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In the title compound, {[Mn(C
2O
4)(H
2O)
2]·H
2O}
n, the octahedrally coordinated Mn atom, lying on a twofold rotation axis, is bonded to four carboxyl O atoms from oxalate groups and two O atoms from two water molecules. By means of the bridging oxalate ligand, the title compound exhibits a one-dimensional chain structure. The crystal packing is stabilized by hydrogen bonds of the type O—H
O(oxalate).
Supporting information
CCDC reference: 277709
Key indicators
- Single-crystal X-ray study
- T = 292 K
- Mean (C-C) = 0.001 Å
- R factor = 0.020
- wR factor = 0.054
- Data-to-parameter ratio = 14.5
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT369_ALERT_2_C Long C(sp2)-C(sp2) Bond C1 - C1_b ... 1.55 Ang.
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.11 Ratio
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: SMART (Bruker, 2000); cell refinement: SMART; data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXTL.
catena-Poly[[[diaquamanganese(II)]-µ-oxalato] monohydrate]
top
Crystal data top
[Mn(C2O4)(H2O)2]·H2O | F(000) = 396 |
Mr = 197.01 | Dx = 1.926 Mg m−3 |
Orthorhombic, Pcca | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P2a2ac | Cell parameters from 2752 reflections |
a = 9.7660 (9) Å | θ = 3.1–28.2° |
b = 6.6155 (6) Å | µ = 1.93 mm−1 |
c = 10.5192 (10) Å | T = 292 K |
V = 679.61 (11) Å3 | Block, pale yellow |
Z = 4 | 0.40 × 0.36 × 0.22 mm |
Data collection top
Bruker SMART CCD area-detector diffractometer | 824 independent reflections |
Radiation source: fine-focus sealed tube | 781 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.017 |
φ and ω scans | θmax = 28.3°, θmin = 3.1° |
Absorption correction: multi-scan (SADABS; Bruker, 2000) | h = −13→11 |
Tmin = 0.474, Tmax = 0.654 | k = −8→6 |
3698 measured reflections | l = −12→14 |
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)] = 0.020 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.054 | w = 1/[σ2(Fo2) + (0.0344P)2 + 0.0879P] where P = (Fo2 + 2Fc2)/3 |
S = 1.07 | (Δ/σ)max = 0.005 |
824 reflections | Δρmax = 0.41 e Å−3 |
57 parameters | Δρmin = −0.27 e Å−3 |
2 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0119 (16) |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Mn1 | 0.2500 | 0.5000 | 0.14108 (2) | 0.02437 (12) | |
O1 | 0.06730 (8) | 0.68075 (13) | 0.10231 (8) | 0.0324 (2) | |
O2 | 0.18709 (9) | 0.30102 (14) | 0.29254 (8) | 0.0372 (2) | |
H2A | 0.2470 | 0.2970 | 0.3471 | 0.056* | |
O3 | 0.13199 (7) | 0.32188 (12) | 0.00141 (7) | 0.0286 (2) | |
C1 | −0.01871 (10) | 0.60430 (15) | 0.02907 (10) | 0.0240 (2) | |
O4 | 0.0000 | 1.01007 (16) | 0.2500 | 0.0309 (3) | |
H2B | 0.1359 (17) | 0.202 (3) | 0.2816 (16) | 0.050 (5)* | |
H4A | 0.0253 (19) | 0.938 (3) | 0.1954 (17) | 0.056 (5)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Mn1 | 0.01871 (17) | 0.03029 (18) | 0.02411 (17) | −0.00044 (7) | 0.000 | 0.000 |
O1 | 0.0259 (4) | 0.0332 (4) | 0.0382 (5) | 0.0037 (3) | −0.0067 (3) | −0.0128 (3) |
O2 | 0.0387 (5) | 0.0418 (5) | 0.0310 (4) | −0.0170 (4) | −0.0059 (3) | 0.0053 (3) |
O3 | 0.0231 (4) | 0.0319 (4) | 0.0308 (4) | 0.0052 (3) | −0.0023 (3) | −0.0055 (3) |
C1 | 0.0207 (4) | 0.0278 (5) | 0.0236 (5) | 0.0003 (4) | 0.0026 (4) | −0.0029 (4) |
O4 | 0.0365 (7) | 0.0214 (5) | 0.0349 (7) | 0.000 | 0.0029 (6) | 0.000 |
Geometric parameters (Å, º) top
Mn1—O2i | 2.1561 (9) | O2—H2A | 0.8200 |
Mn1—O2 | 2.1561 (9) | O2—H2B | 0.834 (17) |
Mn1—O1i | 2.1862 (8) | O3—C1ii | 1.2511 (12) |
Mn1—O1 | 2.1862 (8) | C1—O3ii | 1.2511 (12) |
Mn1—O3i | 2.2080 (8) | C1—C1ii | 1.553 (2) |
Mn1—O3 | 2.2080 (8) | O4—H4A | 0.785 (17) |
O1—C1 | 1.2470 (12) | | |
| | | |
O2i—Mn1—O2 | 84.71 (5) | O1i—Mn1—O3 | 90.57 (3) |
O2i—Mn1—O1i | 103.84 (4) | O1—Mn1—O3 | 75.03 (3) |
O2—Mn1—O1i | 92.09 (3) | O3i—Mn1—O3 | 96.58 (4) |
O2i—Mn1—O1 | 92.09 (3) | C1—O1—Mn1 | 116.31 (7) |
O2—Mn1—O1 | 103.84 (4) | Mn1—O2—H2A | 109.5 |
O1i—Mn1—O1 | 158.50 (5) | Mn1—O2—H2B | 123.4 (12) |
O2i—Mn1—O3i | 90.98 (3) | H2A—O2—H2B | 119.9 |
O2—Mn1—O3i | 165.07 (3) | C1ii—O3—Mn1 | 115.07 (6) |
O1i—Mn1—O3i | 75.04 (3) | O1—C1—O3ii | 126.56 (10) |
O1—Mn1—O3i | 90.57 (3) | O1—C1—C1ii | 116.43 (11) |
O2i—Mn1—O3 | 165.07 (3) | O3ii—C1—C1ii | 117.01 (11) |
O2—Mn1—O3 | 90.98 (3) | | |
| | | |
O2i—Mn1—O1—C1 | −169.19 (8) | O2—Mn1—O3—C1ii | 100.72 (8) |
O2—Mn1—O1—C1 | −84.13 (8) | O1i—Mn1—O3—C1ii | −167.18 (7) |
O1i—Mn1—O1—C1 | 52.58 (8) | O1—Mn1—O3—C1ii | −3.35 (7) |
O3i—Mn1—O1—C1 | 99.80 (8) | O3i—Mn1—O3—C1ii | −92.18 (8) |
O3—Mn1—O1—C1 | 3.14 (8) | Mn1—O1—C1—O3ii | 176.92 (8) |
O2i—Mn1—O3—C1ii | 27.79 (17) | Mn1—O1—C1—C1ii | −2.60 (15) |
Symmetry codes: (i) −x+1/2, −y+1, z; (ii) −x, −y+1, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O2—H2A···O3iii | 0.82 | 2.01 | 2.8228 (11) | 169 |
O2—H2B···O4iv | 0.83 (2) | 1.87 (2) | 2.6913 (12) | 171 (2) |
O4—H4A···O1 | 0.79 (2) | 2.01 (2) | 2.7554 (11) | 159 (2) |
Symmetry codes: (iii) −x+1/2, y, z+1/2; (iv) x, y−1, z. |
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