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The title compound, (C2H8N)2(C8H20N)2[H2V10O28], contains two crystallographically independent centrosymmetric polyvanadate clusters, each with a composition [V10O28H2]4−, with the H atoms attached to μ2-O atoms. A variety of O—H...O and N—H...O hydrogen bonds generate a two-dimensional network.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807004758/br2025sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807004758/br2025Isup2.hkl
Contains datablock I

CCDC reference: 640265

Key indicators

  • Single-crystal X-ray study
  • T = 173 K
  • Mean [sigma](C-C) = 0.010 Å
  • R factor = 0.042
  • wR factor = 0.090
  • Data-to-parameter ratio = 17.9

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ? PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.29 PLAT202_ALERT_3_C Isotropic non-H Atoms in Anion/Solvent ......... 1 PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.74 Ratio PLAT221_ALERT_4_C Large Solvent/Anion C Ueq(max)/Ueq(min) ... 3.19 Ratio PLAT223_ALERT_4_C Large Solvent/Anion H Ueq(max)/Ueq(min) ... 3.45 Ratio PLAT231_ALERT_4_C Hirshfeld Test (Solvent) C11 - C12 .. 5.55 su PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for C1 PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for C9 PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for C11 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for N1 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for N2 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C15 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for N4 PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 3.11 PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 10 PLAT480_ALERT_4_C Long H...A H-Bond Reported H4D .. O7 .. 2.65 Ang. PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.30 Ratio
Alert level G FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: C20 H58 N4 O28 V10 Atom count from _chemical_formula_moiety:C20 H58 N2 O28 V10
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 19 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 12 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: CrystalClear (Rigaku, 2000); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXTL.

Bis(tetraethylammonium) bis(dimethylammonium) dihydrogendecavanadate top
Crystal data top
(C2H8N)2(C8H20N)2[H2V10O28]F(000) = 2640
Mr = 1312.10Dx = 1.950 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -p 2ybcCell parameters from 8685 reflections
a = 22.342 (5) Åθ = 2.1–27.5°
b = 17.134 (4) ŵ = 2.08 mm1
c = 11.673 (3) ÅT = 173 K
β = 90.149 (3)°Prism, yellow
V = 4468.2 (18) Å30.30 × 0.25 × 0.15 mm
Z = 4
Data collection top
Mercury70 (2x2 bin mode)
diffractometer
10215 independent reflections
Radiation source: fine-focus sealed tube9041 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.028
Detector resolution: 14.6306 pixels mm-1θmax = 27.5°, θmin = 2.2°
CCD–profile–fitting scansh = 2928
Absorption correction: multi-scan
(CrystalClear; Rigaku, 2000)
k = 1022
Tmin = 0.541, Tmax = 0.732l = 1515
32458 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)] = 0.042Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.090H atoms treated by a mixture of independent and constrained refinement
S = 1.01 w = 1/[σ2(Fo2) + (0.0198P)2 + 14.9963P]
where P = (Fo2 + 2Fc2)/3
10250 reflections(Δ/σ)max = 0.001
574 parametersΔρmax = 1.47 e Å3
0 restraintsΔρmin = 0.64 e Å3
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
xyzUiso*/Ueq
V10.56239 (3)0.37206 (3)0.30827 (5)0.03020 (13)
V20.46684 (2)0.49239 (3)0.37560 (4)0.01974 (11)
V30.37359 (2)0.61056 (3)0.46039 (6)0.03199 (14)
V40.39590 (2)0.46498 (3)0.61078 (5)0.02394 (12)
V50.48267 (2)0.34451 (3)0.52392 (5)0.02205 (11)
V60.11375 (2)0.36487 (3)0.99625 (5)0.02619 (12)
V70.03923 (2)0.49383 (3)0.88269 (4)0.01936 (11)
V80.03827 (3)0.62632 (3)0.78528 (5)0.02678 (12)
V90.03348 (2)0.65165 (3)1.01157 (5)0.02311 (11)
V100.10172 (2)0.52120 (3)1.12636 (5)0.02297 (11)
O10.57081 (12)0.32151 (16)0.1927 (2)0.0459 (7)
O20.48629 (10)0.43418 (13)0.26599 (18)0.0282 (5)
O30.50398 (10)0.30753 (12)0.3888 (2)0.0273 (5)
O40.52460 (9)0.57438 (12)0.34728 (18)0.0225 (4)
O50.40526 (10)0.54200 (13)0.3336 (2)0.0285 (5)
O60.42380 (9)0.41519 (11)0.46542 (17)0.0203 (4)
O70.55961 (11)0.32191 (14)0.5964 (2)0.0335 (6)
H70.5663 (19)0.283 (3)0.622 (4)0.044 (13)*
O80.44412 (11)0.27531 (13)0.5789 (2)0.0338 (5)
O90.46058 (9)0.55488 (11)0.53266 (17)0.0195 (4)
O100.39786 (10)0.53659 (14)0.7251 (2)0.0322 (5)
O110.35379 (11)0.39708 (14)0.6592 (2)0.0363 (6)
O120.37916 (10)0.66279 (14)0.5996 (2)0.0366 (6)
O130.34257 (10)0.52459 (13)0.5234 (2)0.0318 (5)
O140.31844 (12)0.65155 (17)0.3982 (3)0.0533 (8)
O150.03603 (13)0.67092 (16)0.6639 (2)0.0436 (7)
O160.03146 (10)0.54936 (13)0.76472 (18)0.0284 (5)
O170.02213 (10)0.68492 (13)0.8702 (2)0.0294 (5)
O180.08576 (9)0.56749 (12)0.97237 (18)0.0216 (4)
O190.03145 (9)0.44046 (11)1.04499 (17)0.0189 (4)
O200.09647 (9)0.43162 (13)0.85715 (18)0.0255 (5)
O210.04279 (10)0.30822 (13)0.9349 (2)0.0308 (5)
H210.048 (2)0.265 (3)0.899 (4)0.055 (14)*
O220.07761 (11)0.71541 (14)1.0659 (2)0.0371 (6)
O230.08631 (10)0.45772 (13)1.24681 (18)0.0276 (5)
O240.14943 (11)0.58179 (15)1.1765 (2)0.0377 (6)
O250.09631 (10)0.32303 (13)1.1381 (2)0.0304 (5)
O260.15146 (9)0.44729 (13)1.05553 (19)0.0268 (5)
O270.16632 (11)0.30969 (16)0.9501 (2)0.0407 (6)
O280.02579 (9)0.42264 (12)0.85044 (17)0.0214 (4)
N10.22734 (13)0.62781 (18)0.8065 (3)0.0382 (7)
N20.27579 (15)0.3447 (2)0.2758 (3)0.0473 (9)
N30.00206 (19)0.8507 (2)0.8550 (3)0.0512 (9)
H3C0.00960.79810.86040.061*
H3D0.00830.86540.78020.061*
N40.50616 (18)0.35346 (19)0.8589 (3)0.0504 (9)
H4E0.49580.30160.86410.060*
H4D0.50260.36800.78330.060*
C10.2119 (2)0.5462 (3)0.8496 (6)0.0807 (19)
H1A0.20450.54940.93310.097*
H1B0.17410.52960.81270.097*
C20.2575 (3)0.4849 (3)0.8292 (6)0.091 (2)
H2A0.25650.46930.74840.137*
H2B0.24890.43960.87750.137*
H2C0.29730.50540.84800.137*
C30.2413 (3)0.6259 (4)0.6800 (5)0.0861 (19)
H3A0.27470.58920.66620.103*
H3B0.25430.67840.65490.103*
C40.1859 (4)0.6001 (6)0.6076 (7)0.141 (4)
H4A0.17970.54380.61630.212*
H4B0.19280.61230.52670.212*
H4C0.15020.62800.63430.212*
C50.2830 (2)0.6574 (3)0.8638 (6)0.0745 (16)
H5A0.29360.70880.83110.089*
H5B0.31640.62100.84760.089*
C60.2759 (4)0.6657 (5)0.9959 (6)0.104 (2)
H6A0.24250.70101.01260.157*
H6B0.31290.68691.02880.157*
H6C0.26770.61441.02950.157*
C70.1738 (2)0.6773 (3)0.8311 (5)0.0621 (13)
H7A0.16590.67640.91450.075*
H7B0.13860.65480.79170.075*
C80.1821 (3)0.7628 (3)0.7919 (6)0.0859 (19)
H8A0.17140.79810.85470.129*
H8B0.15620.77310.72570.129*
H8C0.22400.77140.77040.129*
C90.3182 (3)0.4078 (5)0.2587 (7)0.129 (4)
H9A0.35880.38530.25170.155*
H9B0.31790.44170.32730.155*
C100.3055 (5)0.4578 (7)0.1534 (9)0.168 (4)*
H10A0.28150.42780.09850.252*
H10B0.34340.47300.11780.252*
H10C0.28340.50460.17630.252*
C110.2668 (2)0.2925 (4)0.1755 (4)0.0736 (16)
H11A0.25110.32450.11160.088*
H11B0.30660.27270.15180.088*
C120.2265 (2)0.2243 (3)0.1900 (4)0.0526 (11)
H12A0.24250.19000.25010.079*
H12B0.22400.19540.11770.079*
H12C0.18660.24240.21180.079*
C130.2971 (2)0.2982 (3)0.3808 (4)0.0608 (12)
H13A0.30630.33540.44330.073*
H13B0.26370.26470.40720.073*
C140.3493 (3)0.2492 (3)0.3620 (5)0.0827 (19)
H14A0.33720.20170.32130.124*
H14B0.36710.23520.43600.124*
H14C0.37870.27780.31610.124*
C150.2135 (3)0.3773 (4)0.3084 (6)0.0804 (18)
H15A0.19400.39830.23870.096*
H15B0.18840.33400.33730.096*
C160.2163 (4)0.4412 (5)0.3988 (9)0.167 (5)
H16A0.23820.42200.46600.250*
H16B0.17560.45570.42130.250*
H16C0.23690.48690.36740.250*
C170.0444 (2)0.8928 (3)0.9288 (4)0.0653 (13)
H17A0.03740.94910.92210.098*
H17B0.08550.88090.90490.098*
H17C0.03880.87651.00850.098*
C180.0611 (2)0.8653 (3)0.8847 (4)0.0632 (13)
H18A0.06840.84880.96380.095*
H18B0.08710.83560.83280.095*
H18C0.06980.92110.87710.095*
C190.5690 (3)0.3625 (3)0.8947 (4)0.0734 (17)
H19A0.58120.41700.88480.110*
H19B0.59440.32880.84770.110*
H19C0.57310.34780.97540.110*
C200.4637 (3)0.4000 (3)0.9278 (5)0.0728 (16)
H20A0.46530.38261.00780.109*
H20B0.42310.39280.89780.109*
H20C0.47460.45530.92350.109*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
V10.0295 (3)0.0231 (3)0.0380 (3)0.0042 (2)0.0103 (2)0.0129 (2)
V20.0220 (2)0.0168 (2)0.0205 (2)0.00227 (19)0.00257 (19)0.00057 (19)
V30.0221 (3)0.0215 (3)0.0524 (4)0.0043 (2)0.0050 (2)0.0017 (3)
V40.0210 (2)0.0194 (2)0.0315 (3)0.0029 (2)0.0065 (2)0.0023 (2)
V50.0241 (2)0.0133 (2)0.0287 (3)0.00118 (19)0.0008 (2)0.00051 (19)
V60.0238 (3)0.0224 (3)0.0323 (3)0.0064 (2)0.0017 (2)0.0044 (2)
V70.0204 (2)0.0185 (2)0.0192 (2)0.00037 (19)0.00339 (18)0.00027 (19)
V80.0332 (3)0.0216 (3)0.0255 (3)0.0009 (2)0.0020 (2)0.0077 (2)
V90.0247 (3)0.0143 (2)0.0303 (3)0.0016 (2)0.0007 (2)0.0000 (2)
V100.0218 (2)0.0192 (2)0.0279 (3)0.0001 (2)0.0040 (2)0.0013 (2)
O10.0488 (16)0.0368 (14)0.0520 (16)0.0099 (12)0.0190 (13)0.0244 (13)
O20.0353 (12)0.0252 (11)0.0242 (11)0.0063 (10)0.0002 (9)0.0040 (9)
O30.0272 (11)0.0175 (10)0.0373 (13)0.0003 (9)0.0032 (9)0.0072 (9)
O40.0248 (10)0.0196 (10)0.0232 (10)0.0042 (8)0.0001 (8)0.0026 (8)
O50.0285 (11)0.0228 (11)0.0343 (12)0.0020 (9)0.0098 (9)0.0037 (9)
O60.0201 (10)0.0158 (9)0.0250 (10)0.0021 (8)0.0000 (8)0.0021 (8)
O70.0340 (13)0.0171 (11)0.0494 (16)0.0011 (10)0.0107 (11)0.0090 (11)
O80.0380 (13)0.0211 (11)0.0423 (14)0.0052 (10)0.0003 (11)0.0062 (10)
O90.0187 (9)0.0148 (9)0.0249 (10)0.0002 (8)0.0003 (8)0.0005 (8)
O100.0329 (12)0.0279 (12)0.0360 (13)0.0068 (10)0.0150 (10)0.0078 (10)
O110.0333 (13)0.0295 (12)0.0462 (15)0.0100 (10)0.0148 (11)0.0027 (11)
O120.0251 (11)0.0221 (12)0.0626 (17)0.0021 (9)0.0057 (11)0.0105 (11)
O130.0195 (10)0.0256 (12)0.0505 (15)0.0007 (9)0.0015 (10)0.0052 (11)
O140.0333 (14)0.0358 (15)0.091 (2)0.0088 (12)0.0202 (15)0.0050 (15)
O150.0611 (18)0.0364 (14)0.0335 (14)0.0019 (13)0.0007 (12)0.0168 (11)
O160.0331 (12)0.0282 (12)0.0237 (11)0.0003 (10)0.0046 (9)0.0035 (9)
O170.0320 (12)0.0197 (11)0.0365 (13)0.0025 (9)0.0007 (10)0.0089 (9)
O180.0199 (10)0.0177 (10)0.0271 (11)0.0024 (8)0.0027 (8)0.0003 (8)
O190.0202 (10)0.0153 (9)0.0213 (10)0.0003 (8)0.0002 (8)0.0006 (8)
O200.0242 (11)0.0271 (11)0.0252 (11)0.0033 (9)0.0043 (8)0.0037 (9)
O210.0297 (12)0.0179 (11)0.0449 (14)0.0042 (9)0.0028 (10)0.0095 (10)
O220.0380 (13)0.0225 (12)0.0507 (16)0.0074 (10)0.0068 (11)0.0033 (11)
O230.0318 (12)0.0262 (11)0.0246 (11)0.0029 (10)0.0057 (9)0.0011 (9)
O240.0329 (13)0.0309 (13)0.0494 (15)0.0041 (11)0.0108 (11)0.0052 (11)
O250.0344 (12)0.0207 (11)0.0360 (13)0.0058 (10)0.0062 (10)0.0031 (9)
O260.0219 (10)0.0251 (11)0.0334 (12)0.0020 (9)0.0017 (9)0.0023 (9)
O270.0361 (13)0.0387 (14)0.0473 (15)0.0164 (12)0.0013 (11)0.0094 (12)
O280.0231 (10)0.0182 (10)0.0227 (10)0.0000 (8)0.0003 (8)0.0030 (8)
N10.0270 (14)0.0325 (16)0.055 (2)0.0027 (12)0.0171 (13)0.0014 (14)
N20.0443 (19)0.046 (2)0.052 (2)0.0077 (16)0.0236 (16)0.0056 (16)
N30.092 (3)0.0313 (17)0.0304 (17)0.0079 (18)0.0047 (17)0.0086 (14)
N40.089 (3)0.0290 (16)0.0333 (17)0.0165 (18)0.0149 (18)0.0088 (14)
C10.069 (3)0.041 (3)0.132 (5)0.008 (2)0.050 (3)0.000 (3)
C20.083 (4)0.038 (3)0.152 (6)0.008 (3)0.064 (4)0.009 (3)
C30.088 (4)0.097 (5)0.074 (4)0.009 (4)0.030 (3)0.003 (3)
C40.155 (8)0.182 (10)0.086 (5)0.002 (7)0.031 (5)0.058 (6)
C50.052 (3)0.059 (3)0.113 (5)0.002 (3)0.003 (3)0.006 (3)
C60.127 (6)0.111 (6)0.075 (4)0.015 (5)0.040 (4)0.006 (4)
C70.043 (2)0.056 (3)0.088 (4)0.005 (2)0.015 (2)0.000 (3)
C80.095 (4)0.048 (3)0.115 (5)0.026 (3)0.005 (4)0.017 (3)
C90.123 (6)0.118 (6)0.145 (7)0.082 (5)0.085 (5)0.074 (5)
C110.064 (3)0.103 (5)0.054 (3)0.015 (3)0.013 (2)0.001 (3)
C120.052 (2)0.050 (3)0.056 (3)0.004 (2)0.011 (2)0.010 (2)
C130.064 (3)0.062 (3)0.057 (3)0.001 (3)0.014 (2)0.003 (2)
C140.079 (4)0.071 (4)0.099 (4)0.020 (3)0.049 (3)0.017 (3)
C150.067 (3)0.068 (4)0.106 (5)0.010 (3)0.034 (3)0.011 (3)
C160.122 (6)0.142 (7)0.235 (11)0.078 (6)0.110 (7)0.135 (8)
C170.081 (4)0.065 (3)0.050 (3)0.007 (3)0.004 (2)0.008 (2)
C180.082 (4)0.061 (3)0.047 (3)0.005 (3)0.004 (2)0.019 (2)
C190.098 (4)0.071 (4)0.051 (3)0.033 (3)0.019 (3)0.021 (3)
C200.112 (5)0.045 (3)0.061 (3)0.002 (3)0.002 (3)0.001 (2)
Geometric parameters (Å, º) top
V1—O11.614 (3)O21—H210.86 (5)
V1—O22.065 (2)O23—V8ii1.834 (2)
V1—O31.953 (2)O25—V8ii1.800 (2)
V1—O9i2.298 (2)O28—V10ii1.970 (2)
V1—O10i1.842 (2)O28—V9ii2.061 (2)
V1—O12i1.792 (3)N1—C71.494 (5)
V1—V3i3.0669 (11)N1—C51.499 (6)
V1—V4i3.0907 (9)N1—C31.510 (6)
V2—O21.680 (2)N1—C11.525 (6)
V2—O41.937 (2)N2—C91.451 (7)
V2—O51.689 (2)N2—C111.486 (6)
V2—O61.944 (2)N2—C131.536 (6)
V2—O92.128 (2)N2—C151.547 (7)
V2—O9i2.103 (2)N3—C171.467 (6)
V3—O52.019 (2)N3—C181.476 (6)
V3—O7i2.003 (3)N3—H3C0.9200
V3—O92.322 (2)N3—H3D0.9200
V3—O121.859 (3)N4—C191.472 (6)
V3—O131.787 (2)N4—C201.479 (7)
V3—O141.592 (3)N4—H4E0.9200
V3—V1i3.0669 (11)N4—H4D0.9200
V4—O4i1.961 (2)C1—C21.483 (7)
V4—O62.000 (2)C1—H1A0.9900
V4—O92.302 (2)C1—H1B0.9900
V4—O101.813 (2)C2—H2A0.9800
V4—O111.600 (2)C2—H2B0.9800
V4—O131.870 (2)C2—H2C0.9800
V4—V1i3.0907 (10)C3—C41.562 (9)
V5—O31.767 (2)C3—H3A0.9900
V5—O4i2.054 (2)C3—H3B0.9900
V5—O61.913 (2)C4—H4A0.9800
V5—O71.953 (3)C4—H4B0.9800
V5—O81.601 (2)C4—H4C0.9800
V5—O9i2.240 (2)C5—C61.557 (9)
V6—O192.321 (2)C5—H5A0.9900
V6—O202.022 (2)C5—H5B0.9900
V6—O211.991 (2)C6—H6A0.9800
V6—O251.847 (2)C6—H6B0.9800
V6—O261.783 (2)C6—H6C0.9800
V6—O271.602 (2)C7—C81.547 (7)
V6—V8ii3.0647 (10)C7—H7A0.9900
V7—O161.682 (2)C7—H7B0.9900
V7—O181.940 (2)C8—H8A0.9800
V7—O192.111 (2)C8—H8B0.9800
V7—O19ii2.117 (2)C8—H8C0.9800
V7—O201.692 (2)C9—C101.524 (11)
V7—O281.933 (2)C9—H9A0.9900
V8—O151.610 (2)C9—H9B0.9900
V8—O162.056 (2)C10—H10A0.9800
V8—O171.951 (2)C10—H10B0.9800
V8—O19ii2.293 (2)C10—H10C0.9800
V8—O23ii1.834 (2)C11—C121.485 (7)
V8—O25ii1.800 (2)C11—H11A0.9900
V8—V6ii3.0647 (10)C11—H11B0.9900
V8—V10ii3.0773 (9)C12—H12A0.9800
V9—O171.763 (2)C12—H12B0.9800
V9—O181.912 (2)C12—H12C0.9800
V9—O19ii2.242 (2)C13—C141.454 (7)
V9—O21ii1.943 (2)C13—H13A0.9900
V9—O221.601 (2)C13—H13B0.9900
V9—O28ii2.061 (2)C14—H14A0.9800
V10—O181.996 (2)C14—H14B0.9800
V10—O192.296 (2)C14—H14C0.9800
V10—O231.811 (2)C15—C161.522 (8)
V10—O241.598 (2)C15—H15A0.9900
V10—O261.878 (2)C15—H15B0.9900
V10—O28ii1.970 (2)C16—H16A0.9800
V10—V8ii3.0773 (9)C16—H16B0.9800
O4—V4i1.961 (2)C16—H16C0.9800
O4—V5i2.054 (2)C17—H17A0.9800
O7—V3i2.003 (3)C17—H17B0.9800
O7—H70.74 (4)C17—H17C0.9800
O9—V2i2.103 (2)C18—H18A0.9800
O9—V5i2.240 (2)C18—H18B0.9800
O9—V1i2.298 (2)C18—H18C0.9800
O10—V1i1.842 (2)C19—H19A0.9800
O12—V1i1.792 (3)C19—H19B0.9800
O19—V7ii2.117 (2)C19—H19C0.9800
O19—V9ii2.242 (2)C20—H20A0.9800
O19—V8ii2.293 (2)C20—H20B0.9800
O21—V9ii1.943 (2)C20—H20C0.9800
O1—V1—O12i103.67 (14)V2—O4—V4i108.15 (10)
O1—V1—O10i102.82 (12)V2—O4—V5i108.17 (10)
O12i—V1—O10i93.39 (11)V4i—O4—V5i97.08 (9)
O1—V1—O3100.24 (12)V2—O5—V3111.50 (12)
O12i—V1—O390.54 (11)V5—O6—V2106.42 (10)
O10i—V1—O3154.96 (10)V5—O6—V4100.52 (10)
O1—V1—O2100.06 (13)V2—O6—V4108.85 (9)
O12i—V1—O2156.01 (10)V5—O7—V3i113.45 (12)
O10i—V1—O284.76 (10)V5—O7—H7122 (3)
O3—V1—O281.72 (9)V3i—O7—H7120 (3)
O1—V1—O9i173.67 (12)V2i—O9—V2101.10 (8)
O12i—V1—O9i81.98 (10)V2i—O9—V5i90.58 (8)
O10i—V1—O9i79.45 (9)V2—O9—V5i95.43 (8)
O3—V1—O9i76.63 (8)V2i—O9—V1i88.39 (8)
O2—V1—O9i74.15 (8)V2—O9—V1i170.17 (10)
O1—V1—V3i137.10 (12)V5i—O9—V1i86.96 (7)
O12i—V1—V3i33.54 (8)V2i—O9—V491.41 (8)
O10i—V1—V3i83.09 (8)V2—O9—V492.71 (8)
O3—V1—V3i86.67 (7)V5i—O9—V4171.09 (10)
O2—V1—V3i122.84 (6)V1i—O9—V484.42 (7)
O9i—V1—V3i48.73 (5)V2i—O9—V3170.69 (10)
O1—V1—V4i134.78 (10)V2—O9—V387.16 (7)
O12i—V1—V4i84.19 (8)V5i—O9—V392.90 (8)
O10i—V1—V4i31.98 (7)V1i—O9—V383.18 (7)
O3—V1—V4i124.45 (7)V4—O9—V383.86 (7)
O2—V1—V4i81.66 (6)V4—O10—V1i115.48 (12)
O9i—V1—V4i47.84 (5)V1i—O12—V3114.28 (12)
V3i—V1—V4i60.234 (19)V3—O13—V4115.30 (12)
O2—V2—O5106.84 (12)V7—O16—V8110.11 (11)
O2—V2—O497.29 (10)V9—O17—V8114.00 (11)
O5—V2—O497.36 (10)V9—O18—V7107.03 (10)
O2—V2—O697.82 (10)V9—O18—V10101.07 (10)
O5—V2—O695.47 (10)V7—O18—V10108.76 (10)
O4—V2—O6156.42 (9)V7—O19—V7ii101.00 (8)
O2—V2—O9i87.62 (10)V7—O19—V9ii95.47 (8)
O5—V2—O9i165.49 (10)V7ii—O19—V9ii90.52 (8)
O4—V2—O9i81.55 (8)V7—O19—V8ii170.47 (10)
O6—V2—O9i81.10 (8)V7ii—O19—V8ii88.21 (7)
O2—V2—O9166.49 (10)V9ii—O19—V8ii86.83 (7)
O5—V2—O986.65 (10)V7—O19—V1093.01 (8)
O4—V2—O980.06 (8)V7ii—O19—V1091.41 (8)
O6—V2—O981.02 (8)V9ii—O19—V10170.78 (10)
O9i—V2—O978.90 (8)V8ii—O19—V1084.23 (7)
O14—V3—O13104.52 (13)V7—O19—V687.40 (7)
O14—V3—O12103.67 (14)V7ii—O19—V6170.68 (10)
O13—V3—O1293.57 (12)V9ii—O19—V692.72 (7)
O14—V3—O7i99.83 (14)V8ii—O19—V683.25 (7)
O13—V3—O7i154.50 (10)V10—O19—V684.05 (7)
O12—V3—O7i87.88 (11)V7—O20—V6110.95 (11)
O14—V3—O5101.21 (14)V9ii—O21—V6114.20 (12)
O13—V3—O587.66 (10)V9ii—O21—H21125 (3)
O12—V3—O5153.91 (10)V6—O21—H21120 (3)
O7i—V3—O580.25 (10)V10—O23—V8ii115.17 (12)
O14—V3—O9173.33 (14)V8ii—O25—V6114.35 (12)
O13—V3—O980.62 (9)V6—O26—V10115.17 (11)
O12—V3—O979.99 (9)V7—O28—V10ii108.19 (10)
O7i—V3—O974.56 (9)V7—O28—V9ii107.56 (10)
O5—V3—O974.50 (8)V10ii—O28—V9ii96.93 (9)
O14—V3—V1i135.84 (12)C7—N1—C5112.7 (4)
O13—V3—V1i84.16 (8)C7—N1—C3111.6 (4)
O12—V3—V1i32.18 (8)C5—N1—C3105.7 (4)
O7i—V3—V1i83.63 (8)C7—N1—C1106.0 (3)
O5—V3—V1i122.58 (7)C5—N1—C1110.5 (4)
O9—V3—V1i48.08 (5)C3—N1—C1110.5 (4)
O11—V4—O10104.21 (12)C9—N2—C11115.3 (5)
O11—V4—O13102.43 (12)C9—N2—C13107.2 (4)
O10—V4—O1392.64 (11)C11—N2—C13110.9 (4)
O11—V4—O4i101.24 (12)C9—N2—C15110.6 (5)
O10—V4—O4i91.65 (10)C11—N2—C15107.0 (4)
O13—V4—O4i154.09 (10)C13—N2—C15105.5 (4)
O11—V4—O6100.03 (11)C17—N3—C18113.3 (4)
O10—V4—O6154.94 (9)C17—N3—H3C108.9
O13—V4—O688.26 (10)C18—N3—H3C108.9
O4i—V4—O677.35 (9)C17—N3—H3D108.9
O11—V4—O9175.27 (10)C18—N3—H3D108.9
O10—V4—O979.90 (9)H3C—N3—H3D107.7
O13—V4—O979.53 (9)C19—N4—C20113.7 (4)
O4i—V4—O976.10 (8)C19—N4—H4E108.8
O6—V4—O975.64 (8)C20—N4—H4E108.8
O11—V4—V1i136.55 (9)C19—N4—H4D108.8
O10—V4—V1i32.54 (7)C20—N4—H4D108.8
O13—V4—V1i82.22 (7)H4E—N4—H4D107.7
O4i—V4—V1i87.83 (6)C2—C1—N1116.1 (4)
O6—V4—V1i123.38 (6)C2—C1—H1A108.3
O9—V4—V1i47.74 (5)N1—C1—H1A108.3
O8—V5—O3103.81 (12)C2—C1—H1B108.3
O8—V5—O6104.00 (11)N1—C1—H1B108.3
O3—V5—O695.45 (10)H1A—C1—H1B107.4
O8—V5—O798.83 (12)C1—C2—H2A109.5
O3—V5—O794.40 (11)C1—C2—H2B109.5
O6—V5—O7152.14 (10)H2A—C2—H2B109.5
O8—V5—O4i99.45 (11)C1—C2—H2C109.5
O3—V5—O4i156.68 (9)H2A—C2—H2C109.5
O6—V5—O4i77.14 (9)H2B—C2—H2C109.5
O7—V5—O4i83.59 (10)N1—C3—C4111.7 (5)
O8—V5—O9i173.52 (11)N1—C3—H3A109.3
O3—V5—O9i81.87 (9)C4—C3—H3A109.3
O6—V5—O9i78.28 (8)N1—C3—H3B109.3
O7—V5—O9i77.41 (9)C4—C3—H3B109.3
O4i—V5—O9i75.00 (8)H3A—C3—H3B107.9
O27—V6—O26104.57 (12)C3—C4—H4A109.5
O27—V6—O25103.23 (13)C3—C4—H4B109.5
O26—V6—O2593.45 (11)H4A—C4—H4B109.5
O27—V6—O21100.09 (12)C3—C4—H4C109.5
O26—V6—O21154.27 (10)H4A—C4—H4C109.5
O25—V6—O2187.92 (11)H4B—C4—H4C109.5
O27—V6—O20101.68 (12)N1—C5—C6112.7 (5)
O26—V6—O2087.29 (10)N1—C5—H5A109.0
O25—V6—O20154.04 (10)C6—C5—H5A109.0
O21—V6—O2080.60 (10)N1—C5—H5B109.0
O27—V6—O19173.52 (11)C6—C5—H5B109.0
O26—V6—O1980.61 (9)H5A—C5—H5B107.8
O25—V6—O1980.08 (9)C5—C6—H6A109.5
O21—V6—O1974.32 (9)C5—C6—H6B109.5
O20—V6—O1974.43 (8)H6A—C6—H6B109.5
O27—V6—V8ii135.58 (11)C5—C6—H6C109.5
O26—V6—V8ii84.18 (8)H6A—C6—H6C109.5
O25—V6—V8ii32.36 (7)H6B—C6—H6C109.5
O21—V6—V8ii83.35 (8)N1—C7—C8112.6 (4)
O20—V6—V8ii122.41 (6)N1—C7—H7A109.1
O19—V6—V8ii47.98 (5)C8—C7—H7A109.1
O16—V7—O20106.77 (11)N1—C7—H7B109.1
O16—V7—O2896.98 (10)C8—C7—H7B109.1
O20—V7—O2897.83 (10)H7A—C7—H7B107.8
O16—V7—O1897.33 (10)C7—C8—H8A109.5
O20—V7—O1895.77 (10)C7—C8—H8B109.5
O28—V7—O18156.48 (9)H8A—C8—H8B109.5
O16—V7—O19166.14 (10)C7—C8—H8C109.5
O20—V7—O1987.10 (9)H8A—C8—H8C109.5
O28—V7—O1980.67 (8)H8B—C8—H8C109.5
O18—V7—O1980.96 (8)N2—C9—C10114.2 (6)
O16—V7—O19ii87.14 (10)N2—C9—H9A108.7
O20—V7—O19ii166.02 (10)C10—C9—H9A108.7
O28—V7—O19ii81.50 (8)N2—C9—H9B108.7
O18—V7—O19ii80.68 (8)C10—C9—H9B108.7
O19—V7—O19ii79.00 (8)H9A—C9—H9B107.6
O15—V8—O25ii103.44 (13)C9—C10—H10A109.5
O15—V8—O23ii102.27 (13)C9—C10—H10B109.5
O25ii—V8—O23ii93.33 (11)H10A—C10—H10B109.5
O15—V8—O17100.35 (13)C9—C10—H10C109.5
O25ii—V8—O1789.86 (11)H10A—C10—H10C109.5
O23ii—V8—O17155.73 (10)H10B—C10—H10C109.5
O15—V8—O16100.17 (12)C12—C11—N2117.7 (4)
O25ii—V8—O16156.11 (10)C12—C11—H11A107.9
O23ii—V8—O1685.17 (10)N2—C11—H11A107.9
O17—V8—O1682.29 (10)C12—C11—H11B107.9
O15—V8—O19ii174.17 (12)N2—C11—H11B107.9
O25ii—V8—O19ii81.80 (9)H11A—C11—H11B107.2
O23ii—V8—O19ii79.76 (9)C11—C12—H12A109.5
O17—V8—O19ii76.90 (8)C11—C12—H12B109.5
O16—V8—O19ii74.46 (8)H12A—C12—H12B109.5
O15—V8—V6ii136.63 (11)C11—C12—H12C109.5
O25ii—V8—V6ii33.29 (7)H12A—C12—H12C109.5
O23ii—V8—V6ii83.43 (7)H12B—C12—H12C109.5
O17—V8—V6ii86.17 (7)C14—C13—N2115.2 (5)
O16—V8—V6ii123.20 (6)C14—C13—H13A108.5
O19ii—V8—V6ii48.77 (5)N2—C13—H13A108.5
O15—V8—V10ii134.43 (11)C14—C13—H13B108.5
O25ii—V8—V10ii84.05 (8)N2—C13—H13B108.5
O23ii—V8—V10ii32.19 (7)H13A—C13—H13B107.5
O17—V8—V10ii124.83 (7)C13—C14—H14A109.5
O16—V8—V10ii82.08 (7)C13—C14—H14B109.5
O19ii—V8—V10ii47.94 (5)H14A—C14—H14B109.5
V6ii—V8—V10ii60.436 (19)C13—C14—H14C109.5
O22—V9—O17103.71 (12)H14A—C14—H14C109.5
O22—V9—O18103.50 (11)H14B—C14—H14C109.5
O17—V9—O1896.10 (10)C16—C15—N2113.3 (5)
O22—V9—O21ii99.83 (12)C16—C15—H15A108.9
O17—V9—O21ii93.59 (11)N2—C15—H15A108.9
O18—V9—O21ii151.76 (10)C16—C15—H15B108.9
O22—V9—O28ii99.46 (11)N2—C15—H15B108.9
O17—V9—O28ii156.79 (10)H15A—C15—H15B107.7
O18—V9—O28ii76.91 (9)C15—C16—H16A109.5
O21ii—V9—O28ii83.80 (10)C15—C16—H16B109.5
O22—V9—O19ii173.77 (11)H16A—C16—H16B109.5
O17—V9—O19ii81.99 (9)C15—C16—H16C109.5
O18—V9—O19ii78.10 (8)H16A—C16—H16C109.5
O21ii—V9—O19ii77.08 (9)H16B—C16—H16C109.5
O28ii—V9—O19ii74.94 (8)N3—C17—H17A109.5
O24—V10—O23103.53 (12)N3—C17—H17B109.5
O24—V10—O26101.79 (12)H17A—C17—H17B109.5
O23—V10—O2692.90 (10)N3—C17—H17C109.5
O24—V10—O28ii101.90 (11)H17A—C17—H17C109.5
O23—V10—O28ii91.21 (10)H17B—C17—H17C109.5
O26—V10—O28ii154.26 (9)N3—C18—H18A109.5
O24—V10—O18100.89 (12)N3—C18—H18B109.5
O23—V10—O18154.66 (10)H18A—C18—H18B109.5
O26—V10—O1888.63 (9)N3—C18—H18C109.5
O28ii—V10—O1877.16 (8)H18A—C18—H18C109.5
O24—V10—O19176.04 (11)H18B—C18—H18C109.5
O23—V10—O1980.10 (9)N4—C19—H19A109.5
O26—V10—O1979.42 (9)N4—C19—H19B109.5
O28ii—V10—O1976.29 (8)H19A—C19—H19B109.5
O18—V10—O1975.32 (8)N4—C19—H19C109.5
O24—V10—V8ii135.93 (10)H19A—C19—H19C109.5
O23—V10—V8ii32.64 (7)H19B—C19—H19C109.5
O26—V10—V8ii82.38 (7)N4—C20—H20A109.5
O28ii—V10—V8ii87.56 (7)N4—C20—H20B109.5
O18—V10—V8ii123.15 (6)H20A—C20—H20B109.5
O19—V10—V8ii47.84 (5)N4—C20—H20C109.5
V2—O2—V1109.78 (11)H20A—C20—H20C109.5
V5—O3—V1114.11 (11)H20B—C20—H20C109.5
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y+1, z+2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O7—H7···O1iii0.74 (4)1.98 (5)2.714 (3)171 (5)
O21—H21···O15iv0.86 (5)1.79 (5)2.624 (3)164 (5)
N3—H3C···O170.921.962.881 (4)178
N3—H3D···O28v0.921.862.749 (4)163
N4—H4E···O3iii0.921.902.781 (4)159
N4—H4D···O4i0.921.912.790 (4)158
N4—H4D···O70.922.653.335 (5)132
Symmetry codes: (i) x+1, y+1, z+1; (iii) x, y+1/2, z+1/2; (iv) x, y1/2, z+3/2; (v) x, y+1/2, z+3/2.
 

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