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The title complex, tetraaquabis[(2-oxo-1,2-dihydropyridin-1-yl)acetato]magnesium(II), [Mg(C
7H
6NO
3)
2(H
2O)
4], is a neutral mononuclear molecule consisting of an Mg
II ion, two (2-oxo-4
H-pyridin-1-yl)acetate ligands and four coordinated water molecules. The Mg
II atom, located on a symmetry center, has octahedral coordination involving two carbonyl O atoms of different (2-oxo-4
H-pyridin-1-yl)acetate ligands and four water molecules. O—H
O intermolecular hydrogen bonds form a layer structure.
Supporting information
CCDC reference: 239089
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.003 Å
- R factor = 0.043
- wR factor = 0.120
- Data-to-parameter ratio = 15.1
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ?
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mg1 - O2W .. 5.01 su
PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... O3
PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... Mg1
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 4
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
5 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
3 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 & Rigaku, 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.
Tetraaquabis[(2-oxo-1,2-dihydropyridin-1-yl)acetato]magnesium(II)
top
Crystal data top
[Mg(C7H6NO3)2(H2O)4] | F(000) = 420 |
Mr = 400.63 | Dx = 1.486 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 5735 reflections |
a = 10.550 (2) Å | θ = 3.3–27.4° |
b = 7.099 (1) Å | µ = 0.16 mm−1 |
c = 13.056 (3) Å | T = 293 K |
β = 113.70 (3)° | Prism, colorless |
V = 895.3 (4) Å3 | 0.38 × 0.24 × 0.20 mm |
Z = 2 | |
Data collection top
Rigaku R-AXIS RAPID diffractometer | 2054 independent reflections |
Radiation source: fine-focus sealed tube | 1839 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.029 |
Detector resolution: 10 pixels mm-1 | θmax = 27.5°, θmin = 3.2° |
ω scan | h = −13→13 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −8→9 |
Tmin = 0.943, Tmax = 0.969 | l = −16→16 |
8176 measured reflections | |
Refinement top
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)] = 0.043 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.120 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.06 | w = 1/[σ2(Fo2) + (0.0672P)2 + 0.2876P] where P = (Fo2 + 2Fc2)/3 |
2054 reflections | (Δ/σ)max < 0.001 |
136 parameters | Δρmax = 0.35 e Å−3 |
6 restraints | Δρmin = −0.27 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Mg1 | 0.0000 | 0.0000 | 0.5000 | 0.0283 (2) | |
O1 | −0.0858 (1) | 0.5007 (2) | 0.64772 (9) | 0.0400 (3) | |
O2 | −0.2552 (1) | 0.5467 (2) | 0.47913 (9) | 0.0393 (3) | |
O3 | −0.1848 (1) | 0.0986 (2) | 0.4904 (1) | 0.0534 (4) | |
O1W | −0.0222 (2) | 0.1439 (2) | 0.3568 (1) | 0.0562 (4) | |
O2W | −0.0941 (1) | −0.2399 (2) | 0.40636 (9) | 0.0359 (3) | |
N1 | −0.3797 (1) | 0.2160 (2) | 0.4944 (1) | 0.0313 (3) | |
C1 | −0.3133 (2) | 0.1091 (2) | 0.4429 (1) | 0.0353 (3) | |
C2 | −0.3995 (2) | 0.0214 (3) | 0.3404 (2) | 0.0456 (4) | |
C3 | −0.5392 (2) | 0.0442 (3) | 0.2976 (2) | 0.0528 (5) | |
C4 | −0.6016 (2) | 0.1527 (3) | 0.3544 (2) | 0.0501 (5) | |
C5 | −0.5201 (2) | 0.2352 (2) | 0.4519 (2) | 0.0398 (4) | |
C6 | −0.2900 (2) | 0.3130 (2) | 0.5961 (1) | 0.0364 (3) | |
C7 | −0.2030 (2) | 0.4663 (2) | 0.5708 (1) | 0.0312 (3) | |
H2 | −0.3598 | −0.0523 | 0.3023 | 0.055* | |
H3 | −0.5940 | −0.0127 | 0.2301 | 0.063* | |
H4 | −0.6972 | 0.1675 | 0.3254 | 0.060* | |
H5 | −0.5604 | 0.3062 | 0.4907 | 0.048* | |
H1W1 | 0.016 (3) | 0.251 (2) | 0.359 (2) | 0.084* | |
H1W2 | −0.039 (3) | 0.093 (3) | 0.293 (1) | 0.084* | |
H2W1 | −0.042 (2) | −0.314 (2) | 0.390 (2) | 0.054* | |
H2W2 | −0.146 (2) | −0.304 (3) | 0.430 (2) | 0.054* | |
H6A | −0.2287 | 0.2225 | 0.6483 | 0.044* | |
H6B | −0.3461 | 0.3705 | 0.6311 | 0.044* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Mg1 | 0.0280 (3) | 0.0269 (3) | 0.0302 (3) | 0.0002 (2) | 0.0119 (3) | −0.0014 (2) |
O1 | 0.0443 (6) | 0.0347 (6) | 0.0348 (6) | −0.0063 (4) | 0.0095 (5) | 0.0005 (4) |
O2 | 0.0382 (6) | 0.0396 (6) | 0.0382 (6) | −0.0012 (4) | 0.0134 (5) | 0.0080 (5) |
O3 | 0.0321 (6) | 0.0529 (8) | 0.0748 (9) | 0.0030 (5) | 0.0210 (6) | −0.0175 (7) |
O1W | 0.094 (1) | 0.0389 (7) | 0.0329 (6) | −0.0205 (7) | 0.0224 (6) | −0.0034 (5) |
O2W | 0.0363 (5) | 0.0319 (5) | 0.0419 (6) | −0.0038 (4) | 0.0182 (5) | −0.0053 (4) |
N1 | 0.0304 (6) | 0.0276 (6) | 0.0369 (6) | 0.0009 (4) | 0.0146 (5) | 0.0016 (5) |
C1 | 0.0334 (7) | 0.0308 (7) | 0.0433 (8) | 0.0008 (6) | 0.0171 (6) | −0.0015 (6) |
C2 | 0.058 (1) | 0.0387 (8) | 0.0423 (9) | −0.0058 (7) | 0.0217 (8) | −0.0067 (7) |
C3 | 0.058 (1) | 0.0445 (9) | 0.0398 (9) | −0.0131 (8) | 0.0030 (8) | 0.0024 (8) |
C4 | 0.0299 (7) | 0.0453 (9) | 0.062 (1) | −0.0009 (7) | 0.0052 (7) | 0.0149 (8) |
C5 | 0.0333 (7) | 0.0315 (7) | 0.058 (1) | 0.0047 (6) | 0.0215 (7) | 0.0096 (7) |
C6 | 0.0434 (8) | 0.0325 (7) | 0.0351 (7) | −0.0032 (6) | 0.0178 (6) | 0.0002 (6) |
C7 | 0.0358 (7) | 0.0257 (6) | 0.0341 (7) | 0.0026 (5) | 0.0161 (6) | −0.0019 (5) |
Geometric parameters (Å, º) top
Mg1—O1W | 2.060 (1) | O2—C7 | 1.238 (2) |
Mg1—O2W | 2.099 (1) | N1—C5 | 1.364 (2) |
Mg1—O3 | 2.027 (1) | N1—C1 | 1.378 (2) |
O3—C1 | 1.246 (2) | N1—C6 | 1.457 (2) |
C2—C3 | 1.360 (3) | C1—C2 | 1.423 (2) |
C4—C5 | 1.351 (3) | C2—H2 | 0.93 |
Mg1—O1Wi | 2.060 (1) | C3—C4 | 1.402 (3) |
Mg1—O2Wi | 2.099 (1) | C3—H3 | 0.93 |
Mg1—O3i | 2.027 (1) | C4—H4 | 0.93 |
O1W—H1W1 | 0.86 (2) | C5—H5 | 0.93 |
O1W—H1W2 | 0.86 (2) | C6—C7 | 1.542 (2) |
O2W—H2W1 | 0.86 (2) | C6—H6A | 0.97 |
O2W—H2W2 | 0.86 (2) | C6—H6B | 0.97 |
O1—C7 | 1.265 (2) | | |
| | | |
O3—Mg1—O1W | 90.97 (7) | N1—C1—C2 | 116.2 (1) |
O3—Mg1—O1Wi | 89.03 (7) | N1—C5—H5 | 119.5 |
O3—Mg1—O2Wi | 88.51 (5) | N1—C6—H6A | 109.4 |
O3—Mg1—O2W | 91.49 (5) | N1—C6—H6B | 109.4 |
O1W—Mg1—O2W | 91.08 (5) | C1—O3—Mg1 | 151.5 (1) |
O1W—Mg1—O2Wi | 88.92 (5) | C1—N1—C6 | 115.7 (1) |
N1—C6—C7 | 111.3 (1) | C1—C2—H2 | 119.6 |
O3i—Mg1—O3 | 180.0 | C2—C3—C4 | 120.6 (2) |
O3i—Mg1—O1W | 89.03 (7) | C2—C3—H3 | 119.7 |
O3i—Mg1—O1Wi | 90.97 (7) | C3—C2—C1 | 120.8 (2) |
O3i—Mg1—O2Wi | 91.49 (5) | C3—C2—H2 | 119.6 |
O3i—Mg1—O2W | 88.51 (5) | C3—C4—H4 | 120.6 |
O1W—Mg1—O1Wi | 180.0 | C4—C3—H3 | 119.7 |
O1Wi—Mg1—O2W | 88.92 (5) | C4—C5—N1 | 121.0 (2) |
O1Wi—Mg1—O2Wi | 91.08 (5) | C4—C5—H5 | 119.5 |
O2W—Mg1—O2Wi | 180.00 (3) | C5—N1—C1 | 122.6 (1) |
Mg1—O1W—H1W1 | 122 (2) | C5—N1—C6 | 121.7 (1) |
Mg1—O1W—H1W2 | 125 (2) | C5—C4—C3 | 118.8 (2) |
Mg1—O2W—H2W1 | 117 (1) | C5—C4—H4 | 120.6 |
Mg1—O2W—H2W2 | 116 (1) | C7—C6—H6A | 109.4 |
O1—C7—C6 | 116.3 (1) | C7—C6—H6B | 109.4 |
O2—C7—O1 | 126.3 (1) | H1W1—O1W—H1W2 | 109 (1) |
O2—C7—C6 | 117.4 (1) | H2W1—O2W—H2W2 | 110 (1) |
O3—C1—N1 | 117.1 (1) | H6A—C6—H6B | 108.0 |
O3—C1—C2 | 126.7 (2) | | |
| | | |
Mg1—O3—C1—N1 | 178.2 (2) | C1—C2—C3—C4 | −0.8 (3) |
Mg1—O3—C1—C2 | −1.6 (4) | C1—N1—C5—C4 | −1.7 (2) |
O3—C1—C2—C3 | 179.8 (2) | C2—C3—C4—C5 | 0.5 (3) |
O1W—Mg1—O3—C1 | 65.2 (3) | C3—C4—C5—N1 | 0.8 (2) |
O1Wi—Mg1—O3—C1 | −114.8 (3) | C5—N1—C1—O3 | −178.6 (1) |
O2W—Mg1—O3—C1 | −25.9 (3) | C5—N1—C6—C7 | −111.8 (1) |
O2Wi—Mg1—O3—C1 | 154.1 (3) | C5—N1—C1—C2 | 1.2 (2) |
N1—C6—C7—O2 | 31.6 (2) | C6—N1—C1—C2 | −176.9 (1) |
N1—C6—C7—O1 | −150.0 (1) | C6—N1—C1—O3 | 3.2 (2) |
N1—C1—C2—C3 | 0.0 (2) | C6—N1—C5—C4 | 176.4 (1) |
C1—N1—C6—C7 | 66.39 (18) | | |
Symmetry code: (i) −x, −y, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W2···O1ii | 0.86 (2) | 1.88 (1) | 2.735 (2) | 175 (3) |
O1W—H1W1···O1iii | 0.86 (2) | 1.93 (1) | 2.779 (2) | 175 (3) |
O2W—H2W2···O2iv | 0.86 (2) | 1.86 (1) | 2.717 (2) | 177 (2) |
O2W—H2W1···O1i | 0.86 (2) | 2.09 (2) | 2.933 (2) | 179 (2) |
Symmetry codes: (i) −x, −y, −z+1; (ii) x, −y+1/2, z−1/2; (iii) −x, −y+1, −z+1; (iv) x, y−1, z. |
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