Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803014211/om6151sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536803014211/om6151Isup2.hkl |
CCDC reference: 217429
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.005 Å
- H-atom completeness 82%
- Disorder in solvent or counterion
- R factor = 0.042
- wR factor = 0.130
- Data-to-parameter ratio = 16.8
checkCIF results
No syntax errors found ADDSYM reports no extra symmetry
Alert Level C:
PLAT_302 Alert C Anion/Solvent Disorder ......................... 50.00 Perc. General Notes
FORMU_01 There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C28 H22 Co1 N3 O4 Atom count from the _atom_site data: C28 H18 Co1 N3 O4 CELLZ_01 From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_sum C28 H22 Co N3 O4 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 112.00 112.00 0.00 H 88.00 72.00 16.00 Co 4.00 4.00 0.00 N 12.00 12.00 0.00 O 16.00 16.00 0.00 Difference between formula and atom_site contents detected. WARNING: H atoms missing from atom site list. Is this intentional?
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check
The complex was prepared by refluxing the methanol solution (15 ml) containing CoCl2·6H2O (0.24 g, 1 mmol) and 8-quinolinol (0.15 g, 1 mmol) for 2 h. The resulting solution was filtered at room temperature. The brown single crystals were obtained from the filtrate after two weeks.
The disordered methanol molecule was refined isotropically and H atoms were not located. Other H atoms were placed in calculated positions with C—H = 0.93 Å and included in the final cycles of refinement using a riding model, with Uiso(H) = 1.2Ueq of the carrier atoms.
Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); 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).
[Co(C9H6NO)3]·CH4O | F(000) = 1080 |
Mr = 523.42 | Dx = 1.466 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71069 Å |
Hall symbol: -P 2yn | Cell parameters from 9762 reflections |
a = 10.9235 (12) Å | θ = 3.0–27.0° |
b = 13.1172 (14) Å | µ = 0.77 mm−1 |
c = 16.6861 (14) Å | T = 298 K |
β = 97.325 (8)° | Prism, brown |
V = 2371.4 (4) Å3 | 0.36 × 0.20 × 0.10 mm |
Z = 4 |
Rigaku R-AXIS-RAPID diffractometer | 5432 independent reflections |
Radiation source: fine-focus sealed tube | 4009 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.020 |
Detector resolution: 10.00 pixels mm-1 | θmax = 27.5°, θmin = 2.0° |
ω scans | h = −14→14 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −17→17 |
Tmin = 0.750, Tmax = 0.918 | l = −21→21 |
10460 measured reflections |
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)] = 0.042 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.130 | H-atom parameters constrained |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0805P)2 + 0.1393P] where P = (Fo2 + 2Fc2)/3 |
5432 reflections | (Δ/σ)max = 0.003 |
323 parameters | Δρmax = 0.59 e Å−3 |
0 restraints | Δρmin = −0.42 e Å−3 |
[Co(C9H6NO)3]·CH4O | V = 2371.4 (4) Å3 |
Mr = 523.42 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 10.9235 (12) Å | µ = 0.77 mm−1 |
b = 13.1172 (14) Å | T = 298 K |
c = 16.6861 (14) Å | 0.36 × 0.20 × 0.10 mm |
β = 97.325 (8)° |
Rigaku R-AXIS-RAPID diffractometer | 5432 independent reflections |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | 4009 reflections with I > 2σ(I) |
Tmin = 0.750, Tmax = 0.918 | Rint = 0.020 |
10460 measured reflections |
R[F2 > 2σ(F2)] = 0.042 | 0 restraints |
wR(F2) = 0.130 | H-atom parameters constrained |
S = 1.04 | Δρmax = 0.59 e Å−3 |
5432 reflections | Δρmin = −0.42 e Å−3 |
323 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 | Occ. (<1) | |
Co | 0.42453 (3) | 0.52085 (3) | 0.240612 (18) | 0.03029 (12) | |
O11 | 0.25371 (17) | 0.51074 (15) | 0.25265 (11) | 0.0397 (4) | |
O21 | 0.59627 (16) | 0.52675 (14) | 0.23257 (11) | 0.0363 (4) | |
O31 | 0.40960 (18) | 0.65942 (14) | 0.20819 (11) | 0.0396 (4) | |
N11 | 0.4467 (2) | 0.56689 (17) | 0.35082 (12) | 0.0363 (5) | |
N21 | 0.45475 (19) | 0.38159 (16) | 0.27347 (12) | 0.0314 (4) | |
N31 | 0.3862 (2) | 0.48847 (16) | 0.12697 (12) | 0.0333 (5) | |
C10 | 0.3259 (3) | 0.6040 (2) | 0.46019 (16) | 0.0498 (8) | |
C12 | 0.5483 (3) | 0.5981 (2) | 0.39558 (17) | 0.0478 (7) | |
H12 | 0.6232 | 0.5969 | 0.3746 | 0.057* | |
C13 | 0.5438 (4) | 0.6332 (3) | 0.47470 (19) | 0.0596 (9) | |
H13 | 0.6158 | 0.6553 | 0.5056 | 0.072* | |
C14 | 0.4372 (4) | 0.6351 (3) | 0.50610 (17) | 0.0610 (9) | |
H14 | 0.4363 | 0.6573 | 0.5590 | 0.073* | |
C15 | 0.2088 (4) | 0.6023 (3) | 0.4859 (2) | 0.0636 (10) | |
H15 | 0.1989 | 0.6222 | 0.5381 | 0.076* | |
C16 | 0.1087 (4) | 0.5712 (3) | 0.4333 (2) | 0.0666 (10) | |
H16 | 0.0313 | 0.5714 | 0.4509 | 0.080* | |
C17 | 0.1182 (3) | 0.5389 (2) | 0.3540 (2) | 0.0524 (8) | |
H17 | 0.0483 | 0.5180 | 0.3203 | 0.063* | |
C18 | 0.2328 (3) | 0.5386 (2) | 0.32625 (16) | 0.0395 (6) | |
C19 | 0.3365 (3) | 0.5703 (2) | 0.38057 (15) | 0.0378 (6) | |
C20 | 0.6257 (3) | 0.2599 (2) | 0.29467 (15) | 0.0384 (6) | |
C22 | 0.3766 (3) | 0.3107 (2) | 0.29318 (16) | 0.0408 (6) | |
H22 | 0.2934 | 0.3266 | 0.2920 | 0.049* | |
C23 | 0.4182 (3) | 0.2123 (2) | 0.31575 (18) | 0.0494 (7) | |
H23 | 0.3626 | 0.1641 | 0.3304 | 0.059* | |
C24 | 0.5394 (3) | 0.1865 (2) | 0.31634 (18) | 0.0482 (7) | |
H24 | 0.5658 | 0.1209 | 0.3309 | 0.058* | |
C25 | 0.7527 (3) | 0.2434 (2) | 0.29262 (17) | 0.0491 (7) | |
H25 | 0.7871 | 0.1796 | 0.3051 | 0.059* | |
C26 | 0.8243 (3) | 0.3213 (3) | 0.27227 (18) | 0.0507 (8) | |
H26 | 0.9081 | 0.3095 | 0.2713 | 0.061* | |
C27 | 0.7772 (3) | 0.4191 (2) | 0.25265 (17) | 0.0454 (7) | |
H27 | 0.8297 | 0.4707 | 0.2398 | 0.054* | |
C28 | 0.6517 (2) | 0.4386 (2) | 0.25241 (14) | 0.0336 (5) | |
C29 | 0.5768 (2) | 0.3571 (2) | 0.27431 (13) | 0.0314 (5) | |
C30 | 0.3434 (2) | 0.5764 (2) | −0.00203 (15) | 0.0412 (6) | |
C32 | 0.3725 (3) | 0.4000 (2) | 0.08936 (16) | 0.0410 (6) | |
H32 | 0.3817 | 0.3402 | 0.1195 | 0.049* | |
C33 | 0.3444 (3) | 0.3934 (3) | 0.00479 (17) | 0.0492 (7) | |
H33 | 0.3353 | 0.3301 | −0.0202 | 0.059* | |
C34 | 0.3306 (3) | 0.4800 (3) | −0.04010 (17) | 0.0493 (7) | |
H34 | 0.3127 | 0.4759 | −0.0960 | 0.059* | |
C35 | 0.3337 (3) | 0.6719 (3) | −0.04178 (18) | 0.0513 (8) | |
H35 | 0.3142 | 0.6752 | −0.0976 | 0.062* | |
C36 | 0.3531 (3) | 0.7587 (3) | 0.00256 (18) | 0.0521 (8) | |
H36 | 0.3482 | 0.8208 | −0.0245 | 0.063* | |
C37 | 0.3801 (3) | 0.7594 (2) | 0.08720 (17) | 0.0445 (6) | |
H37 | 0.3923 | 0.8208 | 0.1149 | 0.053* | |
C38 | 0.3886 (2) | 0.6677 (2) | 0.12899 (16) | 0.0359 (6) | |
C39 | 0.3721 (2) | 0.5767 (2) | 0.08324 (14) | 0.0336 (5) | |
C1a | 0.0264 (11) | 0.3915 (10) | 0.0861 (8) | 0.111 (4)* | 0.50 |
C1b | 0.0423 (8) | 0.3573 (7) | 0.1223 (6) | 0.073 (2)* | 0.50 |
O1a | 0.0379 (6) | 0.4409 (5) | 0.1711 (4) | 0.0774 (17)* | 0.50 |
O1b | 0.0416 (6) | 0.4653 (6) | 0.1382 (5) | 0.088 (2)* | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co | 0.03250 (19) | 0.03052 (19) | 0.02821 (17) | 0.00119 (14) | 0.00521 (12) | −0.00099 (14) |
O11 | 0.0334 (10) | 0.0475 (11) | 0.0384 (9) | 0.0051 (8) | 0.0056 (7) | −0.0030 (8) |
O21 | 0.0341 (9) | 0.0346 (10) | 0.0412 (9) | −0.0022 (8) | 0.0086 (7) | 0.0054 (8) |
O31 | 0.0512 (12) | 0.0320 (10) | 0.0352 (9) | 0.0027 (8) | 0.0038 (8) | −0.0026 (7) |
N11 | 0.0451 (13) | 0.0316 (12) | 0.0319 (10) | 0.0005 (10) | 0.0043 (9) | 0.0006 (9) |
N21 | 0.0322 (11) | 0.0320 (11) | 0.0311 (10) | −0.0020 (9) | 0.0078 (8) | −0.0015 (8) |
N31 | 0.0335 (11) | 0.0356 (11) | 0.0318 (10) | 0.0016 (9) | 0.0078 (8) | −0.0020 (9) |
C10 | 0.080 (2) | 0.0380 (16) | 0.0342 (14) | 0.0080 (15) | 0.0183 (14) | 0.0010 (11) |
C12 | 0.0527 (18) | 0.0476 (18) | 0.0412 (15) | −0.0076 (14) | −0.0007 (13) | −0.0024 (12) |
C13 | 0.079 (2) | 0.056 (2) | 0.0405 (16) | −0.0138 (18) | −0.0039 (16) | −0.0074 (14) |
C14 | 0.103 (3) | 0.0487 (19) | 0.0312 (15) | −0.0030 (19) | 0.0095 (16) | −0.0074 (13) |
C15 | 0.088 (3) | 0.059 (2) | 0.0511 (18) | 0.0156 (19) | 0.0366 (19) | 0.0006 (16) |
C16 | 0.070 (2) | 0.066 (2) | 0.073 (2) | 0.0205 (19) | 0.047 (2) | 0.0168 (19) |
C17 | 0.0449 (17) | 0.052 (2) | 0.0638 (19) | 0.0102 (14) | 0.0198 (14) | 0.0119 (15) |
C18 | 0.0435 (15) | 0.0343 (15) | 0.0425 (14) | 0.0089 (11) | 0.0123 (12) | 0.0047 (11) |
C19 | 0.0505 (16) | 0.0299 (14) | 0.0347 (12) | 0.0060 (11) | 0.0124 (11) | 0.0030 (10) |
C20 | 0.0480 (16) | 0.0353 (14) | 0.0319 (12) | 0.0043 (12) | 0.0056 (11) | −0.0016 (10) |
C22 | 0.0414 (15) | 0.0382 (15) | 0.0441 (15) | −0.0064 (12) | 0.0111 (12) | −0.0007 (11) |
C23 | 0.0589 (19) | 0.0345 (15) | 0.0572 (18) | −0.0131 (14) | 0.0162 (15) | −0.0005 (13) |
C24 | 0.065 (2) | 0.0308 (15) | 0.0485 (16) | 0.0015 (13) | 0.0073 (14) | −0.0016 (12) |
C25 | 0.0506 (18) | 0.0488 (18) | 0.0475 (16) | 0.0179 (14) | 0.0043 (13) | 0.0030 (13) |
C26 | 0.0341 (15) | 0.069 (2) | 0.0485 (16) | 0.0134 (14) | 0.0037 (12) | 0.0028 (15) |
C27 | 0.0323 (14) | 0.0585 (19) | 0.0455 (15) | −0.0028 (13) | 0.0057 (12) | 0.0049 (13) |
C28 | 0.0345 (13) | 0.0391 (14) | 0.0276 (11) | 0.0002 (11) | 0.0056 (10) | 0.0001 (10) |
C29 | 0.0353 (13) | 0.0343 (13) | 0.0252 (11) | 0.0005 (10) | 0.0065 (10) | −0.0022 (9) |
C30 | 0.0367 (14) | 0.0532 (18) | 0.0343 (13) | −0.0004 (13) | 0.0064 (11) | 0.0031 (12) |
C32 | 0.0469 (16) | 0.0390 (15) | 0.0376 (13) | 0.0021 (12) | 0.0072 (11) | −0.0034 (11) |
C33 | 0.0559 (19) | 0.0528 (19) | 0.0390 (15) | −0.0056 (14) | 0.0066 (13) | −0.0143 (13) |
C34 | 0.0537 (18) | 0.063 (2) | 0.0313 (13) | −0.0060 (15) | 0.0052 (12) | −0.0062 (13) |
C35 | 0.0533 (18) | 0.063 (2) | 0.0372 (15) | −0.0011 (15) | 0.0038 (13) | 0.0132 (13) |
C36 | 0.0498 (18) | 0.0522 (19) | 0.0547 (18) | 0.0015 (15) | 0.0081 (14) | 0.0219 (15) |
C37 | 0.0436 (16) | 0.0384 (15) | 0.0521 (16) | −0.0003 (12) | 0.0081 (13) | 0.0062 (12) |
C38 | 0.0307 (13) | 0.0374 (14) | 0.0401 (14) | 0.0025 (11) | 0.0070 (10) | 0.0025 (11) |
C39 | 0.0311 (13) | 0.0373 (14) | 0.0330 (12) | 0.0007 (11) | 0.0062 (10) | 0.0015 (10) |
Co—O31 | 1.8975 (19) | C20—C25 | 1.409 (4) |
Co—O21 | 1.8994 (18) | C20—C24 | 1.425 (4) |
Co—O11 | 1.9066 (19) | C22—C23 | 1.404 (4) |
Co—N11 | 1.921 (2) | C22—H22 | 0.93 |
Co—N21 | 1.924 (2) | C23—C24 | 1.366 (4) |
Co—N31 | 1.936 (2) | C23—H23 | 0.93 |
O11—C18 | 1.329 (3) | C24—H24 | 0.93 |
O21—C28 | 1.327 (3) | C25—C26 | 1.356 (5) |
O31—C38 | 1.317 (3) | C25—H25 | 0.93 |
N11—C12 | 1.321 (4) | C26—C27 | 1.405 (4) |
N11—C19 | 1.361 (3) | C26—H26 | 0.93 |
N21—C22 | 1.332 (3) | C27—C28 | 1.395 (4) |
N21—C29 | 1.369 (3) | C27—H27 | 0.93 |
N31—C32 | 1.319 (3) | C28—C29 | 1.422 (4) |
N31—C39 | 1.366 (3) | C30—C34 | 1.414 (4) |
C10—C15 | 1.400 (5) | C30—C35 | 1.415 (4) |
C10—C14 | 1.412 (5) | C30—C39 | 1.417 (3) |
C10—C19 | 1.419 (4) | C32—C33 | 1.408 (4) |
C12—C13 | 1.405 (4) | C32—H32 | 0.93 |
C12—H12 | 0.93 | C33—C34 | 1.359 (4) |
C13—C14 | 1.337 (5) | C33—H33 | 0.93 |
C13—H13 | 0.93 | C34—H34 | 0.93 |
C14—H14 | 0.93 | C35—C36 | 1.359 (5) |
C15—C16 | 1.374 (5) | C35—H35 | 0.93 |
C15—H15 | 0.93 | C36—C37 | 1.406 (4) |
C16—C17 | 1.405 (5) | C36—H36 | 0.93 |
C16—H16 | 0.93 | C37—C38 | 1.387 (4) |
C17—C18 | 1.389 (4) | C37—H37 | 0.93 |
C17—H17 | 0.93 | C38—C39 | 1.416 (4) |
C18—C19 | 1.420 (4) | C1a—O1a | 1.551 (14) |
C20—C29 | 1.407 (4) | C1b—O1b | 1.442 (12) |
O31—Co—O21 | 89.46 (8) | C29—C20—C25 | 118.6 (3) |
O31—Co—O11 | 92.70 (8) | C29—C20—C24 | 115.5 (3) |
O21—Co—O11 | 177.41 (8) | C25—C20—C24 | 125.9 (3) |
O31—Co—N11 | 88.14 (9) | N21—C22—C23 | 120.9 (3) |
O21—Co—N11 | 92.83 (9) | N21—C22—H22 | 119.6 |
O11—Co—N11 | 85.81 (9) | C23—C22—H22 | 119.6 |
O31—Co—N21 | 175.06 (8) | C24—C23—C22 | 120.6 (3) |
O21—Co—N21 | 85.62 (8) | C24—C23—H23 | 119.7 |
O11—Co—N21 | 92.21 (8) | C22—C23—H23 | 119.7 |
N11—Co—N21 | 91.69 (9) | C23—C24—C20 | 120.2 (3) |
O31—Co—N31 | 86.04 (8) | C23—C24—H24 | 119.9 |
O21—Co—N31 | 91.83 (8) | C20—C24—H24 | 119.9 |
O11—Co—N31 | 89.75 (8) | C26—C25—C20 | 119.4 (3) |
N11—Co—N31 | 172.51 (9) | C26—C25—H25 | 120.3 |
N21—Co—N31 | 94.51 (9) | C20—C25—H25 | 120.3 |
C18—O11—Co | 111.35 (17) | C25—C26—C27 | 122.7 (3) |
C28—O21—Co | 111.71 (15) | C25—C26—H26 | 118.7 |
C38—O31—Co | 111.28 (16) | C27—C26—H26 | 118.7 |
C12—N11—C19 | 120.1 (2) | C28—C27—C26 | 120.0 (3) |
C12—N11—Co | 129.3 (2) | C28—C27—H27 | 120.0 |
C19—N11—Co | 110.48 (17) | C26—C27—H27 | 120.0 |
C22—N21—C29 | 119.2 (2) | O21—C28—C27 | 125.3 (2) |
C22—N21—Co | 129.90 (19) | O21—C28—C29 | 117.4 (2) |
C29—N21—Co | 110.91 (16) | C27—C28—C29 | 117.3 (2) |
C32—N31—C39 | 119.5 (2) | N21—C29—C20 | 123.6 (2) |
C32—N31—Co | 131.02 (19) | N21—C29—C28 | 114.4 (2) |
C39—N31—Co | 109.45 (17) | C20—C29—C28 | 122.0 (2) |
C15—C10—C14 | 126.5 (3) | C34—C30—C35 | 125.7 (3) |
C15—C10—C19 | 118.0 (3) | C34—C30—C39 | 116.7 (3) |
C14—C10—C19 | 115.5 (3) | C35—C30—C39 | 117.5 (3) |
N11—C12—C13 | 120.4 (3) | N31—C32—C33 | 121.8 (3) |
N11—C12—H12 | 119.8 | N31—C32—H32 | 119.1 |
C13—C12—H12 | 119.8 | C33—C32—H32 | 119.1 |
C14—C13—C12 | 120.7 (3) | C34—C33—C32 | 119.7 (3) |
C14—C13—H13 | 119.6 | C34—C33—H33 | 120.1 |
C12—C13—H13 | 119.6 | C32—C33—H33 | 120.1 |
C13—C14—C10 | 121.0 (3) | C33—C34—C30 | 120.2 (3) |
C13—C14—H14 | 119.5 | C33—C34—H34 | 119.9 |
C10—C14—H14 | 119.5 | C30—C34—H34 | 119.9 |
C16—C15—C10 | 119.5 (3) | C36—C35—C30 | 119.3 (3) |
C16—C15—H15 | 120.2 | C36—C35—H35 | 120.4 |
C10—C15—H15 | 120.2 | C30—C35—H35 | 120.4 |
C15—C16—C17 | 122.8 (3) | C35—C36—C37 | 123.4 (3) |
C15—C16—H16 | 118.6 | C35—C36—H36 | 118.3 |
C17—C16—H16 | 118.6 | C37—C36—H36 | 118.3 |
C18—C17—C16 | 119.5 (3) | C38—C37—C36 | 119.4 (3) |
C18—C17—H17 | 120.2 | C38—C37—H37 | 120.3 |
C16—C17—H17 | 120.2 | C36—C37—H37 | 120.3 |
O11—C18—C17 | 125.3 (3) | O31—C38—C37 | 124.6 (3) |
O11—C18—C19 | 117.0 (2) | O31—C38—C39 | 117.7 (2) |
C17—C18—C19 | 117.8 (3) | C37—C38—C39 | 117.6 (2) |
N11—C19—C10 | 122.3 (3) | N31—C39—C38 | 115.3 (2) |
N11—C19—C18 | 115.4 (2) | N31—C39—C30 | 122.0 (2) |
C10—C19—C18 | 122.4 (3) | C38—C39—C30 | 122.7 (2) |
D—H···A | D—H | H···A | D···A | D—H···A |
C12—H12···O21 | 0.93 | 2.52 | 2.985 (3) | 111 |
C22—H22···O11 | 0.93 | 2.53 | 2.985 (3) | 111 |
C24—H24···O1b | 0.93 | 2.44 | 3.154 (8) | 133 |
C25—H25···O21 | 0.93 | 2.50 | 3.339 (4) | 151 |
Experimental details
Crystal data | |
Chemical formula | [Co(C9H6NO)3]·CH4O |
Mr | 523.42 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 298 |
a, b, c (Å) | 10.9235 (12), 13.1172 (14), 16.6861 (14) |
β (°) | 97.325 (8) |
V (Å3) | 2371.4 (4) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.77 |
Crystal size (mm) | 0.36 × 0.20 × 0.10 |
Data collection | |
Diffractometer | Rigaku R-AXIS-RAPID diffractometer |
Absorption correction | Multi-scan (ABSCOR; Higashi, 1995) |
Tmin, Tmax | 0.750, 0.918 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 10460, 5432, 4009 |
Rint | 0.020 |
(sin θ/λ)max (Å−1) | 0.650 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.042, 0.130, 1.04 |
No. of reflections | 5432 |
No. of parameters | 323 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.59, −0.42 |
Computer programs: PROCESS-AUTO (Rigaku, 1998), PROCESS-AUTO, CrystalStructure (Rigaku/MSC, 2002), SIR92 (Altomare et al., 1993), SHELXL97 (Sheldrick, 1997), ORTEP-3 for Windows (Farrugia, 1997), WinGX (Farrugia, 1999).
Co—O31 | 1.8975 (19) | Co—N11 | 1.921 (2) |
Co—O21 | 1.8994 (18) | Co—N21 | 1.924 (2) |
Co—O11 | 1.9066 (19) | Co—N31 | 1.936 (2) |
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As a part of an investigation on the π–π-stacking interaction in metal complexes, several 8-quinolinolate metal complexes have been prepared in our laboratory (Li et al., 2003). Compound (I) is a representative of this group.
The structure of (I) is shown in Fig. 1. Three 8-quinolinolate monoanions chelate to the CoIII atom with an octahedral coordination geometry. The planar 8-quinolinolate are nearly perpendicular to each other with dihedral angles of 93.80 (7), 95.34 (6) and 91.49 (7)°. The overlapped arrangement of neighboring parallel quinoline rings is shown in Fig. 2. The quinoline plane containing N11 is separated from the quinoline plane containing N11(1 − x, 1 − y, 1 − z) by 3.404 (15) Å. Likewise, the quinoline plane containing N31 atom is separated from the quinoline plane containing N31(1 − x, 1 − y, −z) by 3.386 (7) Å. These findings indicate the existence of the π–π stacking between the neighboring complex molecules.
The solvate methanol is disordered, either C or O atoms located in two sites with 0.5 occupancy factors. Although H atoms of the disordered methanol were not located, the O1a···O11 distance of 2.726 (7) Å and the O1b···O11 distance of 2.871 (8) Å suggest the existence of hydrogen bonding between the quinolinol hydroxyl group and the disordered methanol molecule. The C24—H24···O1b(0.5 − x, −0.5 + y, 0.5 − z) angle of 133° and the C24···O1b distance of 3.154 (8) Å suggest that the disordered methanol molecule is also involved in the weak hydrogen bonding.
Compound (I) is isomorphous with the manganese(III) compound (Hems & Mackay, 1975). The major difference between the Co and Mn complexes is the length of the coordination bonds: Mn—O distances range from 1.905 to 1.924 Å and Co—O distances range from 1.8975 (19) to 1.9066 (19) Å; Mn—N distances range from 2.059 to 2.266 Å, while Co—N distances range from 1.921 (2) to 1.936 (2) Å. The other difference between two structures is that the solvent methanol molecule in the Mn structrue was not treated with a disorder model, even though the C—O distance of 1.352 Å is shorter than the expected value.