Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100004534/qa0262sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270100004534/qa0262Isup2.hkl |
CCDC reference: 145635
To a hot methanol solution (50 ml) of vanadium(IV) oxide sulfate (0.25 g, 1 mmol) were added H2(3-tBu-sal-meso-stien) (0.53 g, 1 mmol) and pyridine (2 ml), and the mixture was stirred for 1 h at 333 K. The resulting green precipitate was collected by filtration and washed with ether (yield 80%). Found: C 72.34, H 6.52, N 4.72%; calculated for C36H38N2O3V: C 72.35, H 6.41, N 4.69%. An analysis of the product by high-performance liquid reverse-phase chromatography suggested that only one of two possible geometrical isomers had been obtained. Crystals of the title compound, exo-[VO(3-tBu-sal-meso-stien)], were grown from an acetonitrile solution.
All H-atom positional parameters were calculated geometrically, and fixed with Uiso(H) = 1.2Ueq(parent atom).
Data collection: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1993); cell refinement: MSC/AFC Diffractometer Control Software; data reduction: TEXSAN (Molecular Structure Corporation, 1999); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); software used to prepare material for publication: TEXSAN.
[VO(C36H38N2O2)] | Dx = 1.268 Mg m−3 |
Mr = 597.65 | Mo Kα radiation, λ = 0.71073 Å |
Monoclinic, C2/c | Cell parameters from 25 reflections |
a = 32.529 (4) Å | θ = 14.8–15.0° |
b = 11.877 (5) Å | µ = 0.35 mm−1 |
c = 18.909 (7) Å | T = 297 K |
β = 121.01 (1)° | Prismatic, green |
V = 6261 (3) Å3 | 0.5 × 0.3 × 0.1 mm |
Z = 8 |
Rigaku AFC-7R diffractometer | Rint = 0.045 |
θ–2θ scans | θmax = 27.5° |
Absorption correction: integration (Coppens et al., 1965) | h = −42→42 |
Tmin = 0.866, Tmax = 0.979 | k = 0→15 |
7427 measured reflections | l = −25→0 |
7203 independent reflections | 3 standard reflections every 150 reflections |
3823 reflections with I > 2σ(I) | intensity decay: none |
Refinement on F2 | H-atom parameters not refined |
R[F2 > 2σ(F2)] = 0.061 | w = 1/[σ2(Fo2) + (0.1616P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.219 | (Δ/σ)max = 0.0001 |
S = 1.18 | Δρmax = 0.81 e Å−3 |
7203 reflections | Δρmin = −0.73 e Å−3 |
379 parameters |
[VO(C36H38N2O2)] | V = 6261 (3) Å3 |
Mr = 597.65 | Z = 8 |
Monoclinic, C2/c | Mo Kα radiation |
a = 32.529 (4) Å | µ = 0.35 mm−1 |
b = 11.877 (5) Å | T = 297 K |
c = 18.909 (7) Å | 0.5 × 0.3 × 0.1 mm |
β = 121.01 (1)° |
Rigaku AFC-7R diffractometer | 3823 reflections with I > 2σ(I) |
Absorption correction: integration (Coppens et al., 1965) | Rint = 0.045 |
Tmin = 0.866, Tmax = 0.979 | 3 standard reflections every 150 reflections |
7427 measured reflections | intensity decay: none |
7203 independent reflections |
R[F2 > 2σ(F2)] = 0.061 | 379 parameters |
wR(F2) = 0.219 | H-atom parameters not refined |
S = 1.18 | Δρmax = 0.81 e Å−3 |
7203 reflections | Δρmin = −0.73 e Å−3 |
Refinement. Refinement using reflections with F2 > 0.0 σ(F2). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F2 > 2.0 σ(F2) is used only for calculating R-factor (gt). |
x | y | z | Uiso*/Ueq | ||
V1 | −0.21722 (2) | −0.13575 (6) | −0.69752 (4) | 0.0278 (2) | |
O2 | −0.2192 (1) | −0.0058 (3) | −0.7218 (2) | 0.0431 (8) | |
O3 | −0.1792 (1) | −0.1420 (3) | −0.5794 (2) | 0.0360 (7) | |
O4 | −0.1653 (1) | −0.2075 (3) | −0.7006 (2) | 0.0374 (7) | |
N5 | −0.2750 (1) | −0.1740 (3) | −0.6837 (2) | 0.0324 (8) | |
N6 | −0.2623 (1) | −0.2212 (3) | −0.8053 (2) | 0.0307 (8) | |
C7 | −0.1902 (2) | −0.1033 (4) | −0.5255 (3) | 0.0328 (9) | |
C8 | −0.1539 (2) | −0.0567 (4) | −0.4502 (3) | 0.0336 (10) | |
C9 | −0.1023 (2) | −0.0449 (4) | −0.4313 (3) | 0.038 (1) | |
C10 | −0.1023 (2) | 0.0336 (5) | −0.4959 (4) | 0.060 (2) | |
C11 | −0.0683 (2) | 0.0068 (5) | −0.3465 (3) | 0.058 (1) | |
C12 | −0.0829 (2) | −0.1609 (5) | −0.4333 (4) | 0.062 (2) | |
C13 | −0.1673 (2) | −0.0197 (4) | −0.3946 (3) | 0.043 (1) | |
C14 | −0.2140 (2) | −0.0315 (5) | −0.4097 (3) | 0.050 (1) | |
C15 | −0.2487 (2) | −0.0779 (5) | −0.4819 (3) | 0.045 (1) | |
C16 | −0.2381 (2) | −0.1124 (4) | −0.5421 (3) | 0.036 (1) | |
C17 | −0.2755 (2) | −0.1593 (4) | −0.6165 (3) | 0.039 (1) | |
C18 | −0.3156 (2) | −0.2385 (3) | −0.7512 (3) | 0.0326 (9) | |
C19 | −0.3649 (1) | −0.2139 (4) | −0.7657 (3) | 0.0354 (10) | |
C20 | −0.3795 (2) | −0.1071 (4) | −0.7592 (3) | 0.046 (1) | |
C21 | −0.4268 (2) | −0.0896 (5) | −0.7788 (4) | 0.063 (2) | |
C22 | −0.4594 (2) | −0.1775 (6) | −0.8074 (4) | 0.074 (2) | |
C23 | −0.4452 (2) | −0.2824 (6) | −0.8158 (4) | 0.072 (2) | |
C24 | −0.3979 (2) | −0.3008 (4) | −0.7933 (4) | 0.055 (1) | |
C25 | −0.3137 (2) | −0.2259 (3) | −0.8319 (3) | 0.0339 (9) | |
C26 | −0.3430 (1) | −0.1313 (4) | −0.8904 (3) | 0.0298 (9) | |
C27 | −0.3249 (2) | −0.0250 (4) | −0.8886 (3) | 0.041 (1) | |
C28 | −0.3528 (2) | 0.0566 (4) | −0.9459 (3) | 0.045 (1) | |
C29 | −0.3987 (2) | 0.0329 (5) | −1.0044 (3) | 0.049 (1) | |
C30 | −0.4184 (2) | −0.0708 (5) | −1.0072 (3) | 0.054 (1) | |
C31 | −0.3904 (2) | −0.1525 (4) | −0.9506 (3) | 0.043 (1) | |
C32 | −0.2494 (2) | −0.2722 (4) | −0.8513 (3) | 0.036 (1) | |
C33 | −0.2018 (2) | −0.2803 (4) | −0.8372 (3) | 0.0370 (10) | |
C34 | −0.1967 (2) | −0.3265 (5) | −0.9012 (3) | 0.050 (1) | |
C35 | −0.1533 (2) | −0.3366 (5) | −0.8929 (3) | 0.053 (1) | |
C36 | −0.1124 (2) | −0.3030 (4) | −0.8179 (3) | 0.044 (1) | |
C37 | −0.1145 (2) | −0.2602 (4) | −0.7517 (3) | 0.0324 (9) | |
C38 | −0.0690 (2) | −0.2289 (4) | −0.6702 (3) | 0.0353 (10) | |
C39 | −0.0700 (2) | −0.1052 (4) | −0.6490 (3) | 0.046 (1) | |
C40 | −0.0233 (2) | −0.2471 (5) | −0.6740 (3) | 0.048 (1) | |
C41 | −0.0646 (2) | −0.3041 (5) | −0.6004 (3) | 0.050 (1) | |
C42 | −0.1613 (2) | −0.2476 (4) | −0.7622 (3) | 0.0334 (10) | |
H10A | −0.1147 | 0.1074 | −0.4945 | 0.0693* | |
H10B | −0.0712 | 0.0444 | −0.4882 | 0.0693* | |
H10C | −0.1230 | 0.0051 | −0.5513 | 0.0693* | |
H11A | −0.0797 | 0.0815 | −0.3435 | 0.0657* | |
H11B | −0.0680 | −0.0378 | −0.3044 | 0.0657* | |
H11C | −0.0366 | 0.0147 | −0.3357 | 0.0657* | |
H12A | −0.1015 | −0.1958 | −0.4860 | 0.0672* | |
H12B | −0.0500 | −0.1556 | −0.4224 | 0.0672* | |
H12C | −0.0820 | −0.2085 | −0.3923 | 0.0672* | |
H13 | −0.1443 | 0.0142 | −0.3447 | 0.0596* | |
H14 | −0.2229 | −0.0077 | −0.3716 | 0.0618* | |
H15 | −0.2808 | −0.0848 | −0.4931 | 0.0540* | |
H17 | −0.3028 | −0.1840 | −0.6164 | 0.0479* | |
H18 | −0.3092 | −0.3149 | −0.7360 | 0.0423* | |
H20 | −0.3565 | −0.0454 | −0.7392 | 0.0585* | |
H21 | −0.4370 | −0.0190 | −0.7753 | 0.0830* | |
H22 | −0.4914 | −0.1662 | −0.8201 | 0.0914* | |
H23 | −0.4669 | −0.3436 | −0.8369 | 0.0840* | |
H24 | −0.3876 | −0.3745 | −0.7977 | 0.0675* | |
H25 | −0.3264 | −0.2929 | −0.8620 | 0.0427* | |
H27 | −0.2923 | −0.0086 | −0.8492 | 0.0542* | |
H28 | −0.3404 | 0.1294 | −0.9424 | 0.0535* | |
H29 | −0.4173 | 0.0878 | −1.0452 | 0.0569* | |
H30 | −0.4504 | −0.0852 | −1.0485 | 0.0641* | |
H31 | −0.4033 | −0.2247 | −0.9538 | 0.0508* | |
H32 | −0.2740 | −0.3097 | −0.8986 | 0.0464* | |
H34 | −0.2260 | −0.3509 | −0.9523 | 0.0579* | |
H35 | −0.1509 | −0.3696 | −0.9366 | 0.0672* | |
H36 | −0.0835 | −0.3134 | −0.8161 | 0.0570* | |
H39A | −0.0980 | −0.0886 | −0.6437 | 0.0568* | |
H39B | −0.0725 | −0.0552 | −0.6908 | 0.0568* | |
H39C | −0.0425 | −0.0820 | −0.5972 | 0.0568* | |
H40A | 0.0060 | −0.2285 | −0.6215 | 0.0631* | |
H40B | −0.0195 | −0.3254 | −0.6843 | 0.0631* | |
H40C | −0.0229 | −0.2028 | −0.7153 | 0.0631* | |
H41A | −0.0613 | −0.3821 | −0.6097 | 0.0599* | |
H41B | −0.0916 | −0.2965 | −0.5937 | 0.0599* | |
H41C | −0.0362 | −0.2848 | −0.5471 | 0.0599* |
U11 | U22 | U33 | U12 | U13 | U23 | |
V1 | 0.0286 (4) | 0.0281 (4) | 0.0294 (4) | −0.0022 (3) | 0.0168 (3) | −0.0044 (3) |
O2 | 0.056 (2) | 0.029 (2) | 0.044 (2) | −0.005 (1) | 0.026 (2) | 0.001 (1) |
O3 | 0.030 (1) | 0.047 (2) | 0.033 (2) | 0.002 (1) | 0.018 (1) | −0.007 (1) |
O4 | 0.034 (2) | 0.048 (2) | 0.036 (2) | 0.003 (1) | 0.023 (1) | −0.007 (1) |
N5 | 0.032 (2) | 0.030 (2) | 0.036 (2) | −0.001 (1) | 0.018 (2) | −0.001 (2) |
N6 | 0.032 (2) | 0.028 (2) | 0.031 (2) | 0.002 (1) | 0.015 (2) | −0.003 (2) |
C7 | 0.040 (2) | 0.029 (2) | 0.034 (2) | 0.005 (2) | 0.023 (2) | 0.000 (2) |
C8 | 0.043 (2) | 0.028 (2) | 0.031 (2) | 0.003 (2) | 0.020 (2) | −0.001 (2) |
C9 | 0.031 (2) | 0.043 (3) | 0.035 (2) | −0.001 (2) | 0.012 (2) | −0.008 (2) |
C10 | 0.058 (3) | 0.072 (4) | 0.054 (3) | −0.019 (3) | 0.031 (3) | −0.003 (3) |
C11 | 0.051 (3) | 0.066 (4) | 0.042 (3) | −0.009 (3) | 0.013 (3) | −0.019 (3) |
C12 | 0.037 (3) | 0.062 (4) | 0.065 (4) | 0.011 (2) | 0.010 (3) | −0.015 (3) |
C13 | 0.048 (3) | 0.046 (3) | 0.031 (2) | 0.000 (2) | 0.017 (2) | −0.007 (2) |
C14 | 0.062 (3) | 0.058 (3) | 0.041 (3) | 0.009 (3) | 0.034 (3) | −0.003 (2) |
C15 | 0.041 (3) | 0.062 (3) | 0.044 (3) | 0.011 (2) | 0.029 (2) | 0.007 (2) |
C16 | 0.042 (2) | 0.037 (3) | 0.036 (2) | 0.004 (2) | 0.025 (2) | 0.000 (2) |
C17 | 0.040 (2) | 0.040 (3) | 0.049 (3) | 0.000 (2) | 0.032 (2) | 0.004 (2) |
C18 | 0.032 (2) | 0.026 (2) | 0.039 (2) | −0.005 (2) | 0.018 (2) | −0.001 (2) |
C19 | 0.025 (2) | 0.041 (3) | 0.038 (2) | −0.006 (2) | 0.015 (2) | 0.004 (2) |
C20 | 0.038 (3) | 0.041 (3) | 0.063 (3) | −0.002 (2) | 0.028 (2) | −0.003 (2) |
C21 | 0.051 (3) | 0.062 (4) | 0.083 (4) | 0.013 (3) | 0.040 (3) | 0.005 (3) |
C22 | 0.020 (2) | 0.096 (5) | 0.101 (5) | 0.000 (3) | 0.028 (3) | 0.014 (4) |
C23 | 0.034 (3) | 0.066 (4) | 0.103 (5) | −0.008 (3) | 0.025 (3) | 0.019 (4) |
C24 | 0.034 (3) | 0.042 (3) | 0.079 (4) | −0.009 (2) | 0.023 (3) | 0.005 (3) |
C25 | 0.032 (2) | 0.026 (2) | 0.040 (2) | −0.005 (2) | 0.016 (2) | −0.008 (2) |
C26 | 0.026 (2) | 0.033 (2) | 0.032 (2) | 0.004 (2) | 0.016 (2) | −0.002 (2) |
C27 | 0.030 (2) | 0.041 (3) | 0.052 (3) | 0.000 (2) | 0.021 (2) | 0.000 (2) |
C28 | 0.042 (3) | 0.031 (2) | 0.062 (3) | 0.005 (2) | 0.026 (3) | 0.005 (2) |
C29 | 0.055 (3) | 0.048 (3) | 0.042 (3) | 0.017 (2) | 0.024 (3) | 0.005 (2) |
C30 | 0.047 (3) | 0.056 (3) | 0.038 (3) | 0.004 (2) | 0.007 (2) | −0.009 (2) |
C31 | 0.035 (2) | 0.038 (3) | 0.044 (3) | 0.001 (2) | 0.012 (2) | −0.004 (2) |
C32 | 0.035 (2) | 0.034 (2) | 0.037 (2) | 0.001 (2) | 0.017 (2) | −0.009 (2) |
C33 | 0.043 (3) | 0.034 (2) | 0.038 (2) | 0.003 (2) | 0.024 (2) | −0.005 (2) |
C34 | 0.054 (3) | 0.055 (3) | 0.041 (3) | 0.005 (2) | 0.024 (2) | −0.013 (2) |
C35 | 0.061 (3) | 0.060 (4) | 0.050 (3) | 0.006 (3) | 0.038 (3) | −0.011 (3) |
C36 | 0.050 (3) | 0.043 (3) | 0.056 (3) | 0.012 (2) | 0.038 (3) | 0.005 (2) |
C37 | 0.039 (2) | 0.029 (2) | 0.039 (2) | 0.005 (2) | 0.027 (2) | 0.005 (2) |
C38 | 0.030 (2) | 0.039 (2) | 0.041 (2) | 0.006 (2) | 0.021 (2) | 0.008 (2) |
C39 | 0.045 (3) | 0.044 (3) | 0.050 (3) | −0.003 (2) | 0.025 (2) | −0.004 (2) |
C40 | 0.033 (2) | 0.062 (3) | 0.060 (3) | 0.009 (2) | 0.032 (2) | 0.016 (3) |
C41 | 0.046 (3) | 0.063 (3) | 0.043 (3) | 0.003 (2) | 0.024 (2) | 0.019 (3) |
C42 | 0.042 (2) | 0.029 (2) | 0.040 (2) | 0.007 (2) | 0.029 (2) | 0.001 (2) |
V1—O2 | 1.601 (3) | C21—H21 | 0.918 |
V1—O3 | 1.917 (3) | C22—C23 | 1.37 (1) |
V1—O4 | 1.918 (4) | C22—H22 | 0.949 |
V1—N5 | 2.077 (5) | C23—C24 | 1.387 (9) |
V1—N6 | 2.063 (3) | C23—H23 | 0.946 |
O3—C7 | 1.325 (7) | C24—H24 | 0.956 |
O4—C42 | 1.326 (7) | C25—C26 | 1.519 (6) |
N5—C17 | 1.291 (8) | C25—H25 | 0.942 |
N5—C18 | 1.491 (5) | C26—C27 | 1.386 (7) |
N6—C25 | 1.480 (6) | C26—C31 | 1.388 (5) |
N6—C32 | 1.294 (7) | C27—C28 | 1.388 (6) |
C7—C8 | 1.412 (5) | C27—H27 | 0.949 |
C7—C16 | 1.428 (8) | C28—C29 | 1.351 (6) |
C8—C9 | 1.533 (8) | C28—H28 | 0.943 |
C8—C13 | 1.400 (9) | C29—C30 | 1.376 (8) |
C9—C10 | 1.536 (9) | C29—H29 | 0.952 |
C9—C11 | 1.531 (7) | C30—C31 | 1.383 (7) |
C9—C12 | 1.525 (8) | C30—H30 | 0.942 |
C10—H10A | 0.972 | C31—H31 | 0.944 |
C10—H10B | 0.953 | C32—C33 | 1.433 (8) |
C10—H10C | 0.969 | C32—H32 | 0.948 |
C11—H11A | 0.975 | C33—C34 | 1.415 (9) |
C11—H11B | 0.953 | C33—C42 | 1.405 (5) |
C11—H11C | 0.946 | C34—C35 | 1.342 (10) |
C12—H12A | 0.954 | C34—H34 | 0.989 |
C12—H12B | 0.980 | C35—C36 | 1.413 (6) |
C12—H12C | 0.948 | C35—H35 | 0.953 |
C13—C14 | 1.401 (9) | C36—C37 | 1.384 (9) |
C13—H13 | 0.940 | C36—H36 | 0.932 |
C14—C15 | 1.361 (6) | C37—C38 | 1.533 (5) |
C14—H14 | 0.947 | C37—C42 | 1.438 (8) |
C15—C16 | 1.411 (9) | C38—C39 | 1.529 (7) |
C15—H15 | 0.953 | C38—C40 | 1.542 (8) |
C16—C17 | 1.416 (6) | C38—C41 | 1.538 (8) |
C17—H17 | 0.937 | C39—H39A | 0.987 |
C18—C19 | 1.510 (7) | C39—H39B | 0.958 |
C18—C25 | 1.564 (8) | C39—H39C | 0.967 |
C18—H18 | 0.942 | C40—H40A | 0.983 |
C19—C20 | 1.383 (7) | C40—H40B | 0.971 |
C19—C24 | 1.384 (7) | C40—H40C | 0.946 |
C20—C21 | 1.398 (9) | C41—H41A | 0.959 |
C20—H20 | 0.975 | C41—H41B | 0.956 |
C21—C22 | 1.385 (9) | C41—H41C | 0.980 |
O2—V1—O3 | 106.1 (1) | C21—C22—C23 | 119.7 (6) |
O2—V1—O4 | 109.0 (2) | C21—C22—H22 | 120.8 |
O2—V1—N5 | 109.9 (2) | C23—C22—H22 | 119.4 |
O2—V1—N6 | 106.7 (1) | C22—C23—C24 | 119.7 (5) |
O3—V1—O4 | 88.2 (1) | C22—C23—H23 | 121.8 |
O3—V1—N5 | 85.9 (1) | C24—C23—H23 | 118.5 |
O3—V1—N6 | 146.6 (1) | C19—C24—C23 | 121.4 (5) |
O4—V1—N5 | 140.7 (1) | C19—C24—H24 | 118.4 |
O4—V1—N6 | 86.6 (1) | C23—C24—H24 | 120.1 |
N5—V1—N6 | 77.8 (2) | N6—C25—C18 | 106.1 (3) |
V1—O3—C7 | 127.9 (2) | N6—C25—C26 | 113.2 (4) |
V1—O4—C42 | 132.3 (2) | N6—C25—H25 | 107.7 |
V1—N5—C17 | 124.4 (3) | C18—C25—C26 | 117.2 (4) |
V1—N5—C18 | 117.6 (4) | C18—C25—H25 | 106.5 |
C17—N5—C18 | 117.3 (4) | C26—C25—H25 | 105.6 |
V1—N6—C25 | 117.3 (3) | C25—C26—C27 | 123.9 (3) |
V1—N6—C32 | 125.6 (3) | C25—C26—C31 | 118.5 (4) |
C25—N6—C32 | 117.1 (3) | C27—C26—C31 | 117.6 (4) |
O3—C7—C8 | 119.8 (5) | C26—C27—C28 | 121.2 (4) |
O3—C7—C16 | 120.1 (3) | C26—C27—H27 | 119.6 |
C8—C7—C16 | 120.1 (5) | C28—C27—H27 | 119.1 |
C7—C8—C9 | 121.1 (5) | C27—C28—C29 | 119.7 (5) |
C7—C8—C13 | 117.3 (5) | C27—C28—H28 | 120.0 |
C9—C8—C13 | 121.6 (4) | C29—C28—H28 | 120.1 |
C8—C9—C10 | 108.6 (4) | C28—C29—C30 | 120.9 (4) |
C8—C9—C11 | 113.2 (5) | C28—C29—H29 | 119.6 |
C8—C9—C12 | 109.2 (4) | C30—C29—H29 | 119.5 |
C10—C9—C11 | 107.1 (4) | C29—C30—C31 | 119.3 (4) |
C10—C9—C12 | 111.0 (6) | C29—C30—H30 | 119.4 |
C11—C9—C12 | 107.6 (4) | C31—C30—H30 | 121.3 |
C9—C10—H10A | 110.8 | C26—C31—C30 | 121.2 (5) |
C9—C10—H10B | 113.3 | C26—C31—H31 | 119.2 |
C9—C10—H10C | 111.3 | C30—C31—H31 | 119.6 |
H10A—C10—H10B | 107.4 | N6—C32—C33 | 126.8 (4) |
H10A—C10—H10C | 106.1 | N6—C32—H32 | 116.5 |
H10B—C10—H10C | 107.7 | C33—C32—H32 | 116.6 |
C9—C11—H11A | 109.6 | C32—C33—C34 | 117.3 (4) |
C9—C11—H11B | 110.1 | C32—C33—C42 | 122.1 (5) |
C9—C11—H11C | 112.6 | C34—C33—C42 | 120.6 (5) |
H11A—C11—H11B | 107.2 | C33—C34—C35 | 121.0 (4) |
H11A—C11—H11C | 107.7 | C33—C34—H34 | 117.9 |
H11B—C11—H11C | 109.5 | C35—C34—H34 | 121.0 |
C9—C12—H12A | 111.7 | C34—C35—C36 | 118.7 (6) |
C9—C12—H12B | 110.9 | C34—C35—H35 | 119.1 |
C9—C12—H12C | 110.9 | C36—C35—H35 | 122.1 |
H12A—C12—H12B | 106.6 | C35—C36—C37 | 123.6 (6) |
H12A—C12—H12C | 109.3 | C35—C36—H36 | 114.1 |
H12B—C12—H12C | 107.2 | C37—C36—H36 | 122.3 |
C8—C13—C14 | 122.6 (4) | C36—C37—C38 | 121.8 (5) |
C8—C13—H13 | 119.4 | C36—C37—C42 | 117.1 (4) |
C14—C13—H13 | 117.9 | C38—C37—C42 | 121.2 (5) |
C13—C14—C15 | 119.9 (6) | C37—C38—C39 | 110.9 (3) |
C13—C14—H14 | 122.6 | C37—C38—C40 | 112.0 (5) |
C15—C14—H14 | 117.6 | C37—C38—C41 | 109.7 (4) |
C14—C15—C16 | 120.3 (6) | C39—C38—C40 | 107.3 (4) |
C14—C15—H15 | 120.4 | C39—C38—C41 | 109.8 (5) |
C16—C15—H15 | 119.2 | C40—C38—C41 | 107.0 (4) |
C7—C16—C15 | 119.6 (4) | C38—C39—H39A | 111.4 |
C7—C16—C17 | 122.0 (5) | C38—C39—H39B | 112.6 |
C15—C16—C17 | 118.3 (5) | C38—C39—H39C | 114.0 |
N5—C17—C16 | 126.3 (5) | H39A—C39—H39B | 105.8 |
N5—C17—H17 | 116.9 | H39A—C39—H39C | 105.2 |
C16—C17—H17 | 116.8 | H39B—C39—H39C | 107.4 |
N5—C18—C19 | 116.4 (4) | C38—C40—H40A | 112.1 |
N5—C18—C25 | 108.9 (4) | C38—C40—H40B | 111.6 |
N5—C18—H18 | 106.0 | C38—C40—H40C | 112.5 |
C19—C18—C25 | 112.0 (3) | H40A—C40—H40B | 105.1 |
C19—C18—H18 | 106.7 | H40A—C40—H40C | 107.1 |
C25—C18—H18 | 106.1 | H40B—C40—H40C | 108.0 |
C18—C19—C20 | 123.0 (4) | C38—C41—H41A | 111.8 |
C18—C19—C24 | 118.0 (4) | C38—C41—H41B | 111.9 |
C20—C19—C24 | 118.8 (5) | C38—C41—H41C | 111.7 |
C19—C20—C21 | 119.6 (5) | H41A—C41—H41B | 108.2 |
C19—C20—H20 | 119.5 | H41A—C41—H41C | 106.3 |
C21—C20—H20 | 120.8 | H41B—C41—H41C | 106.5 |
C20—C21—C22 | 120.6 (6) | O4—C42—C33 | 121.4 (5) |
C20—C21—H21 | 120.5 | O4—C42—C37 | 119.6 (3) |
C22—C21—H21 | 118.8 | C33—C42—C37 | 119.1 (5) |
Experimental details
Crystal data | |
Chemical formula | [VO(C36H38N2O2)] |
Mr | 597.65 |
Crystal system, space group | Monoclinic, C2/c |
Temperature (K) | 297 |
a, b, c (Å) | 32.529 (4), 11.877 (5), 18.909 (7) |
β (°) | 121.01 (1) |
V (Å3) | 6261 (3) |
Z | 8 |
Radiation type | Mo Kα |
µ (mm−1) | 0.35 |
Crystal size (mm) | 0.5 × 0.3 × 0.1 |
Data collection | |
Diffractometer | Rigaku AFC-7R diffractometer |
Absorption correction | Integration (Coppens et al., 1965) |
Tmin, Tmax | 0.866, 0.979 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 7427, 7203, 3823 |
Rint | 0.045 |
(sin θ/λ)max (Å−1) | 0.650 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.061, 0.219, 1.18 |
No. of reflections | 7203 |
No. of parameters | 379 |
No. of restraints | ? |
H-atom treatment | H-atom parameters not refined |
Δρmax, Δρmin (e Å−3) | 0.81, −0.73 |
Computer programs: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1993), MSC/AFC Diffractometer Control Software, TEXSAN (Molecular Structure Corporation, 1999), SIR92 (Altomare et al., 1994), SHELXL97 (Sheldrick, 1997), TEXSAN.
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The crystal structure and the thermal isomerization of [VO(3-EtO-sal-meso-stien)] have been investigated by the authors (Hoshina et al., 1999), together with the thermal dehydrogenation in the solid state (Hoshina et al., 1998, 2000).
In the crystals of [VO(3-tBu,5-Me-salen)], (I), the complex has an asymmetric distortion with a tBu—C···C—tBu torsion angle of 25.1° (Cornman et al., 1997). Distortion of the title compound in the crystal is moderate and the C9—C8···C37—C38 torsion angle is 10.1 (3)°°.