In the asymmetric unit of the title compound, [Mn(C10H8O6)(H2O)3]n, the two half-MnII atoms lie on inversion centres. One MnII atom is in an octahedral configuration, defined by two O atoms from two monodentate carboxylate groups and four water molecules, and the other MnII atom exists in a different octahedral coordination environment, defined by four O atoms from four monodentate carboxylate groups and two water molecules. The MnII atoms are bridged by a benzene-1,3-dioxyacetate dianion in monodentate and bridging-bidentate modes, forming a two-dimensional layer structure.
Supporting information
CCDC reference: 254349
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.005 Å
- R factor = 0.043
- wR factor = 0.133
- Data-to-parameter ratio = 14.1
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ !
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ !
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ !
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ !
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
0 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
4 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.
Poly[triaqua[µ-
m-phenylenebis(oxyacetato)]manganese(II)]
top
Crystal data top
[Mn(C10H8O6)(H2O)3] | Z = 2 |
Mr = 333.15 | F(000) = 342 |
Triclinic, P1 | Dx = 1.771 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 4.770 (1) Å | Cell parameters from 5921 reflections |
b = 5.797 (2) Å | θ = 3.7–27.5° |
c = 22.923 (7) Å | µ = 1.10 mm−1 |
α = 83.65 (2)° | T = 293 K |
β = 84.16 (1)° | Prism, colourless |
γ = 84.92 (1)° | 0.38 × 0.25 × 0.19 mm |
V = 624.8 (3) Å3 | |
Data collection top
Rigaku R-AXIS RAPID diffractometer | 2841 independent reflections |
Radiation source: fine-focus sealed tube | 2278 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.031 |
Detector resolution: 10 pixels mm-1 | θmax = 27.5°, θmin = 3.6° |
ω scans | h = −6→5 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −7→7 |
Tmin = 0.679, Tmax = 0.818 | l = −29→29 |
6030 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) = 0.133 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0669P)2 + 1.0201P] where P = (Fo2 + 2Fc2)/3 |
2841 reflections | (Δ/σ)max < 0.001 |
202 parameters | Δρmax = 0.48 e Å−3 |
9 restraints | Δρmin = −0.55 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Mn1 | 1.0000 | 0.5000 | 0.5000 | 0.02615 (19) | |
Mn2 | −0.5000 | −0.5000 | 1.0000 | 0.02215 (18) | |
O1 | 0.7336 (5) | 0.3480 (4) | 0.57526 (10) | 0.0323 (5) | |
O2 | 1.0028 (5) | 0.0387 (4) | 0.61097 (10) | 0.0348 (6) | |
O3 | 0.3982 (5) | 0.3519 (4) | 0.67319 (10) | 0.0327 (5) | |
O4 | −0.0685 (5) | 0.0262 (4) | 0.85906 (11) | 0.0392 (6) | |
O5 | −0.2285 (4) | −0.2940 (4) | 0.93834 (10) | 0.0282 (5) | |
O6 | 0.1878 (5) | −0.5059 (4) | 0.93369 (10) | 0.0272 (5) | |
O1W | 0.7348 (5) | 0.8176 (4) | 0.49539 (12) | 0.0360 (6) | |
O2W | 0.7548 (5) | 0.3546 (4) | 0.43823 (11) | 0.0333 (5) | |
O3W | −0.7483 (5) | −0.1842 (4) | 1.02398 (11) | 0.0354 (6) | |
C1 | 0.7924 (7) | 0.1846 (6) | 0.61384 (14) | 0.0264 (6) | |
C2 | 0.5917 (7) | 0.1516 (6) | 0.66945 (14) | 0.0290 (7) | |
C3 | 0.2004 (7) | 0.3546 (6) | 0.72090 (13) | 0.0271 (6) | |
C4 | 0.0114 (7) | 0.5491 (6) | 0.72157 (15) | 0.0329 (7) | |
C5 | −0.1982 (8) | 0.5640 (6) | 0.76744 (15) | 0.0348 (8) | |
C6 | −0.2210 (7) | 0.3859 (6) | 0.81308 (14) | 0.0307 (7) | |
C7 | −0.0276 (7) | 0.1947 (5) | 0.81230 (13) | 0.0272 (7) | |
C8 | 0.1848 (7) | 0.1742 (6) | 0.76672 (14) | 0.0281 (7) | |
C9 | 0.1384 (7) | −0.1637 (6) | 0.86786 (14) | 0.0293 (7) | |
C10 | 0.0210 (6) | −0.3334 (5) | 0.91771 (12) | 0.0231 (6) | |
H2A | 0.4890 | 0.0151 | 0.6686 | 0.035* | |
H2B | 0.6982 | 0.1281 | 0.7038 | 0.035* | |
H4 | 0.0252 | 0.6694 | 0.6913 | 0.040* | |
H5 | −0.3258 | 0.6949 | 0.7678 | 0.042* | |
H6 | −0.3642 | 0.3955 | 0.8436 | 0.037* | |
H8 | 0.3134 | 0.0439 | 0.7666 | 0.034* | |
H9A | 0.3115 | −0.1081 | 0.8779 | 0.035* | |
H9B | 0.1804 | −0.2401 | 0.8321 | 0.035* | |
H10 | 0.776 (8) | 0.877 (8) | 0.4602 (8) | 0.054* | |
H11 | 0.563 (3) | 0.788 (8) | 0.4999 (17) | 0.054* | |
H12 | 0.646 (7) | 0.447 (6) | 0.4179 (14) | 0.050* | |
H13 | 0.841 (8) | 0.254 (5) | 0.4170 (14) | 0.050* | |
H14 | −0.909 (5) | −0.237 (7) | 1.0336 (18) | 0.053* | |
H15 | −0.722 (8) | −0.082 (6) | 1.0460 (15) | 0.053* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Mn1 | 0.0237 (3) | 0.0263 (3) | 0.0253 (3) | 0.0025 (3) | 0.0035 (3) | 0.0024 (3) |
Mn2 | 0.0183 (3) | 0.0229 (3) | 0.0231 (3) | −0.0004 (2) | 0.0025 (2) | 0.0021 (2) |
O1 | 0.0294 (12) | 0.0362 (12) | 0.0254 (11) | 0.0037 (10) | 0.0051 (9) | 0.0114 (9) |
O2 | 0.0364 (13) | 0.0332 (12) | 0.0302 (12) | 0.0087 (10) | 0.0031 (10) | 0.0021 (10) |
O3 | 0.0314 (12) | 0.0348 (12) | 0.0255 (11) | 0.0060 (10) | 0.0090 (9) | 0.0076 (9) |
O4 | 0.0371 (14) | 0.0359 (13) | 0.0342 (13) | 0.0095 (11) | 0.0165 (11) | 0.0153 (10) |
O5 | 0.0204 (11) | 0.0314 (11) | 0.0287 (11) | −0.0013 (9) | 0.0055 (9) | 0.0070 (9) |
O6 | 0.0256 (11) | 0.0283 (11) | 0.0262 (11) | 0.0002 (9) | −0.0029 (9) | 0.0022 (9) |
O1W | 0.0254 (12) | 0.0299 (12) | 0.0483 (15) | 0.0050 (10) | 0.0067 (11) | 0.0009 (11) |
O2W | 0.0313 (13) | 0.0333 (13) | 0.0335 (12) | 0.0064 (10) | −0.0024 (10) | −0.0029 (10) |
O3W | 0.0317 (13) | 0.0315 (12) | 0.0426 (14) | 0.0008 (10) | 0.0020 (11) | −0.0093 (10) |
C1 | 0.0238 (15) | 0.0304 (16) | 0.0247 (15) | −0.0034 (12) | 0.0003 (12) | −0.0023 (12) |
C2 | 0.0263 (15) | 0.0315 (16) | 0.0261 (15) | −0.0005 (13) | 0.0024 (12) | 0.0050 (13) |
C3 | 0.0243 (15) | 0.0340 (16) | 0.0215 (14) | −0.0031 (13) | 0.0018 (12) | 0.0013 (12) |
C4 | 0.0371 (18) | 0.0308 (16) | 0.0265 (16) | 0.0032 (14) | 0.0026 (13) | 0.0067 (13) |
C5 | 0.0342 (18) | 0.0321 (17) | 0.0335 (17) | 0.0106 (14) | 0.0028 (14) | 0.0010 (14) |
C6 | 0.0293 (16) | 0.0343 (17) | 0.0253 (15) | −0.0003 (13) | 0.0071 (13) | 0.0011 (13) |
C7 | 0.0281 (16) | 0.0283 (15) | 0.0225 (14) | −0.0027 (12) | 0.0023 (12) | 0.0054 (12) |
C8 | 0.0254 (15) | 0.0286 (16) | 0.0266 (15) | 0.0035 (12) | 0.0013 (12) | 0.0061 (12) |
C9 | 0.0235 (15) | 0.0317 (16) | 0.0288 (16) | −0.0004 (13) | 0.0037 (13) | 0.0067 (13) |
C10 | 0.0240 (15) | 0.0249 (14) | 0.0198 (14) | −0.0033 (12) | −0.0004 (11) | −0.0001 (11) |
Geometric parameters (Å, º) top
Mn1—O1 | 2.187 (2) | O1W—H11 | 0.85 (3) |
Mn1—O1W | 2.138 (2) | O2W—H12 | 0.85 (3) |
Mn1—O2W | 2.204 (3) | O2W—H13 | 0.85 (3) |
Mn2—O5 | 2.152 (2) | O3W—H14 | 0.85 (3) |
Mn2—O6i | 2.238 (2) | O3W—H15 | 0.85 (4) |
Mn2—O3W | 2.182 (2) | C1—C2 | 1.519 (4) |
O1—C1 | 1.256 (4) | C2—H2A | 0.9700 |
O2—C1 | 1.255 (4) | C2—H2B | 0.9700 |
O5—C10 | 1.246 (4) | C3—C4 | 1.381 (5) |
O6—C10 | 1.267 (4) | C3—C8 | 1.399 (4) |
Mn1—O1ii | 2.187 (2) | C4—C5 | 1.379 (5) |
Mn1—O1Wii | 2.138 (2) | C4—H4 | 0.9300 |
Mn1—O2Wii | 2.204 (3) | C5—C6 | 1.389 (5) |
Mn2—O5iii | 2.152 (2) | C5—H5 | 0.9300 |
Mn2—O6iv | 2.238 (2) | C6—C7 | 1.378 (5) |
Mn2—O3Wiii | 2.182 (2) | C6—H6 | 0.9300 |
O3—C2 | 1.422 (4) | C7—C8 | 1.386 (4) |
O3—C3 | 1.370 (4) | C8—H8 | 0.9300 |
O4—C7 | 1.379 (4) | C9—C10 | 1.519 (4) |
O4—C9 | 1.423 (4) | C9—H9A | 0.9700 |
O6—Mn2v | 2.238 (2) | C9—H9B | 0.9700 |
O1W—H10 | 0.85 (3) | | |
| | | |
O1ii—Mn1—O1 | 180.000 (1) | O5iii—Mn2—O3Wiii | 90.13 (9) |
O1—Mn1—O2W | 90.86 (10) | O5—Mn2—O3Wiii | 89.87 (9) |
O1ii—Mn1—O2W | 89.14 (10) | O5—C10—O6 | 126.1 (3) |
O5iii—Mn2—O5 | 180.000 (1) | O5—C10—C9 | 117.9 (3) |
O5—Mn2—O6iv | 88.04 (9) | O6—C10—C9 | 116.0 (3) |
O5—Mn2—O6i | 91.96 (9) | O1W—Mn1—O1ii | 88.14 (9) |
O5iii—Mn2—O3W | 89.87 (9) | O1Wii—Mn1—O1ii | 91.86 (9) |
O5—Mn2—O3W | 90.13 (9) | O1W—Mn1—O2Wii | 88.76 (10) |
O6iv—Mn2—O6i | 180.000 (1) | O1Wii—Mn1—O2Wii | 91.24 (10) |
O1W—Mn1—O1 | 91.86 (9) | O3Wiii—Mn2—O6iv | 85.10 (9) |
O1Wii—Mn1—O1 | 88.14 (9) | O3Wiii—Mn2—O6i | 94.90 (9) |
O1W—Mn1—O1Wii | 180.000 (1) | C1—O1—Mn1 | 129.8 (2) |
O1W—Mn1—O2W | 91.24 (10) | C1—C2—H2A | 109.8 |
O1Wii—Mn1—O2W | 88.76 (10) | C1—C2—H2B | 109.8 |
O2W—Mn1—O2Wii | 180.000 (1) | C3—O3—C2 | 118.0 (2) |
O3W—Mn2—O6i | 85.10 (9) | C3—C4—H4 | 120.2 |
O3W—Mn2—O6iv | 94.90 (9) | C3—C8—H8 | 120.9 |
O3W—Mn2—O3Wiii | 180.00 (13) | C4—C3—C8 | 120.7 (3) |
Mn1—O1W—H10 | 103 (3) | C4—C5—C6 | 120.8 (3) |
Mn1—O1W—H11 | 110 (3) | C4—C5—H5 | 119.6 |
Mn1—O2W—H12 | 119 (3) | C5—C4—C3 | 119.6 (3) |
Mn1—O2W—H13 | 117 (3) | C5—C4—H4 | 120.2 |
Mn2—O3W—H14 | 100 (3) | C5—C6—H6 | 120.6 |
Mn2—O3W—H15 | 133 (3) | C6—C5—H5 | 119.6 |
O1ii—Mn1—O2Wii | 90.86 (10) | C6—C7—O4 | 114.7 (3) |
O1—Mn1—O2Wii | 89.14 (10) | C6—C7—C8 | 121.7 (3) |
O1—C1—C2 | 118.6 (3) | C7—O4—C9 | 120.1 (2) |
O2—C1—O1 | 126.3 (3) | C7—C6—C5 | 118.9 (3) |
O2—C1—C2 | 115.1 (3) | C7—C6—H6 | 120.6 |
O3—C2—C1 | 109.5 (3) | C7—C8—C3 | 118.3 (3) |
O3—C2—H2A | 109.8 | C7—C8—H8 | 120.9 |
O3—C2—H2B | 109.8 | C10—O5—Mn2 | 131.5 (2) |
O3—C3—C4 | 115.8 (3) | C10—O6—Mn2v | 124.1 (2) |
O3—C3—C8 | 123.4 (3) | C10—C9—H9A | 110.1 |
O4—C7—C8 | 123.6 (3) | C10—C9—H9B | 110.1 |
O4—C9—C10 | 108.1 (2) | H10—O1W—H11 | 110 (4) |
O4—C9—H9A | 110.1 | H12—O2W—H13 | 109.7 (17) |
O4—C9—H9B | 110.1 | H14—O3W—H15 | 110 (4) |
O5iii—Mn2—O6iv | 91.96 (9) | H2A—C2—H2B | 108.2 |
O5iii—Mn2—O6i | 88.04 (9) | H9A—C9—H9B | 108.4 |
| | | |
Mn1—O1—C1—O2 | −16.0 (5) | O2W—Mn1—O1—C1 | 110.9 (3) |
Mn1—O1—C1—C2 | 165.3 (2) | O2Wii—Mn1—O1—C1 | −69.1 (3) |
Mn2—O5—C10—O6 | −7.3 (5) | O3W—Mn2—O5—C10 | 155.4 (3) |
Mn2—O5—C10—C9 | 171.3 (2) | O3Wiii—Mn2—O5—C10 | −24.6 (3) |
Mn2v—O6—C10—O5 | −95.2 (4) | C2—O3—C3—C4 | −177.9 (3) |
Mn2v—O6—C10—C9 | 86.1 (3) | C2—O3—C3—C8 | 2.0 (5) |
O1—C1—C2—O3 | −13.3 (4) | C3—O3—C2—C1 | −179.7 (3) |
O2—C1—C2—O3 | 167.9 (3) | C3—C4—C5—C6 | 0.2 (6) |
O3—C3—C4—C5 | 178.8 (3) | C4—C3—C8—C7 | 0.8 (5) |
O3—C3—C8—C7 | −179.0 (3) | C4—C5—C6—C7 | 1.0 (6) |
O4—C7—C8—C3 | 178.4 (3) | C5—C6—C7—O4 | −179.4 (3) |
O4—C9—C10—O5 | 5.7 (4) | C5—C6—C7—C8 | −1.2 (5) |
O4—C9—C10—O6 | −175.6 (3) | C6—C7—C8—C3 | 0.3 (5) |
O6iv—Mn2—O5—C10 | 60.5 (3) | C7—O4—C9—C10 | −173.5 (3) |
O6i—Mn2—O5—C10 | −119.5 (3) | C8—C3—C4—C5 | −1.1 (6) |
O1W—Mn1—O1—C1 | −157.9 (3) | C9—O4—C7—C6 | −171.2 (3) |
O1Wii—Mn1—O1—C1 | 22.1 (3) | C9—O4—C7—C8 | 10.6 (5) |
Symmetry codes: (i) x−1, y, z; (ii) −x+2, −y+1, −z+1; (iii) −x−1, −y−1, −z+2; (iv) −x, −y−1, −z+2; (v) x+1, y, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H10···O2ii | 0.85 (3) | 1.89 (3) | 2.706 (3) | 159 (4) |
O1W—H11···O1vi | 0.85 (3) | 2.57 (3) | 3.161 (4) | 128 (3) |
O1W—H11···O2Wvi | 0.85 (3) | 2.13 (2) | 2.849 (4) | 143 (3) |
O2W—H12···O1vi | 0.85 (3) | 2.08 (2) | 2.795 (3) | 142 (3) |
O2W—H12···O3vi | 0.85 (3) | 2.30 (3) | 3.025 (3) | 144 (3) |
O2W—H13···O2vii | 0.85 (3) | 1.94 (3) | 2.765 (3) | 162 (4) |
O3W—H14···O6iii | 0.85 (3) | 2.11 (2) | 2.903 (4) | 155 (4) |
O3W—H15···O4viii | 0.85 (4) | 2.35 (3) | 2.952 (4) | 129 (3) |
O3W—H15···O5viii | 0.85 (4) | 2.23 (3) | 2.983 (4) | 147 (4) |
Symmetry codes: (ii) −x+2, −y+1, −z+1; (iii) −x−1, −y−1, −z+2; (vi) −x+1, −y+1, −z+1; (vii) −x+2, −y, −z+1; (viii) −x−1, −y, −z+2. |