In the title compound, [Mg(H
2O)
6](C
7H
6NO
3)
2·2H
2O, the Mg
II atom lies on a centre of symmetry and is coordinated by six water molecules in an octahedral geometry. A three-dimensional supramolecular framework is formed
via O—H
O hydrogen bonds between the anions and cations.
Supporting information
CCDC reference: 259090
Key indicators
- Single-crystal X-ray study
- T = 296 K
- Mean (C-C) = 0.004 Å
- R factor = 0.055
- wR factor = 0.177
- Data-to-parameter ratio = 14.9
checkCIF/PLATON results
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Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
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
1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
0 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.
Hexaaquamagnesium(II) bis[(4-oxo-4
H-pyridin-1-yl)acetate] dihydrate
top
Crystal data top
[Mg(H2O)6](C7H6NO3)2·2H2O | F(000) = 500 |
Mr = 472.69 | Dx = 1.449 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 9023 reflections |
a = 12.486 (3) Å | θ = 3.2–27.5° |
b = 12.904 (3) Å | µ = 0.16 mm−1 |
c = 6.8131 (14) Å | T = 296 K |
β = 99.21 (3)° | Prism, colourless |
V = 1083.6 (4) Å3 | 0.38 × 0.26 × 0.17 mm |
Z = 2 | |
Data collection top
Rigaku RAXIS-RAPID diffractometer | 2477 independent reflections |
Radiation source: fine-focus sealed tube | 2212 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.022 |
Detector resolution: 10 pixels mm-1 | θmax = 27.5°, θmin = 3.2° |
ω scans | h = −16→16 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −16→16 |
Tmin = 0.953, Tmax = 0.974 | l = −8→8 |
9164 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)] = 0.055 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.177 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.08 | w = 1/[σ2(Fo2) + (0.0802P)2 + 1.5072P] where P = (Fo2 + 2Fc2)/3 |
2477 reflections | (Δ/σ)max < 0.001 |
166 parameters | Δρmax = 0.39 e Å−3 |
12 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 | 0.5000 | 0.5000 | 0.5000 | 0.0267 (3) | |
O1 | 0.60425 (14) | 0.69911 (14) | 0.0391 (3) | 0.0348 (4) | |
O1W | 0.47098 (16) | 0.57432 (17) | 0.7562 (3) | 0.0423 (5) | |
H1W2 | 0.5206 (18) | 0.607 (3) | 0.830 (5) | 0.063* | |
H1W1 | 0.4092 (12) | 0.597 (3) | 0.772 (6) | 0.063* | |
O2W | 0.50916 (16) | 0.35966 (14) | 0.6474 (3) | 0.0354 (4) | |
H2W2 | 0.486 (3) | 0.3068 (19) | 0.579 (4) | 0.053* | |
H2W1 | 0.481 (3) | 0.362 (3) | 0.753 (3) | 0.053* | |
O2 | 0.75820 (15) | 0.79120 (14) | 0.0894 (3) | 0.0367 (5) | |
O3W | 0.66402 (15) | 0.51860 (15) | 0.5824 (3) | 0.0389 (5) | |
H3W2 | 0.702 (2) | 0.4714 (18) | 0.645 (5) | 0.058* | |
H3W1 | 0.698 (2) | 0.5751 (14) | 0.587 (6) | 0.058* | |
O3 | 1.21238 (15) | 0.62126 (17) | 0.1734 (3) | 0.0454 (5) | |
O4W | 0.2800 (2) | 0.6657 (2) | 0.8086 (4) | 0.0634 (7) | |
H4W2 | 0.273 (4) | 0.657 (3) | 0.930 (3) | 0.095* | |
H4W1 | 0.279 (4) | 0.7305 (11) | 0.783 (6) | 0.095* | |
N1 | 0.88334 (17) | 0.61402 (16) | 0.1406 (3) | 0.0308 (5) | |
C1 | 0.9483 (2) | 0.6049 (2) | 0.3185 (4) | 0.0381 (6) | |
H1 | 0.9170 | 0.5960 | 0.4322 | 0.046* | |
C2 | 1.0577 (2) | 0.6085 (2) | 0.3358 (4) | 0.0395 (6) | |
H2 | 1.0999 | 0.6023 | 0.4608 | 0.047* | |
C3 | 1.1098 (2) | 0.62184 (19) | 0.1643 (4) | 0.0325 (5) | |
C4 | 1.0376 (2) | 0.6355 (2) | −0.0185 (4) | 0.0351 (6) | |
H4 | 1.0656 | 0.6471 | −0.1351 | 0.042* | |
C5 | 0.9286 (2) | 0.6316 (2) | −0.0240 (4) | 0.0358 (6) | |
H5 | 0.8835 | 0.6413 | −0.1451 | 0.043* | |
C6 | 0.7654 (2) | 0.6055 (2) | 0.1220 (4) | 0.0346 (6) | |
H6A | 0.7474 | 0.5768 | 0.2443 | 0.041* | |
H6B | 0.7396 | 0.5574 | 0.0155 | 0.041* | |
C7 | 0.70524 (19) | 0.70910 (18) | 0.0793 (3) | 0.0267 (5) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Mg1 | 0.0231 (5) | 0.0242 (5) | 0.0315 (6) | −0.0028 (4) | 0.0007 (4) | −0.0008 (4) |
O1 | 0.0250 (8) | 0.0356 (10) | 0.0422 (10) | 0.0025 (7) | 0.0005 (7) | 0.0004 (8) |
O1W | 0.0336 (10) | 0.0495 (12) | 0.0426 (11) | 0.0005 (9) | 0.0025 (8) | −0.0166 (9) |
O2W | 0.0386 (10) | 0.0302 (9) | 0.0367 (10) | −0.0047 (7) | 0.0043 (8) | 0.0024 (7) |
O2 | 0.0320 (9) | 0.0258 (9) | 0.0505 (11) | 0.0020 (7) | 0.0011 (8) | −0.0021 (8) |
O3W | 0.0262 (9) | 0.0307 (9) | 0.0561 (12) | −0.0036 (7) | −0.0049 (8) | 0.0067 (9) |
O3 | 0.0287 (9) | 0.0491 (12) | 0.0562 (13) | 0.0039 (8) | 0.0003 (9) | 0.0093 (10) |
O4W | 0.0622 (15) | 0.0567 (15) | 0.0784 (18) | 0.0162 (13) | 0.0325 (14) | 0.0099 (13) |
N1 | 0.0293 (10) | 0.0270 (10) | 0.0360 (11) | 0.0068 (8) | 0.0052 (9) | 0.0035 (8) |
C1 | 0.0382 (14) | 0.0410 (14) | 0.0351 (13) | 0.0080 (11) | 0.0058 (11) | 0.0024 (11) |
C2 | 0.0375 (14) | 0.0453 (15) | 0.0328 (13) | 0.0058 (12) | −0.0030 (11) | −0.0003 (11) |
C3 | 0.0304 (12) | 0.0244 (11) | 0.0413 (14) | 0.0047 (9) | 0.0019 (10) | 0.0022 (10) |
C4 | 0.0325 (13) | 0.0378 (14) | 0.0354 (13) | 0.0040 (10) | 0.0067 (10) | 0.0077 (11) |
C5 | 0.0360 (13) | 0.0383 (14) | 0.0313 (13) | 0.0049 (11) | 0.0000 (10) | 0.0060 (10) |
C6 | 0.0281 (12) | 0.0285 (12) | 0.0466 (15) | 0.0023 (9) | 0.0045 (10) | 0.0031 (11) |
C7 | 0.0283 (11) | 0.0266 (11) | 0.0249 (10) | 0.0022 (9) | 0.0034 (8) | −0.0009 (9) |
Geometric parameters (Å, º) top
Mg1—O1W | 2.0735 (19) | O3W—H3W1 | 0.84 (3) |
Mg1—O2W | 2.0652 (19) | O4W—H4W2 | 0.85 (3) |
Mg1—O3W | 2.0490 (18) | O4W—H4W1 | 0.85 (3) |
O1—C7 | 1.253 (3) | N1—C1 | 1.351 (4) |
O2—C7 | 1.245 (3) | N1—C5 | 1.353 (3) |
O3—C3 | 1.272 (3) | N1—C6 | 1.462 (3) |
C1—C2 | 1.353 (4) | C1—H1 | 0.9300 |
C4—C5 | 1.356 (4) | C2—C3 | 1.435 (4) |
Mg1—O1Wi | 2.0735 (19) | C2—H2 | 0.9300 |
Mg1—O2Wi | 2.0652 (19) | C3—C4 | 1.427 (4) |
Mg1—O3Wi | 2.0490 (18) | C4—H4 | 0.9300 |
O1W—H1W2 | 0.85 (3) | C5—H5 | 0.9300 |
O1W—H1W1 | 0.85 (3) | C6—C7 | 1.538 (3) |
O2W—H2W2 | 0.85 (3) | C6—H6A | 0.9700 |
O2W—H2W1 | 0.85 (3) | C6—H6B | 0.9700 |
O3W—H3W2 | 0.85 (3) | | |
| | | |
O2W—Mg1—O1W | 89.98 (9) | O1—C7—C6 | 113.3 (2) |
O2W—Mg1—O1Wi | 90.02 (9) | O2—C7—O1 | 127.3 (2) |
O3W—Mg1—O1W | 90.97 (9) | O2—C7—C6 | 119.4 (2) |
O3W—Mg1—O1Wi | 89.03 (9) | O3—C3—C4 | 122.2 (3) |
O3W—Mg1—O2W | 89.68 (8) | O3—C3—C2 | 122.9 (3) |
O3W—Mg1—O2Wi | 90.32 (8) | N1—C1—C2 | 121.9 (3) |
N1—C6—C7 | 113.9 (2) | N1—C1—H1 | 119.1 |
O1W—Mg1—O1Wi | 180.00 (6) | N1—C5—C4 | 122.3 (2) |
O2Wi—Mg1—O1W | 90.02 (9) | N1—C5—H5 | 118.9 |
O2Wi—Mg1—O1Wi | 89.98 (9) | N1—C6—H6A | 108.8 |
O2W—Mg1—O2Wi | 180.0 | N1—C6—H6B | 108.8 |
O3Wi—Mg1—O1W | 89.03 (9) | C1—N1—C5 | 119.1 (2) |
O3Wi—Mg1—O1Wi | 90.97 (9) | C1—N1—C6 | 121.5 (2) |
O3Wi—Mg1—O2W | 90.32 (8) | C1—C2—C3 | 121.1 (3) |
O3Wi—Mg1—O2Wi | 89.68 (8) | C1—C2—H2 | 119.5 |
O3W—Mg1—O3Wi | 180.00 (3) | C2—C1—H1 | 119.1 |
Mg1—O1W—H1W2 | 121 (2) | C3—C2—H2 | 119.5 |
Mg1—O1W—H1W1 | 123 (2) | C3—C4—H4 | 119.6 |
Mg1—O2W—H2W2 | 117 (2) | C4—C3—C2 | 114.8 (2) |
Mg1—O2W—H2W1 | 112 (2) | C4—C5—H5 | 118.9 |
Mg1—O3W—H3W2 | 121 (2) | C5—N1—C6 | 119.3 (2) |
Mg1—O3W—H3W1 | 126 (2) | C5—C4—C3 | 120.7 (2) |
H1W2—O1W—H1W1 | 110.5 (17) | C5—C4—H4 | 119.6 |
H2W2—O2W—H2W1 | 110.2 (16) | C7—C6—H6A | 108.8 |
H3W2—O3W—H3W1 | 111.1 (17) | C7—C6—H6B | 108.8 |
H4W2—O4W—H4W1 | 109 (4) | H6A—C6—H6B | 107.7 |
| | | |
C5—N1—C1—C2 | −2.8 (4) | C1—N1—C5—C4 | 3.2 (4) |
C6—N1—C1—C2 | 177.3 (3) | C6—N1—C5—C4 | −176.9 (2) |
N1—C1—C2—C3 | −0.3 (4) | C3—C4—C5—N1 | −0.5 (4) |
C1—C2—C3—O3 | −177.0 (3) | C1—N1—C6—C7 | 107.8 (3) |
C1—C2—C3—C4 | 2.8 (4) | C5—N1—C6—C7 | −72.1 (3) |
O3—C3—C4—C5 | 177.4 (3) | N1—C6—C7—O2 | −9.2 (3) |
C2—C3—C4—C5 | −2.4 (4) | N1—C6—C7—O1 | 171.6 (2) |
Symmetry code: (i) −x+1, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1w—H1w1···O4w | 0.85 (3) | 1.89 (3) | 2.734 (3) | 172 (4) |
O1w—H1w2···O1ii | 0.85 (3) | 2.01 (3) | 2.837 (3) | 164 (3) |
O2w—H2w2···O1iii | 0.85 (3) | 1.89 (3) | 2.709 (3) | 162 (3) |
O2w—H2w1···O1i | 0.85 (3) | 2.06 (3) | 2.847 (3) | 153 (3) |
O3w—H3w2···O3iv | 0.85 (3) | 1.92 (3) | 2.754 (3) | 170 (4) |
O3w—H3w1···O2v | 0.84 (3) | 1.88 (3) | 2.719 (3) | 173 (3) |
O4w—H4w2···O3vi | 0.85 (3) | 1.98 (3) | 2.809 (4) | 163 (5) |
O4w—H4w1···O3vii | 0.85 (3) | 2.17 (2) | 2.978 (4) | 158 (5) |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x, y, z+1; (iii) −x+1, y−1/2, −z+1/2; (iv) −x+2, −y+1, −z+1; (v) x, −y+3/2, z+1/2; (vi) x−1, y, z+1; (vii) x−1, −y+3/2, z+1/2. |