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metal-organic compounds
The structure refined as [H3O]+·[[(C12H8N2)VIV(=O)O]2(H2AsO4)]− by Zheng, Zhang & Yang [J. Chem. Crystallogr. (2005). 34, 267–273] is rerefined as [V2O4(HAsO4)(C12H8N2)2]·H2O, whose crystal structure features a disordered [HAsO4]2− group that links the dinuclear molecules through O—HO hydrogen bonds into a chain running along the a axis.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807010082/xu2216sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807010082/xu2216Isup2.hkl |
CCDC reference: 643676
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.007 Å
- R factor = 0.050
- wR factor = 0.113
- Data-to-parameter ratio = 15.2
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT432_ALERT_2_B Short Inter X...Y Contact O1W .. C13 .. 2.91 Ang.
Alert level C CRYSC01_ALERT_1_C The word below has not been recognised as a standard identifier. Yellowish PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ? PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 2
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Computing details top
Data collection: CrystalClear (Rigaku Corporation, 2000); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: atomic coordinates from published structure; program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2007).
µ-Hydrogenarsenato-κ2O:O'-di-µ-oxo-κ4O:O-bis[oxo(1,10- phenanthroline-κ2N,N')vanadium(V)] monohydrate top
Crystal data top
[V2O4(HAsO4)(C12H8N2)2]·H2O | F(000) = 1368 |
Mr = 684.23 | Dx = 1.879 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 7834 reflections |
a = 9.175 (2) Å | θ = 2.5–27.5° |
b = 18.638 (5) Å | µ = 2.20 mm−1 |
c = 14.482 (4) Å | T = 295 K |
β = 102.333 (3)° | Prism, yellow–green |
V = 2419 (1) Å3 | 0.45 × 0.13 × 0.10 mm |
Z = 4 |
Data collection top
Rigaku Mercury diffractometer | 5517 independent reflections |
Radiation source: medium-focus sealed tube | 5151 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.031 |
ω scans | θmax = 27.5°, θmin = 2.5° |
Absorption correction: multi-scan (Jacobson, 1998) | h = −11→11 |
Tmin = 0.717, Tmax = 0.803 | k = −24→24 |
18641 measured reflections | l = −18→18 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.050 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.113 | H-atom parameters constrained |
S = 1.24 | w = 1/[σ2(Fo2) + (0.0158P)2 + 13.118P] where P = (Fo2 + 2Fc2)/3 |
5517 reflections | (Δ/σ)max = 0.001 |
363 parameters | Δρmax = 0.65 e Å−3 |
6 restraints | Δρmin = −0.91 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | Occ. (<1) | |
As1 | 0.71488 (5) | 0.49891 (2) | 0.41755 (3) | 0.0124 (1) | |
V1 | 0.71507 (8) | 0.48151 (4) | 0.19344 (5) | 0.0146 (2) | |
V2 | 0.68297 (8) | 0.34485 (4) | 0.30780 (5) | 0.0136 (2) | |
O1 | 0.8636 (3) | 0.5141 (2) | 0.5051 (2) | 0.0218 (7) | |
O2 | 0.5651 (3) | 0.5401 (2) | 0.4433 (2) | 0.0189 (6) | |
O3 | 0.6744 (3) | 0.4102 (2) | 0.4076 (2) | 0.0171 (6) | |
O4 | 0.7488 (4) | 0.5293 (2) | 0.3142 (2) | 0.0182 (6) | |
O5 | 0.7396 (4) | 0.2733 (2) | 0.3684 (2) | 0.0223 (7) | |
O6 | 0.8279 (3) | 0.3767 (2) | 0.2689 (2) | 0.0166 (6) | |
O7 | 0.5698 (3) | 0.4295 (2) | 0.1992 (2) | 0.0178 (6) | |
O8 | 0.6495 (4) | 0.5477 (2) | 0.1255 (2) | 0.0213 (7) | |
O1w | 0.9109 (6) | 0.1756 (3) | 0.2749 (5) | 0.077 (2) | |
N1 | 0.7692 (4) | 0.4237 (2) | 0.0762 (2) | 0.0177 (7) | |
N2 | 0.9576 (4) | 0.4974 (2) | 0.2056 (2) | 0.0151 (7) | |
N3 | 0.6018 (4) | 0.2786 (2) | 0.1874 (3) | 0.0169 (7) | |
N4 | 0.4401 (4) | 0.3327 (2) | 0.3012 (2) | 0.0140 (7) | |
C1 | 0.6709 (5) | 0.3903 (3) | 0.0096 (3) | 0.0220 (9) | |
C2 | 0.7128 (6) | 0.3516 (3) | −0.0632 (3) | 0.027 (1) | |
C3 | 0.8603 (6) | 0.3465 (3) | −0.0666 (3) | 0.026 (1) | |
C4 | 0.9675 (5) | 0.3830 (2) | 0.0008 (3) | 0.020 (1) | |
C5 | 0.9162 (5) | 0.4217 (2) | 0.0711 (3) | 0.015 (1) | |
C6 | 1.0183 (5) | 0.4618 (2) | 0.1404 (3) | 0.015 (1) | |
C7 | 1.1250 (6) | 0.3849 (2) | 0.0011 (3) | 0.024 (1) | |
C8 | 1.2204 (5) | 0.4239 (3) | 0.0662 (3) | 0.023 (1) | |
C9 | 1.1698 (5) | 0.4636 (2) | 0.1385 (3) | 0.019 (1) | |
C10 | 1.2640 (5) | 0.5040 (2) | 0.2087 (3) | 0.021 (1) | |
C11 | 1.2044 (5) | 0.5385 (2) | 0.2758 (3) | 0.022 (1) | |
C12 | 1.0506 (5) | 0.5342 (2) | 0.2725 (3) | 0.020 (1) | |
C13 | 0.6879 (5) | 0.2497 (2) | 0.1346 (3) | 0.021 (1) | |
C14 | 0.6348 (5) | 0.1994 (3) | 0.0637 (3) | 0.023 (1) | |
C15 | 0.4863 (5) | 0.1806 (2) | 0.0443 (3) | 0.021 (1) | |
C16 | 0.3914 (5) | 0.2114 (2) | 0.0980 (3) | 0.017 (1) | |
C17 | 0.4551 (5) | 0.2589 (2) | 0.1700 (3) | 0.014 (1) | |
C18 | 0.2342 (5) | 0.1954 (2) | 0.0845 (3) | 0.020 (1) | |
C19 | 0.1507 (5) | 0.2248 (2) | 0.1413 (3) | 0.019 (1) | |
C20 | 0.3676 (5) | 0.2891 (2) | 0.2305 (3) | 0.013 (1) | |
C21 | 0.2136 (5) | 0.2735 (2) | 0.2156 (3) | 0.015 (1) | |
C22 | 0.1320 (5) | 0.3083 (2) | 0.2750 (3) | 0.016 (1) | |
C23 | 0.2056 (5) | 0.3546 (2) | 0.3438 (3) | 0.017 (1) | |
C24 | 0.3594 (5) | 0.3640 (2) | 0.3562 (3) | 0.017 (1) | |
H1o | 0.9417 | 0.5160 | 0.4825 | 0.026* | 0.50 |
H2o | 0.5305 | 0.5148 | 0.4825 | 0.023* | 0.50 |
H1w1 | 0.8627 | 0.2071 | 0.2997 | 0.092* | |
H1w2 | 0.8974 | 0.1352 | 0.3019 | 0.092* | |
H1 | 0.5703 | 0.3928 | 0.0113 | 0.026* | |
H2 | 0.6407 | 0.3292 | −0.1091 | 0.033* | |
H3 | 0.8894 | 0.3192 | −0.1132 | 0.032* | |
H7 | 1.1613 | 0.3591 | −0.0441 | 0.028* | |
H8 | 1.3210 | 0.4250 | 0.0642 | 0.028* | |
H10 | 1.3654 | 0.5073 | 0.2097 | 0.025* | |
H11 | 1.2658 | 0.5647 | 0.3234 | 0.027* | |
H12 | 1.0121 | 0.5579 | 0.3185 | 0.023* | |
H13 | 0.7875 | 0.2634 | 0.1451 | 0.025* | |
H14 | 0.6995 | 0.1787 | 0.0298 | 0.028* | |
H15 | 0.4492 | 0.1480 | −0.0036 | 0.025* | |
H18 | 0.1898 | 0.1645 | 0.0362 | 0.024* | |
H19 | 0.0500 | 0.2131 | 0.1318 | 0.023* | |
H22 | 0.0302 | 0.3001 | 0.2678 | 0.019* | |
H23 | 0.1529 | 0.3794 | 0.3817 | 0.020* | |
H24 | 0.4077 | 0.3934 | 0.4051 | 0.020* |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
As1 | 0.0129 (2) | 0.0140 (2) | 0.0107 (2) | −0.0022 (2) | 0.0037 (2) | −0.0022 (2) |
V1 | 0.0133 (4) | 0.0186 (4) | 0.0129 (3) | 0.0021 (3) | 0.0051 (3) | 0.0015 (3) |
V2 | 0.0135 (3) | 0.0147 (3) | 0.0124 (3) | −0.0008 (3) | 0.0022 (3) | −0.0021 (3) |
O1 | 0.015 (2) | 0.030 (2) | 0.019 (2) | −0.003 (1) | 0.000 (1) | −0.006 (13) |
O2 | 0.017 (2) | 0.020 (2) | 0.022 (2) | 0.0041 (2) | 0.010 (1) | 0.001 (1) |
O3 | 0.022 (2) | 0.016 (1) | 0.01 (1) | −0.003 (1) | 0.005 (12) | −0.001 (11) |
O4 | 0.026 (2) | 0.017 (2) | 0.015 (2) | −0.003 (1) | 0.011 (1) | −0.001 (1) |
O5 | 0.029 (2) | 0.017 (2) | 0.020 (2) | 0.001 (1) | 0.003 (1) | −0.001 (1) |
O6 | 0.014 (2) | 0.019 (2) | 0.016 (1) | 0.000 (1) | 0.002 (1) | −0.002 (1) |
O7 | 0.014 (2) | 0.022 (2) | 0.017 (2) | 0.002 (1) | 0.00 (1) | 0.001 (1) |
O8 | 0.021 (2) | 0.026 (2) | 0.019 (2) | 0.006 (1) | 0.008 (1) | 0.006 (1) |
O1w | 0.060 (3) | 0.061 (3) | 0.108 (4) | 0.001 (3) | 0.016 (3) | 0.029 (3) |
N1 | 0.018 (2) | 0.022 (2) | 0.013 (2) | 0.001 (2) | 0.003 (1) | 0.002 (1) |
N2 | 0.017 (2) | 0.017 (2) | 0.013 (2) | 0.002 (1) | 0.007 (2) | 0.001 (1) |
N3 | 0.016 (2) | 0.018 (2) | 0.017 (2) | −0.001 (1) | 0.005 (2) | −0.004 (1) |
N4 | 0.014 (2) | 0.013 (2) | 0.016 (2) | −0.002 (1) | 0.005 (1) | −0.001 (1) |
C1 | 0.019 (2) | 0.028 (2) | 0.018 (2) | −0.001 (2) | 0.000 (2) | 0.002 (2) |
C2 | 0.034 (3) | 0.030 (3) | 0.017 (2) | −0.005 (2) | 0.003 (2) | −0.004 (2) |
C3 | 0.043 (3) | 0.023 (2) | 0.015 (2) | 0.005 (2) | 0.010 (2) | −0.001 (2) |
C4 | 0.031 (3) | 0.017 (2) | 0.015 (2) | 0.006 (2) | 0.009 (2) | 0.004 (2) |
C5 | 0.016 (2) | 0.016 (2) | 0.016 (2) | 0.002 (2) | 0.006 (2) | 0.004 (2) |
C6 | 0.016 (2) | 0.017 (2) | 0.013 (2) | 0.003 (2) | 0.005 (2) | 0.004 (2) |
C7 | 0.032 (3) | 0.022 (2) | 0.021 (2) | 0.012 (2) | 0.016 (2) | 0.006 (2) |
C8 | 0.023 (2) | 0.027 (2) | 0.025 (2) | 0.010 (2) | 0.014 (2) | 0.008 (2) |
C9 | 0.020 (2) | 0.019 (2) | 0.019 (2) | 0.005 (2) | 0.008 (2) | 0.009 (2) |
C10 | 0.011 (2) | 0.021 (2) | 0.031 (2) | 0.000 (2) | 0.005 (2) | 0.009 (2) |
C11 | 0.021 (2) | 0.019 (2) | 0.026 (2) | −0.005 (2) | 0.006 (2) | 0.000 (2) |
C12 | 0.023 (2) | 0.019 (2) | 0.018 (2) | −0.004 (2) | 0.006 (2) | −0.003 (2) |
C13 | 0.018 (2) | 0.025 (2) | 0.021 (2) | −0.001 (2) | 0.005 (2) | −0.008 (2) |
C14 | 0.026 (2) | 0.025 (2) | 0.021 (2) | 0.002 (2) | 0.010 (2) | −0.009 (2) |
C15 | 0.024 (2) | 0.019 (2) | 0.017 (2) | 0.002 (2) | 0.000 (2) | −0.004 (2) |
C16 | 0.018 (2) | 0.0152 (19) | 0.015 (2) | 0.002 (2) | 0.000 (2) | 0.000 (2) |
C17 | 0.015 (2) | 0.0120 (19) | 0.014 (2) | 0.000 (2) | 0.002 (2) | 0.001 (2) |
C18 | 0.020 (2) | 0.019 (2) | 0.018 (2) | −0.002 (2) | −0.002 (2) | −0.005 (2) |
C19 | 0.015 (2) | 0.021 (2) | 0.021 (2) | −0.002 (2) | 0.001 (2) | −0.002 (2) |
C20 | 0.014 (2) | 0.0193 (2) | 0.012 (2) | −0.003 (2) | 0.001 (2) | 0.000 (1) |
C21 | 0.015 (2) | 0.013 (2) | 0.016 (2) | 0.000 (2) | 0.002 (2) | 0.001 (2) |
C22 | 0.011 (2) | 0.018 (2) | 0.019 (2) | 0.001 (2) | 0.004 (2) | 0.004 (2) |
C23 | 0.021 (2) | 0.017 (2) | 0.015 (2) | 0.005 (2) | 0.008 (2) | 0.003 (2) |
C24 | 0.020 (2) | 0.017 (2) | 0.013 (2) | −0.003 (2) | 0.003 (2) | −0.002 (2) |
Geometric parameters (Å, º) top
As1—O1 | 1.676 (3) | C10—C11 | 1.374 (6) |
As1—O2 | 1.684 (3) | C11—C12 | 1.403 (6) |
As1—O3 | 1.694 (3) | C13—C14 | 1.400 (6) |
As1—O4 | 1.690 (3) | C14—C15 | 1.376 (7) |
V1—O4 | 1.928 (3) | C15—C16 | 1.408 (6) |
V1—O6 | 2.367 (3) | C16—C17 | 1.397 (6) |
V1—O7 | 1.664 (3) | C16—C18 | 1.444 (6) |
V1—O8 | 1.612 (3) | C17—C20 | 1.425 (6) |
V1—N1 | 2.156 (4) | C18—C19 | 1.354 (6) |
V1—N2 | 2.214 (4) | C19—C21 | 1.431 (6) |
V2—O3 | 1.904 (3) | C20—C21 | 1.413 (6) |
V2—O5 | 1.620 (3) | C21—C22 | 1.413 (6) |
V2—O6 | 1.661 (3) | C22—C23 | 1.381 (6) |
V2—N3 | 2.137 (4) | C23—C24 | 1.394 (6) |
V2—N4 | 2.222 (4) | O1—H1o | 0.85 |
V2—O7 | 2.312 (3) | O2—H2o | 0.85 |
N1—C1 | 1.327 (6) | O1w—H1w1 | 0.86 |
N1—C5 | 1.367 (6) | O1w—H1w2 | 0.87 |
N2—C12 | 1.336 (6) | C1—H1 | 0.93 |
N2—C6 | 1.367 (5) | C2—H2 | 0.93 |
N3—C13 | 1.324 (6) | C3—H3 | 0.93 |
N3—C17 | 1.366 (5) | C7—H7 | 0.93 |
N4—C24 | 1.332 (5) | C8—H8 | 0.93 |
N4—C20 | 1.364 (5) | C10—H10 | 0.93 |
C1—C2 | 1.397 (7) | C11—H11 | 0.93 |
C2—C3 | 1.368 (7) | C12—H12 | 0.93 |
C3—C4 | 1.404 (7) | C13—H13 | 0.93 |
C4—C5 | 1.408 (6) | C14—H14 | 0.93 |
C4—C7 | 1.445 (7) | C15—H15 | 0.93 |
C5—C6 | 1.429 (6) | C18—H18 | 0.93 |
C6—C9 | 1.397 (6) | C19—H19 | 0.93 |
C7—C8 | 1.353 (7) | C22—H22 | 0.93 |
C8—C9 | 1.437 (6) | C23—H23 | 0.93 |
C9—C10 | 1.404 (7) | C24—H24 | 0.93 |
O1—As1—O2 | 109.0 (2) | C8—C7—C4 | 120.9 (4) |
O1—As1—O3 | 111.0 (2) | C7—C8—C9 | 121.5 (4) |
O1—As1—O4 | 109.8 (2) | C6—C9—C10 | 117.3 (4) |
O2—As1—O3 | 106.8 (2) | C6—C9—C8 | 118.7 (4) |
O2—As1—O4 | 110.9 (2) | C10—C9—C8 | 124.0 (4) |
O3—As1—O4 | 109.3 (1) | C11—C10—C9 | 119.2 (4) |
O4—V1—O6 | 89.6 (1) | C10—C11—C12 | 119.9 (4) |
O4—V1—O7 | 101.5 (1) | N2—C12—C11 | 122.5 (4) |
O4—V1—O8 | 99.6 (2) | N3—C13—C14 | 122.6 (4) |
O4—V1—N1 | 157.8 (1) | C15—C14—C13 | 119.6 (4) |
O4—V1—N2 | 84.4 (1) | C14—C15—C16 | 119.1 (4) |
O6—V1—O7 | 76.8 (1) | C17—C16—C15 | 117.4 (4) |
O6—V1—O8 | 169.4 (1) | C17—C16—C18 | 118.6 (4) |
O6—V1—N1 | 78.5 (1) | C15—C16—C18 | 124.0 (4) |
O6—V1—N2 | 75.0 (1) | N3—C17—C16 | 123.1 (4) |
O7—V1—O8 | 106.1 (2) | N3—C17—C20 | 116.3 (4) |
O7—V1—N1 | 94.0 (2) | C16—C17—C20 | 120.6 (4) |
O7—V1—N2 | 151.2 (1) | C19—C18—C16 | 120.9 (4) |
O8—V1—N1 | 91.1 (2) | C18—C19—C21 | 121.5 (4) |
O8—V1—N2 | 100.6 (2) | N4—C20—C21 | 123.3 (4) |
N1—V1—N2 | 74.5 (1) | N4—C20—C17 | 116.7 (4) |
O3—V2—O5 | 100.2 (2) | C21—C20—C17 | 120.0 (4) |
O3—V2—O6 | 101.2 (1) | C22—C21—C20 | 117.0 (4) |
O3—V2—O7 | 89.7 (1) | C22—C21—C19 | 124.6 (4) |
O3—V2—N3 | 157.7 (1) | C20—C21—C19 | 118.4 (4) |
O3—V2—N4 | 83.9 (1) | C23—C22—C21 | 119.0 (4) |
O5—V2—O6 | 106.9 (2) | C22—C23—C24 | 119.9 (4) |
O5—V2—O7 | 167.4 (1) | N4—C24—C23 | 122.9 (4) |
O5—V2—N3 | 88.9 (2) | As1—O1—H1o | 109.5 |
O5—V2—N4 | 98.2 (2) | As1—O2—H2o | 109.5 |
O6—V2—O7 | 78.5 (1) | H1w1—O1w—H1w2 | 105.6 |
O6—V2—N3 | 95.4 (1) | N1—C1—H1 | 118.8 |
O6—V2—N4 | 152.9 (1) | C2—C1—H1 | 118.8 |
O7—V2—N3 | 79.1 (1) | C3—C2—H2 | 120.1 |
O7—V2—N4 | 74.9 (1) | C1—C2—H2 | 120.1 |
N3—V2—N4 | 74.6 (1) | C2—C3—H3 | 120.2 |
As1—O3—V2 | 130.2 (2) | C4—C3—H3 | 120.2 |
As1—O4—V1 | 128.6 (2) | C8—C7—H7 | 119.6 |
V2—O6—V1 | 98.5 (1) | C4—C7—H7 | 119.6 |
V1—O7—V2 | 100.6 (1) | C7—C8—H8 | 119.3 |
C1—N1—C5 | 118.2 (4) | C9—C8—H8 | 119.3 |
C1—N1—V1 | 124.9 (3) | C11—C10—H10 | 120.4 |
C5—N1—V1 | 116.9 (3) | C9—C10—H10 | 120.4 |
C12—N2—C6 | 117.3 (4) | C10—C11—H11 | 120.1 |
C12—N2—V1 | 127.0 (3) | C12—C11—H11 | 120.1 |
C6—N2—V1 | 115.5 (3) | N2—C12—H12 | 118.8 |
C13—N3—C17 | 118.0 (4) | C11—C12—H12 | 118.8 |
C13—N3—V2 | 124.0 (3) | N3—C13—H13 | 118.7 |
C17—N3—V2 | 117.6 (3) | C14—C13—H13 | 118.7 |
C24—N4—C20 | 117.7 (4) | C15—C14—H14 | 120.2 |
C24—N4—V2 | 127.6 (3) | C13—C14—H14 | 120.2 |
C20—N4—V2 | 114.6 (3) | C14—C15—H15 | 120.5 |
N1—C1—C2 | 122.5 (5) | C16—C15—H15 | 120.5 |
C3—C2—C1 | 119.8 (5) | C19—C18—H18 | 119.6 |
C2—C3—C4 | 119.6 (4) | C16—C18—H18 | 119.6 |
C3—C4—C5 | 117.2 (4) | C18—C19—H19 | 119.2 |
C3—C4—C7 | 124.5 (4) | C21—C19—H19 | 119.2 |
C5—C4—C7 | 118.3 (4) | C23—C22—H22 | 120.5 |
N1—C5—C4 | 122.7 (4) | C21—C22—H22 | 120.5 |
N1—C5—C6 | 117.0 (4) | C22—C23—H23 | 120.1 |
C4—C5—C6 | 120.4 (4) | C24—C23—H23 | 120.1 |
N2—C6—C9 | 123.8 (4) | N4—C24—H24 | 118.5 |
N2—C6—C5 | 115.9 (4) | C23—C24—H24 | 118.5 |
C9—C6—C5 | 120.3 (4) | ||
O1—As1—O3—V2 | −114.2 (2) | O5—V2—N4—C20 | −83.9 (3) |
O2—As1—O3—V2 | 127.1 (2) | O6—V2—N4—C20 | 73.8 (4) |
O4—As1—O3—V2 | 7.1 (3) | O3—V2—N4—C20 | 176.7 (3) |
O5—V2—O3—As1 | 143.5 (2) | N3—V2—N4—C20 | 2.7 (3) |
O6—V2—O3—As1 | 33.9 (3) | O7—V2—N4—C20 | 85.4 (3) |
N3—V2—O3—As1 | −103.7 (4) | V1—V2—N4—C20 | 94.2 (3) |
N4—V2—O3—As1 | −119.2 (2) | C5—N1—C1—C2 | 2.1 (7) |
O7—V2—O3—As1 | −44.4 (2) | V1—N1—C1—C2 | −177.7 (3) |
V1—V2—O3—As1 | −12.8 (2) | N1—C1—C2—C3 | 0.7 (7) |
O1—As1—O4—V1 | 132.8 (2) | C1—C2—C3—C4 | −2.7 (7) |
O2—As1—O4—V1 | −106.6 (2) | C2—C3—C4—C5 | 1.9 (7) |
O3—As1—O4—V1 | 10.9 (3) | C2—C3—C4—C7 | −176.4 (4) |
O8—V1—O4—As1 | 138.6 (2) | C1—N1—C5—C4 | −2.9 (6) |
O7—V1—O4—As1 | 29.8 (3) | V1—N1—C5—C4 | 176.9 (3) |
N1—V1—O4—As1 | −103.6 (4) | C1—N1—C5—C6 | 176.2 (4) |
N2—V1—O4—As1 | −121.6 (2) | V1—N1—C5—C6 | −4.0 (5) |
O6—V1—O4—As1 | −46.7 (2) | C3—C4—C5—N1 | 0.9 (6) |
V2—V1—O4—As1 | −14.8 (2) | C7—C4—C5—N1 | 179.4 (4) |
O5—V2—O6—V1 | −176.9 (1) | C3—C4—C5—C6 | −178.2 (4) |
O3—V2—O6—V1 | −72.5 (1) | C7—C4—C5—C6 | 0.3 (6) |
N3—V2—O6—V1 | 92.6 (1) | C12—N2—C6—C9 | −1.8 (6) |
N4—V2—O6—V1 | 26.2 (3) | V1—N2—C6—C9 | −178.0 (3) |
O7—V2—O6—V1 | 14.9 (1) | C12—N2—C6—C5 | 178.6 (4) |
O8—V1—O6—V2 | −128.4 (8) | V1—N2—C6—C5 | 2.4 (5) |
O7—V1—O6—V2 | −21.0 (2) | N1—C5—C6—N2 | 0.9 (5) |
O4—V1—O6—V2 | 80.9 (2) | C4—C5—C6—N2 | −179.9 (4) |
N1—V1—O6—V2 | −118.0 (2) | N1—C5—C6—C9 | −178.6 (4) |
N2—V1—O6—V2 | 165.2 (2) | C4—C5—C6—C9 | 0.5 (6) |
O8—V1—O7—V2 | −175.5 (1) | C3—C4—C7—C8 | 177.2 (4) |
O4—V1—O7—V2 | −71.8 (1) | C5—C4—C7—C8 | −1.1 (6) |
N1—V1—O7—V2 | 92.2 (1) | C4—C7—C8—C9 | 1.2 (7) |
N2—V1—O7—V2 | 27.5 (3) | N2—C6—C9—C10 | 0.6 (6) |
O6—V1—O7—V2 | 15.0 (1) | C5—C6—C9—C10 | −179.9 (4) |
O5—V2—O7—V1 | −138.3 (6) | N2—C6—C9—C8 | −180.0 (4) |
O6—V2—O7—V1 | −21.5 (2) | C5—C6—C9—C8 | −0.5 (6) |
O3—V2—O7—V1 | 80.0 (2) | C7—C8—C9—C6 | −0.4 (6) |
N3—V2—O7—V1 | −119.4 (2) | C7—C8—C9—C10 | 179.0 (4) |
N4—V2—O7—V1 | 163.8 (2) | C6—C9—C10—C11 | 1.0 (6) |
O8—V1—N1—C1 | −75.6 (4) | C8—C9—C10—C11 | −178.4 (4) |
O7—V1—N1—C1 | 30.6 (4) | C9—C10—C11—C12 | −1.2 (7) |
O4—V1—N1—C1 | 165.0 (4) | C6—N2—C12—C11 | 1.6 (6) |
N2—V1—N1—C1 | −176.3 (4) | V1—N2—C12—C11 | 177.3 (3) |
O6—V1—N1—C1 | 106.3 (4) | C10—C11—C12—N2 | −0.1 (7) |
V2—V1—N1—C1 | 78.1 (4) | C17—N3—C13—C14 | −1.2 (7) |
O8—V1—N1—C5 | 104.5 (3) | V2—N3—C13—C14 | 171.7 (4) |
O7—V1—N1—C5 | −149.2 (3) | N3—C13—C14—C15 | 2.7 (7) |
O4—V1—N1—C5 | −14.8 (5) | C13—C14—C15—C16 | −1.4 (7) |
N2—V1—N1—C5 | 3.9 (3) | C14—C15—C16—C17 | −1.2 (6) |
O6—V1—N1—C5 | −73.6 (3) | C14—C15—C16—C18 | −179.5 (4) |
V2—V1—N1—C5 | −101.7 (3) | C13—N3—C17—C16 | −1.6 (6) |
O8—V1—N2—C12 | 92.7 (4) | V2—N3—C17—C16 | −175.0 (3) |
O7—V1—N2—C12 | −109.7 (4) | C13—N3—C17—C20 | 177.7 (4) |
O4—V1—N2—C12 | −6.1 (4) | V2—N3—C17—C20 | 4.4 (5) |
N1—V1—N2—C12 | −179.1 (4) | C15—C16—C17—N3 | 2.8 (6) |
O6—V1—N2—C12 | −97.2 (4) | C18—C16—C17—N3 | −178.8 (4) |
V2—V1—N2—C12 | −89.0 (4) | C15—C16—C17—C20 | −176.5 (4) |
O8—V1—N2—C6 | −91.5 (3) | C18—C16—C17—C20 | 1.9 (6) |
O7—V1—N2—C6 | 66.0 (4) | C17—C16—C18—C19 | −1.1 (6) |
O4—V1—N2—C6 | 169.7 (3) | C15—C16—C18—C19 | 177.2 (4) |
N1—V1—N2—C6 | −3.3 (3) | C16—C18—C19—C21 | 1.0 (7) |
O6—V1—N2—C6 | 78.6 (3) | C24—N4—C20—C21 | −2.5 (6) |
V2—V1—N2—C6 | 86.7 (3) | V2—N4—C20—C21 | 178.9 (3) |
O5—V2—N3—C13 | −77.9 (4) | C24—N4—C20—C17 | 177.2 (4) |
O6—V2—N3—C13 | 28.9 (4) | V2—N4—C20—C17 | −1.4 (5) |
O3—V2—N3—C13 | 167.3 (4) | N3—C17—C20—N4 | −1.8 (5) |
N4—V2—N3—C13 | −176.7 (4) | C16—C17—C20—N4 | 177.5 (4) |
O7—V2—N3—C13 | 106.1 (4) | N3—C17—C20—C21 | 177.9 (4) |
V1—V2—N3—C13 | 78.5 (4) | C16—C17—C20—C21 | −2.7 (6) |
O5—V2—N3—C17 | 95.0 (3) | N4—C20—C21—C22 | 3.1 (6) |
O6—V2—N3—C17 | −158.2 (3) | C17—C20—C21—C22 | −176.6 (4) |
O3—V2—N3—C17 | −19.8 (6) | N4—C20—C21—C19 | −177.7 (4) |
N4—V2—N3—C17 | −3.8 (3) | C17—C20—C21—C19 | 2.6 (6) |
O7—V2—N3—C17 | −80.9 (3) | C18—C19—C21—C22 | 177.4 (4) |
V1—V2—N3—C17 | −108.6 (3) | C18—C19—C21—C20 | −1.8 (6) |
O5—V2—N4—C24 | 97.6 (4) | C20—C21—C22—C23 | −0.4 (6) |
O6—V2—N4—C24 | −104.6 (4) | C19—C21—C22—C23 | −179.6 (4) |
O3—V2—N4—C24 | −1.8 (3) | C21—C22—C23—C24 | −2.6 (6) |
N3—V2—N4—C24 | −175.8 (4) | C20—N4—C24—C23 | −0.8 (6) |
O7—V2—N4—C24 | −93.1 (4) | V2—N4—C24—C23 | 177.7 (3) |
V1—V2—N4—C24 | −84.3 (3) | C22—C23—C24—N4 | 3.4 (6) |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1o···O1i | 0.85 | 1.84 | 2.593 (6) | 146 |
O2—H2o···O2ii | 0.85 | 1.84 | 2.683 (6) | 173 |
O1w—H1w1···O5 | 0.86 | 2.06 | 2.920 (7) | 173 |
O1w—H1w2···O8iii | 0.87 | 2.04 | 2.901 (6) | 173 |
Symmetry codes: (i) −x+2, −y+1, −z+1; (ii) −x+1, −y+1, −z+1; (iii) −x+3/2, y−1/2, −z+1/2. |
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