The title complex, [Co(H
2O)
6](C
7H
6NO
3)
2·2H
2O, was synthesized by the reaction of Co(CH
3COO)
2·4H
2O and 4-oxo-4
H-pyridine-1-acetic acid in an aqueous solution. The cobalt(II) ion, which lies on a center of symmetry, is coordinated by six water molecules to form an octahedron [Co—O = 2.077 (1)–2.084 (1) Å]. A three-dimensional supramolecular framework is formed
via O—H
O hydrogen bonds between the anions and cations.
Supporting information
CCDC reference: 239088
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.002 Å
- R factor = 0.027
- wR factor = 0.080
- Data-to-parameter ratio = 14.7
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Co1 - O3W .. 8.54 su
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 8
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
2 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
0 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
Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
Hexaaquacobalt(II) bis[(4-oxo-4
H-pyridin-1-yl)acetate] dihydrate
top
Crystal data top
[Co(H2O)6](C7H6NO3)2·2H2O | F(000) = 530 |
Mr = 507.31 | Dx = 1.586 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 8329 reflections |
a = 12.387 (3) Å | θ = 3.7–27.5° |
b = 12.816 (3) Å | µ = 0.88 mm−1 |
c = 6.766 (1) Å | T = 293 K |
β = 98.42 (3)° | Prism, pink |
V = 1062.6 (4) Å3 | 0.37 × 0.26 × 0.17 mm |
Z = 2 | |
Data collection top
Rigaku R-AXIS RAPID diffractometer | 2452 independent reflections |
Radiation source: fine-focus sealed tube | 2312 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.020 |
Detector resolution: 10 pixels mm-1 | θmax = 27.6°, θmin = 3.2° |
ω scans | h = −16→15 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −16→16 |
Tmin = 0.736, Tmax = 0.865 | l = −8→8 |
10160 measured reflections | |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.027 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.080 | w = 1/[σ2(Fo2) + (0.0539P)2 + 0.226P] where P = (Fo2 + 2Fc2)/3 |
S = 1.04 | (Δ/σ)max < 0.001 |
2452 reflections | Δρmax = 0.25 e Å−3 |
167 parameters | Δρmin = −0.41 e Å−3 |
12 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.049 (3) |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Co1 | 0.0000 | 0.5000 | 0.0000 | 0.0259 (1) | |
O1 | 0.25714 (8) | 0.79061 (7) | 0.5950 (2) | 0.0366 (2) | |
O2 | 0.10209 (7) | 0.69885 (7) | 0.5411 (1) | 0.0343 (2) | |
O3 | 0.71376 (8) | 0.61956 (9) | 0.6743 (2) | 0.0443 (3) | |
O1W | −0.02889 (8) | 0.56991 (9) | 0.2653 (2) | 0.0421 (3) | |
H1W1 | −0.0891 (9) | 0.599 (2) | 0.273 (3) | 0.063* | |
H1W2 | 0.021 (1) | 0.602 (2) | 0.342 (3) | 0.063* | |
O2W | 0.16756 (9) | 0.51828 (8) | 0.0752 (2) | 0.0398 (3) | |
H2W1 | 0.200 (1) | 0.5769 (8) | 0.090 (3) | 0.060* | |
H2W2 | 0.208 (2) | 0.473 (1) | 0.141 (3) | 0.060* | |
O3W | 0.01462 (8) | 0.35625 (7) | 0.1444 (1) | 0.0346 (2) | |
H3W1 | −0.011 (1) | 0.361 (2) | 0.256 (2) | 0.052* | |
H3W2 | −0.022 (1) | 0.309 (1) | 0.076 (2) | 0.052* | |
O4W | 0.2182 (1) | 0.1669 (1) | 0.1906 (2) | 0.0611 (4) | |
H4W1 | 0.224 (2) | 0.153 (2) | 0.068 (2) | 0.092* | |
H4W2 | 0.222 (2) | 0.2334 (8) | 0.200 (4) | 0.092* | |
N1 | 0.38275 (9) | 0.61391 (8) | 0.6406 (2) | 0.0310 (2) | |
C1 | 0.20418 (1) | 0.70853 (9) | 0.5826 (2) | 0.0272 (2) | |
C2 | 0.2639 (1) | 0.6051 (1) | 0.6221 (2) | 0.0336 (3) | |
H2A | 0.2450 | 0.5752 | 0.7442 | 0.040* | |
H2B | 0.2387 | 0.5574 | 0.5138 | 0.040* | |
C3 | 0.4297 (1) | 0.63152 (1) | 0.4757 (2) | 0.0356 (3) | |
H3 | 0.3853 | 0.6411 | 0.3537 | 0.043* | |
C4 | 0.5392 (1) | 0.6357 (1) | 0.4824 (2) | 0.0356 (3) | |
H4 | 0.5685 | 0.6483 | 0.3657 | 0.043* | |
C5 | 0.6103 (1) | 0.6210 (1) | 0.6651 (2) | 0.0328 (3) | |
C6 | 0.5576 (1) | 0.6080 (1) | 0.8362 (2) | 0.0388 (3) | |
H6 | 0.5994 | 0.6017 | 0.9615 | 0.047* | |
C7 | 0.4472 (1) | 0.6048 (1) | 0.8192 (2) | 0.0376 (3) | |
H7 | 0.4148 | 0.5960 | 0.9337 | 0.045* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0248 (2) | 0.0230 (2) | 0.0288 (2) | −0.00195 (7) | 0.0003 (1) | −0.00062 (7) |
O1 | 0.0325 (5) | 0.0265 (4) | 0.0488 (6) | 0.0015 (4) | −0.0008 (4) | −0.0020 (4) |
O2 | 0.0263 (4) | 0.0345 (5) | 0.0410 (5) | 0.0028 (3) | 0.0007 (4) | 0.0009 (4) |
O3 | 0.0285 (5) | 0.0480 (6) | 0.0549 (6) | 0.0036 (4) | 0.0006 (4) | 0.0087 (5) |
O1W | 0.0367 (5) | 0.0493 (6) | 0.0391 (5) | 0.0016 (5) | 0.0017 (4) | −0.0160 (5) |
O2W | 0.0271 (5) | 0.0306 (4) | 0.0576 (7) | −0.0049 (4) | −0.0076 (4) | 0.0069 (4) |
O3W | 0.0388 (5) | 0.0285 (4) | 0.0360 (5) | −0.0047 (4) | 0.0040 (4) | 0.0015 (4) |
O4W | 0.0639 (8) | 0.0507 (7) | 0.0756 (9) | −0.0129 (6) | 0.0326 (7) | −0.0082 (6) |
N1 | 0.0285 (5) | 0.0279 (5) | 0.0361 (6) | 0.0060 (4) | 0.0028 (4) | 0.0031 (4) |
C1 | 0.0290 (6) | 0.0275 (6) | 0.0247 (5) | 0.0034 (4) | 0.0027 (4) | −0.0018 (4) |
C2 | 0.0290 (6) | 0.0266 (6) | 0.0451 (7) | 0.0025 (5) | 0.0055 (5) | 0.0028 (5) |
C3 | 0.0348 (7) | 0.0366 (7) | 0.0339 (6) | 0.0053 (5) | 0.0000 (5) | 0.0066 (5) |
C4 | 0.0347 (7) | 0.0368 (7) | 0.0355 (7) | 0.0039 (6) | 0.0057 (5) | 0.0076 (5) |
C5 | 0.0309 (6) | 0.0253 (6) | 0.0410 (7) | 0.0036 (5) | 0.0009 (5) | 0.0024 (5) |
C6 | 0.0374 (7) | 0.0445 (8) | 0.0322 (6) | 0.0055 (6) | −0.0027 (5) | 0.0004 (5) |
C7 | 0.0403 (7) | 0.0408 (7) | 0.0318 (6) | 0.0072 (6) | 0.0057 (5) | 0.0020 (5) |
Geometric parameters (Å, º) top
Co1—O1W | 2.084 (1) | O3W—H3W2 | 0.852 (9) |
Co1—O2W | 2.077 (1) | O4W—H4W1 | 0.865 (9) |
Co1—O3W | 2.081 (1) | O4W—H4W2 | 0.855 (9) |
O1—C1 | 1.236 (2) | N1—C3 | 1.351 (2) |
O2—C1 | 1.261 (2) | N1—C7 | 1.352 (2) |
O3—C5 | 1.274 (2) | N1—C2 | 1.464 (2) |
C3—C4 | 1.352 (2) | C1—C2 | 1.522 (2) |
C6—C7 | 1.357 (2) | C2—H2A | 0.97 |
Co1—O1Wi | 2.084 (1) | C2—H2B | 0.97 |
Co1—O2Wi | 2.077 (1) | C3—H3 | 0.93 |
Co1—O3Wi | 2.081 (1) | C4—C5 | 1.421 (2) |
O1W—H1W1 | 0.845 (9) | C4—H4 | 0.93 |
O1W—H1W2 | 0.852 (19) | C5—C6 | 1.420 (2) |
O2W—H2W1 | 0.850 (9) | C6—H6 | 0.93 |
O2W—H2W2 | 0.849 (19) | C7—H7 | 0.93 |
O3W—H3W1 | 0.859 (9) | | |
| | | |
O2W—Co1—O1W | 91.84 (5) | O1—C1—O2 | 127.2 (1) |
O2W—Co1—O1Wi | 88.16 (5) | O1—C1—C2 | 119.3 (1) |
O2W—Co1—O3W | 88.27 (4) | O2—C1—C2 | 113.5 (1) |
O2W—Co1—O3Wi | 91.74 (4) | O3—C5—C6 | 122.6 (1) |
O3W—Co1—O1W | 89.45 (4) | O3—C5—C4 | 122.4 (1) |
O3W—Co1—O1Wi | 90.55 (4) | N1—C2—H2A | 108.8 |
N1—C2—C1 | 113.9 (1) | N1—C2—H2B | 108.8 |
O1Wi—Co1—O1W | 180.00 (6) | N1—C3—C4 | 122.0 (1) |
O2Wi—Co1—O1Wi | 91.84 (5) | N1—C3—H3 | 119.0 |
O2Wi—Co1—O1W | 88.16 (5) | N1—C7—C6 | 121.9 (1) |
O2W—Co1—O2Wi | 180.00 (2) | N1—C7—H7 | 119.0 |
O2Wi—Co1—O3W | 91.73 (4) | C1—C2—H2A | 108.8 |
O2Wi—Co1—O3Wi | 88.27 (4) | C1—C2—H2B | 108.8 |
O3Wi—Co1—O1Wi | 89.45 (4) | C3—N1—C2 | 119.5 (1) |
O3Wi—Co1—O1W | 90.55 (4) | C3—N1—C7 | 118.9 (1) |
O3W—Co1—O3Wi | 180.00 (2) | C3—C4—C5 | 121.0 (1) |
Co1—O1W—H1W1 | 121 (1) | C3—C4—H4 | 119.5 |
Co1—O1W—H1W2 | 122 (1) | C4—C3—H3 | 119.0 |
H1W1—O1W—H1W2 | 109 (1) | C5—C4—H4 | 119.5 |
Co1—O2W—H2W1 | 124 (1) | C5—C6—H6 | 119.6 |
Co1—O2W—H2W2 | 122 (1) | C6—C5—C4 | 115.1 (1) |
H2W1—O2W—H2W2 | 109 (1) | C6—C7—H7 | 119.0 |
Co1—O3W—H3W1 | 109 (1) | C7—N1—C2 | 121.6 (1) |
Co1—O3W—H3W2 | 112 (1) | C7—C6—C5 | 120.9 (1) |
H3W1—O3W—H3W2 | 107 (1) | C7—C6—H6 | 119.6 |
H4W1—O4W—H4W2 | 106 (1) | H2A—C2—H2B | 107.7 |
| | | |
O1—C1—C2—N1 | −9.3 (2) | C3—N1—C7—C6 | −3.1 (2) |
O2—C1—C2—N1 | 171.3 (1) | C3—C4—C5—O3 | 176.6 (1) |
O3—C5—C6—C7 | −176.7 (1) | C3—C4—C5—C6 | −3.4 (2) |
N1—C3—C4—C5 | 0.4 (2) | C4—C5—C6—C7 | 3.3 (2) |
C2—N1—C3—C4 | −177.0 (1) | C5—C6—C7—N1 | −0.2 (2) |
C2—N1—C7—C6 | 176.9 (1) | C7—N1—C2—C1 | 107.0 (1) |
C3—N1—C2—C1 | −73.1 (2) | C7—N1—C3—C4 | 3.0 (2) |
Symmetry code: (i) −x, −y+1, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W2···O2 | 0.85 (2) | 1.99 (1) | 2.821 (2) | 164 (2) |
O1W—H1W1···O4Wii | 0.85 (1) | 1.87 (1) | 2.709 (2) | 176 (2) |
O2W—H2W1···O1iii | 0.85 (1) | 1.84 (1) | 2.684 (2) | 173 (2) |
O2W—H2W2···O3iv | 0.85 (2) | 1.88 (1) | 2.725 (2) | 170 (2) |
O3W—H3W1···O2v | 0.86 (1) | 2.06 (1) | 2.832 (2) | 150 (2) |
O3W—H3W2···O2vi | 0.85 (1) | 1.84 (1) | 2.684 (1) | 173 (2) |
O4W—H4W1···O3vii | 0.87 (1) | 1.95 (1) | 2.790 (2) | 162 (2) |
O4W—H4W2···O3iv | 0.86 (1) | 2.17 (1) | 2.969 (2) | 155 (2) |
Symmetry codes: (ii) −x, y+1/2, −z+1/2; (iii) x, −y+3/2, z−1/2; (iv) −x+1, −y+1, −z+1; (v) −x, −y+1, −z+1; (vi) −x, y−1/2, −z+1/2; (vii) −x+1, y−1/2, −z+1/2. |