The coordination geometry around the V atom in the title complex, [VO(C11H19O2)2], is square pyramidal with the basal plane defined by four O atoms from two chelating β-diketonate ligands and the axial position occupied by an oxo group.
Supporting information
CCDC reference: 170278
Key indicators
- Single-crystal X-ray study
- T = 149 K
- Mean (C-C) = 0.010 Å
- Disorder in main residue
- R factor = 0.074
- wR factor = 0.187
- Data-to-parameter ratio = 16.0
checkCIF results
No syntax errors found
ADDSYM reports no extra symmetry
Alert Level B:
PLAT_213 Alert B Atom C18 has ADP max/min Ratio ........... 4.40
Alert Level C:
PLAT_213 Alert C Atom C22 has ADP max/min Ratio ........... 3.10
PLAT_301 Alert C Main Residue Disorder ........................ 10.00 Perc.
General Notes
REFLT_03
From the CIF: _diffrn_reflns_theta_max 26.50
From the CIF: _reflns_number_total 4217
Count of symmetry unique reflns 2689
Completeness (_total/calc) 156.82%
TEST3: Check Friedels for noncentro structure
Estimate of Friedel pairs measured 1528
Fraction of Friedel pairs measured 0.568
Are heavy atom types Z>Si present yes
Please check that the estimate of the number of Friedel pairs is
correct. If it is not, please give the correct count in the
_publ_section_exptl_refinement section of the submitted CIF.
0 Alert Level A = Potentially serious problem
1 Alert Level B = Potential problem
2 Alert Level C = Please check
Data collection: XSCANS (Fait, 1991); cell refinement: XSCANS; data reduction: XSCANS; program(s) used to solve structure: SHELXS86 (Sheldrick, 1985); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Johnson, 1976; Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).
oxobis(2,2,6,6-tetramethyl-3,5-heptadionato)vanadium(IV)
top
Crystal data top
[VO(C11H19O2)2] | F(000) = 466 |
Mr = 433.46 | Dx = 1.171 Mg m−3 |
Monoclinic, P21 | Mo Kα radiation, λ = 0.71073 Å |
a = 9.4515 (2) Å | Cell parameters from 25 reflections |
b = 10.7953 (3) Å | θ = 8–15° |
c = 12.7494 (4) Å | µ = 0.43 mm−1 |
β = 109.025 (1)° | T = 149 K |
V = 1229.79 (6) Å3 | Prism, green |
Z = 2 | 0.50 × 0.40 × 0.40 mm |
Data collection top
Siemens P4 diffractometer | Rint = 0.093 |
Radiation source: fine-focus sealed tube | θmax = 26.5°, θmin = 1.7° |
Graphite monochromator | h = −11→11 |
ω scans | k = −9→13 |
7897 measured reflections | l = −15→14 |
4217 independent reflections | 3 standard reflections every 120 min |
2751 reflections with I > 2σ(I) | intensity decay: no decay |
Refinement top
Refinement on F2 | H atoms treated by a mixture of independent and constrained refinement |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0898P)2] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.074 | (Δ/σ)max < 0.001 |
wR(F2) = 0.187 | Δρmax = 0.95 e Å−3 |
S = 0.92 | Δρmin = −1.01 e Å−3 |
4217 reflections | Absolute structure: Flack (1983) |
263 parameters | Absolute structure parameter: 0.03 (5) |
1 restraint | |
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
V1 | 0.71881 (10) | 0.26486 (9) | 0.31402 (8) | 0.0238 (3) | |
O2 | 0.6290 (4) | 0.1734 (4) | 0.4098 (3) | 0.0278 (10) | |
O4 | 0.8731 (4) | 0.2700 (5) | 0.2425 (3) | 0.0295 (9) | |
O1 | 0.8863 (5) | 0.3000 (4) | 0.4482 (3) | 0.0306 (12) | |
O3 | 0.6198 (4) | 0.1396 (4) | 0.2014 (3) | 0.0272 (11) | |
C1 | 0.8940 (6) | 0.2958 (5) | 0.5501 (5) | 0.0230 (15) | |
C15 | 0.5284 (7) | 0.0200 (6) | 0.0366 (5) | 0.0246 (15) | |
C19 | 0.9992 (6) | 0.2808 (8) | 0.1103 (5) | 0.0328 (16) | |
C18 | 0.6081 (8) | −0.0684 (6) | −0.0209 (6) | 0.0353 (17) | |
H18A | 0.6418 | −0.0227 | −0.0729 | 0.053* | |
H18B | 0.5396 | −0.1318 | −0.0595 | 0.053* | |
H18C | 0.6924 | −0.1058 | 0.0338 | 0.053* | |
C12 | 0.8661 (6) | 0.2364 (5) | 0.1459 (5) | 0.0196 (14) | |
C3 | 0.6589 (7) | 0.1788 (6) | 0.5143 (5) | 0.0235 (14) | |
C13 | 0.7560 (6) | 0.1642 (6) | 0.0780 (5) | 0.0236 (14) | |
H13 | 0.7579 | 0.1482 | 0.0068 | 0.028* | |
C8 | 1.0346 (7) | 0.3479 (7) | 0.6322 (6) | 0.0334 (17) | |
C4 | 0.5548 (7) | 0.1020 (6) | 0.5605 (5) | 0.0265 (15) | |
C2 | 0.7811 (6) | 0.2412 (6) | 0.5838 (5) | 0.0296 (17) | |
H2 | 0.7893 | 0.2474 | 0.6583 | 0.035* | |
C14 | 0.6381 (6) | 0.1118 (6) | 0.1100 (5) | 0.0206 (13) | |
C17 | 0.4572 (9) | −0.0566 (7) | 0.1066 (6) | 0.044 (2) | |
H17A | 0.5325 | −0.1066 | 0.1579 | 0.066* | |
H17B | 0.3812 | −0.1092 | 0.0591 | 0.066* | |
H17C | 0.4131 | −0.0023 | 0.147 | 0.066* | |
C7 | 0.3971 (8) | 0.1048 (8) | 0.4806 (7) | 0.051 (2) | |
H7A | 0.3349 | 0.0517 | 0.5074 | 0.077* | |
H7B | 0.3966 | 0.0765 | 0.4091 | 0.077* | |
H7C | 0.3594 | 0.188 | 0.4744 | 0.077* | |
O5 | 0.6249 (5) | 0.3889 (4) | 0.2791 (4) | 0.0401 (13) | |
C6 | 0.6123 (9) | −0.0323 (7) | 0.5697 (8) | 0.056 (3) | |
H6A | 0.554 | −0.0832 | 0.6019 | 0.084* | |
H6B | 0.7154 | −0.0345 | 0.6158 | 0.084* | |
H6C | 0.6035 | −0.0629 | 0.4972 | 0.084* | |
C16 | 0.4075 (8) | 0.0918 (7) | −0.0501 (6) | 0.045 (2) | |
H16A | 0.3578 | 0.1464 | −0.0139 | 0.068* | |
H16B | 0.3361 | 0.0349 | −0.0965 | 0.068* | |
H16C | 0.452 | 0.1394 | −0.0947 | 0.068* | |
C5 | 0.5558 (9) | 0.1487 (8) | 0.6727 (6) | 0.051 (2) | |
H5A | 0.5334 | 0.2357 | 0.668 | 0.077* | |
H5B | 0.6528 | 0.1351 | 0.7264 | 0.077* | |
H5C | 0.4817 | 0.1049 | 0.6949 | 0.077* | |
C21 | 1.1383 (8) | 0.2221 (8) | 0.1837 (8) | 0.061 (3) | |
H21A | 1.1345 | 0.1345 | 0.1701 | 0.092* | |
H21B | 1.1473 | 0.2371 | 0.2598 | 0.092* | |
H21C | 1.2232 | 0.2567 | 0.1686 | 0.092* | |
C20 | 1.0133 (9) | 0.4237 (7) | 0.1325 (8) | 0.058 (2) | |
H20A | 1.0186 | 0.4398 | 0.2077 | 0.087* | |
H20B | 0.9276 | 0.4649 | 0.0828 | 0.087* | |
H20C | 1.1024 | 0.4539 | 0.1207 | 0.087* | |
C22 | 0.9772 (9) | 0.2583 (12) | −0.0111 (6) | 0.072 (3) | |
H22A | 1.0551 | 0.2993 | −0.0309 | 0.109* | |
H22B | 0.8817 | 0.2904 | −0.0555 | 0.109* | |
H22C | 0.9809 | 0.171 | −0.0241 | 0.109* | |
C9A | 1.1227 (15) | 0.2348 (14) | 0.7071 (12) | 0.060 (3)* | 0.580 (7) |
H9A1 | 1.2182 | 0.2632 | 0.7549 | 0.089* | 0.580 (7) |
H9A2 | 1.1372 | 0.1701 | 0.66 | 0.089* | 0.580 (7) |
H9A3 | 1.0654 | 0.2035 | 0.7511 | 0.089* | 0.580 (7) |
C10A | 0.9955 (15) | 0.4329 (15) | 0.7119 (12) | 0.048 (3)* | 0.580 (7) |
H10A | 0.9496 | 0.386 | 0.7561 | 0.072* | 0.580 (7) |
H10B | 0.927 | 0.4952 | 0.6711 | 0.072* | 0.580 (7) |
H10C | 1.0847 | 0.4718 | 0.7593 | 0.072* | 0.580 (7) |
C11A | 1.1368 (16) | 0.4022 (15) | 0.5784 (13) | 0.056 (3)* | 0.580 (7) |
H11A | 1.0932 | 0.4765 | 0.5398 | 0.084* | 0.580 (7) |
H11B | 1.1528 | 0.3439 | 0.5265 | 0.084* | 0.580 (7) |
H11C | 1.2307 | 0.4216 | 0.6337 | 0.084* | 0.580 (7) |
C10B | 1.1622 (16) | 0.267 (2) | 0.6225 (14) | 0.048 (3)* | 0.420 (7) |
H10D | 1.2551 | 0.2948 | 0.6746 | 0.072* | 0.420 (7) |
H10E | 1.1671 | 0.2729 | 0.5486 | 0.072* | 0.420 (7) |
H10F | 1.1448 | 0.1824 | 0.6381 | 0.072* | 0.420 (7) |
C11B | 1.033 (2) | 0.358 (2) | 0.7442 (17) | 0.056 (3)* | 0.420 (7) |
H11D | 1.1244 | 0.397 | 0.7892 | 0.084* | 0.420 (7) |
H11E | 1.0258 | 0.2772 | 0.7728 | 0.084* | 0.420 (7) |
H11F | 0.9494 | 0.4075 | 0.7454 | 0.084* | 0.420 (7) |
C9B | 1.055 (2) | 0.482 (2) | 0.5859 (18) | 0.060 (3)* | 0.420 (7) |
H9B1 | 0.9805 | 0.5375 | 0.5954 | 0.089* | 0.420 (7) |
H9B2 | 1.0442 | 0.4765 | 0.5085 | 0.089* | 0.420 (7) |
H9B3 | 1.1528 | 0.5137 | 0.6261 | 0.089* | 0.420 (7) |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
V1 | 0.0401 (5) | 0.0192 (5) | 0.0170 (5) | −0.0041 (5) | 0.0160 (4) | −0.0037 (6) |
O2 | 0.043 (2) | 0.027 (3) | 0.018 (3) | −0.011 (2) | 0.015 (2) | −0.007 (2) |
O4 | 0.043 (2) | 0.032 (3) | 0.018 (2) | −0.010 (3) | 0.0168 (17) | −0.009 (3) |
O1 | 0.044 (2) | 0.031 (3) | 0.023 (2) | −0.016 (2) | 0.021 (2) | −0.0082 (19) |
O3 | 0.039 (2) | 0.028 (3) | 0.020 (2) | −0.0117 (19) | 0.016 (2) | −0.008 (2) |
C1 | 0.040 (3) | 0.018 (4) | 0.016 (3) | 0.004 (3) | 0.015 (3) | −0.001 (2) |
C15 | 0.041 (4) | 0.018 (4) | 0.017 (4) | −0.002 (3) | 0.012 (3) | −0.008 (3) |
C19 | 0.041 (3) | 0.036 (5) | 0.028 (3) | −0.004 (4) | 0.021 (3) | −0.006 (4) |
C18 | 0.059 (5) | 0.016 (4) | 0.035 (4) | −0.009 (3) | 0.021 (4) | −0.020 (3) |
C12 | 0.034 (3) | 0.010 (4) | 0.015 (3) | 0.004 (2) | 0.008 (2) | 0.000 (2) |
C3 | 0.037 (3) | 0.018 (3) | 0.021 (4) | 0.004 (3) | 0.016 (3) | 0.006 (3) |
C13 | 0.038 (3) | 0.022 (4) | 0.014 (3) | −0.003 (3) | 0.013 (3) | −0.006 (3) |
C8 | 0.042 (4) | 0.035 (4) | 0.025 (4) | −0.012 (3) | 0.014 (3) | −0.009 (3) |
C4 | 0.043 (4) | 0.022 (4) | 0.022 (4) | −0.007 (3) | 0.020 (3) | −0.002 (3) |
C2 | 0.043 (3) | 0.034 (5) | 0.015 (3) | −0.006 (3) | 0.015 (3) | −0.001 (3) |
C14 | 0.033 (3) | 0.015 (3) | 0.017 (3) | 0.003 (2) | 0.012 (3) | 0.004 (3) |
C17 | 0.069 (5) | 0.030 (5) | 0.039 (5) | −0.024 (4) | 0.026 (4) | −0.009 (4) |
C7 | 0.054 (5) | 0.045 (5) | 0.065 (6) | −0.009 (4) | 0.035 (5) | 0.013 (5) |
O5 | 0.067 (3) | 0.025 (3) | 0.033 (3) | 0.014 (2) | 0.023 (3) | 0.011 (2) |
C6 | 0.065 (5) | 0.032 (5) | 0.086 (7) | 0.007 (4) | 0.046 (5) | 0.021 (5) |
C16 | 0.043 (4) | 0.032 (5) | 0.049 (5) | 0.003 (3) | −0.004 (4) | −0.007 (4) |
C5 | 0.074 (5) | 0.048 (5) | 0.045 (5) | −0.026 (4) | 0.038 (4) | −0.004 (4) |
C21 | 0.053 (5) | 0.046 (6) | 0.093 (7) | 0.006 (4) | 0.036 (5) | 0.022 (5) |
C20 | 0.065 (5) | 0.030 (5) | 0.095 (7) | −0.005 (4) | 0.048 (5) | 0.008 (5) |
C22 | 0.082 (5) | 0.100 (7) | 0.063 (5) | −0.046 (7) | 0.061 (5) | −0.035 (7) |
Geometric parameters (Å, º) top
V1—O5 | 1.588 (5) | C19—C22 | 1.513 (9) |
V1—O1 | 1.952 (4) | C19—C12 | 1.546 (7) |
V1—O4 | 1.957 (3) | C19—C20 | 1.566 (11) |
V1—O2 | 1.965 (4) | C12—C13 | 1.361 (8) |
V1—O3 | 1.972 (4) | C3—C2 | 1.381 (8) |
O2—C3 | 1.270 (7) | C3—C4 | 1.543 (8) |
O4—C12 | 1.264 (6) | C13—C14 | 1.423 (8) |
O1—C1 | 1.279 (7) | C8—C11B | 1.44 (2) |
O3—C14 | 1.269 (7) | C8—C11A | 1.476 (15) |
C1—C2 | 1.403 (8) | C8—C10A | 1.502 (15) |
C1—C8 | 1.507 (8) | C8—C10B | 1.526 (19) |
C15—C14 | 1.516 (8) | C8—C9B | 1.60 (2) |
C15—C16 | 1.518 (9) | C8—C9A | 1.605 (16) |
C15—C17 | 1.526 (8) | C4—C7 | 1.506 (10) |
C15—C18 | 1.541 (8) | C4—C5 | 1.514 (9) |
C19—C21 | 1.485 (10) | C4—C6 | 1.539 (10) |
| | | |
O5—V1—O1 | 107.5 (2) | C2—C3—C4 | 121.4 (5) |
O5—V1—O4 | 106.2 (2) | C12—C13—C14 | 123.6 (5) |
O1—V1—O4 | 83.59 (16) | C11B—C8—C11A | 130.5 (12) |
O5—V1—O2 | 106.4 (2) | C11B—C8—C10A | 36.5 (10) |
O1—V1—O2 | 86.81 (16) | C11A—C8—C10A | 114.5 (10) |
O4—V1—O2 | 147.4 (2) | C11B—C8—C1 | 115.4 (10) |
O5—V1—O3 | 106.6 (2) | C11A—C8—C1 | 112.8 (8) |
O1—V1—O3 | 145.88 (18) | C10A—C8—C1 | 109.9 (7) |
O4—V1—O3 | 85.92 (18) | C11B—C8—C10B | 112.8 (12) |
O2—V1—O3 | 84.78 (17) | C11A—C8—C10B | 62.3 (11) |
C3—O2—V1 | 129.5 (4) | C10A—C8—C10B | 141.3 (10) |
C12—O4—V1 | 129.5 (3) | C1—C8—C10B | 105.8 (8) |
C1—O1—V1 | 130.2 (4) | C11B—C8—C9B | 109.7 (14) |
C14—O3—V1 | 131.0 (4) | C11A—C8—C9B | 45.0 (9) |
O1—C1—C2 | 121.9 (6) | C10A—C8—C9B | 77.4 (10) |
O1—C1—C8 | 115.9 (5) | C1—C8—C9B | 105.5 (9) |
C2—C1—C8 | 122.1 (5) | C10B—C8—C9B | 107.2 (12) |
C14—C15—C16 | 108.5 (5) | C11B—C8—C9A | 68.8 (11) |
C14—C15—C17 | 109.6 (5) | C11A—C8—C9A | 106.7 (9) |
C16—C15—C17 | 109.4 (6) | C10A—C8—C9A | 104.9 (9) |
C14—C15—C18 | 110.9 (5) | C1—C8—C9A | 107.4 (7) |
C16—C15—C18 | 109.8 (5) | C10B—C8—C9A | 48.9 (8) |
C17—C15—C18 | 108.6 (6) | C9B—C8—C9A | 143.8 (10) |
C21—C19—C22 | 112.0 (7) | C7—C4—C5 | 109.4 (6) |
C21—C19—C12 | 108.7 (6) | C7—C4—C6 | 108.5 (6) |
C22—C19—C12 | 113.4 (5) | C5—C4—C6 | 110.4 (7) |
C21—C19—C20 | 107.5 (6) | C7—C4—C3 | 110.2 (5) |
C22—C19—C20 | 108.6 (8) | C5—C4—C3 | 111.9 (5) |
C12—C19—C20 | 106.3 (5) | C6—C4—C3 | 106.4 (5) |
O4—C12—C13 | 124.7 (5) | C3—C2—C1 | 124.7 (5) |
O4—C12—C19 | 114.1 (5) | O3—C14—C13 | 121.6 (5) |
C13—C12—C19 | 121.1 (5) | O3—C14—C15 | 116.8 (5) |
O2—C3—C2 | 123.3 (5) | C13—C14—C15 | 121.6 (5) |
O2—C3—C4 | 115.1 (5) | | |