The title complex, [Mn(H
2O)
6](C
7H
6NO
3)
2·2H
2O, was synthesized by the reaction of MnCl
2·4H
2O and (4-oxo-4
H-pyrindin-1-yl)acetic acid in aqueous solution. The manganese(II) ion, which lies on a center of symmetry, is octahedrally coordinated by six water molecules [Mn—O = 2.166 (1)–2.177 (1) Å]. A three-dimensional supramolecular framework is formed
via O—H
O hydrogen bonds between the anions and cations.
Supporting information
CCDC reference: 262248
Key indicators
- Single-crystal X-ray study
- T = 296 K
- Mean (C-C) = 0.002 Å
- R factor = 0.032
- wR factor = 0.085
- Data-to-parameter ratio = 15.1
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mn1 - O3W .. 5.85 su
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 8
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2
C7 H6 N O3
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
4 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
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
2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: RAPID-AUTO (Rigaku Corporation, 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.
Hexaaquamanganese(II) bis[(4-oxo-4
H-pyridin-1-yl)acetate] dihydrate
top
Crystal data top
[Mn(H2O)6](C7H6NO3)2·2H2O | F(000) = 526 |
Mr = 503.32 | Dx = 1.517 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 10242 reflections |
a = 12.561 (3) Å | θ = 3.0–27.5° |
b = 12.949 (3) Å | µ = 0.67 mm−1 |
c = 6.855 (1) Å | T = 296 K |
β = 98.68 (3)° | Prism, colorless |
V = 1102.2 (4) Å3 | 0.39 × 0.26 × 0.19 mm |
Z = 2 | |
Data collection top
Rigaku R-AXIS RAPID diffractometer | 2509 independent reflections |
Radiation source: fine-focus sealed tube | 2273 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.024 |
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 = 0.780, Tmax = 0.883 | l = −8→8 |
10259 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)] = 0.032 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.085 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.04 | w1/[σ2(Fo2) + (0.047P)2 + 0.3365P] where P(Fo2 + 2Fc2)/3 |
2509 reflections | (Δ/σ)max < 0.001 |
166 parameters | Δρmax = 0.29 e Å−3 |
12 restraints | Δρmin = −0.34 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Mn1 | 0.0000 | 0.5000 | 0.0000 | 0.0313 (1) | |
O1W | −0.0296 (1) | 0.4260 (1) | 0.2719 (2) | 0.0498 (3) | |
H1W1 | −0.0906 (9) | 0.4004 (2) | 0.284 (3) | 0.075* | |
H1W2 | 0.019 (1) | 0.392 (2) | 0.345 (3) | 0.075* | |
O2W | 0.17244 (9) | 0.48079 (9) | 0.0791 (2) | 0.0475 (3) | |
H2W1 | 0.201 (2) | 0.4217 (9) | 0.089 (3) | 0.071* | |
H2W2 | 0.211 (2) | 0.525 (1) | 0.148 (3) | 0.071* | |
O3W | 0.01204 (9) | 0.64785 (8) | 0.1499 (2) | 0.0407 (3) | |
H3W1 | −0.023 (2) | 0.694 (1) | 0.077 (2) | 0.061* | |
H3W2 | −0.012 (2) | 0.648 (2) | 0.261 (2) | 0.061* | |
O4W | 0.2189 (1) | 0.8330 (1) | 0.1817 (3) | 0.0697 (4) | |
H4W1 | 0.219 (2) | 0.7675 (9) | 0.199 (4) | 0.105* | |
H4W2 | 0.223 (2) | 0.843 (2) | 0.058 (2) | 0.105* | |
O1 | −0.10557 (8) | 0.80018 (8) | −0.0420 (2) | 0.0389 (3) | |
O2 | −0.25982 (8) | 0.70991 (8) | −0.0938 (2) | 0.0412 (3) | |
O3 | −0.71104 (9) | 0.8799 (1) | −0.1775 (2) | 0.0498 (3) | |
N1 | −0.3831 (1) | 0.88615 (9) | −0.1402 (2) | 0.0354 (3) | |
C1 | −0.4464 (1) | 0.8955 (1) | −0.3168 (2) | 0.0417 (4) | |
H1 | −0.4143 | 0.9046 | −0.4293 | 0.050* | |
C2 | −0.5557 (1) | 0.8920 (1) | −0.3353 (3) | 0.0436 (4) | |
H2 | −0.5966 | 0.8983 | −0.4596 | 0.052* | |
C3 | −0.6084 (1) | 0.8788 (1) | −0.1665 (2) | 0.0372 (3) | |
C4 | −0.5383 (1) | 0.8642 (1) | 0.0143 (2) | 0.0402 (3) | |
H4 | −0.5673 | 0.8515 | 0.1291 | 0.048* | |
C5 | −0.4298 (1) | 0.8683 (1) | 0.0227 (2) | 0.0397 (3) | |
H5 | −0.3862 | 0.8587 | 0.1435 | 0.048* | |
C6 | −0.2652 (1) | 0.8942 (1) | −0.1207 (3) | 0.0387 (3) | |
H6A | −0.2400 | 0.9410 | −0.0131 | 0.046* | |
H6B | −0.2464 | 0.9240 | −0.2408 | 0.046* | |
C7 | −0.2068 (1) | 0.7911 (1) | −0.0822 (2) | 0.0315 (3) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Mn1 | 0.0289 (2) | 0.0276 (2) | 0.0359 (2) | 0.0024 (1) | 0.0006 (1) | 0.0003 (1) |
O1W | 0.0412 (6) | 0.0581 (8) | 0.0488 (7) | −0.0004 (5) | 0.0032 (5) | 0.0203 (6) |
O2W | 0.0328 (6) | 0.0345 (6) | 0.0698 (9) | 0.0051 (4) | −0.0100 (5) | −0.0081 (5) |
O3W | 0.0458 (6) | 0.0338 (6) | 0.0420 (6) | 0.0051 (4) | 0.0051 (5) | −0.0029 (5) |
O4W | 0.0714 (9) | 0.0580 (9) | 0.0874 (12) | 0.0149 (7) | 0.0364 (9) | 0.0105 (8) |
O1 | 0.0295 (5) | 0.0393 (6) | 0.0468 (6) | 0.0027 (4) | 0.0016 (4) | 0.0004 (5) |
O2 | 0.0359 (5) | 0.0300 (5) | 0.0555 (7) | 0.0016 (4) | −0.0001 (5) | −0.0020 (5) |
O3 | 0.0313 (6) | 0.0546 (7) | 0.0621 (8) | 0.0045 (5) | 0.0019 (5) | 0.0112 (6) |
N1 | 0.0322 (6) | 0.0312 (6) | 0.0422 (7) | 0.0066 (5) | 0.0036 (5) | 0.0034 (5) |
C1 | 0.0443 (8) | 0.0449 (8) | 0.0366 (8) | 0.0079 (7) | 0.0078 (6) | 0.0035 (6) |
C2 | 0.0424 (8) | 0.0490 (9) | 0.0370 (8) | 0.0065 (7) | −0.0024 (6) | 0.0015 (7) |
C3 | 0.0354 (7) | 0.0278 (7) | 0.0474 (9) | 0.0044 (5) | 0.0025 (6) | 0.0037 (6) |
C4 | 0.0394 (8) | 0.0408 (8) | 0.0410 (8) | 0.0048 (6) | 0.0080 (6) | 0.0078 (7) |
C5 | 0.0393 (8) | 0.0411 (8) | 0.0372 (8) | 0.0060 (6) | 0.0006 (6) | 0.0075 (6) |
C6 | 0.0315 (7) | 0.0322 (7) | 0.0523 (9) | 0.0034 (6) | 0.0059 (6) | 0.0026 (6) |
C7 | 0.0325 (7) | 0.0323 (7) | 0.0290 (7) | 0.0037 (5) | 0.0027 (5) | −0.0013 (5) |
Geometric parameters (Å, º) top
Mn1—O1W | 2.177 (1) | O3W—H3W2 | 0.86 (2) |
Mn1—O2W | 2.166 (1) | O4W—H4W1 | 0.86 (2) |
Mn1—O3W | 2.167 (1) | O4W—H4W2 | 0.86 (2) |
O1—C7 | 1.265 (2) | N1—C1 | 1.350 (2) |
O2—C7 | 1.241 (2) | N1—C5 | 1.358 (2) |
O3—C3 | 1.280 (2) | N1—C6 | 1.471 (2) |
C1—C2 | 1.360 (2) | C1—H1 | 0.9300 |
C4—C5 | 1.356 (2) | C2—C3 | 1.427 (2) |
Mn1—O1Wi | 2.177 (1) | C2—H2 | 0.9300 |
Mn1—O2Wi | 2.166 (1) | C3—C4 | 1.421 (2) |
Mn1—O3Wi | 2.167 (1) | C4—H4 | 0.9300 |
O1W—H1W1 | 0.85 (2) | C5—H5 | 0.9300 |
O1W—H1W2 | 0.85 (2) | C6—C7 | 1.527 (2) |
O2W—H2W1 | 0.84 (2) | C6—H6A | 0.9700 |
O2W—H2W2 | 0.85 (2) | C6—H6B | 0.9700 |
O3W—H3W1 | 0.86 (2) | | |
| | | |
O2W—Mn1—O1W | 91.64 (6) | O1—C7—C6 | 113.4 (1) |
O2W—Mn1—O1Wi | 88.36 (6) | O2—C7—O1 | 127.2 (1) |
O2W—Mn1—O3W | 89.27 (5) | O2—C7—C6 | 119.4 (1) |
O2W—Mn1—O3Wi | 90.73 (5) | O3—C3—C2 | 122.5 (2) |
O3W—Mn1—O1W | 89.51 (5) | O3—C3—C4 | 122.6 (2) |
O3W—Mn1—O1Wi | 90.49 (5) | N1—C1—H1 | 119.0 |
N1—C6—C7 | 113.9 (1) | N1—C1—C2 | 122.0 (2) |
O1W—Mn1—O1Wi | 180.00 (6) | N1—C5—H5 | 119.1 |
O2Wi—Mn1—O1W | 88.36 (6) | N1—C6—H6A | 108.8 |
O2Wi—Mn1—O1Wi | 91.64 (6) | N1—C6—H6B | 108.8 |
O2Wi—Mn1—O2W | 180.00 (6) | C1—N1—C5 | 118.9 (1) |
O2Wi—Mn1—O3Wi | 89.27 (5) | C1—N1—C6 | 121.6 (1) |
O2Wi—Mn1—O3W | 90.73 (5) | C1—C2—H2 | 119.5 |
O3Wi—Mn1—O1W | 90.49 (5) | C1—C2—C3 | 120.9 (2) |
O3Wi—Mn1—O1Wi | 89.51 (5) | C2—C1—H1 | 119.0 |
O3Wi—Mn1—O3W | 180.00 (6) | C3—C2—H2 | 119.5 |
Mn1—O1W—H1W1 | 122 (2) | C3—C4—H4 | 119.4 |
Mn1—O1W—H1W2 | 122 (2) | C4—C3—C2 | 114.9 (1) |
Mn1—O2W—H2W1 | 122 (1) | C4—C5—N1 | 121.9 (2) |
Mn1—O2W—H2W2 | 122 (2) | C4—C5—H5 | 119.1 |
Mn1—O3W—H3W1 | 110.3 (9) | C5—N1—C6 | 119.5 (1) |
Mn1—O3W—H3W2 | 114 (2) | C5—C4—C3 | 121.2 (2) |
H1W1—O1W—H1W2 | 109 (1) | C5—C4—H4 | 119.4 |
H2W1—O2W—H2W2 | 111 (1) | C7—C6—H6A | 108.8 |
H3W1—O3W—H3W2 | 107 (1) | C7—C6—H6B | 108.8 |
H4W1—O4W—H4W2 | 106 (2) | H6A—C6—H6B | 107.7 |
| | | |
O3—C3—C4—C5 | −176.9 (2) | C1—C2—C3—C4 | −3.4 (2) |
N1—C1—C2—C3 | 0.4 (3) | C2—C3—C4—C5 | 3.3 (2) |
N1—C6—C7—O2 | 8.5 (2) | C3—C4—C5—N1 | −0.3 (2) |
N1—C6—C7—O1 | −171.9 (1) | C5—N1—C1—C2 | 2.9 (2) |
C1—N1—C5—C4 | −2.9 (2) | C5—N1—C6—C7 | 72.9 (2) |
C1—N1—C6—C7 | −106.7 (2) | C6—N1—C1—C2 | −177.5 (2) |
C1—C2—C3—O3 | 176.8 (2) | C6—N1—C5—C4 | 177.4 (1) |
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—H1W1···O4Wii | 0.85 (2) | 1.88 (1) | 2.727 (2) | 175 (2) |
O1W—H1W2···O1ii | 0.85 (2) | 1.99 (2) | 2.831 (2) | 167 (2) |
O2W—H2W1···O2i | 0.84 (2) | 1.85 (2) | 2.698 (2) | 176 (2) |
O2W—H2W2···O3iii | 0.85 (2) | 1.89 (2) | 2.728 (2) | 174 (3) |
O3W—H3W1···O1 | 0.86 (2) | 1.84 (2) | 2.687 (2) | 171 (2) |
O3W—H3W2···O1iv | 0.86 (2) | 2.03 (2) | 2.835 (2) | 155 (2) |
O4W—H4W1···O3iii | 0.86 (2) | 2.22 (3) | 3.007 (2) | 154 (3) |
O4W—H4W2···O3v | 0.86 (2) | 1.99 (3) | 2.804 (2) | 158 (3) |
Symmetry codes: (i) −x, −y+1, −z; (ii) −x, y−1/2, −z+1/2; (iii) x+1, −y+3/2, z+1/2; (iv) x, −y+3/2, z+1/2; (v) x+1, y, z. |