The title complex, alternatively called hexaaquamagnesium(II) p-phenylenebis(oxyacetate), [Mg(H2O)6](C10H8O6), has been synthesized by the reaction of Mg(NO3)2·6H2O and benzene-1,4-dioxyacetic acid in an aqueous solution. The MgII atom is coordinated by six water molecules to form an octahedron [Mg-O = 2.0433 (16)-2.1281 (18) Å]. The cations and anions, which lie on centres of symmetry, are linked by hydrogen bonds into a three-dimensional network structure.
Supporting information
CCDC reference: 263545
Key indicators
- Single-crystal X-ray study
- T = 296 K
- Mean (C-C) = 0.003 Å
- R factor = 0.046
- wR factor = 0.122
- Data-to-parameter ratio = 13.8
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT733_ALERT_1_B Torsion Calc -178.8(2), Rep -179.1(15) ...... 7.50 su-Rat
C4 -O3 -C2 -C1 1.555 1.555 1.555 1.555
Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.52
PLAT703_ALERT_1_C Torsion Calc -178.8(2), Rep -179.1(15), Dev.. 1.50 Sigma
C4 -O3 -C2 -C1 1.555 1.555 1.555 1.555
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 6
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 1
C10 H8 O6
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
6 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
3 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
1 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, 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)
p-phenylenebis(oxyacetate)
top
Crystal data top
[Mg(H2O)6](C10H8O6) | Z = 1 |
Mr = 356.57 | F(000) = 188 |
Triclinic, P1 | Dx = 1.557 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 5.5677 (11) Å | Cell parameters from 3689 reflections |
b = 6.3662 (13) Å | θ = 3.5–27.5° |
c = 11.620 (2) Å | µ = 0.18 mm−1 |
α = 102.11 (3)° | T = 296 K |
β = 95.59 (3)° | Prism, colorless |
γ = 106.68 (3)° | 0.37 × 0.25 × 0.18 mm |
V = 380.26 (16) Å3 | |
Data collection top
Rigaku R-AXIS RAPID diffractometer | 1710 independent reflections |
Radiation source: fine-focus sealed tube | 1321 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.027 |
Detector resolution: 10 pixels mm-1 | θmax = 27.5°, θmin = 3.5° |
ω scans | h = −7→7 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −8→8 |
Tmin = 0.947, Tmax = 0.968 | l = −14→14 |
3747 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)] = 0.046 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.122 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0638P)2 + 0.1773P] where P = (Fo2 + 2Fc2)/3 |
1710 reflections | (Δ/σ)max < 0.001 |
124 parameters | Δρmax = 0.49 e Å−3 |
9 restraints | Δρmin = −0.30 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 | 0.0238 (2) | |
O1 | 0.2118 (3) | 0.5640 (3) | 0.20508 (14) | 0.0406 (4) | |
O2 | 0.1323 (3) | 0.8429 (3) | 0.32875 (13) | 0.0324 (4) | |
O3 | −0.1693 (3) | 0.9040 (3) | 0.16086 (13) | 0.0359 (4) | |
O1W | 0.3654 (3) | 0.3596 (3) | 0.63313 (15) | 0.0415 (4) | |
O2W | 0.3078 (3) | 0.7349 (3) | 0.52992 (14) | 0.0364 (4) | |
O3W | 0.1747 (3) | 0.2879 (3) | 0.37269 (13) | 0.0327 (4) | |
C1 | 0.1087 (3) | 0.7127 (3) | 0.22690 (18) | 0.0254 (4) | |
C2 | −0.0627 (4) | 0.7318 (3) | 0.12087 (17) | 0.0269 (4) | |
C3 | −0.3339 (4) | 0.9452 (3) | 0.07751 (17) | 0.0258 (4) | |
C4 | −0.4347 (4) | 1.1132 (4) | 0.12022 (18) | 0.0297 (4) | |
C5 | −0.3983 (4) | 0.8299 (4) | −0.04327 (18) | 0.0284 (4) | |
H1W1 | 0.225 (3) | 0.262 (4) | 0.635 (3) | 0.062* | |
H1W2 | 0.480 (4) | 0.357 (5) | 0.686 (2) | 0.062* | |
H2W1 | 0.181 (4) | 0.714 (5) | 0.567 (2) | 0.055* | |
H2W2 | 0.270 (5) | 0.788 (5) | 0.4705 (17) | 0.055* | |
H3W1 | 0.160 (5) | 0.341 (4) | 0.3126 (16) | 0.049* | |
H3W2 | 0.149 (5) | 0.1465 (18) | 0.351 (2) | 0.049* | |
H2A | 0.0359 | 0.7676 | 0.0592 | 0.032* | |
H2B | −0.1967 | 0.5889 | 0.0874 | 0.032* | |
H4 | −0.3920 | 1.1896 | 0.2006 | 0.036* | |
H5 | −0.3304 | 0.7158 | −0.0724 | 0.034* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Mg1 | 0.0243 (4) | 0.0283 (5) | 0.0215 (5) | 0.0116 (4) | 0.0021 (3) | 0.0082 (4) |
O1 | 0.0523 (9) | 0.0456 (10) | 0.0341 (8) | 0.0344 (8) | −0.0004 (7) | 0.0084 (7) |
O2 | 0.0381 (8) | 0.0381 (9) | 0.0253 (7) | 0.0207 (7) | −0.0007 (6) | 0.0081 (6) |
O3 | 0.0465 (9) | 0.0428 (9) | 0.0246 (7) | 0.0311 (7) | −0.0060 (6) | 0.0035 (6) |
O1W | 0.0283 (8) | 0.0647 (12) | 0.0379 (9) | 0.0121 (8) | 0.0051 (7) | 0.0301 (8) |
O2W | 0.0435 (9) | 0.0444 (10) | 0.0322 (8) | 0.0272 (8) | 0.0076 (7) | 0.0132 (7) |
O3W | 0.0376 (8) | 0.0298 (8) | 0.0291 (8) | 0.0108 (7) | −0.0010 (6) | 0.0065 (6) |
C1 | 0.0253 (9) | 0.0276 (10) | 0.0266 (10) | 0.0106 (8) | 0.0023 (7) | 0.0113 (8) |
C2 | 0.0311 (10) | 0.0279 (10) | 0.0246 (9) | 0.0150 (8) | −0.0005 (8) | 0.0069 (8) |
C3 | 0.0277 (9) | 0.0290 (10) | 0.0231 (9) | 0.0132 (8) | −0.0017 (7) | 0.0085 (8) |
C4 | 0.0374 (10) | 0.0330 (11) | 0.0197 (9) | 0.0178 (9) | −0.0025 (8) | 0.0025 (8) |
C5 | 0.0334 (10) | 0.0287 (10) | 0.0264 (10) | 0.0184 (8) | 0.0006 (8) | 0.0037 (8) |
Geometric parameters (Å, º) top
Mg1—O1w | 2.0433 (16) | O2W—H2W2 | 0.86 (2) |
Mg1—O2w | 2.0677 (16) | O3W—H3W1 | 0.84 (2) |
Mg1—O3w | 2.1281 (18) | O3W—H3W2 | 0.85 (2) |
O1—C1 | 1.237 (2) | C1—C2 | 1.531 (3) |
O2—C1 | 1.265 (3) | C2—H2A | 0.9700 |
Mg1—O1Wi | 2.0433 (16) | C2—H2B | 0.9700 |
Mg1—O2Wi | 2.0677 (16) | C3—C4 | 1.372 (3) |
Mg1—O3Wi | 2.1281 (18) | C3—C5 | 1.398 (3) |
O3—C2 | 1.408 (2) | C4—C5ii | 1.401 (3) |
O3—C3 | 1.385 (2) | C4—H4 | 0.9300 |
O1W—H1W1 | 0.85 (2) | C5—C4ii | 1.401 (3) |
O1W—H1W2 | 0.84 (2) | C5—H5 | 0.9300 |
O2W—H2W1 | 0.86 (2) | | |
| | | |
O1w—Mg1—O1wi | 180 | O1W—Mg1—O2Wi | 87.50 (7) |
O1w—Mg1—O2w | 92.50 (7) | O1Wi—Mg1—O2Wi | 92.50 (7) |
O1w—Mg1—O3w | 92.03 (7) | O1W—Mg1—O3Wi | 87.97 (7) |
O1wi—Mg1—O2w | 87.50 (7) | O1Wi—Mg1—O3Wi | 92.03 (7) |
O1wi—Mg1—O3w | 87.97 (7) | O2Wi—Mg1—O3Wi | 86.91 (7) |
O2wi—Mg1—O2w | 180 | O2W—Mg1—O3Wi | 93.09 (7) |
O2wi—Mg1—O3w | 93.09 (7) | C1—C2—H2A | 110.0 |
O2w—Mg1—O3w | 86.91 (7) | C1—C2—H2B | 110.0 |
O3wi—Mg1—O3w | 180 | C3—O3—C2 | 117.38 (15) |
Mg1—O1W—H1W1 | 131.6 (19) | C3—C4—C5ii | 120.27 (18) |
Mg1—O1W—H1W2 | 114.4 (19) | C3—C4—H4 | 119.9 |
Mg1—O2W—H2W1 | 121.2 (19) | C3—C5—C4ii | 119.84 (18) |
Mg1—O2W—H2W2 | 117.1 (18) | C3—C5—H5 | 120.1 |
Mg1—O3W—H3W1 | 110.9 (18) | C4—C3—O3 | 115.55 (17) |
Mg1—O3W—H3W2 | 120.1 (18) | C4—C3—C5 | 119.89 (17) |
O1—C1—O2 | 124.82 (18) | C4ii—C5—H5 | 120.1 |
O1—C1—C2 | 115.75 (18) | C5ii—C4—H4 | 119.9 |
O2—C1—C2 | 119.41 (17) | H1W1—O1W—H1W2 | 109.8 (16) |
O3—C2—C1 | 108.70 (16) | H2W1—O2W—H2W2 | 108 (3) |
O3—C2—H2A | 110.0 | H3W1—O3W—H3W2 | 110.6 (15) |
O3—C2—H2B | 110.0 | H2A—C2—H2B | 108.3 |
O3—C3—C5 | 124.55 (18) | | |
| | | |
O1—C1—C2—O3 | 178.66 (17) | C2—O3—C3—C5 | −0.9 (3) |
O2—C1—C2—O3 | −0.1 (3) | C3—O3—C2—C1 | −179.20 (16) |
O3—C3—C4—C5ii | 179.43 (19) | C4—O3—C2—C1 | −179.1 (15) |
O3—C3—C5—C4ii | −179.39 (19) | C4—C3—C5—C4ii | 0.1 (3) |
C2—O3—C3—C4 | 179.61 (18) | C5—C3—C4—C5ii | −0.1 (3) |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x−1, −y+2, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1w—H1w1···O2iii | 0.85 (2) | 2.03 (2) | 2.823 (2) | 155 (3) |
O1w—H1w2···O1i | 0.84 (2) | 1.90 (2) | 2.722 (2) | 163 (3) |
O2w—H2w1···O3wiii | 0.86 (2) | 2.16 (2) | 2.993 (2) | 164 (2) |
O2w—H2w2···O2 | 0.86 (2) | 1.89 (2) | 2.740 (2) | 168 (3) |
O3w—H3w1···O1 | 0.84 (2) | 2.06 (2) | 2.869 (2) | 161 (2) |
O3w—H3w2···O2iv | 0.85 (2) | 1.87 (2) | 2.707 (2) | 170 (2) |
O3w—H3w2···O3iv | 0.85 (2) | 2.58 (2) | 3.094 (3) | 120 (2) |
Symmetry codes: (i) −x+1, −y+1, −z+1; (iii) −x, −y+1, −z+1; (iv) x, y−1, z. |