (10)
V13—O341.832 (3)C23'—H23D0.9900
V13—O511.963 (3)C23'—H23C0.9900
V13—O332.018 (3)C24—H24A0.9800
V13—O402.367 (3)C24—H24B0.9800
V14—O351.595 (3)C24—H24C0.9800
V14—O341.822 (3)C24'—H24D0.9800
V14—O521.870 (3)C24'—H24E0.9800
V14—O461.880 (3)C24'—H24F0.9800
V14—O362.060 (3)C25—C261.516 (7)
V14—O402.306 (3)C25—H25A0.9900
V15—O361.682 (3)C25—H25B0.9900
V15—O371.693 (3)C25'—C26'1.501 (10)
V15—O471.861 (3)C25'—H25C0.9900
V15—O542.050 (3)C25'—H25D0.9900
V15—O402.076 (3)C26—H26A0.9800
V15—O392.124 (3)C26—H26B0.9800
V16—O381.593 (3)C26—H26C0.9800
V16—O481.793 (3)C26'—H26D0.9800
V16—O291.853 (3)C26'—H26E0.9800
V16—O561.993 (3)C26'—H26F0.9800
V16—O372.015 (3)C27—C281.478 (6)
V16—O392.284 (3)C27—H27A0.9900
V17—O421.594 (3)C27—H27B0.9900
V17—O411.815 (3)C27'—C28'1.490 (10)
V17—O481.868 (3)C27'—H27C0.9900
V17—O431.952 (3)C27'—H27D0.9900
V17—O472.006 (3)C28—H28A0.9800
V17—O392.328 (3)C28—H28B0.9800
V18—O441.606 (3)C28—H28C0.9800
V18—O461.796 (3)C28'—H28D0.9800
V18—O451.841 (3)C28'—H28E0.9800
V18—O471.999 (3)C28'—H28F0.9800
V18—O432.014 (3)C29—C301.516 (6)
V18—O402.330 (3)C29—H29A0.9900
V19—O551.620 (3)C29—H29B0.9900
V19—O491.722 (3)C29'—C30'1.504 (10)
V19—O501.897 (3)C29'—H29C0.9900
V19—O561.940 (3)C29'—H29D0.9900
V19—O542.125 (3)C30—H30A0.9800
V19—O392.213 (3)C30—H30B0.9800
V20—O531.617 (3)C30—H30C0.9800
V20—O511.763 (3)C30'—H30D0.9800
V20—O521.830 (3)C30'—H30E0.9800
V20—O501.989 (3)C30'—H30F0.9800
V20—O542.114 (3)C31—C321.516 (7)
V20—O402.214 (3)C31—H31A0.9900
O15—H150.8400C31—H31B0.9900
O17—H170.8400C32—H32A0.9800
O54—H540.8400C32—H32B0.9800
O56—H560.8400C32—H32C0.9800
N1—C51.506 (5)C33—C341.512 (7)
N1—C11.508 (4)C33—H33A0.9900
N1—C31.509 (5)C33—H33B0.9900
N1—H10.8800C34—H34A0.9800
N2—C111.498 (5)C34—H34B0.9800
N2—C91.499 (5)C34—H34C0.9800
N2—C71.512 (5)C35—C361.527 (7)
N2—H20.8800C35—H35A0.9900
N3—C131.487 (5)C35—H35B0.9900
N3—C151.497 (5)C36—H36A0.9800
N3—C171.499 (5)C36—H36B0.9800
N3—H30.8800C36—H36C0.9800
N4—C211.432 (8)C37—C381.514 (6)
N4—C231.459 (7)C37—H37A0.9900
N4—C191.477 (7)C37—H37B0.9900
N4—H40.8800C38—H38A0.9800
N4'—C21'1.439 (9)C38—H38B0.9800
N4'—C23'1.455 (9)C38—H38C0.9800
N4'—C19'1.461 (9)C39—C401.519 (6)
N4'—H4'0.8800C39—H39A0.9900
N5—C291.454 (6)C39—H39B0.9900
N5—C251.476 (5)C40—H40A0.9800
N5—C271.480 (5)C40—H40B0.9800
N5—H50.8800C40—H40C0.9800
N5'—C27'1.469 (9)C41—C421.508 (6)
N5'—C29'1.489 (9)C41—H41A0.9900
N5'—C25'1.489 (9)C41—H41B0.9900
N5'—H5'0.8800C42—H42A0.9800
N6—C391.498 (5)C42—H42B0.9800
N6—C411.503 (5)C42—H42C0.9800
N6—C371.504 (5)C43—C441.501 (6)
N6—H60.8800C43—H43A0.9900
N7—C311.504 (6)C43—H43B0.9900
N7—C351.513 (6)C44—H44A0.9800
N7—C331.515 (6)C44—H44B0.9800
N7—H70.8800C44—H44C0.9800
N8—C431.502 (5)C45—C461.488 (6)
N8—C451.506 (5)C45—H45A0.9900
N8—C471.509 (5)C45—H45B0.9900
N8—H80.8800C46—H46A0.9800
C1—C21.508 (5)C46—H46B0.9800
C1—H1A0.9900C46—H46C0.9800
C1—H1B0.9900C47—C481.508 (6)
C2—H2A0.9800C47—H47A0.9900
C2—H2B0.9800C47—H47B0.9900
C2—H2C0.9800C48—H48A0.9800
C3—C41.503 (6)C48—H48B0.9800
C3—H3A0.9900C48—H48C0.9800
O1—V1—O2104.40 (14)V16—O56—H56123.4
O1—V1—O21102.78 (13)C5—N1—C1112.7 (3)
O2—V1—O2192.67 (12)C5—N1—C3111.9 (3)
O1—V1—O13100.67 (13)C1—N1—C3113.1 (3)
O2—V1—O1391.25 (11)C5—N1—H1106.2
O21—V1—O13154.43 (12)C1—N1—H1106.2
O1—V1—O10101.55 (13)C3—N1—H1106.2
O2—V1—O10153.89 (12)C11—N2—C9114.1 (3)
O21—V1—O1084.32 (11)C11—N2—C7109.8 (3)
O13—V1—O1081.13 (11)C9—N2—C7112.6 (3)
O1—V1—O11174.52 (12)C11—N2—H2106.6
O2—V1—O1180.22 (11)C9—N2—H2106.6
O21—V1—O1179.72 (11)C7—N2—H2106.6
O13—V1—O1176.08 (10)C13—N3—C15110.5 (4)
O10—V1—O1173.72 (10)C13—N3—C17112.6 (4)
O10—V2—O9106.94 (13)C15—N3—C17113.9 (3)
O10—V2—O2797.70 (12)C13—N3—H3106.4
O9—V2—O2798.10 (12)C15—N3—H3106.4
O10—V2—O2096.18 (12)C17—N3—H3106.4
O9—V2—O2096.89 (12)C21—N4—C23109.9 (6)
O27—V2—O20155.62 (12)C21—N4—C19112.3 (7)
O10—V2—O12163.29 (12)C23—N4—C19111.6 (5)
O9—V2—O1289.61 (12)C21—N4—H4107.6
O27—V2—O1281.83 (11)C23—N4—H4107.6
O20—V2—O1279.16 (10)C19—N4—H4107.6
O10—V2—O1185.72 (12)C21'—N4'—C23'110.0 (8)
O9—V2—O11167.15 (12)C21'—N4'—C19'110.8 (9)
O27—V2—O1181.93 (11)C23'—N4'—C19'110.7 (8)
O20—V2—O1179.22 (10)C21'—N4'—H4'108.4
O12—V2—O1177.66 (10)C23'—N4'—H4'108.4
O8—V3—O25103.01 (13)C19'—N4'—H4'108.4
O8—V3—O7104.72 (14)C29—N5—C25113.2 (4)
O25—V3—O793.32 (12)C29—N5—C27113.9 (4)
O8—V3—O19102.39 (13)C25—N5—C27110.9 (4)
O25—V3—O19153.24 (12)C29—N5—H5106.0
O7—V3—O1988.24 (11)C25—N5—H5106.0
O8—V3—O9100.74 (13)C27—N5—H5106.0
O25—V3—O985.47 (11)C27'—N5'—C29'106.8 (8)
O7—V3—O9154.09 (12)C27'—N5'—C25'107.2 (8)
O19—V3—O981.69 (11)C29'—N5'—C25'105.1 (8)
O8—V3—O12173.91 (13)C27'—N5'—H5'112.4
O25—V3—O1279.06 (10)C29'—N5'—H5'112.4
O7—V3—O1280.75 (11)C25'—N5'—H5'112.4
O19—V3—O1274.84 (10)C39—N6—C41110.2 (3)
O9—V3—O1273.61 (10)C39—N6—C37112.1 (3)
O6—V4—O7104.97 (14)C41—N6—C37110.7 (3)
O6—V4—O14101.65 (13)C39—N6—H6107.9
O7—V4—O1492.98 (12)C41—N6—H6107.9
O6—V4—O24101.85 (13)C37—N6—H6107.9
O7—V4—O2490.39 (12)C31—N7—C35111.1 (4)
O14—V4—O24154.50 (12)C31—N7—C33112.9 (4)
O6—V4—O599.00 (13)C35—N7—C33110.4 (4)
O7—V4—O5155.89 (12)C31—N7—H7107.4
O14—V4—O584.62 (11)C35—N7—H7107.4
O24—V4—O582.08 (11)C33—N7—H7107.4
O6—V4—O12171.96 (13)C43—N8—C45111.9 (3)
O7—V4—O1283.06 (11)C43—N8—C47112.7 (3)
O14—V4—O1277.85 (10)C45—N8—C47110.9 (3)
O24—V4—O1277.49 (10)C43—N8—H8107.0
O5—V4—O1272.97 (10)C45—N8—H8107.0
O5—V5—O4106.57 (13)C47—N8—H8107.0
O5—V5—O23101.53 (12)C2—C1—N1112.8 (3)
O4—V5—O2399.54 (12)C2—C1—H1A109.0
O5—V5—O1793.84 (11)N1—C1—H1A109.0
O4—V5—O1793.43 (11)C2—C1—H1B109.0
O23—V5—O17156.06 (12)N1—C1—H1B109.0
O5—V5—O1288.25 (12)H1A—C1—H1B107.8
O4—V5—O12163.32 (12)C1—C2—H2A109.5
O23—V5—O1284.53 (11)C1—C2—H2B109.5
O17—V5—O1277.65 (10)H2A—C2—H2B109.5
O5—V5—O11165.37 (12)C1—C2—H2C109.5
O4—V5—O1185.68 (12)H2A—C2—H2C109.5
O23—V5—O1183.82 (11)H2B—C2—H2C109.5
O17—V5—O1177.15 (10)C4—C3—N1113.2 (4)
O12—V5—O1178.64 (10)C4—C3—H3A108.9
O3—V6—O22105.10 (13)N1—C3—H3A108.9
O3—V6—O2105.55 (13)C4—C3—H3B108.9
O22—V6—O293.48 (12)N1—C3—H3B108.9
O3—V6—O1596.42 (12)H3A—C3—H3B107.8
O22—V6—O15157.47 (12)C3—C4—H4A109.5
O2—V6—O1586.99 (11)C3—C4—H4B109.5
O3—V6—O495.51 (13)H4A—C4—H4B109.5
O22—V6—O488.42 (11)C3—C4—H4C109.5
O2—V6—O4157.54 (12)H4A—C4—H4C109.5
O15—V6—O482.89 (11)H4B—C4—H4C109.5
O3—V6—O11168.28 (12)N1—C5—C6111.9 (4)
O22—V6—O1182.70 (11)N1—C5—H5A109.2
O2—V6—O1182.32 (11)C6—C5—H5A109.2
O15—V6—O1175.03 (10)N1—C5—H5B109.2
O4—V6—O1175.72 (10)C6—C5—H5B109.2
O16—V7—O13105.63 (13)H5A—C5—H5B107.9
O16—V7—O20103.96 (12)C5—C6—H6A109.5
O13—V7—O2097.78 (12)C5—C6—H6B109.5
O16—V7—O1597.43 (12)H6A—C6—H6B109.5
O13—V7—O1594.28 (12)C5—C6—H6C109.5
O20—V7—O15151.50 (11)H6A—C6—H6C109.5
O16—V7—O1796.17 (12)H6B—C6—H6C109.5
O13—V7—O17158.17 (11)C8—C7—N2113.1 (3)
O20—V7—O1775.42 (11)C8—C7—H7A109.0
O15—V7—O1783.84 (11)N2—C7—H7A109.0
O16—V7—O11169.05 (12)C8—C7—H7B109.0
O13—V7—O1184.23 (11)N2—C7—H7B109.0
O20—V7—O1178.92 (10)H7A—C7—H7B107.8
O15—V7—O1176.73 (10)C7—C8—H8A109.5
O17—V7—O1174.15 (10)C7—C8—H8B109.5
O18—V8—O19107.20 (13)H8A—C8—H8B109.5
O18—V8—O14101.55 (13)C7—C8—H8C109.5
O19—V8—O1497.62 (12)H8A—C8—H8C109.5
O18—V8—O2099.80 (12)H8B—C8—H8C109.5
O19—V8—O2093.20 (12)N2—C9—C10112.7 (3)
O14—V8—O20151.95 (11)N2—C9—H9A109.1
O18—V8—O1795.59 (12)C10—C9—H9A109.1
O19—V8—O17155.43 (11)N2—C9—H9B109.1
O14—V8—O1786.38 (11)C10—C9—H9B109.1
O20—V8—O1773.58 (10)H9A—C9—H9B107.8
O18—V8—O12168.37 (12)C9—C10—H10A109.5
O19—V8—O1283.73 (11)C9—C10—H10B109.5
O14—V8—O1280.41 (10)H10A—C10—H10B109.5
O20—V8—O1275.13 (10)C9—C10—H10C109.5
O17—V8—O1273.00 (10)H10A—C10—H10C109.5
O28—V9—O21103.48 (13)H10B—C10—H10C109.5
O28—V9—O22103.92 (13)N2—C11—C12113.8 (4)
O21—V9—O2293.07 (12)N2—C11—H11A108.8
O28—V9—O27101.40 (13)C12—C11—H11A108.8
O21—V9—O2792.61 (12)N2—C11—H11B108.8
O22—V9—O27151.94 (11)C12—C11—H11B108.8
O28—V9—O23100.91 (13)H11A—C11—H11B107.7
O21—V9—O23154.82 (12)C11—C12—H12A109.5
O22—V9—O2387.04 (11)C11—C12—H12B109.5
O27—V9—O2376.43 (11)H12A—C12—H12B109.5
O28—V9—O11175.30 (13)C11—C12—H12C109.5
O21—V9—O1180.74 (11)H12A—C12—H12C109.5
O22—V9—O1177.70 (10)H12B—C12—H12C109.5
O27—V9—O1176.15 (10)N3—C13—C14112.1 (4)
O23—V9—O1174.68 (10)N3—C13—H13A109.2
O26—V10—O24105.10 (13)C14—C13—H13A109.2
O26—V10—O25103.03 (13)N3—C13—H13B109.2
O24—V10—O2594.98 (13)C14—C13—H13B109.2
O26—V10—O2399.23 (13)H13A—C13—H13B107.9
O24—V10—O2392.22 (12)C13—C14—H14A109.5
O25—V10—O23153.89 (12)C13—C14—H14B109.5
O26—V10—O2799.72 (13)H14A—C14—H14B109.5
O24—V10—O27153.59 (11)C13—C14—H14C109.5
O25—V10—O2788.01 (12)H14A—C14—H14C109.5
O23—V10—O2774.84 (11)H14B—C14—H14C109.5
O26—V10—O12172.44 (12)N3—C15—C16111.9 (4)
O24—V10—O1280.67 (11)N3—C15—H15A109.2
O25—V10—O1281.03 (11)C16—C15—H15A109.2
O23—V10—O1275.42 (10)N3—C15—H15B109.2
O27—V10—O1273.87 (10)C16—C15—H15B109.2
O30—V11—O29104.27 (14)H15A—C15—H15B107.9
O30—V11—O41101.57 (13)C15—C16—H16A109.5
O29—V11—O4192.07 (12)C15—C16—H16B109.5
O30—V11—O49101.62 (13)H16A—C16—H16B109.5
O29—V11—O4991.83 (12)C15—C16—H16C109.5
O41—V11—O49154.74 (12)H16A—C16—H16C109.5
O30—V11—O31101.81 (13)H16B—C16—H16C109.5
O29—V11—O31153.90 (12)N3—C17—C18114.6 (4)
O41—V11—O3183.68 (11)N3—C17—H17A108.6
O49—V11—O3181.89 (11)C18—C17—H17A108.6
O30—V11—O39175.03 (12)N3—C17—H17B108.6
O29—V11—O3980.54 (11)C18—C17—H17B108.6
O41—V11—O3979.32 (10)H17A—C17—H17B107.6
O49—V11—O3976.73 (10)C17—C18—H18A109.5
O31—V11—O3973.37 (10)C17—C18—H18B109.5
O31—V12—O33107.24 (13)H18A—C18—H18B109.5
O31—V12—O4397.90 (12)C17—C18—H18C109.5
O33—V12—O4398.20 (12)H18A—C18—H18C109.5
O31—V12—O5096.89 (12)H18B—C18—H18C109.5
O33—V12—O5095.29 (12)N4—C19—C20110.1 (6)
O43—V12—O50156.03 (12)N4—C19—H19A109.6
O31—V12—O40164.78 (12)C20—C19—H19A109.6
O33—V12—O4087.76 (12)N4—C19—H19B109.6
O43—V12—O4082.09 (11)C20—C19—H19B109.6
O50—V12—O4078.72 (10)H19A—C19—H19B108.2
O31—V12—O3986.90 (12)N4'—C19'—C20'104.9 (8)
O33—V12—O39165.51 (12)N4'—C19'—H19C110.8
O43—V12—O3982.54 (11)C20'—C19'—H19C110.8
O50—V12—O3979.54 (10)N4'—C19'—H19D110.8
O40—V12—O3977.98 (10)C20'—C19'—H19D110.8
O32—V13—O45102.99 (13)H19C—C19'—H19D108.8
O32—V13—O34104.03 (14)C19—C20—H20A109.5
O45—V13—O3492.07 (12)C19—C20—H20B109.5
O32—V13—O51100.42 (13)H20A—C20—H20B109.5
O45—V13—O51155.67 (12)C19—C20—H20C109.5
O34—V13—O5188.62 (12)H20A—C20—H20C109.5
O32—V13—O33101.13 (13)H20B—C20—H20C109.5
O45—V13—O3386.70 (12)C19'—C20'—H20D109.5
O34—V13—O33154.43 (12)C19'—C20'—H20E109.5
O51—V13—O3382.36 (11)H20D—C20'—H20E109.5
O32—V13—O40174.28 (12)C19'—C20'—H20F109.5
O45—V13—O4079.72 (11)H20D—C20'—H20F109.5
O34—V13—O4080.77 (11)H20E—C20'—H20F109.5
O51—V13—O4076.38 (10)C22—C21—N4119.9 (8)
O33—V13—O4073.87 (10)C22—C21—H21A107.4
O35—V14—O34103.00 (13)N4—C21—H21A107.4
O35—V14—O52102.32 (13)C22—C21—H21B107.4
O34—V14—O5292.20 (12)N4—C21—H21B107.4
O35—V14—O46101.73 (13)H21A—C21—H21B106.9
O34—V14—O4689.85 (12)C22'—C21'—N4'114.6 (10)
O52—V14—O46154.73 (12)C22'—C21'—H21C108.6
O35—V14—O36100.53 (13)N4'—C21'—H21C108.6
O34—V14—O36156.38 (12)C22'—C21'—H21D108.6
O52—V14—O3684.77 (11)N4'—C21'—H21D108.6
O46—V14—O3683.35 (11)H21C—C21'—H21D107.6
O35—V14—O40174.30 (13)C21—C22—H22A109.5
O34—V14—O4082.70 (11)C21—C22—H22B109.5
O52—V14—O4076.94 (10)H22A—C22—H22B109.5
O46—V14—O4078.35 (11)C21—C22—H22C109.5
O36—V14—O4073.79 (10)H22A—C22—H22C109.5
O36—V15—O37106.43 (13)H22B—C22—H22C109.5
O36—V15—O47100.70 (12)C21'—C22'—H22D109.5
O37—V15—O4799.52 (12)C21'—C22'—H22E109.5
O36—V15—O5494.43 (12)H22D—C22'—H22E109.5
O37—V15—O5493.40 (12)C21'—C22'—H22F109.5
O47—V15—O54156.37 (12)H22D—C22'—H22F109.5
O36—V15—O4088.13 (12)H22E—C22'—H22F109.5
O37—V15—O40163.68 (12)N4—C23—C24116.7 (7)
O47—V15—O4084.58 (11)N4—C23—H23A108.1
O54—V15—O4077.84 (10)C24—C23—H23A108.1
O36—V15—O39165.37 (12)N4—C23—H23B108.1
O37—V15—O3986.34 (12)C24—C23—H23B108.1
O47—V15—O3983.75 (11)H23A—C23—H23B107.3
O54—V15—O3977.38 (10)N4'—C23'—C24'110.0 (9)
O40—V15—O3978.36 (10)N4'—C23'—H23D109.7
O38—V16—O48105.15 (14)C24'—C23'—H23D109.7
O38—V16—O29103.52 (14)N4'—C23'—H23C109.7
O48—V16—O2992.80 (12)C24'—C23'—H23C109.7
O38—V16—O5698.58 (13)H23D—C23'—H23C108.2
O48—V16—O56155.65 (12)C23—C24—H24A109.5
O29—V16—O5686.83 (11)C23—C24—H24B109.5
O38—V16—O37100.13 (13)H24A—C24—H24B109.5
O48—V16—O3787.75 (12)C23—C24—H24C109.5
O29—V16—O37155.31 (12)H24A—C24—H24C109.5
O56—V16—O3782.72 (11)H24B—C24—H24C109.5
O38—V16—O39171.78 (13)C23'—C24'—H24D109.5
O48—V16—O3981.61 (11)C23'—C24'—H24E109.5
O29—V16—O3980.49 (11)H24D—C24'—H24E109.5
O56—V16—O3974.31 (10)C23'—C24'—H24F109.5
O37—V16—O3975.17 (10)H24D—C24'—H24F109.5
O42—V17—O41102.84 (14)H24E—C24'—H24F109.5
O42—V17—O48102.41 (14)N5—C25—C26113.8 (5)
O41—V17—O4893.44 (12)N5—C25—H25A108.8
O42—V17—O43102.11 (13)C26—C25—H25A108.8
O41—V17—O4391.65 (12)N5—C25—H25B108.8
O48—V17—O43153.15 (12)C26—C25—H25B108.8
O42—V17—O47100.97 (13)H25A—C25—H25B107.7
O41—V17—O47155.28 (12)N5'—C25'—C26'106.1 (9)
O48—V17—O4787.87 (11)N5'—C25'—H25C110.5
O43—V17—O4776.87 (11)C26'—C25'—H25C110.5
O42—V17—O39176.32 (13)N5'—C25'—H25D110.5
O41—V17—O3980.45 (11)C26'—C25'—H25D110.5
O48—V17—O3978.90 (10)H25C—C25'—H25D108.7
O43—V17—O3975.99 (10)C25—C26—H26A109.5
O47—V17—O3975.58 (10)C25—C26—H26B109.5
O44—V18—O46104.23 (14)H26A—C26—H26B109.5
O44—V18—O45102.53 (13)C25—C26—H26C109.5
O46—V18—O4593.58 (12)H26A—C26—H26C109.5
O44—V18—O47101.47 (13)H26B—C26—H26C109.5
O46—V18—O4791.17 (12)C25'—C26'—H26D109.5
O45—V18—O47153.55 (11)C25'—C26'—H26E109.5
O44—V18—O43101.83 (13)H26D—C26'—H26E109.5
O46—V18—O43152.67 (12)C25'—C26'—H26F109.5
O45—V18—O4388.69 (12)H26D—C26'—H26F109.5
O47—V18—O4375.62 (11)H26E—C26'—H26F109.5
O44—V18—O40175.31 (12)C28—C27—N5114.1 (4)
O46—V18—O4079.29 (11)C28—C27—H27A108.7
O45—V18—O4080.19 (10)N5—C27—H27A108.7
O47—V18—O4075.17 (10)C28—C27—H27B108.7
O43—V18—O4074.28 (10)N5—C27—H27B108.7
O55—V19—O49104.51 (13)H27A—C27—H27B107.6
O55—V19—O50102.61 (12)N5'—C27'—C28'107.9 (9)
O49—V19—O5098.40 (12)N5'—C27'—H27C110.1
O55—V19—O5699.35 (12)C28'—C27'—H27C110.1
O49—V19—O5694.41 (12)N5'—C27'—H27D110.1
O50—V19—O56150.82 (12)C28'—C27'—H27D110.1
O55—V19—O5497.27 (12)H27C—C27'—H27D108.4
O49—V19—O54158.17 (11)C27—C28—H28A109.5
O50—V19—O5475.18 (11)C27—C28—H28B109.5
O56—V19—O5483.22 (11)H28A—C28—H28B109.5
O55—V19—O39170.72 (12)C27—C28—H28C109.5
O49—V19—O3984.37 (11)H28A—C28—H28C109.5
O50—V19—O3978.33 (10)H28B—C28—H28C109.5
O56—V19—O3976.98 (10)C27'—C28'—H28D109.5
O54—V19—O3973.94 (10)C27'—C28'—H28E109.5
O53—V20—O51106.05 (13)H28D—C28'—H28E109.5
O53—V20—O52101.71 (13)C27'—C28'—H28F109.5
O51—V20—O5296.88 (12)H28D—C28'—H28F109.5
O53—V20—O5099.68 (12)H28E—C28'—H28F109.5
O51—V20—O5093.84 (12)N5—C29—C30113.9 (5)
O52—V20—O50152.33 (11)N5—C29—H29A108.8
O53—V20—O5495.49 (12)C30—C29—H29A108.8
O51—V20—O54156.75 (11)N5—C29—H29B108.8
O52—V20—O5487.01 (11)C30—C29—H29B108.8
O50—V20—O5473.62 (10)H29A—C29—H29B107.7
O53—V20—O40168.82 (12)N5'—C29'—C30'105.6 (9)
O51—V20—O4084.53 (11)N5'—C29'—H29C110.6
O52—V20—O4080.16 (11)C30'—C29'—H29C110.6
O50—V20—O4075.55 (10)N5'—C29'—H29D110.6
O54—V20—O4073.53 (10)C30'—C29'—H29D110.6
V1—O2—V6113.17 (14)H29C—C29'—H29D108.8
V5—O4—V6109.31 (14)C29—C30—H30A109.5
V5—O5—V4109.84 (14)C29—C30—H30B109.5
V4—O7—V3114.90 (14)H30A—C30—H30B109.5
V2—O9—V3110.17 (14)C29—C30—H30C109.5
V2—O10—V1112.93 (14)H30A—C30—H30C109.5
V5—O11—V299.73 (11)H30B—C30—H30C109.5
V5—O11—V7101.37 (11)C29'—C30'—H30D109.5
V2—O11—V790.47 (10)C29'—C30'—H30E109.5
V5—O11—V688.33 (10)H30D—C30'—H30E109.5
V2—O11—V6169.28 (13)C29'—C30'—H30F109.5
V7—O11—V694.88 (10)H30D—C30'—H30F109.5
V5—O11—V990.21 (9)H30E—C30'—H30F109.5
V2—O11—V988.57 (9)N7—C31—C32114.4 (4)
V7—O11—V9168.37 (13)N7—C31—H31A108.7
V6—O11—V984.31 (9)C32—C31—H31A108.7
V5—O11—V1169.96 (13)N7—C31—H31B108.7
V2—O11—V187.43 (9)C32—C31—H31B108.7
V7—O11—V185.49 (9)H31A—C31—H31B107.6
V6—O11—V183.75 (9)C31—C32—H32A109.5
V9—O11—V182.88 (8)C31—C32—H32B109.5
V5—O12—V2103.41 (11)H32A—C32—H32B109.5
V5—O12—V8101.39 (10)C31—C32—H32C109.5
V2—O12—V894.15 (10)H32A—C32—H32C109.5
V5—O12—V1089.55 (10)H32B—C32—H32C109.5
V2—O12—V1092.89 (10)C34—C33—N7113.8 (4)
V8—O12—V10165.24 (13)C34—C33—H33A108.8
V5—O12—V488.76 (10)N7—C33—H33A108.8
V2—O12—V4167.59 (13)C34—C33—H33B108.8
V8—O12—V485.69 (9)N7—C33—H33B108.8
V10—O12—V484.66 (9)H33A—C33—H33B107.7
V5—O12—V3167.75 (13)C33—C34—H34A109.5
V2—O12—V386.41 (9)C33—C34—H34B109.5
V8—O12—V384.94 (9)H34A—C34—H34B109.5
V10—O12—V382.57 (8)C33—C34—H34C109.5
V4—O12—V381.21 (8)H34A—C34—H34C109.5
V7—O13—V1113.93 (14)H34B—C34—H34C109.5
V4—O14—V8113.36 (14)N7—C35—C36114.4 (4)
V7—O15—V6111.75 (12)N7—C35—H35A108.7
V7—O15—H15124.1C36—C35—H35A108.7
V6—O15—H15124.1N7—C35—H35B108.7
V5—O17—V7106.45 (11)C36—C35—H35B108.7
V5—O17—V8105.39 (11)H35A—C35—H35B107.6
V7—O17—V896.11 (11)C35—C36—H36A109.5
V5—O17—H17115.6C35—C36—H36B109.5
V7—O17—H17115.6H36A—C36—H36B109.5
V8—O17—H17115.6C35—C36—H36C109.5
V8—O19—V3115.53 (14)H36A—C36—H36C109.5
V7—O20—V2106.70 (12)H36B—C36—H36C109.5
V7—O20—V8108.45 (13)N6—C37—C38112.9 (4)
V2—O20—V8106.69 (12)N6—C37—H37A109.0
V9—O21—V1116.12 (14)C38—C37—H37A109.0
V6—O22—V9114.37 (14)N6—C37—H37B109.0
V5—O23—V10106.66 (13)C38—C37—H37B109.0
V5—O23—V9109.81 (13)H37A—C37—H37B107.8
V10—O23—V999.20 (12)C37—C38—H38A109.5
V10—O24—V4115.97 (14)C37—C38—H38B109.5
V3—O25—V10115.91 (14)H38A—C38—H38B109.5
V2—O27—V9110.10 (13)C37—C38—H38C109.5
V2—O27—V10108.32 (12)H38A—C38—H38C109.5
V9—O27—V10100.89 (12)H38B—C38—H38C109.5
V11—O29—V16115.20 (14)N6—C39—C40115.4 (4)
V12—O31—V11111.69 (14)N6—C39—H39A108.4
V12—O33—V13111.47 (14)C40—C39—H39A108.4
V14—O34—V13114.32 (14)N6—C39—H39B108.4
V15—O36—V14109.37 (14)C40—C39—H39B108.4
V15—O37—V16110.25 (14)H39A—C39—H39B107.5
V12—O39—V15100.64 (11)C39—C40—H40A109.5
V12—O39—V1990.95 (10)C39—C40—H40B109.5
V15—O39—V19101.05 (11)H40A—C40—H40B109.5
V12—O39—V16169.70 (14)C39—C40—H40C109.5
V15—O39—V1687.41 (9)H40A—C40—H40C109.5
V19—O39—V1693.81 (10)H40B—C40—H40C109.5
V12—O39—V1789.64 (10)N6—C41—C42114.2 (4)
V15—O39—V1789.89 (9)N6—C41—H41A108.7
V19—O39—V17168.74 (13)C42—C41—H41A108.7
V16—O39—V1783.92 (9)N6—C41—H41B108.7
V12—O39—V1187.92 (9)C42—C41—H41B108.7
V15—O39—V11169.44 (13)H41A—C41—H41B107.6
V19—O39—V1184.85 (9)C41—C42—H42A109.5
V16—O39—V1183.43 (9)C41—C42—H42B109.5
V17—O39—V1183.93 (9)H42A—C42—H42B109.5
V15—O40—V12102.47 (11)C41—C42—H42C109.5
V15—O40—V20100.88 (11)H42A—C42—H42C109.5
V12—O40—V2094.44 (10)H42B—C42—H42C109.5
V15—O40—V1488.50 (10)C44—C43—N8112.5 (4)
V12—O40—V14168.52 (14)C44—C43—H43A109.1
V20—O40—V1486.67 (9)N8—C43—H43A109.1
V15—O40—V1889.66 (10)C44—C43—H43B109.1
V12—O40—V1891.78 (10)N8—C43—H43B109.1
V20—O40—V18166.28 (13)H43A—C43—H43B107.8
V14—O40—V1884.84 (9)C43—C44—H44A109.5
V15—O40—V13168.43 (13)C43—C44—H44B109.5
V12—O40—V1386.56 (9)H44A—C44—H44B109.5
V20—O40—V1385.42 (9)C43—C44—H44C109.5
V14—O40—V1382.14 (9)H44A—C44—H44C109.5
V18—O40—V1382.76 (9)H44B—C44—H44C109.5
V17—O41—V11115.55 (14)C46—C45—N8113.3 (4)
V12—O43—V17108.85 (13)C46—C45—H45A108.9
V12—O43—V18109.07 (13)N8—C45—H45A108.9
V17—O43—V18100.10 (12)C46—C45—H45B108.9
V13—O45—V18116.34 (14)N8—C45—H45B108.9
V18—O46—V14116.53 (14)H45A—C45—H45B107.7
V15—O47—V18107.37 (12)C45—C46—H46A109.5
V15—O47—V17108.97 (13)C45—C46—H46B109.5
V18—O47—V1798.80 (12)H46A—C46—H46B109.5
V16—O48—V17114.74 (14)C45—C46—H46C109.5
V19—O49—V11113.73 (14)H46A—C46—H46C109.5
V19—O50—V12106.19 (12)H46B—C46—H46C109.5
V19—O50—V20108.62 (12)C48—C47—N8113.0 (3)
V12—O50—V20106.87 (12)C48—C47—H47A109.0
V20—O51—V13112.99 (13)N8—C47—H47A109.0
V20—O52—V14113.96 (14)C48—C47—H47B109.0
V15—O54—V20105.19 (11)N8—C47—H47B109.0
V15—O54—V19106.63 (11)H47A—C47—H47B107.8
V20—O54—V1996.22 (10)C47—C48—H48A109.5
V15—O54—H54115.5C47—C48—H48B109.5
V20—O54—H54115.5H48A—C48—H48B109.5
V19—O54—H54115.5C47—C48—H48C109.5
V19—O56—V16113.25 (13)H48A—C48—H48C109.5
V19—O56—H56123.4H48B—C48—H48C109.5
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1···O30.882.062.937 (4)175
N2—H2···O140.881.892.765 (4)176
N3—H3···O410.881.822.699 (4)175
N4—H4···O90.882.132.968 (9)160
N4—H4···O90.881.992.830 (16)158
N5—H5···O260.882.392.981 (5)125
N5—H5···O280.882.383.187 (5)153
N6—H6···O510.881.962.823 (4)167
N7—H7···O340.882.333.061 (4)141
N7—H7···O450.882.443.156 (5)139
N7—H7···O460.882.403.139 (4)142
N8—H8···O520.881.912.766 (4)162
O15—H15···O18i0.841.992.819 (4)171
O17—H17···O16i0.841.902.715 (4)162
O54—H54···O55ii0.841.882.686 (4)159
O56—H56···O53ii0.841.942.775 (4)177
Symmetry codes: (i) x+1, y+1, z; (ii) x+2, y, z+2.

Experimental details

Crystal data
Chemical formula(C6H16N)4[H2V10O28]
Mr1368.21
Crystal system, space groupTriclinic, P1
Temperature (K)100
a, b, c (Å)13.1735 (4), 20.0061 (7), 20.2427 (7)
α, β, γ (°)62.669 (3), 86.263 (3), 76.979 (3)
V3)4613.0 (3)
Z4
Radiation typeMo Kα
µ (mm1)2.02
Crystal size (mm)0.20 × 0.15 × 0.10
Data collection
DiffractometerAgilent SuperNova Dual
diffractometer with an Atlas detector
Absorption correctionMulti-scan
(CrysAlis PRO; Agilent, 2010)
Tmin, Tmax0.688, 0.824
No. of measured, independent and
observed [I > 2σ(I)] reflections
38533, 20465, 13087
Rint0.041
(sin θ/λ)max1)0.650
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.049, 0.133, 1.04
No. of reflections20465
No. of parameters1230
No. of restraints132
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.47, 0.79

Computer programs: CrysAlis PRO (Agilent, 2010), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), X-SEED (Barbour, 2001), publCIF (Westrip, 2010).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1···O30.882.062.937 (4)175
N2—H2···O140.881.892.765 (4)176
N3—H3···O410.881.822.699 (4)175
N4—H4···O90.882.132.968 (9)160
N4'—H4'···O90.881.992.830 (16)158
N5—H5···O260.882.392.981 (5)125
N5—H5···O280.882.383.187 (5)153
N6—H6···O510.881.962.823 (4)167
N7—H7···O340.882.333.061 (4)141
N7—H7···O450.882.443.156 (5)139
N7—H7···O460.882.403.139 (4)142
N8—H8···O520.881.912.766 (4)162
O15—H15···O18i0.841.992.819 (4)171
O17—H17···O16i0.841.902.715 (4)162
O54—H54···O55ii0.841.882.686 (4)159
O56—H56···O53ii0.841.942.775 (4)177
Symmetry codes: (i) x+1, y+1, z; (ii) x+2, y, z+2.
 

Acknowledgements

I thank the University of Malaya for supporting this study.

References

First citationAgilent (2010). CrysAlis PRO. Agilent Technologies, Yarnton, England.
First citationBarbour, L. J. (2001). J. Supramol. Chem. 1, 189–191.  CrossRef CAS
First citationCorreia, I., Avecilla, F., Marcão, S. & Pessoa, J. C. (2004). Inorg. Chim. Acta, 357, 4476–4487.  Web of Science CSD CrossRef CAS
First citationSarkar, A. & Pal, S. (2008). Polyhedron, 27, 3472–3476.  CrossRef CAS
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals
First citationWestrip, S. P. (2010). J. Appl. Cryst. 43, 920–925.  Web of Science CrossRef CAS IUCr Journals

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Volume 67| Part 6| June 2011| Pages m811-m812
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