metal-organic compounds
The title complex, [Mg(H2O)6](1,3-BDOA)·3H2O (1,3-BDOA2- = benzene-1,3-dioxyacetate, C10H8O62-), consists of an [Mg(H2O)6]2+ cation, a benzene-1,3-dioxyacetate dianion and three uncoordinated water molecules. The MgII atom is coordinated by six water molecules, forming a slightly distorted octahedral coordination. A two-dimensional supramolecular network structure is constructed by hydrogen bonds.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804012176/ww6210sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804012176/ww6210Isup2.hkl |
CCDC reference: 242279
Computing details top
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) benzene-1,3-dioxyacetate trihydrate top
Crystal data top
[Mg(H2O)6](C10H8O6)·3H2O | F(000) = 872 |
Mr = 410.62 | Dx = 1.456 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 12616 reflections |
a = 6.134 (1) Å | θ = 3.5–27.4° |
b = 26.020 (5) Å | µ = 0.17 mm−1 |
c = 12.028 (2) Å | T = 293 K |
β = 102.64 (3)° | Prism, colorless |
V = 1873.3 (6) Å3 | 0.39 × 0.26 × 0.18 mm |
Z = 4 |
Data collection top
Rigaku R-AXIS RAPID diffractometer | 4240 independent reflections |
Radiation source: fine-focus sealed tube | 3547 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.019 |
Detector resolution: 10 pixels mm-1 | θmax = 27.4°, θmin = 3.1° |
ω scans | h = −7→7 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −33→33 |
Tmin = 0.937, Tmax = 0.971 | l = −15→15 |
17782 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)] = 0.039 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.097 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.09 | w = 1/[σ2(Fo2) + (0.0482P)2 + 0.4786P] where P = (Fo2 + 2Fc2)/3 |
4240 reflections | (Δ/σ)max < 0.001 |
289 parameters | Δρmax = 0.39 e Å−3 |
27 restraints | Δρmin = −0.15 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | ||
Mg1 | 0.01334 (7) | 0.02970 (2) | 0.28843 (4) | 0.0262 (1) | |
O1 | −0.0344 (2) | −0.04813 (4) | 0.2962 (1) | 0.0367 (2) | |
O2 | 0.0546 (2) | 0.10786 (4) | 0.27631 (9) | 0.0409 (3) | |
O3 | −0.2690 (2) | 0.03999 (4) | 0.3602 (1) | 0.0372 (2) | |
O4 | 0.2112 (2) | 0.03234 (4) | 0.44934 (8) | 0.0349 (2) | |
O5 | −0.1873 (2) | 0.02464 (4) | 0.12787 (9) | 0.0389 (3) | |
O6 | 0.3008 (2) | 0.01848 (4) | 0.22099 (9) | 0.0338 (2) | |
O7 | 0.1306 (2) | 0.17563 (4) | 0.4738 (1) | 0.0443 (3) | |
O8 | 0.3883 (2) | 0.11828 (4) | 0.5476 (1) | 0.0446 (3) | |
O9 | 0.6335 (2) | 0.18094 (4) | 0.6807 (1) | 0.0422 (3) | |
O10 | 1.3464 (2) | 0.17117 (4) | 0.9099 (1) | 0.0428 (3) | |
O11 | 1.8874 (2) | 0.16075 (5) | 1.0840 (1) | 0.0569 (4) | |
O12 | 1.6421 (2) | 0.10336 (4) | 0.9967 (1) | 0.0512 (3) | |
O13 | 0.8232 (2) | 0.10828 (4) | 0.5271 (1) | 0.0386 (3) | |
O14 | 0.2117 (2) | 0.06742 (5) | 0.0098 (1) | 0.0497 (3) | |
O15 | 0.5128 (2) | −0.07450 (4) | 0.2293 (1) | 0.0402 (3) | |
C1 | 0.3114 (2) | 0.16312 (5) | 0.5368 (1) | 0.0295 (3) | |
C2 | 0.4526 (2) | 0.20528 (5) | 0.6045 (1) | 0.0323 (3) | |
C3 | 0.8157 (2) | 0.20920 (5) | 0.7338 (1) | 0.0298 (3) | |
C4 | 0.8294 (2) | 0.26230 (5) | 0.7304 (1) | 0.0349 (3) | |
C5 | 1.0256 (3) | 0.28531 (6) | 0.7895 (1) | 0.0408 (4) | |
C6 | 1.2036 (2) | 0.25699 (6) | 0.8513 (1) | 0.0358 (3) | |
C7 | 1.1837 (2) | 0.20390 (5) | 0.8532 (1) | 0.0303 (3) | |
C8 | 0.9908 (2) | 0.17990 (5) | 0.7950 (1) | 0.0323 (3) | |
C9 | 1.5501 (2) | 0.19235 (5) | 0.9723 (1) | 0.0327 (3) | |
C10 | 1.7061 (2) | 0.14874 (6) | 1.0223 (1) | 0.0343 (3) | |
H2 | 0.5086 | 0.2283 | 0.5537 | 0.039* | |
H3 | 0.3641 | 0.2251 | 0.6468 | 0.039* | |
H4 | 0.7116 | 0.2819 | 0.6900 | 0.042* | |
H5 | 1.0380 | 0.3209 | 0.7875 | 0.049* | |
H6 | 1.3328 | 0.2732 | 0.8904 | 0.043* | |
H8 | 0.9785 | 0.1443 | 0.7968 | 0.039* | |
H9 | 1.5213 | 0.2141 | 1.0330 | 0.039* | |
H10 | 1.6187 | 0.2132 | 0.9225 | 0.039* | |
H11 | 0.028 (3) | −0.0679 (6) | 0.351 (1) | 0.055* | |
H12 | −0.169 (2) | −0.0572 (7) | 0.272 (2) | 0.055* | |
H13 | 0.001 (3) | 0.1244 (7) | 0.215 (1) | 0.061* | |
H14 | 0.081 (3) | 0.1288 (6) | 0.332 (1) | 0.061* | |
H15 | −0.398 (2) | 0.0411 (7) | 0.316 (1) | 0.056* | |
H16 | −0.258 (3) | 0.0658 (6) | 0.406 (1) | 0.056* | |
H17 | 0.266 (3) | 0.0608 (4) | 0.478 (2) | 0.052* | |
H18 | 0.225 (3) | 0.0102 (5) | 0.502 (1) | 0.052* | |
H19 | −0.232 (3) | 0.0507 (5) | 0.087 (1) | 0.058* | |
H20 | −0.185 (4) | −0.0013 (5) | 0.086 (1) | 0.058* | |
H21 | 0.281 (3) | 0.0327 (6) | 0.156 (1) | 0.051* | |
H22 | 0.349 (3) | −0.0118 (4) | 0.217 (2) | 0.051* | |
H23 | 0.703 (2) | 0.1201 (7) | 0.540 (2) | 0.058* | |
H24 | 0.904 (3) | 0.1327 (6) | 0.513 (2) | 0.058* | |
H25 | 0.325 (2) | 0.0840 (7) | 0.000 (2) | 0.075* | |
H26 | 0.104 (2) | 0.0879 (7) | 0.009 (2) | 0.075* | |
H27 | 0.475 (3) | −0.0887 (7) | 0.1647 (9) | 0.060* | |
H28 | 0.502 (3) | −0.0961 (6) | 0.281 (1) | 0.060* |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
Mg1 | 0.0250 (2) | 0.0265 (2) | 0.0250 (2) | −0.0007 (2) | 0.0011 (2) | 0.0009 (2) |
O1 | 0.0346 (5) | 0.0295 (5) | 0.0415 (6) | −0.0017 (4) | −0.0012 (5) | 0.0036 (4) |
O2 | 0.0580 (7) | 0.0280 (5) | 0.0314 (6) | −0.0024 (5) | −0.0019 (5) | 0.0020 (4) |
O3 | 0.0277 (5) | 0.0419 (6) | 0.0401 (6) | −0.0012 (4) | 0.0030 (4) | −0.0086 (5) |
O4 | 0.0405 (6) | 0.0319 (5) | 0.0274 (5) | −0.0055 (4) | −0.0037 (4) | 0.0016 (4) |
O5 | 0.0457 (6) | 0.0341 (5) | 0.0303 (5) | 0.0036 (5) | −0.0059 (5) | 0.0005 (4) |
O6 | 0.0310 (5) | 0.0375 (5) | 0.0329 (5) | 0.0028 (4) | 0.0070 (4) | 0.0025 (4) |
O7 | 0.0315 (5) | 0.0374 (6) | 0.0536 (7) | 0.0015 (4) | −0.0131 (5) | 0.0041 (5) |
O8 | 0.0348 (6) | 0.0300 (5) | 0.0587 (7) | 0.0020 (4) | −0.0125 (5) | −0.0074 (5) |
O9 | 0.0332 (5) | 0.0293 (5) | 0.0530 (7) | −0.0026 (4) | −0.0148 (5) | 0.0020 (5) |
O10 | 0.0314 (5) | 0.0287 (5) | 0.0574 (7) | −0.0001 (4) | −0.0138 (5) | 0.0003 (5) |
O11 | 0.0417 (7) | 0.0510 (7) | 0.0629 (8) | −0.0101 (5) | −0.0214 (6) | 0.0211 (6) |
O12 | 0.0551 (7) | 0.0328 (6) | 0.0525 (7) | 0.0047 (5) | −0.0173 (6) | 0.0032 (5) |
O13 | 0.0328 (5) | 0.0390 (6) | 0.0439 (6) | 0.0034 (4) | 0.0083 (5) | −0.0029 (5) |
O14 | 0.0538 (7) | 0.0476 (7) | 0.0489 (7) | −0.0056 (6) | 0.0138 (6) | 0.0070 (6) |
O15 | 0.0457 (6) | 0.0357 (6) | 0.0378 (6) | −0.0016 (5) | 0.0060 (5) | 0.0004 (5) |
C1 | 0.0248 (6) | 0.0308 (7) | 0.0310 (7) | −0.0008 (5) | 0.0018 (5) | 0.0018 (5) |
C2 | 0.0280 (7) | 0.0287 (7) | 0.0360 (7) | 0.0030 (5) | −0.0023 (6) | −0.0003 (6) |
C3 | 0.0272 (6) | 0.0293 (7) | 0.0301 (7) | −0.0018 (5) | 0.0002 (5) | −0.0044 (5) |
C4 | 0.0329 (7) | 0.0290 (7) | 0.0380 (8) | 0.0044 (5) | −0.0029 (6) | −0.0002 (6) |
C5 | 0.0430 (9) | 0.0241 (7) | 0.0496 (9) | −0.0018 (6) | −0.0023 (7) | −0.0018 (6) |
C6 | 0.0314 (7) | 0.0301 (7) | 0.0405 (8) | −0.0043 (6) | −0.0039 (6) | −0.0043 (6) |
C7 | 0.0284 (7) | 0.0290 (7) | 0.0304 (7) | 0.0023 (5) | −0.0002 (5) | −0.0010 (5) |
C8 | 0.0316 (7) | 0.0249 (6) | 0.0365 (8) | −0.0008 (5) | −0.0009 (6) | −0.0016 (5) |
C9 | 0.0293 (7) | 0.0303 (7) | 0.0340 (7) | −0.0022 (5) | −0.0032 (6) | −0.0009 (6) |
C10 | 0.0324 (7) | 0.0356 (7) | 0.0304 (7) | −0.0011 (6) | −0.0024 (6) | 0.0060 (6) |
Geometric parameters (Å, º) top
Mg1—O1 | 2.051 (1) | O11—C10 | 1.235 (2) |
Mg1—O2 | 2.059 (1) | O12—C10 | 1.261 (2) |
Mg1—O3 | 2.114 (1) | O13—H23 | 0.848 (9) |
Mg1—O4 | 2.048 (1) | O13—H24 | 0.846 (9) |
Mg1—O5 | 2.055 (1) | O14—H25 | 0.849 (9) |
Mg1—O6 | 2.117 (1) | O14—H26 | 0.845 (9) |
O1—H11 | 0.853 (9) | O15—H27 | 0.846 (9) |
O1—H12 | 0.844 (9) | O15—H28 | 0.847 (9) |
O2—H13 | 0.855 (9) | C1—C2 | 1.519 (2) |
O2—H14 | 0.849 (9) | C2—H2 | 0.9700 |
O3—H15 | 0.851 (9) | C2—H3 | 0.9700 |
O3—H16 | 0.859 (9) | C3—C4 | 1.385 (2) |
O4—H17 | 0.853 (9) | C3—C8 | 1.389 (2) |
O4—H18 | 0.845 (9) | C4—C5 | 1.392 (2) |
O5—H19 | 0.851 (9) | C4—H4 | 0.9300 |
O5—H20 | 0.843 (9) | C5—C6 | 1.391 (2) |
O6—H21 | 0.848 (9) | C5—H5 | 0.9300 |
O6—H22 | 0.847 (9) | C6—C7 | 1.387 (2) |
O7—C1 | 1.242 (2) | C6—H6 | 0.9300 |
O8—C1 | 1.255 (2) | C7—C8 | 1.385 (2) |
O9—C2 | 1.424 (2) | C8—H8 | 0.9300 |
O9—C3 | 1.373 (2) | C9—C10 | 1.521 (2) |
O10—C7 | 1.374 (2) | C9—H9 | 0.9700 |
O10—C9 | 1.421 (2) | C9—H10 | 0.9700 |
O1—Mg1—O2 | 178.36 (5) | O10—C9—C10 | 108.9 (1) |
O1—Mg1—O3 | 88.20 (5) | O10—C9—H9 | 109.9 |
O1—Mg1—O5 | 85.25 (5) | O10—C9—H10 | 109.9 |
O1—Mg1—O6 | 91.18 (5) | O11—C10—O12 | 125.1 (1) |
O2—Mg1—O3 | 91.61 (5) | O11—C10—C9 | 117.1 (1) |
O2—Mg1—O6 | 89.05 (5) | O12—C10—C9 | 117.8 (1) |
O3—Mg1—O6 | 178.39 (5) | C1—C2—H2 | 110.3 |
O4—Mg1—O1 | 92.94 (5) | C1—C2—H3 | 110.3 |
O4—Mg1—O2 | 88.69 (4) | C3—O9—C2 | 120.1 (1) |
O4—Mg1—O3 | 88.81 (5) | C3—C4—C5 | 117.7 (1) |
O4—Mg1—O5 | 178.18 (5) | C3—C4—H4 | 121.1 |
O4—Mg1—O6 | 89.74 (5) | C3—C8—H8 | 120.1 |
O5—Mg1—O2 | 93.12 (5) | C4—C3—C8 | 121.2 (1) |
O5—Mg1—O3 | 90.91 (5) | C4—C5—H5 | 118.8 |
O5—Mg1—O6 | 90.52 (5) | C5—C4—H4 | 121.1 |
Mg1—O1—H11 | 126 (1) | C5—C6—H6 | 120.8 |
Mg1—O1—H12 | 113 (1) | C6—C5—C4 | 122.4 (1) |
Mg1—O2—H13 | 122 (1) | C6—C5—H5 | 118.8 |
Mg1—O2—H14 | 126 (1) | C7—O10—C9 | 118.8 (1) |
Mg1—O3—H15 | 119 (1) | C7—C6—C5 | 118.3 (1) |
Mg1—O3—H16 | 114 (1) | C7—C6—H6 | 120.8 |
Mg1—O4—H17 | 121 (1) | C7—C8—C3 | 119.8 (1) |
Mg1—O4—H18 | 129 (1) | C7—C8—H8 | 120.1 |
Mg1—O5—H19 | 123 (1) | C8—C7—C6 | 120.6 (1) |
Mg1—O5—H20 | 122 (1) | C10—C9—H9 | 109.9 |
Mg1—O6—H21 | 109 (1) | C10—C9—H10 | 109.9 |
Mg1—O6—H22 | 119 (1) | H2—C2—H3 | 108.5 |
O7—C1—O8 | 124.9 (1) | H9—C9—H10 | 108.3 |
O7—C1—C2 | 117.8 (1) | H11—O1—H12 | 110 (1) |
O8—C1—C2 | 117.3 (1) | H13—O2—H14 | 109 (1) |
O9—C2—C1 | 107.3 (1) | H15—O3—H16 | 108 (1) |
O9—C2—H2 | 110.3 | H17—O4—H18 | 109 (1) |
O9—C2—H3 | 110.3 | H19—O5—H20 | 110 (1) |
O9—C3—C4 | 124.7 (1) | H21—O6—H22 | 110 (1) |
O9—C3—C8 | 114.1 (1) | H23—O13—H24 | 110 (1) |
O10—C7—C6 | 124.6 (1) | H25—O14—H26 | 110 (1) |
O10—C7—C8 | 114.8 (1) | H27—O15—H28 | 109 (1) |
O7—C1—C2—O9 | 172.3 (1) | C3—C4—C5—C6 | −0.6 (2) |
O8—C1—C2—O9 | −8.8 (2) | C4—C3—C8—C7 | −0.4 (2) |
O9—C3—C4—C5 | 179.6 (2) | C4—C5—C6—C7 | 0.3 (3) |
O9—C3—C8—C7 | −179.5 (1) | C5—C6—C7—O10 | 179.5 (2) |
O10—C7—C8—C3 | −179.5 (1) | C5—C6—C7—C8 | −0.2 (2) |
O10—C9—C10—O11 | −176.6 (2) | C6—C7—C8—C3 | 0.2 (2) |
O10—C9—C10—O12 | 4.2 (2) | C7—O10—C9—C10 | −177.3 (1) |
C2—O9—C3—C4 | 8.2 (2) | C8—C3—C4—C5 | 0.6 (2) |
C2—O9—C3—C8 | −172.7 (1) | C9—O10—C7—C6 | 0.5 (2) |
C3—O9—C2—C1 | 165.0 (1) | C9—O10—C7—C8 | −179.8 (1) |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H11···O13i | 0.85 (1) | 1.88 (1) | 2.728 (2) | 177 (2) |
O1—H12···O15ii | 0.84 (1) | 1.96 (1) | 2.803 (2) | 174 (2) |
O2—H13···O11iii | 0.86 (1) | 1.84 (1) | 2.694 (2) | 179 (2) |
O2—H14···O7 | 0.85 (1) | 2.07 (1) | 2.913 (2) | 175 (2) |
O3—H15···O6ii | 0.85 (1) | 2.04 (1) | 2.854 (2) | 161 (2) |
O3—H16···O13ii | 0.86 (1) | 1.81 (1) | 2.648 (2) | 163 (2) |
O4—H17···O8 | 0.85 (1) | 1.80 (1) | 2.649 (2) | 176 (2) |
O4—H18···O3iv | 0.85 (1) | 2.08 (1) | 2.926 (2) | 176 (2) |
O5—H19···O12iii | 0.85 (1) | 1.81 (1) | 2.657 (2) | 174 (2) |
O5—H20···O14v | 0.84 (1) | 2.06 (1) | 2.897 (2) | 173 (2) |
O6—H21···O14 | 0.85 (1) | 1.94 (1) | 2.787 (2) | 175 (2) |
O6—H22···O15 | 0.85 (1) | 1.90 (1) | 2.738 (2) | 168 (2) |
O13—H23···O8 | 0.85 (1) | 1.95 (1) | 2.745 (2) | 156 (2) |
O13—H23···O9 | 0.85 (1) | 2.42 (2) | 3.047 (2) | 132 (2) |
O13—H24···O7vi | 0.85 (1) | 1.92 (1) | 2.751 (2) | 167 (2) |
O14—H25···O10vii | 0.85 (1) | 2.53 (2) | 3.138 (2) | 129 (2) |
O14—H25···O12vii | 0.85 (1) | 2.02 (1) | 2.837 (2) | 162 (2) |
O14—H26···O11iii | 0.85 (1) | 2.59 (1) | 3.381 (2) | 156 (2) |
O15—H27···O10viii | 0.85 (1) | 2.65 (2) | 3.242 (2) | 128 (2) |
O15—H27···O12viii | 0.85 (1) | 1.96 (1) | 2.779 (2) | 165 (2) |
O15—H28···O8i | 0.85 (1) | 2.11 (1) | 2.856 (2) | 147 (2) |
O15—H28···O9i | 0.85 (1) | 2.44 (1) | 3.174 (2) | 145 (2) |
Symmetry codes: (i) −x+1, −y, −z+1; (ii) x−1, y, z; (iii) x−2, y, z−1; (iv) −x, −y, −z+1; (v) −x, −y, −z; (vi) x+1, y, z; (vii) x−1, y, z−1; (viii) −x+2, −y, −z+1. |