| Literature DB >> 21582056 |
Caixia Yuan1, Liping Lu, Miaoli Zhu, Qi Ma, Yanbo Wu.
Abstract
In the title compound, (C(5)H(7)N(2))(6)[V(10)O(28)]·2H(2)O, the [V(10)O(28)](6-) anion is generated by crystallographic inversion symmetry and each of the five vanadium centres adopts a distorted VO(6) octa-hedral geometry. In the crystal structure, a network of N-H⋯O, N-H⋯(O,O) and O-H⋯O hydrogen bonds helps to establish the packing.Entities:
Year: 2009 PMID: 21582056 PMCID: PMC2968550 DOI: 10.1107/S1600536809004334
Source DB: PubMed Journal: Acta Crystallogr Sect E Struct Rep Online ISSN: 1600-5368
| (C5H7N2)6[V10O28]·2H2O | |
| Monoclinic, | Mo |
| Hall symbol: -P 2ybc | Cell parameters from 3889 reflections |
| θ = 2.2–27.0° | |
| µ = 1.86 mm−1 | |
| β = 97.416 (4)° | Block, yellow |
| 0.40 × 0.20 × 0.20 mm | |
| Bruker SMART 1K CCD diffractometer | 4341 independent reflections |
| Radiation source: fine-focus sealed tube | 3949 reflections with |
| graphite | |
| ω scans | θmax = 25.0°, θmin = 2.9° |
| Absorption correction: multi-scan ( | |
| 9858 measured reflections |
| Refinement on | Primary atom site location: structure-invariant direct methods |
| Least-squares matrix: full | Secondary atom site location: difference Fourier map |
| Hydrogen site location: inferred from neighbouring sites | |
| H-atom parameters constrained | |
| 4341 reflections | (Δ/σ)max = 0.002 |
| 370 parameters | Δρmax = 0.53 e Å−3 |
| 0 restraints | Δρmin = −0.45 e Å−3 |
| 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 |
| V1 | 0.92911 (10) | 1.06195 (6) | 0.82727 (7) | 0.0219 (3) | |
| V2 | 0.93856 (11) | 0.85376 (6) | 0.99424 (7) | 0.0223 (3) | |
| V3 | 1.01726 (11) | 0.90023 (6) | 0.79935 (8) | 0.0261 (3) | |
| V4 | 0.84711 (10) | 1.01767 (6) | 1.02703 (7) | 0.0207 (3) | |
| V5 | 0.72947 (11) | 0.93367 (6) | 0.84923 (8) | 0.0248 (3) | |
| O1 | 0.9456 (4) | 0.9637 (2) | 0.9237 (3) | 0.0187 (9) | |
| O2 | 0.8818 (4) | 1.1018 (2) | 0.9486 (3) | 0.0200 (9) | |
| O3 | 0.7620 (4) | 1.0262 (2) | 0.7977 (3) | 0.0260 (10) | |
| O4 | 0.6972 (4) | 0.9938 (2) | 0.9652 (3) | 0.0257 (10) | |
| O5 | 1.1928 (4) | 0.9330 (2) | 0.8810 (3) | 0.0262 (10) | |
| O6 | 1.0166 (4) | 0.8267 (2) | 0.8929 (3) | 0.0258 (10) | |
| O7 | 0.9299 (4) | 1.1366 (2) | 0.7659 (3) | 0.0302 (10) | |
| O8 | 1.0138 (4) | 0.9970 (2) | 0.7546 (3) | 0.0244 (10) | |
| O9 | 0.9418 (5) | 0.7791 (2) | 1.0547 (3) | 0.0307 (11) | |
| O10 | 0.7627 (4) | 0.8570 (2) | 0.9357 (3) | 0.0263 (10) | |
| O11 | 1.0796 (5) | 0.8564 (3) | 0.7182 (3) | 0.0357 (11) | |
| O12 | 1.1132 (4) | 1.0743 (2) | 0.9091 (3) | 0.0196 (9) | |
| O13 | 0.5753 (5) | 0.9180 (3) | 0.8055 (3) | 0.0356 (11) | |
| O14 | 0.8326 (4) | 0.8887 (2) | 0.7676 (3) | 0.0257 (10) | |
| N1 | 0.4744 (8) | 0.6382 (4) | 0.4937 (6) | 0.075 (3) | |
| H1A | 0.4151 | 0.6036 | 0.4825 | 0.090* | |
| H1B | 0.5513 | 0.6357 | 0.4713 | 0.090* | |
| N2 | 0.3280 (5) | 0.6980 (3) | 0.5806 (4) | 0.0319 (13) | |
| H2A | 0.2685 | 0.6638 | 0.5665 | 0.038* | |
| N3 | 0.8180 (6) | 0.7312 (3) | 0.7329 (4) | 0.0397 (15) | |
| H3A | 0.8710 | 0.7189 | 0.6922 | 0.048* | |
| H3B | 0.8259 | 0.7738 | 0.7591 | 0.048* | |
| N4 | 0.7146 (5) | 0.6182 (3) | 0.7122 (4) | 0.0301 (13) | |
| H4A | 0.7710 | 0.6077 | 0.6730 | 0.036* | |
| C1 | 0.4480 (7) | 0.6944 (4) | 0.5460 (5) | 0.0361 (17) | |
| C2 | 0.5431 (7) | 0.7514 (4) | 0.5687 (5) | 0.0387 (18) | |
| H2 | 0.6274 | 0.7507 | 0.5459 | 0.046* | |
| C3 | 0.5103 (8) | 0.8073 (4) | 0.6245 (6) | 0.0442 (19) | |
| H3 | 0.5722 | 0.8456 | 0.6388 | 0.053* | |
| C4 | 0.3861 (7) | 0.8082 (4) | 0.6606 (6) | 0.0424 (19) | |
| H4 | 0.3651 | 0.8458 | 0.7003 | 0.051* | |
| C5 | 0.2971 (7) | 0.7535 (4) | 0.6369 (5) | 0.0355 (17) | |
| H5 | 0.2127 | 0.7538 | 0.6597 | 0.043* | |
| C6 | 0.7244 (7) | 0.6848 (4) | 0.7549 (5) | 0.0291 (15) | |
| C7 | 0.6326 (7) | 0.7000 (4) | 0.8184 (5) | 0.0418 (19) | |
| H7 | 0.6362 | 0.7453 | 0.8489 | 0.050* | |
| C8 | 0.5373 (7) | 0.6501 (5) | 0.8361 (5) | 0.045 (2) | |
| H8 | 0.4777 | 0.6604 | 0.8798 | 0.054* | |
| C9 | 0.5284 (8) | 0.5829 (5) | 0.7885 (6) | 0.048 (2) | |
| H9 | 0.4607 | 0.5490 | 0.7979 | 0.057* | |
| C10 | 0.6201 (7) | 0.5680 (4) | 0.7286 (5) | 0.0387 (18) | |
| H10 | 0.6179 | 0.5226 | 0.6983 | 0.046* | |
| N5 | 0.9609 (7) | 0.6459 (4) | 0.9265 (5) | 0.0518 (18) | |
| H5A | 0.9958 | 0.6421 | 0.8746 | 0.062* | |
| H5B | 0.9708 | 0.6859 | 0.9587 | 0.062* | |
| N6 | 0.8778 (6) | 0.5280 (3) | 0.9057 (4) | 0.0324 (13) | |
| H6 | 0.9138 | 0.5261 | 0.8540 | 0.039* | |
| C11 | 0.8923 (7) | 0.5903 (4) | 0.9568 (5) | 0.0301 (15) | |
| C12 | 0.8313 (8) | 0.5922 (4) | 1.0402 (5) | 0.0388 (18) | |
| H12 | 0.8382 | 0.6344 | 1.0773 | 0.047* | |
| C13 | 0.7629 (8) | 0.5333 (5) | 1.0668 (5) | 0.049 (2) | |
| H13 | 0.7232 | 0.5351 | 1.1224 | 0.058* | |
| C14 | 0.7509 (9) | 0.4700 (5) | 1.0124 (6) | 0.052 (2) | |
| H14 | 0.7034 | 0.4293 | 1.0305 | 0.062* | |
| C15 | 0.8107 (8) | 0.4690 (4) | 0.9313 (6) | 0.046 (2) | |
| H15 | 0.8048 | 0.4270 | 0.8939 | 0.055* | |
| O15 | 0.2400 (7) | 0.7219 (4) | 0.8838 (5) | 0.083 (2) | |
| H15A | 0.1820 | 0.7567 | 0.8795 | 0.125* | |
| H15B | 0.1917 | 0.6976 | 0.8409 | 0.125* |
| V1 | 0.0254 (6) | 0.0199 (6) | 0.0200 (6) | −0.0005 (4) | 0.0013 (4) | 0.0038 (4) |
| V2 | 0.0268 (6) | 0.0164 (5) | 0.0237 (6) | −0.0012 (4) | 0.0038 (5) | 0.0001 (4) |
| V3 | 0.0308 (6) | 0.0240 (6) | 0.0242 (6) | −0.0007 (5) | 0.0068 (5) | −0.0047 (5) |
| V4 | 0.0211 (5) | 0.0193 (5) | 0.0223 (6) | 0.0022 (4) | 0.0047 (4) | 0.0013 (4) |
| V5 | 0.0229 (6) | 0.0272 (6) | 0.0238 (6) | −0.0033 (5) | 0.0008 (5) | −0.0018 (5) |
| O1 | 0.019 (2) | 0.018 (2) | 0.020 (2) | −0.0005 (16) | 0.0022 (17) | 0.0005 (17) |
| O2 | 0.022 (2) | 0.018 (2) | 0.021 (2) | 0.0030 (17) | 0.0057 (17) | 0.0021 (17) |
| O3 | 0.025 (2) | 0.028 (2) | 0.024 (2) | 0.0028 (18) | −0.0015 (19) | 0.0031 (19) |
| O4 | 0.019 (2) | 0.028 (2) | 0.031 (3) | 0.0003 (18) | 0.0050 (18) | 0.0031 (19) |
| O5 | 0.023 (2) | 0.027 (2) | 0.030 (3) | 0.0042 (18) | 0.0085 (19) | −0.0017 (19) |
| O6 | 0.034 (2) | 0.016 (2) | 0.029 (3) | 0.0033 (18) | 0.008 (2) | −0.0041 (18) |
| O7 | 0.032 (2) | 0.029 (3) | 0.030 (3) | −0.001 (2) | 0.003 (2) | 0.008 (2) |
| O8 | 0.032 (2) | 0.024 (2) | 0.018 (2) | −0.0013 (19) | 0.0040 (18) | −0.0012 (18) |
| O9 | 0.044 (3) | 0.022 (2) | 0.027 (3) | −0.005 (2) | 0.006 (2) | 0.0011 (19) |
| O10 | 0.030 (2) | 0.022 (2) | 0.028 (3) | −0.0047 (19) | 0.0069 (19) | −0.0013 (19) |
| O11 | 0.048 (3) | 0.033 (3) | 0.028 (3) | −0.001 (2) | 0.014 (2) | −0.005 (2) |
| O12 | 0.024 (2) | 0.017 (2) | 0.019 (2) | −0.0020 (17) | 0.0035 (17) | 0.0010 (17) |
| O13 | 0.031 (3) | 0.040 (3) | 0.033 (3) | 0.000 (2) | −0.006 (2) | −0.003 (2) |
| O14 | 0.032 (2) | 0.021 (2) | 0.023 (2) | −0.0006 (19) | 0.0014 (19) | −0.0029 (18) |
| N1 | 0.053 (4) | 0.072 (6) | 0.109 (7) | −0.026 (4) | 0.043 (4) | −0.056 (5) |
| N2 | 0.026 (3) | 0.032 (3) | 0.038 (4) | −0.011 (2) | 0.005 (3) | −0.013 (3) |
| N3 | 0.040 (3) | 0.034 (3) | 0.047 (4) | −0.002 (3) | 0.013 (3) | −0.013 (3) |
| N4 | 0.025 (3) | 0.036 (3) | 0.032 (3) | 0.002 (2) | 0.011 (2) | −0.002 (3) |
| C1 | 0.033 (4) | 0.040 (4) | 0.037 (4) | −0.005 (3) | 0.008 (3) | −0.009 (3) |
| C2 | 0.032 (4) | 0.049 (5) | 0.036 (4) | −0.018 (3) | 0.008 (3) | 0.002 (4) |
| C3 | 0.039 (4) | 0.033 (4) | 0.058 (5) | −0.017 (3) | −0.003 (4) | −0.001 (4) |
| C4 | 0.037 (4) | 0.031 (4) | 0.057 (5) | 0.001 (3) | 0.000 (4) | −0.012 (4) |
| C5 | 0.035 (4) | 0.031 (4) | 0.041 (4) | −0.002 (3) | 0.006 (3) | −0.002 (3) |
| C6 | 0.027 (3) | 0.033 (4) | 0.027 (4) | 0.005 (3) | −0.001 (3) | 0.000 (3) |
| C7 | 0.036 (4) | 0.048 (5) | 0.042 (5) | 0.012 (4) | 0.010 (4) | −0.014 (4) |
| C8 | 0.030 (4) | 0.067 (6) | 0.042 (5) | 0.001 (4) | 0.019 (3) | −0.010 (4) |
| C9 | 0.040 (4) | 0.049 (5) | 0.057 (5) | −0.013 (4) | 0.015 (4) | −0.010 (4) |
| C10 | 0.045 (4) | 0.032 (4) | 0.038 (4) | −0.008 (3) | 0.003 (4) | −0.014 (3) |
| N5 | 0.068 (5) | 0.035 (4) | 0.054 (5) | −0.001 (3) | 0.016 (4) | −0.005 (3) |
| N6 | 0.039 (3) | 0.037 (3) | 0.022 (3) | 0.008 (3) | 0.008 (3) | −0.008 (3) |
| C11 | 0.027 (3) | 0.037 (4) | 0.024 (4) | 0.011 (3) | −0.008 (3) | −0.005 (3) |
| C12 | 0.049 (5) | 0.044 (5) | 0.024 (4) | 0.016 (4) | 0.008 (3) | −0.006 (3) |
| C13 | 0.051 (5) | 0.066 (6) | 0.033 (5) | 0.007 (4) | 0.019 (4) | −0.001 (4) |
| C14 | 0.056 (5) | 0.051 (5) | 0.052 (5) | −0.009 (4) | 0.021 (4) | 0.003 (4) |
| C15 | 0.056 (5) | 0.036 (4) | 0.047 (5) | −0.004 (4) | 0.009 (4) | −0.014 (4) |
| O15 | 0.062 (4) | 0.098 (6) | 0.086 (5) | 0.022 (4) | −0.004 (4) | −0.013 (4) |
| V1—O7 | 1.616 (4) | N2—H2A | 0.8600 |
| V1—O3 | 1.767 (4) | N3—C6 | 1.316 (9) |
| V1—O8 | 1.842 (4) | N3—H3A | 0.8600 |
| V1—O2 | 1.991 (4) | N3—H3B | 0.8599 |
| V1—O12 | 2.038 (4) | N4—C10 | 1.345 (9) |
| V1—O1 | 2.250 (4) | N4—C6 | 1.353 (8) |
| V2—O9 | 1.608 (4) | N4—H4A | 0.8599 |
| V2—O6 | 1.794 (4) | C1—C2 | 1.405 (9) |
| V2—O10 | 1.823 (4) | C2—C3 | 1.357 (11) |
| V2—O12i | 2.015 (4) | C2—H2 | 0.9299 |
| V2—O2i | 2.017 (4) | C3—C4 | 1.387 (11) |
| V2—O1 | 2.243 (4) | C3—H3 | 0.9300 |
| V3—O11 | 1.594 (4) | C4—C5 | 1.339 (10) |
| V3—O14 | 1.827 (4) | C4—H4 | 0.9300 |
| V3—O8 | 1.871 (4) | C5—H5 | 0.9300 |
| V3—O6 | 1.891 (4) | C6—C7 | 1.389 (9) |
| V3—O5 | 2.045 (4) | C7—C8 | 1.352 (11) |
| V3—O1 | 2.305 (4) | C7—H7 | 0.9300 |
| V4—O4 | 1.676 (4) | C8—C9 | 1.396 (11) |
| V4—O5i | 1.680 (4) | C8—H8 | 0.9300 |
| V4—O12i | 1.921 (4) | C9—C10 | 1.349 (10) |
| V4—O2 | 1.953 (4) | C9—H9 | 0.9300 |
| V4—O1i | 2.097 (4) | C10—H10 | 0.9300 |
| V4—O1 | 2.111 (4) | N5—C11 | 1.319 (9) |
| V5—O13 | 1.590 (5) | N5—H5A | 0.8600 |
| V5—O14 | 1.835 (4) | N5—H5B | 0.8601 |
| V5—O10 | 1.864 (4) | N6—C15 | 1.335 (9) |
| V5—O3 | 1.881 (4) | N6—C11 | 1.346 (8) |
| V5—O4 | 2.045 (4) | N6—H6 | 0.8600 |
| V5—O1 | 2.318 (4) | C11—C12 | 1.403 (9) |
| O1—V4i | 2.097 (4) | C12—C13 | 1.346 (11) |
| O2—V2i | 2.017 (4) | C12—H12 | 0.9300 |
| O5—V4i | 1.680 (4) | C13—C14 | 1.386 (11) |
| O12—V4i | 1.921 (4) | C13—H13 | 0.9300 |
| O12—V2i | 2.015 (4) | C14—C15 | 1.366 (11) |
| N1—C1 | 1.312 (9) | C14—H14 | 0.9300 |
| N1—H1A | 0.8599 | C15—H15 | 0.9300 |
| N1—H1B | 0.8600 | O15—H15A | 0.8499 |
| N2—C1 | 1.339 (8) | O15—H15B | 0.8496 |
| N2—C5 | 1.350 (8) | ||
| O7—V1—O3 | 104.4 (2) | V1—O1—V3 | 85.95 (14) |
| O7—V1—O8 | 101.4 (2) | V4i—O1—V5 | 170.8 (2) |
| O3—V1—O8 | 95.96 (19) | V4—O1—V5 | 87.36 (14) |
| O7—V1—O2 | 100.7 (2) | V2—O1—V5 | 85.25 (13) |
| O3—V1—O2 | 91.58 (18) | V1—O1—V5 | 85.16 (14) |
| O8—V1—O2 | 154.05 (18) | V3—O1—V5 | 83.19 (13) |
| O7—V1—O12 | 98.8 (2) | V4—O2—V1 | 107.04 (19) |
| O3—V1—O12 | 155.27 (18) | V4—O2—V2i | 106.87 (19) |
| O8—V1—O12 | 87.81 (17) | V1—O2—V2i | 101.98 (17) |
| O2—V1—O12 | 75.49 (16) | V1—O3—V5 | 115.8 (2) |
| O7—V1—O1 | 173.8 (2) | V4—O4—V5 | 110.3 (2) |
| O3—V1—O1 | 81.16 (17) | V4i—O5—V3 | 109.7 (2) |
| O8—V1—O1 | 80.48 (16) | V2—O6—V3 | 114.8 (2) |
| O2—V1—O1 | 76.19 (15) | V1—O8—V3 | 113.5 (2) |
| O12—V1—O1 | 75.36 (15) | V2—O10—V5 | 113.8 (2) |
| O9—V2—O6 | 102.8 (2) | V4i—O12—V2i | 107.03 (18) |
| O9—V2—O10 | 103.1 (2) | V4i—O12—V1 | 106.72 (18) |
| O6—V2—O10 | 96.7 (2) | V2i—O12—V1 | 100.42 (17) |
| O9—V2—O12i | 99.71 (19) | V3—O14—V5 | 113.9 (2) |
| O6—V2—O12i | 154.72 (18) | C1—N1—H1A | 119.8 |
| O10—V2—O12i | 89.15 (18) | C1—N1—H1B | 120.1 |
| O9—V2—O2i | 99.5 (2) | H1A—N1—H1B | 120.0 |
| O6—V2—O2i | 89.59 (18) | C1—N2—C5 | 122.3 (6) |
| O10—V2—O2i | 154.54 (18) | C1—N2—H2A | 119.0 |
| O12i—V2—O2i | 75.43 (16) | C5—N2—H2A | 118.7 |
| O9—V2—O1 | 173.9 (2) | C6—N3—H3A | 120.0 |
| O6—V2—O1 | 80.77 (17) | C6—N3—H3B | 120.0 |
| O10—V2—O1 | 81.23 (16) | H3A—N3—H3B | 120.0 |
| O12i—V2—O1 | 75.85 (15) | C10—N4—C6 | 122.6 (6) |
| O2i—V2—O1 | 75.47 (15) | C10—N4—H4A | 118.8 |
| O11—V3—O14 | 103.0 (2) | C6—N4—H4A | 118.6 |
| O11—V3—O8 | 102.3 (2) | N1—C1—N2 | 119.8 (7) |
| O14—V3—O8 | 92.79 (19) | N1—C1—C2 | 122.0 (7) |
| O11—V3—O6 | 101.5 (2) | N2—C1—C2 | 118.1 (6) |
| O14—V3—O6 | 90.05 (19) | C3—C2—C1 | 119.1 (7) |
| O8—V3—O6 | 154.81 (18) | C3—C2—H2 | 120.5 |
| O11—V3—O5 | 100.7 (2) | C1—C2—H2 | 120.4 |
| O14—V3—O5 | 156.20 (18) | C2—C3—C4 | 121.0 (7) |
| O8—V3—O5 | 84.18 (18) | C2—C3—H3 | 119.4 |
| O6—V3—O5 | 83.21 (18) | C4—C3—H3 | 119.6 |
| O11—V3—O1 | 175.1 (2) | C5—C4—C3 | 118.5 (7) |
| O14—V3—O1 | 81.71 (16) | C5—C4—H4 | 120.8 |
| O8—V3—O1 | 78.46 (16) | C3—C4—H4 | 120.8 |
| O6—V3—O1 | 77.20 (16) | C4—C5—N2 | 121.0 (7) |
| O5—V3—O1 | 74.55 (15) | C4—C5—H5 | 119.5 |
| O4—V4—O5i | 105.8 (2) | N2—C5—H5 | 119.5 |
| O4—V4—O12i | 97.83 (19) | N3—C6—N4 | 118.4 (6) |
| O5i—V4—O12i | 98.45 (19) | N3—C6—C7 | 124.3 (7) |
| O4—V4—O2 | 96.17 (19) | N4—C6—C7 | 117.3 (6) |
| O5i—V4—O2 | 96.12 (19) | C8—C7—C6 | 120.9 (7) |
| O12i—V4—O2 | 156.20 (17) | C8—C7—H7 | 119.4 |
| O4—V4—O1i | 166.03 (18) | C6—C7—H7 | 119.7 |
| O5i—V4—O1i | 88.08 (18) | C7—C8—C9 | 119.9 (7) |
| O12i—V4—O1i | 81.50 (16) | C7—C8—H8 | 120.3 |
| O2—V4—O1i | 80.29 (16) | C9—C8—H8 | 119.9 |
| O4—V4—O1 | 87.89 (18) | C10—C9—C8 | 118.7 (7) |
| O5i—V4—O1 | 166.22 (19) | C10—C9—H9 | 120.7 |
| O12i—V4—O1 | 81.02 (16) | C8—C9—H9 | 120.6 |
| O2—V4—O1 | 80.36 (16) | N4—C10—C9 | 120.5 (7) |
| O1i—V4—O1 | 78.21 (17) | N4—C10—H10 | 119.7 |
| O13—V5—O14 | 104.4 (2) | C9—C10—H10 | 119.7 |
| O13—V5—O10 | 101.8 (2) | C11—N5—H5A | 120.0 |
| O14—V5—O10 | 91.43 (19) | C11—N5—H5B | 120.0 |
| O13—V5—O3 | 102.0 (2) | H5A—N5—H5B | 120.0 |
| O14—V5—O3 | 90.73 (19) | C15—N6—C11 | 123.3 (6) |
| O10—V5—O3 | 154.79 (19) | C15—N6—H6 | 118.4 |
| O13—V5—O4 | 100.0 (2) | C11—N6—H6 | 118.3 |
| O14—V5—O4 | 155.60 (18) | N5—C11—N6 | 119.3 (6) |
| O10—V5—O4 | 83.94 (18) | N5—C11—C12 | 123.6 (7) |
| O3—V5—O4 | 83.79 (18) | N6—C11—C12 | 117.1 (7) |
| O13—V5—O1 | 174.4 (2) | C13—C12—C11 | 120.4 (7) |
| O14—V5—O1 | 81.21 (17) | C13—C12—H12 | 119.8 |
| O10—V5—O1 | 78.41 (16) | C11—C12—H12 | 119.8 |
| O3—V5—O1 | 77.12 (16) | C12—C13—C14 | 120.8 (7) |
| O4—V5—O1 | 74.39 (15) | C12—C13—H13 | 119.6 |
| V4i—O1—V4 | 101.79 (16) | C14—C13—H13 | 119.6 |
| V4i—O1—V2 | 94.50 (15) | C15—C14—C13 | 118.2 (8) |
| V4—O1—V2 | 93.22 (15) | C15—C14—H14 | 120.9 |
| V4i—O1—V1 | 93.87 (15) | C13—C14—H14 | 120.9 |
| V4—O1—V1 | 93.23 (15) | N6—C15—C14 | 120.3 (7) |
| V2—O1—V1 | 168.2 (2) | N6—C15—H15 | 119.9 |
| V4i—O1—V3 | 87.65 (14) | C14—C15—H15 | 119.9 |
| V4—O1—V3 | 170.6 (2) | H15A—O15—H15B | 91.4 |
| V2—O1—V3 | 86.07 (14) |
| H··· | ||||
| N1—H1A···O4ii | 0.86 | 2.44 | 3.217 (9) | 150 |
| N1—H1A···O5iii | 0.86 | 2.55 | 3.286 (8) | 144 |
| N1—H1B···O10iv | 0.86 | 2.21 | 3.058 (8) | 169 |
| N2—H2A···O2ii | 0.86 | 1.85 | 2.697 (7) | 168 |
| N3—H3A···O9iv | 0.86 | 2.17 | 2.969 (7) | 155 |
| N3—H3A···O7v | 0.86 | 2.48 | 3.017 (7) | 122 |
| N3—H3B···O14 | 0.86 | 2.09 | 2.908 (7) | 158 |
| N4—H4A···O12v | 0.86 | 1.84 | 2.698 (6) | 174 |
| N5—H5A···O7v | 0.86 | 2.23 | 3.085 (8) | 175 |
| N5—H5B···O9 | 0.86 | 2.22 | 3.057 (8) | 164 |
| N6—H6···O8v | 0.86 | 1.87 | 2.709 (7) | 166 |
| O15—H15A···O6vi | 0.85 | 2.09 | 2.926 (8) | 166 |
| O15—H15B···O7ii | 0.85 | 2.13 | 2.977 (8) | 180 |
Selected bond lengths (Å)
| V1—O7 | 1.616 (4) |
| V1—O3 | 1.767 (4) |
| V1—O8 | 1.842 (4) |
| V1—O2 | 1.991 (4) |
| V1—O12 | 2.038 (4) |
| V1—O1 | 2.250 (4) |
| V2—O9 | 1.608 (4) |
| V2—O6 | 1.794 (4) |
| V2—O10 | 1.823 (4) |
| V2—O12i | 2.015 (4) |
| V2—O2i | 2.017 (4) |
| V2—O1 | 2.243 (4) |
| V3—O11 | 1.594 (4) |
| V3—O14 | 1.827 (4) |
| V3—O8 | 1.871 (4) |
| V3—O6 | 1.891 (4) |
| V3—O5 | 2.045 (4) |
| V3—O1 | 2.305 (4) |
| V4—O4 | 1.676 (4) |
| V4—O5i | 1.680 (4) |
| V4—O12i | 1.921 (4) |
| V4—O2 | 1.953 (4) |
| V4—O1i | 2.097 (4) |
| V4—O1 | 2.111 (4) |
| V5—O13 | 1.590 (5) |
| V5—O14 | 1.835 (4) |
| V5—O10 | 1.864 (4) |
| V5—O3 | 1.881 (4) |
| V5—O4 | 2.045 (4) |
| V5—O1 | 2.318 (4) |
Symmetry code: (i) .
Hydrogen-bond geometry (Å, °)
| H⋯ | ||||
|---|---|---|---|---|
| N1—H1 | 0.86 | 2.44 | 3.217 (9) | 150 |
| N1—H1 | 0.86 | 2.55 | 3.286 (8) | 144 |
| N1—H1 | 0.86 | 2.21 | 3.058 (8) | 169 |
| N2—H2 | 0.86 | 1.85 | 2.697 (7) | 168 |
| N3—H3 | 0.86 | 2.17 | 2.969 (7) | 155 |
| N3—H3 | 0.86 | 2.48 | 3.017 (7) | 122 |
| N3—H3 | 0.86 | 2.09 | 2.908 (7) | 158 |
| N4—H4 | 0.86 | 1.84 | 2.698 (6) | 174 |
| N5—H5 | 0.86 | 2.23 | 3.085 (8) | 175 |
| N5—H5 | 0.86 | 2.22 | 3.057 (8) | 164 |
| N6—H6⋯O8v | 0.86 | 1.87 | 2.709 (7) | 166 |
| O15—H15 | 0.85 | 2.09 | 2.926 (8) | 166 |
| O15—H15 | 0.85 | 2.13 | 2.977 (8) | 180 |
Symmetry codes: (ii) ; (iii) ; (iv) ; (v) ; (vi) .