Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803008742/wn6150sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536803008742/wn6150Isup2.hkl |
CCDC reference: 214573
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.006 Å
- R factor = 0.058
- wR factor = 0.162
- Data-to-parameter ratio = 13.1
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
The title complex was prepared by refluxing an ethanol solution (15 ml) containing CrCl3·6H2O (0.27 g, 1 mmol), 8-quinolinol (0.29 g, 2 mmol) and imidazole (0.14 g, 2 mmol) for 2 h. The resulting solution was filtered at room temperature. Green single crystals were obtained from the filtrate after 2 weeks.
The hydroxyl H atom was located in a difference Fourier map, and included in the final cycles of refinement with fixed positional parameters and displacement parameter Uiso = 0.08 Å2. Other H atoms were placed in calculated positions, with C—H = 0.93–0.97 Å, and included in the final cycles of refinement as riding, with Uiso(H) = 1.2Ueq or 1.5Ueq of the carrier atoms.
Data collection: SMART (Bruker, 1999); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT; program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).
[Cr(C9H6NO)3]·C2H6O | F(000) = 1100 |
Mr = 530.51 | Dx = 1.409 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 8818 reflections |
a = 11.2683 (11) Å | θ = 2.5–24.5° |
b = 13.2572 (11) Å | µ = 0.50 mm−1 |
c = 16.8041 (18) Å | T = 298 K |
β = 94.783 (6)° | Prism, green |
V = 2501.6 (4) Å3 | 0.36 × 0.32 × 0.20 mm |
Z = 4 |
Bruker SMART CCD diffractometer | 4362 independent reflections |
Radiation source: fine-focus sealed tube | 3346 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.039 |
ω and ϕ scans | θmax = 25.0°, θmin = 2.0° |
Absorption correction: multi-scan (SADABS; Bruker, 1999) | h = −13→8 |
Tmin = 0.84, Tmax = 0.91 | k = −13→15 |
8913 measured reflections | l = −19→19 |
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)] = 0.058 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.162 | H-atom parameters constrained |
S = 1.10 | w = 1/[σ2(Fo2) + (0.0725P)2 + 2.5324P] where P = (Fo2 + 2Fc2)/3 |
4362 reflections | (Δ/σ)max < 0.001 |
334 parameters | Δρmax = 0.47 e Å−3 |
0 restraints | Δρmin = −0.44 e Å−3 |
[Cr(C9H6NO)3]·C2H6O | V = 2501.6 (4) Å3 |
Mr = 530.51 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 11.2683 (11) Å | µ = 0.50 mm−1 |
b = 13.2572 (11) Å | T = 298 K |
c = 16.8041 (18) Å | 0.36 × 0.32 × 0.20 mm |
β = 94.783 (6)° |
Bruker SMART CCD diffractometer | 4362 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 1999) | 3346 reflections with I > 2σ(I) |
Tmin = 0.84, Tmax = 0.91 | Rint = 0.039 |
8913 measured reflections |
R[F2 > 2σ(F2)] = 0.058 | 0 restraints |
wR(F2) = 0.162 | H-atom parameters constrained |
S = 1.10 | Δρmax = 0.47 e Å−3 |
4362 reflections | Δρmin = −0.44 e Å−3 |
334 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
Cr | 0.06841 (5) | −0.01785 (4) | 0.25614 (3) | 0.0387 (2) | |
O11 | −0.1047 (2) | −0.00813 (19) | 0.26518 (15) | 0.0460 (6) | |
O21 | 0.0771 (2) | −0.15728 (19) | 0.29316 (15) | 0.0496 (6) | |
O31 | 0.2358 (2) | −0.01254 (19) | 0.22972 (14) | 0.0465 (6) | |
N11 | 0.0461 (2) | 0.1328 (2) | 0.22680 (17) | 0.0412 (7) | |
N21 | 0.1125 (3) | 0.0116 (2) | 0.37607 (17) | 0.0413 (7) | |
N31 | 0.0427 (3) | −0.0669 (2) | 0.14009 (17) | 0.0438 (7) | |
C10 | −0.1127 (4) | 0.2590 (3) | 0.2115 (2) | 0.0511 (10) | |
C12 | 0.1243 (3) | 0.2019 (3) | 0.2089 (2) | 0.0531 (10) | |
H12 | 0.2038 | 0.1837 | 0.2076 | 0.064* | |
C13 | 0.0902 (4) | 0.3019 (3) | 0.1918 (3) | 0.0635 (12) | |
H13 | 0.1468 | 0.3491 | 0.1793 | 0.076* | |
C14 | −0.0255 (4) | 0.3296 (3) | 0.1935 (3) | 0.0625 (11) | |
H14 | −0.0476 | 0.3962 | 0.1827 | 0.075* | |
C15 | −0.2363 (4) | 0.2789 (3) | 0.2140 (3) | 0.0614 (11) | |
H15 | −0.2654 | 0.3440 | 0.2053 | 0.074* | |
C16 | −0.3117 (4) | 0.2026 (4) | 0.2292 (3) | 0.0632 (12) | |
H16 | −0.3928 | 0.2160 | 0.2283 | 0.076* | |
C17 | −0.2710 (3) | 0.1040 (3) | 0.2463 (2) | 0.0559 (10) | |
H17 | −0.3256 | 0.0541 | 0.2569 | 0.067* | |
C18 | −0.1497 (3) | 0.0795 (3) | 0.2476 (2) | 0.0443 (9) | |
C19 | −0.0724 (3) | 0.1603 (3) | 0.2284 (2) | 0.0407 (8) | |
C20 | 0.1518 (3) | −0.0819 (3) | 0.5007 (2) | 0.0512 (10) | |
C22 | 0.1283 (3) | 0.0965 (3) | 0.4162 (2) | 0.0499 (9) | |
H22 | 0.1209 | 0.1572 | 0.3885 | 0.060* | |
C23 | 0.1558 (4) | 0.0993 (3) | 0.4989 (2) | 0.0571 (11) | |
H23 | 0.1658 | 0.1608 | 0.5252 | 0.069* | |
C24 | 0.1677 (4) | 0.0116 (3) | 0.5404 (2) | 0.0576 (11) | |
H24 | 0.1865 | 0.0131 | 0.5954 | 0.069* | |
C25 | 0.1595 (4) | −0.1789 (4) | 0.5374 (3) | 0.0620 (11) | |
H25 | 0.1787 | −0.1845 | 0.5921 | 0.074* | |
C26 | 0.1388 (4) | −0.2627 (4) | 0.4927 (3) | 0.0630 (12) | |
H26 | 0.1439 | −0.3252 | 0.5178 | 0.076* | |
C27 | 0.1098 (3) | −0.2593 (3) | 0.4094 (3) | 0.0542 (10) | |
H27 | 0.0957 | −0.3188 | 0.3808 | 0.065* | |
C28 | 0.1022 (3) | −0.1674 (3) | 0.3702 (2) | 0.0442 (9) | |
C29 | 0.1237 (3) | −0.0785 (3) | 0.4173 (2) | 0.0407 (8) | |
C30 | 0.1548 (4) | −0.1113 (3) | 0.0270 (2) | 0.0598 (11) | |
C32 | −0.0564 (4) | −0.0946 (3) | 0.0987 (2) | 0.0580 (11) | |
H32 | −0.1283 | −0.0883 | 0.1217 | 0.070* | |
C33 | −0.0565 (5) | −0.1331 (4) | 0.0210 (3) | 0.0720 (13) | |
H33 | −0.1274 | −0.1542 | −0.0062 | 0.086* | |
C34 | 0.0462 (5) | −0.1396 (4) | −0.0139 (3) | 0.0705 (13) | |
H34 | 0.0453 | −0.1632 | −0.0661 | 0.085* | |
C35 | 0.2678 (5) | −0.1146 (4) | −0.0028 (3) | 0.0722 (13) | |
H35 | 0.2755 | −0.1377 | −0.0543 | 0.087* | |
C36 | 0.3654 (5) | −0.0839 (4) | 0.0436 (3) | 0.0759 (15) | |
H36 | 0.4390 | −0.0855 | 0.0224 | 0.091* | |
C37 | 0.3600 (4) | −0.0495 (3) | 0.1230 (3) | 0.0628 (12) | |
H37 | 0.4294 | −0.0305 | 0.1531 | 0.075* | |
C38 | 0.2516 (3) | −0.0442 (3) | 0.1559 (2) | 0.0479 (9) | |
C39 | 0.1486 (3) | −0.0749 (3) | 0.1065 (2) | 0.0447 (9) | |
O1 | 0.4443 (4) | 0.0801 (4) | 0.2883 (3) | 0.1187 (16) | |
C1 | 0.4784 (10) | 0.0899 (8) | 0.4279 (6) | 0.190 (5) | |
H1A | 0.4724 | 0.1335 | 0.4730 | 0.284* | |
H1B | 0.5602 | 0.0711 | 0.4246 | 0.284* | |
H1C | 0.4315 | 0.0304 | 0.4341 | 0.284* | |
C2 | 0.4346 (7) | 0.1426 (6) | 0.3549 (5) | 0.128 (3) | |
H2A | 0.3520 | 0.1616 | 0.3581 | 0.153* | |
H2B | 0.4806 | 0.2037 | 0.3492 | 0.153* | |
H1 | 0.3769 | 0.0487 | 0.2777 | 0.080* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cr | 0.0394 (3) | 0.0414 (4) | 0.0352 (3) | 0.0015 (2) | 0.0024 (2) | −0.0009 (2) |
O11 | 0.0432 (13) | 0.0444 (15) | 0.0514 (15) | −0.0050 (11) | 0.0093 (11) | 0.0043 (12) |
O21 | 0.0604 (16) | 0.0438 (15) | 0.0439 (15) | −0.0010 (12) | 0.0011 (12) | −0.0030 (12) |
O31 | 0.0403 (13) | 0.0575 (16) | 0.0417 (15) | 0.0053 (11) | 0.0023 (11) | −0.0064 (12) |
N11 | 0.0432 (16) | 0.0458 (18) | 0.0343 (15) | −0.0015 (14) | 0.0023 (12) | 0.0005 (13) |
N21 | 0.0401 (16) | 0.0473 (18) | 0.0367 (16) | 0.0002 (13) | 0.0050 (12) | −0.0017 (13) |
N31 | 0.0489 (18) | 0.0455 (18) | 0.0366 (16) | 0.0004 (14) | 0.0007 (14) | 0.0001 (13) |
C10 | 0.060 (2) | 0.048 (2) | 0.045 (2) | 0.0069 (19) | 0.0015 (18) | −0.0009 (18) |
C12 | 0.046 (2) | 0.061 (3) | 0.052 (2) | −0.0109 (19) | 0.0050 (17) | −0.003 (2) |
C13 | 0.074 (3) | 0.046 (3) | 0.071 (3) | −0.014 (2) | 0.009 (2) | 0.002 (2) |
C14 | 0.081 (3) | 0.041 (2) | 0.065 (3) | 0.004 (2) | 0.006 (2) | −0.001 (2) |
C15 | 0.069 (3) | 0.056 (3) | 0.059 (3) | 0.023 (2) | 0.006 (2) | 0.001 (2) |
C16 | 0.045 (2) | 0.081 (3) | 0.063 (3) | 0.021 (2) | 0.0012 (19) | 0.001 (2) |
C17 | 0.042 (2) | 0.076 (3) | 0.050 (2) | −0.001 (2) | 0.0078 (17) | 0.003 (2) |
C18 | 0.0406 (19) | 0.057 (3) | 0.0359 (19) | −0.0038 (17) | 0.0075 (15) | −0.0014 (17) |
C19 | 0.0433 (19) | 0.046 (2) | 0.0328 (18) | 0.0040 (16) | 0.0029 (15) | −0.0022 (15) |
C20 | 0.041 (2) | 0.069 (3) | 0.044 (2) | 0.0023 (18) | 0.0053 (16) | 0.0053 (19) |
C22 | 0.052 (2) | 0.048 (2) | 0.050 (2) | −0.0017 (18) | 0.0098 (18) | −0.0066 (18) |
C23 | 0.061 (3) | 0.067 (3) | 0.045 (2) | −0.007 (2) | 0.0088 (19) | −0.017 (2) |
C24 | 0.058 (2) | 0.078 (3) | 0.038 (2) | −0.005 (2) | 0.0057 (18) | −0.006 (2) |
C25 | 0.059 (3) | 0.078 (3) | 0.048 (2) | −0.001 (2) | 0.0006 (19) | 0.015 (2) |
C26 | 0.058 (2) | 0.061 (3) | 0.070 (3) | 0.001 (2) | 0.007 (2) | 0.025 (2) |
C27 | 0.052 (2) | 0.046 (2) | 0.066 (3) | 0.0005 (18) | 0.0067 (19) | 0.0065 (19) |
C28 | 0.0362 (18) | 0.047 (2) | 0.049 (2) | −0.0004 (16) | 0.0035 (16) | 0.0013 (17) |
C29 | 0.0329 (17) | 0.051 (2) | 0.0391 (19) | 0.0006 (15) | 0.0060 (14) | 0.0036 (16) |
C30 | 0.090 (3) | 0.049 (2) | 0.042 (2) | 0.011 (2) | 0.018 (2) | 0.0030 (18) |
C32 | 0.058 (2) | 0.063 (3) | 0.051 (2) | −0.007 (2) | −0.0047 (19) | −0.003 (2) |
C33 | 0.078 (3) | 0.078 (3) | 0.056 (3) | −0.018 (3) | −0.011 (2) | −0.006 (2) |
C34 | 0.100 (4) | 0.072 (3) | 0.037 (2) | −0.007 (3) | −0.007 (2) | −0.011 (2) |
C35 | 0.094 (4) | 0.075 (3) | 0.051 (3) | 0.014 (3) | 0.025 (3) | −0.002 (2) |
C36 | 0.075 (3) | 0.082 (4) | 0.077 (3) | 0.021 (3) | 0.044 (3) | 0.010 (3) |
C37 | 0.052 (2) | 0.068 (3) | 0.070 (3) | 0.013 (2) | 0.016 (2) | 0.000 (2) |
C38 | 0.050 (2) | 0.043 (2) | 0.052 (2) | 0.0094 (17) | 0.0120 (18) | 0.0046 (17) |
C39 | 0.058 (2) | 0.037 (2) | 0.039 (2) | 0.0061 (17) | 0.0057 (17) | 0.0024 (15) |
O1 | 0.079 (3) | 0.131 (4) | 0.147 (4) | −0.028 (2) | 0.013 (2) | −0.054 (3) |
C1 | 0.281 (14) | 0.162 (9) | 0.124 (8) | 0.051 (8) | 0.005 (8) | 0.022 (7) |
C2 | 0.125 (6) | 0.109 (6) | 0.153 (7) | −0.021 (4) | 0.038 (5) | −0.060 (5) |
Cr—O21 | 1.950 (3) | C22—H22 | 0.930 |
Cr—O11 | 1.974 (3) | C23—C24 | 1.357 (6) |
Cr—O31 | 1.975 (2) | C23—H23 | 0.930 |
Cr—N31 | 2.053 (3) | C24—H24 | 0.930 |
Cr—N11 | 2.068 (3) | C25—C26 | 1.350 (6) |
Cr—N21 | 2.072 (3) | C25—H25 | 0.930 |
O11—C18 | 1.292 (5) | C26—C27 | 1.411 (6) |
O21—C28 | 1.308 (4) | C26—H26 | 0.930 |
O31—C38 | 1.336 (4) | C27—C28 | 1.385 (5) |
N11—C12 | 1.322 (5) | C27—H27 | 0.930 |
N11—C19 | 1.387 (4) | C28—C29 | 1.430 (5) |
N21—C22 | 1.317 (5) | C30—C34 | 1.404 (7) |
N21—C29 | 1.381 (5) | C30—C35 | 1.407 (6) |
N31—C32 | 1.318 (5) | C30—C39 | 1.428 (5) |
N31—C39 | 1.365 (5) | C32—C33 | 1.402 (6) |
C10—C19 | 1.407 (5) | C32—H32 | 0.930 |
C10—C14 | 1.408 (6) | C33—C34 | 1.343 (7) |
C10—C15 | 1.421 (6) | C33—H33 | 0.930 |
C12—C13 | 1.404 (6) | C34—H34 | 0.930 |
C12—H12 | 0.9300 | C35—C36 | 1.356 (7) |
C13—C14 | 1.358 (6) | C35—H35 | 0.930 |
C13—H13 | 0.930 | C36—C37 | 1.417 (7) |
C14—H14 | 0.930 | C36—H36 | 0.930 |
C15—C16 | 1.360 (6) | C37—C38 | 1.383 (5) |
C15—H15 | 0.930 | C37—H37 | 0.930 |
C16—C17 | 1.407 (6) | C38—C39 | 1.428 (5) |
C16—H16 | 0.930 | O1—C2 | 1.404 (7) |
C17—C18 | 1.403 (5) | O1—H1 | 0.871 |
C17—H17 | 0.930 | C1—C2 | 1.462 (11) |
C18—C19 | 1.434 (5) | C1—H1A | 0.960 |
C20—C24 | 1.411 (6) | C1—H1B | 0.960 |
C20—C29 | 1.412 (5) | C1—H1C | 0.960 |
C20—C25 | 1.426 (6) | C2—H2A | 0.970 |
C22—C23 | 1.398 (5) | C2—H2B | 0.970 |
O21—Cr—O11 | 93.51 (11) | C24—C23—H23 | 120.2 |
O21—Cr—O31 | 94.69 (11) | C22—C23—H23 | 120.2 |
O11—Cr—O31 | 169.68 (10) | C23—C24—C20 | 120.4 (4) |
O21—Cr—N31 | 90.13 (11) | C23—C24—H24 | 119.8 |
O11—Cr—N31 | 91.83 (11) | C20—C24—H24 | 119.8 |
O31—Cr—N31 | 81.91 (11) | C26—C25—C20 | 120.0 (4) |
O21—Cr—N11 | 173.52 (11) | C26—C25—H25 | 120.0 |
O11—Cr—N11 | 81.62 (11) | C20—C25—H25 | 120.0 |
O31—Cr—N11 | 90.64 (11) | C25—C26—C27 | 122.8 (4) |
N31—Cr—N11 | 94.28 (12) | C25—C26—H26 | 118.6 |
O21—Cr—N21 | 82.35 (11) | C27—C26—H26 | 118.6 |
O11—Cr—N21 | 94.09 (11) | C28—C27—C26 | 120.0 (4) |
O31—Cr—N21 | 93.20 (10) | C28—C27—H27 | 120.0 |
N31—Cr—N21 | 170.69 (12) | C26—C27—H27 | 120.0 |
N11—Cr—N21 | 93.69 (12) | O21—C28—C27 | 124.1 (4) |
C18—O11—Cr | 114.4 (2) | O21—C28—C29 | 118.4 (3) |
C28—O21—Cr | 114.4 (2) | C27—C28—C29 | 117.5 (3) |
C38—O31—Cr | 113.7 (2) | N21—C29—C20 | 121.9 (3) |
C12—N11—C19 | 118.9 (3) | N21—C29—C28 | 115.5 (3) |
C12—N11—Cr | 130.8 (3) | C20—C29—C28 | 122.5 (3) |
C19—N11—Cr | 110.3 (2) | C34—C30—C35 | 126.5 (4) |
C22—N21—C29 | 118.6 (3) | C34—C30—C39 | 116.1 (4) |
C22—N21—Cr | 132.1 (3) | C35—C30—C39 | 117.4 (4) |
C29—N21—Cr | 109.2 (2) | N31—C32—C33 | 121.8 (4) |
C32—N31—C39 | 119.5 (3) | N31—C32—H32 | 119.1 |
C32—N31—Cr | 129.4 (3) | C33—C32—H32 | 119.1 |
C39—N31—Cr | 111.0 (2) | C34—C33—C32 | 119.8 (4) |
C19—C10—C14 | 116.3 (4) | C34—C33—H33 | 120.1 |
C19—C10—C15 | 117.9 (4) | C32—C33—H33 | 120.1 |
C14—C10—C15 | 125.8 (4) | C33—C34—C30 | 121.1 (4) |
N11—C12—C13 | 121.6 (4) | C33—C34—H34 | 119.5 |
N11—C12—H12 | 119.2 | C30—C34—H34 | 119.5 |
C13—C12—H12 | 119.2 | C36—C35—C30 | 120.1 (4) |
C14—C13—C12 | 119.9 (4) | C36—C35—H35 | 120.0 |
C14—C13—H13 | 120.1 | C30—C35—H35 | 120.0 |
C12—C13—H13 | 120.1 | C35—C36—C37 | 122.8 (4) |
C13—C14—C10 | 120.9 (4) | C35—C36—H36 | 118.6 |
C13—C14—H14 | 119.6 | C37—C36—H36 | 118.6 |
C10—C14—H14 | 119.6 | C38—C37—C36 | 120.0 (4) |
C16—C15—C10 | 119.8 (4) | C38—C37—H37 | 120.0 |
C16—C15—H15 | 120.1 | C36—C37—H37 | 120.0 |
C10—C15—H15 | 120.1 | O31—C38—C37 | 125.2 (4) |
C15—C16—C17 | 122.1 (4) | O31—C38—C39 | 117.6 (3) |
C15—C16—H16 | 118.9 | C37—C38—C39 | 117.1 (4) |
C17—C16—H16 | 118.9 | N31—C39—C30 | 121.7 (4) |
C18—C17—C16 | 121.2 (4) | N31—C39—C38 | 115.7 (3) |
C18—C17—H17 | 119.4 | C30—C39—C38 | 122.6 (4) |
C16—C17—H17 | 119.4 | C2—O1—H1 | 108.7 |
O11—C18—C17 | 125.1 (4) | C2—C1—H1A | 109.5 |
O11—C18—C19 | 119.3 (3) | C2—C1—H1B | 109.5 |
C17—C18—C19 | 115.6 (4) | H1A—C1—H1B | 109.5 |
N11—C19—C10 | 122.3 (3) | C2—C1—H1C | 109.5 |
N11—C19—C18 | 114.4 (3) | H1A—C1—H1C | 109.5 |
C10—C19—C18 | 123.3 (3) | H1B—C1—H1C | 109.5 |
C24—C20—C29 | 116.8 (4) | O1—C2—C1 | 110.1 (7) |
C24—C20—C25 | 126.0 (4) | O1—C2—H2A | 109.6 |
C29—C20—C25 | 117.3 (4) | C1—C2—H2A | 109.6 |
N21—C22—C23 | 122.7 (4) | O1—C2—H2B | 109.6 |
N21—C22—H22 | 118.6 | C1—C2—H2B | 109.6 |
C23—C22—H22 | 118.6 | H2A—C2—H2B | 108.2 |
C24—C23—C22 | 119.5 (4) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1···O31 | 0.87 | 1.90 | 2.758 (5) | 167 |
C15—H15···O11i | 0.93 | 2.52 | 3.377 (5) | 153 |
C24—H24···O11ii | 0.93 | 2.59 | 3.401 (4) | 146 |
Symmetry codes: (i) −x−1/2, y+1/2, −z+1/2; (ii) −x, −y, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [Cr(C9H6NO)3]·C2H6O |
Mr | 530.51 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 298 |
a, b, c (Å) | 11.2683 (11), 13.2572 (11), 16.8041 (18) |
β (°) | 94.783 (6) |
V (Å3) | 2501.6 (4) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.50 |
Crystal size (mm) | 0.36 × 0.32 × 0.20 |
Data collection | |
Diffractometer | Bruker SMART CCD diffractometer |
Absorption correction | Multi-scan (SADABS; Bruker, 1999) |
Tmin, Tmax | 0.84, 0.91 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 8913, 4362, 3346 |
Rint | 0.039 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.058, 0.162, 1.10 |
No. of reflections | 4362 |
No. of parameters | 334 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.47, −0.44 |
Computer programs: SMART (Bruker, 1999), SAINT (Bruker, 1999), SAINT, SIR92 (Altomare et al., 1993), SHELXL97 (Sheldrick, 1997), ORTEP-3 for Windows (Farrugia, 1997), WinGX (Farrugia, 1999).
Cr—O21 | 1.950 (3) | Cr—N31 | 2.053 (3) |
Cr—O11 | 1.974 (3) | Cr—N11 | 2.068 (3) |
Cr—O31 | 1.975 (2) | Cr—N21 | 2.072 (3) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1···O31 | 0.87 | 1.90 | 2.758 (5) | 167 |
C15—H15···O11i | 0.93 | 2.52 | 3.377 (5) | 153 |
C24—H24···O11ii | 0.93 | 2.59 | 3.401 (4) | 146 |
Symmetry codes: (i) −x−1/2, y+1/2, −z+1/2; (ii) −x, −y, −z+1. |
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As part of a series of investigations on π–π-stacking interactions in metal complexes, several 8-quinolinolate–metal complexes have been synthesized in the laboratory.
The structure of the title complex, (I), is shown in Fig. 1. Three 8-quinolinolate ligands chelate to the CrIII atom in an octahedral coordination geometry. The planar 8-quinolinolate ligands are almost perpendicular to each other, with dihedral angles of 85.84 (10), 85.40 (11) and 81.91 (14)°. The overlapped disposition of neighboring parallel quinoline rings is shown in Fig. 2. The quinoline plane containing atom N21 is separated from the quinoline plane containing N21(-x, −y, 1 − z) by 3.426 (19) Å. Likewise, the plane containing atom 31 and the plane containing N31(-x, −y, −z) are separated by 3.368 (4) Å. These findings strongly suggest the existence of π–π stacking in the crystal structure.
The ethanol solvent molecule is hydrogen bonded to the CrIII complex, with an O1···O31 distance of 2.758 (5) Å and an O1—H1···O31 angle of 167° (Table 2). Weak C—H···O hydrogen bonding occurs between atom O11 and quinoline atoms C15 and C24.