Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270104012867/na1658sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270104012867/na1658Isup2.hkl |
CCDC reference: 245872
All chemicals were of A·R. grade, commercially available from the Beijing Chemical Reagents Company in China, and were used without further purification. The ligand Cl-HXTA was synthesized following a modification of the published procedures of Murch et al. (1987) and Branum et al. (2001). To an aqueous solution (100 ml) of iminodiacetic acid (16.7 g, 0.125 mol) and p-chlorophenol (8.07 g, 0.063 mol) was added NaOH (10.5 g, 0.25 mol) in water (40 ml) in an ice-water bath. Upon dissolution, formaldehyde (15 ml, 37%) was added dropwise at 273 K. The solution was stirred for 30 min, heated at 343 K for 4 h and then concentrated to dryness. Recrystallization of the solid from methanol produced light-yellow crystals of Na4(Cl-HXTA) (yield 90%). MgSO4·7H2O (0.4929 g, 2 mmol) and Na4(Cl-HXTA) (0.5165 g, 1 mmol) were each dissolved in H2O (5.0 ml). The two solutions were mixed at 323 K with stirring and kept agitating for 2 h. The resulting colourless solution was filtered and the filtrate was used to grow crystals at room temperature over anhydrous CaCl2 in a desiccator. Colourless crystals of (I) suitable for X-ray crystallography were obtained after 10 d by slow evaporation of the solvent.
H atoms attached to C atoms were placed in geometrically idealized positions, with Csp3—H = 0.970 (for methylene) and Csp2 = 0.930 Å, and constrained to ride on their parent atoms, with Uiso(H) = 1.2Ueq(C). H atoms attached to O atoms (in water molecules) were located in difference Fourier maps and constrained to ride on their parent atoms, with Uiso(H) = 1.2Ueq(O).
Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL/PC (Sheldrick, 1999); software used to prepare material for publication: SHELXTL/PC.
[Mg(H2O)6]0.5[Mg2(C16H14ClN2O9)(H2O)4]·10H2O | Z = 2 |
Mr = 780.79 | F(000) = 826 |
Triclinic, P1 | Dx = 1.507 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 9.871 (2) Å | Cell parameters from 3324 reflections |
b = 13.119 (3) Å | θ = 2.2–26.4° |
c = 13.438 (3) Å | µ = 0.25 mm−1 |
α = 88.421 (3)° | T = 183 K |
β = 84.029 (2)° | Block, colourless |
γ = 84.050 (3)° | 0.30 × 0.20 × 0.20 mm |
V = 1721.2 (6) Å3 |
Bruker SMART 1K CCD area-detector diffractometer | 5921 independent reflections |
Radiation source: fine-focus sealed tube | 4743 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.016 |
ϕ and ω scans | θmax = 25.0°, θmin = 1.5° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2000) | h = −11→11 |
Tmin = 0.928, Tmax = 0.951 | k = −15→14 |
7116 measured reflections | l = −15→15 |
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)] = 0.050 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.137 | H-atom parameters constrained |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0783P)2] where P = (Fo2 + 2Fc2)/3 |
5921 reflections | (Δ/σ)max = 0.001 |
430 parameters | Δρmax = 1.22 e Å−3 |
0 restraints | Δρmin = −1.12 e Å−3 |
[Mg(H2O)6]0.5[Mg2(C16H14ClN2O9)(H2O)4]·10H2O | γ = 84.050 (3)° |
Mr = 780.79 | V = 1721.2 (6) Å3 |
Triclinic, P1 | Z = 2 |
a = 9.871 (2) Å | Mo Kα radiation |
b = 13.119 (3) Å | µ = 0.25 mm−1 |
c = 13.438 (3) Å | T = 183 K |
α = 88.421 (3)° | 0.30 × 0.20 × 0.20 mm |
β = 84.029 (2)° |
Bruker SMART 1K CCD area-detector diffractometer | 5921 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 2000) | 4743 reflections with I > 2σ(I) |
Tmin = 0.928, Tmax = 0.951 | Rint = 0.016 |
7116 measured reflections |
R[F2 > 2σ(F2)] = 0.050 | 0 restraints |
wR(F2) = 0.137 | H-atom parameters constrained |
S = 1.05 | Δρmax = 1.22 e Å−3 |
5921 reflections | Δρmin = −1.12 e Å−3 |
430 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
Mg1 | 0.25058 (9) | 0.28947 (7) | 0.12477 (6) | 0.0208 (2) | |
N1 | 0.0853 (2) | 0.28325 (17) | 0.02677 (15) | 0.0208 (5) | |
O1 | 0.23642 (18) | 0.13804 (13) | 0.16583 (13) | 0.0215 (4) | |
O3 | 0.36293 (18) | 0.27078 (15) | −0.01291 (13) | 0.0259 (4) | |
O4 | 0.07700 (18) | 0.34135 (14) | 0.21915 (13) | 0.0240 (4) | |
O10 | 0.3892 (2) | 0.28969 (16) | 0.22468 (15) | 0.0339 (5) | |
H10C | 0.4084 | 0.2352 | 0.2642 | 0.041* | |
H10D | 0.4552 | 0.3212 | 0.2184 | 0.041* | |
O11 | 0.2600 (2) | 0.44749 (15) | 0.09321 (15) | 0.0331 (5) | |
H11A | 0.3257 | 0.4710 | 0.0613 | 0.040* | |
H11B | 0.2223 | 0.4921 | 0.1328 | 0.040* | |
Mg2 | 0.20534 (9) | 0.06441 (7) | 0.30351 (6) | 0.0212 (2) | |
N2 | 0.3662 (2) | −0.05934 (17) | 0.25833 (16) | 0.0211 (5) | |
O6 | 0.09101 (18) | −0.04285 (14) | 0.25160 (14) | 0.0266 (5) | |
O8 | 0.38225 (18) | 0.11556 (14) | 0.35318 (13) | 0.0254 (4) | |
O12 | 0.0679 (2) | 0.17992 (16) | 0.34937 (15) | 0.0405 (6) | |
H12C | 0.0237 | 0.1855 | 0.4033 | 0.049* | |
H12D | 0.0468 | 0.2317 | 0.3086 | 0.049* | |
O13 | 0.1598 (2) | −0.00291 (15) | 0.44291 (14) | 0.0328 (5) | |
H13C | 0.1236 | −0.0564 | 0.4516 | 0.039* | |
H13D | 0.1596 | 0.0243 | 0.5011 | 0.039* | |
C1 | 0.2575 (3) | −0.0548 (2) | −0.0725 (2) | 0.0240 (6) | |
C2 | 0.3467 (3) | −0.0766 (2) | −0.0005 (2) | 0.0239 (6) | |
H2 | 0.4101 | −0.1342 | −0.0061 | 0.029* | |
C3 | 0.3412 (3) | −0.0117 (2) | 0.08065 (19) | 0.0215 (6) | |
C4 | 0.2432 (3) | 0.0748 (2) | 0.08794 (19) | 0.0199 (6) | |
C5 | 0.1515 (3) | 0.0932 (2) | 0.01519 (19) | 0.0211 (6) | |
C6 | 0.1596 (3) | 0.0283 (2) | −0.0659 (2) | 0.0251 (6) | |
H6 | 0.0997 | 0.0408 | −0.1149 | 0.030* | |
C7 | 0.0381 (3) | 0.1787 (2) | 0.0323 (2) | 0.0234 (6) | |
H7A | −0.0259 | 0.1746 | −0.0172 | 0.028* | |
H7B | −0.0107 | 0.1688 | 0.0977 | 0.028* | |
C8 | −0.0287 (3) | 0.3570 (2) | 0.0667 (2) | 0.0255 (6) | |
H8A | −0.1144 | 0.3353 | 0.0498 | 0.031* | |
H8B | −0.0182 | 0.4238 | 0.0356 | 0.031* | |
C9 | −0.0337 (3) | 0.3658 (2) | 0.1802 (2) | 0.0267 (6) | |
C10 | 0.1442 (3) | 0.3070 (2) | −0.07600 (19) | 0.0256 (6) | |
H10A | 0.1211 | 0.3791 | −0.0908 | 0.031* | |
H10B | 0.1035 | 0.2677 | −0.1231 | 0.031* | |
C11 | 0.2994 (3) | 0.2828 (2) | −0.0902 (2) | 0.0238 (6) | |
C12 | 0.4376 (3) | −0.0312 (2) | 0.15924 (19) | 0.0228 (6) | |
H12A | 0.4833 | 0.0297 | 0.1664 | 0.027* | |
H12B | 0.5069 | −0.0864 | 0.1381 | 0.027* | |
C13 | 0.2991 (3) | −0.1535 (2) | 0.2522 (2) | 0.0244 (6) | |
H13A | 0.3025 | −0.1915 | 0.3150 | 0.029* | |
H13B | 0.3487 | −0.1960 | 0.1998 | 0.029* | |
C14 | 0.1497 (3) | −0.1308 (2) | 0.2303 (2) | 0.0263 (6) | |
C15 | 0.4633 (3) | −0.0623 (2) | 0.3341 (2) | 0.0255 (6) | |
H15A | 0.5509 | −0.0964 | 0.3075 | 0.031* | |
H15B | 0.4295 | −0.1008 | 0.3925 | 0.031* | |
C16 | 0.4810 (3) | 0.0469 (2) | 0.36380 (19) | 0.0243 (6) | |
Cl1 | 0.27111 (8) | −0.13582 (6) | −0.17551 (5) | 0.0364 (2) | |
Mg3 | 0.0000 | 0.5000 | 0.5000 | 0.0260 (3) | |
O24 | 0.1462 (2) | 0.41896 (16) | 0.40522 (15) | 0.0362 (5) | |
H24A | 0.1328 | 0.3977 | 0.3461 | 0.043* | |
H24B | 0.2083 | 0.3829 | 0.4286 | 0.043* | |
O25 | 0.0093 (2) | 0.62042 (15) | 0.39533 (14) | 0.0321 (5) | |
H25A | 0.0623 | 0.6088 | 0.3437 | 0.039* | |
H25B | −0.0674 | 0.6530 | 0.3734 | 0.039* | |
O26 | 0.1566 (2) | 0.55080 (17) | 0.56955 (15) | 0.0386 (5) | |
H26A | 0.1498 | 0.5649 | 0.6312 | 0.046* | |
H26B | 0.2315 | 0.5615 | 0.5394 | 0.046* | |
O2 | 0.3547 (2) | 0.28069 (17) | −0.17779 (14) | 0.0334 (5) | |
O5 | −0.1428 (2) | 0.3975 (2) | 0.22821 (16) | 0.0484 (7) | |
O7 | 0.0927 (2) | −0.20135 (16) | 0.19791 (18) | 0.0420 (6) | |
O9 | 0.58955 (19) | 0.06212 (16) | 0.39794 (15) | 0.0328 (5) | |
O14 | 0.5885 (5) | 0.3831 (5) | 0.9885 (3) | 0.265 (5) | |
H14A | 0.5675 | 0.3274 | 0.9685 | 0.318* | |
H14B | 0.5225 | 0.4246 | 0.9975 | 0.318* | |
O15 | 0.5924 (2) | 0.41402 (19) | 0.1864 (2) | 0.0590 (7) | |
H15C | 0.5568 | 0.4670 | 0.2233 | 0.071* | |
H15D | 0.6756 | 0.4053 | 0.1981 | 0.071* | |
O16 | 0.3590 (2) | 0.29611 (17) | 0.47508 (16) | 0.0425 (6) | |
H16A | 0.3611 | 0.2437 | 0.4469 | 0.051* | |
H16B | 0.3234 | 0.2863 | 0.5328 | 0.051* | |
O17 | 0.6855 (3) | 0.2471 (2) | 0.3979 (2) | 0.0598 (7) | |
H17A | 0.6430 | 0.1880 | 0.3900 | 0.072* | |
H17B | 0.6923 | 0.2762 | 0.3440 | 0.072* | |
O18 | 0.8911 (2) | 0.20793 (17) | 0.51810 (16) | 0.0404 (5) | |
H18A | 0.8241 | 0.2314 | 0.4819 | 0.049* | |
H18B | 0.9207 | 0.2584 | 0.5425 | 0.049* | |
O19 | 0.2159 (2) | 0.26359 (16) | 0.65840 (15) | 0.0353 (5) | |
H19A | 0.2568 | 0.2685 | 0.7079 | 0.042* | |
H19B | 0.1906 | 0.2058 | 0.6625 | 0.042* | |
O20 | 0.5854 (3) | 0.4155 (2) | 0.5270 (2) | 0.0601 (7) | |
H20A | 0.5218 | 0.4586 | 0.5166 | 0.072* | |
H20B | 0.5573 | 0.3553 | 0.5079 | 0.072* | |
O21 | 0.5410 (2) | 0.40710 (18) | 0.73326 (18) | 0.0472 (6) | |
H21A | 0.4934 | 0.3644 | 0.7585 | 0.057* | |
H21B | 0.5382 | 0.4079 | 0.6731 | 0.057* | |
O22 | 0.1886 (2) | 0.60382 (16) | 0.22587 (16) | 0.0387 (5) | |
H22A | 0.2766 | 0.6061 | 0.2389 | 0.046* | |
H22B | 0.1641 | 0.6623 | 0.2124 | 0.046* | |
O23 | 0.8368 (2) | 0.93689 (16) | 0.36189 (15) | 0.0355 (5) | |
H23A | 0.8995 | 0.9515 | 0.3226 | 0.043* | |
H23B | 0.7696 | 0.9767 | 0.3507 | 0.043* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mg1 | 0.0205 (5) | 0.0215 (5) | 0.0209 (5) | −0.0039 (4) | −0.0019 (4) | −0.0016 (4) |
N1 | 0.0184 (11) | 0.0235 (12) | 0.0199 (11) | −0.0016 (9) | 0.0000 (9) | −0.0009 (9) |
O1 | 0.0253 (10) | 0.0206 (10) | 0.0194 (9) | −0.0038 (8) | −0.0040 (8) | −0.0026 (8) |
O3 | 0.0229 (10) | 0.0329 (11) | 0.0222 (10) | −0.0059 (8) | −0.0002 (8) | −0.0022 (8) |
O4 | 0.0222 (10) | 0.0259 (11) | 0.0238 (10) | −0.0012 (8) | −0.0022 (8) | −0.0024 (8) |
O10 | 0.0330 (12) | 0.0328 (12) | 0.0399 (12) | −0.0133 (9) | −0.0145 (9) | 0.0069 (10) |
O11 | 0.0359 (12) | 0.0261 (11) | 0.0366 (12) | −0.0084 (9) | 0.0059 (9) | −0.0032 (9) |
Mg2 | 0.0210 (5) | 0.0220 (5) | 0.0206 (5) | −0.0031 (4) | −0.0013 (4) | −0.0016 (4) |
N2 | 0.0205 (12) | 0.0223 (12) | 0.0215 (12) | −0.0039 (9) | −0.0044 (9) | −0.0001 (10) |
O6 | 0.0232 (10) | 0.0268 (11) | 0.0306 (11) | −0.0047 (8) | −0.0045 (8) | 0.0002 (9) |
O8 | 0.0256 (10) | 0.0273 (11) | 0.0247 (10) | −0.0048 (9) | −0.0061 (8) | −0.0036 (8) |
O12 | 0.0478 (13) | 0.0332 (12) | 0.0329 (12) | 0.0109 (10) | 0.0158 (10) | 0.0047 (10) |
O13 | 0.0449 (13) | 0.0322 (12) | 0.0228 (10) | −0.0137 (10) | 0.0001 (9) | −0.0007 (9) |
C1 | 0.0249 (15) | 0.0274 (16) | 0.0203 (14) | −0.0107 (12) | 0.0046 (12) | −0.0080 (12) |
C2 | 0.0245 (15) | 0.0199 (15) | 0.0266 (15) | −0.0055 (11) | 0.0043 (12) | −0.0046 (12) |
C3 | 0.0210 (14) | 0.0237 (15) | 0.0200 (14) | −0.0070 (11) | 0.0013 (11) | 0.0012 (11) |
C4 | 0.0221 (14) | 0.0199 (14) | 0.0182 (13) | −0.0086 (11) | 0.0031 (11) | −0.0028 (11) |
C5 | 0.0219 (14) | 0.0199 (14) | 0.0222 (14) | −0.0074 (11) | 0.0001 (11) | −0.0001 (11) |
C6 | 0.0257 (15) | 0.0307 (16) | 0.0208 (14) | −0.0122 (13) | −0.0020 (12) | −0.0012 (12) |
C7 | 0.0208 (14) | 0.0275 (16) | 0.0234 (14) | −0.0082 (12) | −0.0037 (11) | −0.0009 (12) |
C8 | 0.0242 (15) | 0.0240 (15) | 0.0280 (15) | 0.0006 (12) | −0.0039 (12) | 0.0004 (12) |
C9 | 0.0266 (16) | 0.0248 (16) | 0.0288 (15) | −0.0023 (12) | −0.0036 (13) | −0.0032 (12) |
C10 | 0.0263 (15) | 0.0311 (16) | 0.0202 (14) | −0.0051 (12) | −0.0046 (12) | 0.0021 (12) |
C11 | 0.0265 (15) | 0.0214 (15) | 0.0246 (15) | −0.0075 (12) | −0.0018 (12) | −0.0026 (12) |
C12 | 0.0181 (14) | 0.0243 (15) | 0.0253 (15) | −0.0022 (11) | 0.0019 (11) | −0.0039 (12) |
C13 | 0.0267 (15) | 0.0208 (15) | 0.0260 (15) | −0.0034 (12) | −0.0029 (12) | −0.0012 (12) |
C14 | 0.0308 (16) | 0.0270 (17) | 0.0229 (14) | −0.0079 (13) | −0.0067 (12) | 0.0028 (12) |
C15 | 0.0228 (14) | 0.0264 (16) | 0.0277 (15) | −0.0004 (12) | −0.0066 (12) | −0.0001 (12) |
C16 | 0.0230 (15) | 0.0314 (16) | 0.0193 (14) | −0.0070 (13) | −0.0018 (12) | 0.0014 (12) |
Cl1 | 0.0364 (4) | 0.0441 (5) | 0.0292 (4) | −0.0091 (3) | 0.0035 (3) | −0.0181 (3) |
Mg3 | 0.0292 (7) | 0.0247 (7) | 0.0248 (7) | −0.0048 (6) | −0.0035 (6) | −0.0035 (6) |
O24 | 0.0405 (13) | 0.0383 (13) | 0.0288 (11) | 0.0059 (10) | −0.0059 (10) | −0.0110 (10) |
O25 | 0.0312 (11) | 0.0325 (12) | 0.0311 (11) | −0.0006 (9) | 0.0009 (9) | 0.0027 (9) |
O26 | 0.0332 (12) | 0.0548 (15) | 0.0301 (11) | −0.0144 (10) | −0.0013 (9) | −0.0101 (10) |
O2 | 0.0297 (11) | 0.0488 (14) | 0.0215 (11) | −0.0086 (10) | 0.0037 (9) | −0.0036 (9) |
O5 | 0.0253 (12) | 0.0821 (19) | 0.0354 (13) | 0.0128 (11) | −0.0026 (10) | −0.0255 (12) |
O7 | 0.0431 (13) | 0.0286 (12) | 0.0603 (15) | −0.0110 (10) | −0.0253 (11) | −0.0041 (11) |
O9 | 0.0267 (11) | 0.0382 (13) | 0.0358 (12) | −0.0064 (9) | −0.0096 (9) | −0.0054 (10) |
O14 | 0.244 (6) | 0.523 (11) | 0.097 (3) | −0.330 (7) | −0.098 (3) | 0.154 (5) |
O15 | 0.0315 (13) | 0.0387 (14) | 0.109 (2) | −0.0071 (11) | −0.0109 (14) | −0.0128 (15) |
O16 | 0.0497 (14) | 0.0402 (14) | 0.0360 (12) | −0.0015 (11) | 0.0031 (10) | −0.0092 (10) |
O17 | 0.0662 (17) | 0.0529 (17) | 0.0643 (17) | −0.0187 (14) | −0.0097 (14) | −0.0141 (14) |
O18 | 0.0484 (14) | 0.0352 (13) | 0.0376 (12) | −0.0103 (10) | 0.0034 (10) | −0.0042 (10) |
O19 | 0.0367 (12) | 0.0385 (13) | 0.0319 (11) | −0.0053 (10) | −0.0084 (9) | −0.0003 (10) |
O20 | 0.0565 (16) | 0.0558 (17) | 0.0675 (18) | −0.0140 (13) | 0.0081 (14) | −0.0147 (14) |
O21 | 0.0398 (13) | 0.0446 (15) | 0.0569 (15) | −0.0101 (11) | 0.0008 (11) | 0.0037 (12) |
O22 | 0.0381 (12) | 0.0279 (12) | 0.0498 (14) | −0.0047 (10) | −0.0017 (10) | −0.0047 (10) |
O23 | 0.0264 (11) | 0.0411 (13) | 0.0382 (12) | −0.0021 (9) | 0.0004 (9) | −0.0023 (10) |
Mg1—O10 | 2.015 (2) | C9—O5 | 1.236 (3) |
Mg1—O1 | 2.062 (2) | C10—C11 | 1.525 (4) |
Mg1—O3 | 2.063 (2) | C10—H10A | 0.9700 |
Mg1—O4 | 2.088 (2) | C10—H10B | 0.9700 |
Mg1—O11 | 2.114 (2) | C11—O2 | 1.245 (3) |
Mg1—N1 | 2.210 (2) | C12—H12A | 0.9700 |
N1—C8 | 1.472 (3) | C12—H12B | 0.9700 |
N1—C10 | 1.480 (3) | C13—C14 | 1.531 (4) |
N1—C7 | 1.490 (3) | C13—H13A | 0.9700 |
O1—C4 | 1.345 (3) | C13—H13B | 0.9700 |
O1—Mg2 | 2.072 (2) | C14—O7 | 1.242 (3) |
O3—C11 | 1.266 (3) | C15—C16 | 1.530 (4) |
O4—C9 | 1.268 (3) | C15—H15A | 0.9700 |
O10—H10C | 0.8944 | C15—H15B | 0.9700 |
O10—H10D | 0.8031 | C16—O9 | 1.245 (3) |
O11—H11A | 0.8216 | Mg3—O24i | 2.051 (2) |
O11—H11B | 0.8336 | Mg3—O24 | 2.051 (2) |
Mg2—O12 | 1.992 (2) | Mg3—O26 | 2.0634 (19) |
Mg2—O6 | 2.071 (2) | Mg3—O26i | 2.0634 (19) |
Mg2—O13 | 2.075 (2) | Mg3—O25i | 2.089 (2) |
Mg2—O8 | 2.111 (2) | Mg3—O25 | 2.089 (2) |
Mg2—N2 | 2.201 (2) | O24—H24A | 0.8757 |
N2—C15 | 1.466 (3) | O24—H24B | 0.8186 |
N2—C13 | 1.469 (3) | O25—H25A | 0.8314 |
N2—C12 | 1.496 (3) | O25—H25B | 0.9034 |
O6—C14 | 1.262 (3) | O26—H26A | 0.8482 |
O8—C16 | 1.274 (3) | O26—H26B | 0.8288 |
O12—H12C | 0.8066 | O14—H14A | 0.8379 |
O12—H12D | 0.8822 | O14—H14B | 0.8060 |
O13—H13C | 0.8207 | O15—H15C | 0.8852 |
O13—H13D | 0.8687 | O15—H15D | 0.8483 |
C1—C6 | 1.378 (4) | O16—H16A | 0.7910 |
C1—C2 | 1.379 (4) | O16—H16B | 0.8295 |
C1—Cl1 | 1.754 (3) | O17—H17A | 0.9329 |
C2—C3 | 1.395 (4) | O17—H17B | 0.8096 |
C2—H2 | 0.9300 | O18—H18A | 0.8861 |
C3—C4 | 1.412 (4) | O18—H18B | 0.8392 |
C3—C12 | 1.493 (4) | O19—H19A | 0.8201 |
C4—C5 | 1.400 (4) | O19—H19B | 0.8215 |
C5—C6 | 1.393 (4) | O20—H20A | 0.8198 |
C5—C7 | 1.505 (4) | O20—H20B | 0.9162 |
C6—H6 | 0.9300 | O21—H21A | 0.8124 |
C7—H7A | 0.9700 | O21—H21B | 0.8120 |
C7—H7B | 0.9700 | O22—H22A | 0.9081 |
C8—C9 | 1.528 (4) | O22—H22B | 0.8010 |
C8—H8A | 0.9700 | O23—H23A | 0.8055 |
C8—H8B | 0.9700 | O23—H23B | 0.8245 |
O10—Mg1—O1 | 86.59 (8) | C5—C7—H7A | 108.7 |
O10—Mg1—O3 | 105.62 (9) | N1—C7—H7B | 108.7 |
O1—Mg1—O3 | 99.82 (8) | C5—C7—H7B | 108.7 |
O10—Mg1—O4 | 97.90 (9) | H7A—C7—H7B | 107.6 |
O1—Mg1—O4 | 93.27 (8) | N1—C8—C9 | 111.6 (2) |
O3—Mg1—O4 | 153.61 (9) | N1—C8—H8A | 109.3 |
O10—Mg1—O11 | 91.51 (9) | C9—C8—H8A | 109.3 |
O1—Mg1—O11 | 175.96 (9) | N1—C8—H8B | 109.3 |
O3—Mg1—O11 | 84.13 (8) | C9—C8—H8B | 109.3 |
O4—Mg1—O11 | 83.45 (8) | H8A—C8—H8B | 108.0 |
O10—Mg1—N1 | 174.52 (9) | O5—C9—O4 | 123.9 (3) |
O1—Mg1—N1 | 90.04 (8) | O5—C9—C8 | 119.0 (3) |
O3—Mg1—N1 | 79.20 (8) | O4—C9—C8 | 117.1 (2) |
O4—Mg1—N1 | 77.97 (8) | N1—C10—C11 | 112.5 (2) |
O11—Mg1—N1 | 91.58 (9) | N1—C10—H10A | 109.1 |
C8—N1—C10 | 114.7 (2) | C11—C10—H10A | 109.1 |
C8—N1—C7 | 108.7 (2) | N1—C10—H10B | 109.1 |
C10—N1—C7 | 110.6 (2) | C11—C10—H10B | 109.1 |
C8—N1—Mg1 | 106.48 (16) | H10A—C10—H10B | 107.8 |
C10—N1—Mg1 | 106.59 (15) | O2—C11—O3 | 124.8 (3) |
C7—N1—Mg1 | 109.68 (16) | O2—C11—C10 | 116.9 (2) |
C4—O1—Mg1 | 113.87 (15) | O3—C11—C10 | 118.2 (2) |
C4—O1—Mg2 | 113.35 (15) | C3—C12—N2 | 112.3 (2) |
Mg1—O1—Mg2 | 132.72 (9) | C3—C12—H12A | 109.1 |
C11—O3—Mg1 | 117.88 (17) | N2—C12—H12A | 109.1 |
C9—O4—Mg1 | 118.00 (17) | C3—C12—H12B | 109.1 |
Mg1—O10—H10C | 121.6 | N2—C12—H12B | 109.1 |
Mg1—O10—H10D | 125.2 | H12A—C12—H12B | 107.9 |
H10C—O10—H10D | 107.4 | N2—C13—C14 | 112.0 (2) |
Mg1—O11—H11A | 123.7 | N2—C13—H13A | 109.2 |
Mg1—O11—H11B | 121.6 | C14—C13—H13A | 109.2 |
H11A—O11—H11B | 108.0 | N2—C13—H13B | 109.2 |
O12—Mg2—O6 | 104.57 (9) | C14—C13—H13B | 109.2 |
O12—Mg2—O1 | 89.45 (8) | H13A—C13—H13B | 107.9 |
O6—Mg2—O1 | 94.33 (8) | O7—C14—O6 | 124.6 (3) |
O12—Mg2—O13 | 86.54 (9) | O7—C14—C13 | 118.0 (3) |
O6—Mg2—O13 | 85.07 (8) | O6—C14—C13 | 117.3 (2) |
O1—Mg2—O13 | 175.66 (9) | N2—C15—C16 | 109.8 (2) |
O12—Mg2—O8 | 99.64 (9) | N2—C15—H15A | 109.7 |
O6—Mg2—O8 | 154.89 (9) | C16—C15—H15A | 109.7 |
O1—Mg2—O8 | 92.44 (8) | N2—C15—H15B | 109.7 |
O13—Mg2—O8 | 89.88 (8) | C16—C15—H15B | 109.7 |
O12—Mg2—N2 | 176.46 (10) | H15A—C15—H15B | 108.2 |
O6—Mg2—N2 | 78.81 (8) | O9—C16—O8 | 124.7 (3) |
O1—Mg2—N2 | 91.36 (8) | O9—C16—C15 | 118.0 (2) |
O13—Mg2—N2 | 92.74 (9) | O8—C16—C15 | 117.3 (2) |
O8—Mg2—N2 | 76.89 (8) | O24i—Mg3—O24 | 180.0 |
C15—N2—C13 | 114.8 (2) | O24i—Mg3—O26 | 91.98 (8) |
C15—N2—C12 | 108.8 (2) | O24—Mg3—O26 | 88.02 (8) |
C13—N2—C12 | 111.3 (2) | O24i—Mg3—O26i | 88.02 (8) |
C15—N2—Mg2 | 105.48 (16) | O24—Mg3—O26i | 91.98 (8) |
C13—N2—Mg2 | 107.35 (15) | O26—Mg3—O26i | 180.00 (12) |
C12—N2—Mg2 | 108.78 (16) | O24i—Mg3—O25i | 86.88 (8) |
C14—O6—Mg2 | 118.44 (17) | O24—Mg3—O25i | 93.12 (8) |
C16—O8—Mg2 | 116.01 (17) | O26—Mg3—O25i | 89.18 (8) |
Mg2—O12—H12C | 127.2 | O26i—Mg3—O25i | 90.82 (8) |
Mg2—O12—H12D | 120.8 | O24i—Mg3—O25 | 93.12 (8) |
H12C—O12—H12D | 112.0 | O24—Mg3—O25 | 86.88 (8) |
Mg2—O13—H13C | 124.0 | O26—Mg3—O25 | 90.82 (8) |
Mg2—O13—H13D | 127.5 | O26i—Mg3—O25 | 89.18 (8) |
H13C—O13—H13D | 107.5 | O25i—Mg3—O25 | 180.0 |
C6—C1—C2 | 122.1 (2) | Mg3—O24—H24A | 124.7 |
C6—C1—Cl1 | 119.6 (2) | Mg3—O24—H24B | 119.3 |
C2—C1—Cl1 | 118.3 (2) | H24A—O24—H24B | 111.0 |
C1—C2—C3 | 119.7 (3) | Mg3—O25—H25A | 115.9 |
C1—C2—H2 | 120.2 | Mg3—O25—H25B | 121.2 |
C3—C2—H2 | 120.2 | H25A—O25—H25B | 104.7 |
C2—C3—C4 | 119.2 (2) | Mg3—O26—H26A | 123.5 |
C2—C3—C12 | 121.5 (2) | Mg3—O26—H26B | 123.1 |
C4—C3—C12 | 119.4 (2) | H26A—O26—H26B | 113.4 |
O1—C4—C5 | 120.2 (2) | H14A—O14—H14B | 111.6 |
O1—C4—C3 | 119.9 (2) | H15C—O15—H15D | 104.5 |
C5—C4—C3 | 119.8 (2) | H16A—O16—H16B | 106.4 |
C6—C5—C4 | 120.2 (2) | H17A—O17—H17B | 107.2 |
C6—C5—C7 | 121.6 (2) | H18A—O18—H18B | 107.9 |
C4—C5—C7 | 118.0 (2) | H19A—O19—H19B | 105.1 |
C1—C6—C5 | 119.1 (3) | H20A—O20—H20B | 104.0 |
C1—C6—H6 | 120.5 | H21A—O21—H21B | 109.0 |
C5—C6—H6 | 120.5 | H22A—O22—H22B | 103.3 |
N1—C7—C5 | 114.3 (2) | H23A—O23—H23B | 106.8 |
N1—C7—H7A | 108.7 | ||
O10—Mg1—N1—C8 | 65.5 (10) | N2—Mg2—O6—C14 | 8.5 (2) |
O1—Mg1—N1—C8 | 117.39 (16) | O12—Mg2—O8—C16 | 159.13 (18) |
O3—Mg1—N1—C8 | −142.62 (17) | O6—Mg2—O8—C16 | −5.4 (3) |
O4—Mg1—N1—C8 | 24.05 (16) | O1—Mg2—O8—C16 | −111.01 (18) |
O11—Mg1—N1—C8 | −58.91 (16) | O13—Mg2—O8—C16 | 72.66 (19) |
O10—Mg1—N1—C10 | −171.7 (9) | N2—Mg2—O8—C16 | −20.18 (18) |
O1—Mg1—N1—C10 | −119.79 (17) | C6—C1—C2—C3 | −1.8 (4) |
O3—Mg1—N1—C10 | −19.79 (16) | Cl1—C1—C2—C3 | 178.02 (19) |
O4—Mg1—N1—C10 | 146.88 (18) | C1—C2—C3—C4 | 0.6 (4) |
O11—Mg1—N1—C10 | 63.92 (17) | C1—C2—C3—C12 | −178.7 (2) |
O10—Mg1—N1—C7 | −52.0 (11) | Mg1—O1—C4—C5 | −55.9 (3) |
O1—Mg1—N1—C7 | −0.07 (16) | Mg2—O1—C4—C5 | 121.6 (2) |
O3—Mg1—N1—C7 | 99.92 (16) | Mg1—O1—C4—C3 | 125.6 (2) |
O4—Mg1—N1—C7 | −93.41 (16) | Mg2—O1—C4—C3 | −56.9 (3) |
O11—Mg1—N1—C7 | −176.36 (16) | C2—C3—C4—O1 | 179.9 (2) |
O10—Mg1—O1—C4 | −132.42 (17) | C12—C3—C4—O1 | −0.8 (4) |
O3—Mg1—O1—C4 | −27.15 (17) | C2—C3—C4—C5 | 1.3 (4) |
O4—Mg1—O1—C4 | 129.85 (16) | C12—C3—C4—C5 | −179.4 (2) |
O11—Mg1—O1—C4 | 165.5 (12) | O1—C4—C5—C6 | 179.4 (2) |
N1—Mg1—O1—C4 | 51.90 (17) | C3—C4—C5—C6 | −2.1 (4) |
O10—Mg1—O1—Mg2 | 50.67 (13) | O1—C4—C5—C7 | −5.8 (4) |
O3—Mg1—O1—Mg2 | 155.95 (12) | C3—C4—C5—C7 | 172.7 (2) |
O4—Mg1—O1—Mg2 | −47.05 (13) | C2—C1—C6—C5 | 1.0 (4) |
O11—Mg1—O1—Mg2 | −11.4 (13) | Cl1—C1—C6—C5 | −178.77 (19) |
N1—Mg1—O1—Mg2 | −125.01 (13) | C4—C5—C6—C1 | 0.9 (4) |
O10—Mg1—O3—C11 | −170.04 (19) | C7—C5—C6—C1 | −173.7 (2) |
O1—Mg1—O3—C11 | 100.78 (19) | C8—N1—C7—C5 | −167.4 (2) |
O4—Mg1—O3—C11 | −17.9 (3) | C10—N1—C7—C5 | 65.9 (3) |
O11—Mg1—O3—C11 | −80.1 (2) | Mg1—N1—C7—C5 | −51.3 (2) |
N1—Mg1—O3—C11 | 12.63 (19) | C6—C5—C7—N1 | −116.8 (3) |
O10—Mg1—O4—C9 | 170.34 (19) | C4—C5—C7—N1 | 68.5 (3) |
O1—Mg1—O4—C9 | −102.66 (19) | C10—N1—C8—C9 | −149.1 (2) |
O3—Mg1—O4—C9 | 17.3 (3) | C7—N1—C8—C9 | 86.6 (3) |
O11—Mg1—O4—C9 | 79.7 (2) | Mg1—N1—C8—C9 | −31.5 (2) |
N1—Mg1—O4—C9 | −13.32 (19) | Mg1—O4—C9—O5 | −180.0 (2) |
C4—O1—Mg2—O12 | −136.41 (17) | Mg1—O4—C9—C8 | −1.2 (3) |
Mg1—O1—Mg2—O12 | 40.50 (14) | N1—C8—C9—O5 | −157.5 (3) |
C4—O1—Mg2—O6 | −31.84 (17) | N1—C8—C9—O4 | 23.7 (3) |
Mg1—O1—Mg2—O6 | 145.07 (12) | C8—N1—C10—C11 | 142.0 (2) |
C4—O1—Mg2—O13 | −113.8 (11) | C7—N1—C10—C11 | −94.7 (3) |
Mg1—O1—Mg2—O13 | 63.1 (12) | Mg1—N1—C10—C11 | 24.5 (3) |
C4—O1—Mg2—O8 | 123.96 (17) | Mg1—O3—C11—O2 | 175.0 (2) |
Mg1—O1—Mg2—O8 | −59.12 (13) | Mg1—O3—C11—C10 | −1.8 (3) |
C4—O1—Mg2—N2 | 47.03 (17) | N1—C10—C11—O2 | 166.1 (2) |
Mg1—O1—Mg2—N2 | −136.05 (13) | N1—C10—C11—O3 | −16.9 (4) |
O12—Mg2—N2—C15 | 20.7 (16) | C2—C3—C12—N2 | −112.7 (3) |
O6—Mg2—N2—C15 | −141.87 (17) | C4—C3—C12—N2 | 68.0 (3) |
O1—Mg2—N2—C15 | 123.98 (16) | C15—N2—C12—C3 | −171.7 (2) |
O13—Mg2—N2—C15 | −57.45 (16) | C13—N2—C12—C3 | 60.8 (3) |
O8—Mg2—N2—C15 | 31.80 (16) | Mg2—N2—C12—C3 | −57.3 (2) |
O12—Mg2—N2—C13 | 143.6 (15) | C15—N2—C13—C14 | 143.2 (2) |
O6—Mg2—N2—C13 | −19.00 (16) | C12—N2—C13—C14 | −92.6 (3) |
O1—Mg2—N2—C13 | −113.15 (16) | Mg2—N2—C13—C14 | 26.3 (2) |
O13—Mg2—N2—C13 | 65.43 (16) | Mg2—O6—C14—O7 | −179.5 (2) |
O8—Mg2—N2—C13 | 154.67 (17) | Mg2—O6—C14—C13 | 4.5 (3) |
O12—Mg2—N2—C12 | −95.9 (15) | N2—C13—C14—O7 | 161.7 (2) |
O6—Mg2—N2—C12 | 101.52 (16) | N2—C13—C14—O6 | −22.1 (3) |
O1—Mg2—N2—C12 | 7.37 (16) | C13—N2—C15—C16 | −156.9 (2) |
O13—Mg2—N2—C12 | −174.06 (15) | C12—N2—C15—C16 | 77.6 (3) |
O8—Mg2—N2—C12 | −84.82 (16) | Mg2—N2—C15—C16 | −39.0 (2) |
O12—Mg2—O6—C14 | −170.4 (2) | Mg2—O8—C16—O9 | −175.5 (2) |
O1—Mg2—O6—C14 | 99.0 (2) | Mg2—O8—C16—C15 | 3.3 (3) |
O13—Mg2—O6—C14 | −85.3 (2) | N2—C15—C16—O9 | −155.1 (2) |
O8—Mg2—O6—C14 | −6.2 (3) | N2—C15—C16—O8 | 26.0 (3) |
Symmetry code: (i) −x, −y+1, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O10—H10C···O8 | 0.89 | 1.97 | 2.828 (3) | 160 |
O10—H10D···O15 | 0.80 | 1.92 | 2.714 (3) | 169 |
O11—H11A···O14ii | 0.82 | 2.23 | 2.932 (4) | 143 |
O11—H11B···O22 | 0.83 | 1.93 | 2.743 (3) | 164 |
O12—H12C···O18iii | 0.81 | 1.93 | 2.723 (3) | 170 |
O12—H12D···O4 | 0.88 | 1.88 | 2.712 (3) | 157 |
O13—H13C···O18iv | 0.82 | 2.03 | 2.812 (3) | 158 |
O13—H13D···O23ii | 0.87 | 1.93 | 2.789 (3) | 171 |
O24—H24A···O4 | 0.88 | 2.03 | 2.897 (3) | 171 |
O24—H24B···O16 | 0.82 | 1.92 | 2.742 (3) | 176 |
O25—H25A···O22 | 0.83 | 1.91 | 2.734 (3) | 171 |
O25—H25B···O19i | 0.90 | 1.82 | 2.712 (3) | 170 |
O26—H26A···O5i | 0.85 | 1.96 | 2.805 (3) | 177 |
O26—H26B···O20ii | 0.83 | 1.98 | 2.807 (3) | 177 |
O14—H14A···O3v | 0.84 | 2.21 | 2.796 (4) | 127 |
O15—H15C···O21ii | 0.89 | 1.90 | 2.759 (3) | 163 |
O15—H15D···O5vi | 0.85 | 1.87 | 2.716 (3) | 175 |
O16—H16A···O8 | 0.79 | 2.11 | 2.893 (3) | 171 |
O16—H16B···O19 | 0.83 | 1.93 | 2.754 (3) | 172 |
O17—H17A···O9 | 0.93 | 1.78 | 2.695 (3) | 166 |
O18—H18A···O17 | 0.89 | 1.85 | 2.722 (4) | 166 |
O18—H18B···O25ii | 0.84 | 2.03 | 2.869 (3) | 179 |
O19—H19A···O2v | 0.82 | 1.92 | 2.737 (3) | 179 |
O19—H19B···O23ii | 0.82 | 1.96 | 2.760 (3) | 164 |
O20—H20A···O20ii | 0.82 | 1.98 | 2.770 (6) | 162 |
O20—H20B···O16 | 0.92 | 2.27 | 3.008 (3) | 138 |
O21—H21A···O2v | 0.81 | 1.96 | 2.762 (3) | 170 |
O21—H21B···O20 | 0.81 | 1.97 | 2.761 (4) | 164 |
O22—H22A···O21ii | 0.91 | 1.87 | 2.769 (3) | 173 |
O22—H22B···O7vii | 0.80 | 1.87 | 2.662 (3) | 173 |
O23—H23A···O6viii | 0.81 | 2.03 | 2.812 (3) | 162 |
O23—H23B···O9vii | 0.82 | 2.05 | 2.803 (3) | 151 |
Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x+1, −y+1, −z+1; (iii) x−1, y, z; (iv) −x+1, −y, −z+1; (v) x, y, z+1; (vi) x+1, y, z; (vii) x, y+1, z; (viii) x+1, y+1, z. |
Experimental details
Crystal data | |
Chemical formula | [Mg(H2O)6]0.5[Mg2(C16H14ClN2O9)(H2O)4]·10H2O |
Mr | 780.79 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 183 |
a, b, c (Å) | 9.871 (2), 13.119 (3), 13.438 (3) |
α, β, γ (°) | 88.421 (3), 84.029 (2), 84.050 (3) |
V (Å3) | 1721.2 (6) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 0.25 |
Crystal size (mm) | 0.30 × 0.20 × 0.20 |
Data collection | |
Diffractometer | Bruker SMART 1K CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 2000) |
Tmin, Tmax | 0.928, 0.951 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 7116, 5921, 4743 |
Rint | 0.016 |
(sin θ/λ)max (Å−1) | 0.595 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.050, 0.137, 1.05 |
No. of reflections | 5921 |
No. of parameters | 430 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.22, −1.12 |
Computer programs: SMART (Bruker, 2000), SAINT (Bruker, 2000), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL/PC (Sheldrick, 1999), SHELXTL/PC.
Mg1—O10 | 2.015 (2) | O1—Mg2 | 2.072 (2) |
Mg1—O1 | 2.062 (2) | Mg2—O12 | 1.992 (2) |
Mg1—O3 | 2.063 (2) | Mg2—O6 | 2.071 (2) |
Mg1—O4 | 2.088 (2) | Mg2—O13 | 2.075 (2) |
Mg1—O11 | 2.114 (2) | Mg2—O8 | 2.111 (2) |
Mg1—N1 | 2.210 (2) | Mg2—N2 | 2.201 (2) |
O10—Mg1—O1 | 86.59 (8) | O12—Mg2—O1 | 89.45 (8) |
O10—Mg1—O3 | 105.62 (9) | O6—Mg2—O1 | 94.33 (8) |
O1—Mg1—O3 | 99.82 (8) | O12—Mg2—O13 | 86.54 (9) |
O10—Mg1—O4 | 97.90 (9) | O6—Mg2—O13 | 85.07 (8) |
O1—Mg1—O4 | 93.27 (8) | O1—Mg2—O13 | 175.66 (9) |
O3—Mg1—O4 | 153.61 (9) | O12—Mg2—O8 | 99.64 (9) |
O10—Mg1—O11 | 91.51 (9) | O6—Mg2—O8 | 154.89 (9) |
O1—Mg1—O11 | 175.96 (9) | O1—Mg2—O8 | 92.44 (8) |
O3—Mg1—O11 | 84.13 (8) | O13—Mg2—O8 | 89.88 (8) |
O4—Mg1—O11 | 83.45 (8) | O12—Mg2—N2 | 176.46 (10) |
O10—Mg1—N1 | 174.52 (9) | O6—Mg2—N2 | 78.81 (8) |
O1—Mg1—N1 | 90.04 (8) | O1—Mg2—N2 | 91.36 (8) |
O3—Mg1—N1 | 79.20 (8) | O13—Mg2—N2 | 92.74 (9) |
O4—Mg1—N1 | 77.97 (8) | O8—Mg2—N2 | 76.89 (8) |
O11—Mg1—N1 | 91.58 (9) | O24—Mg3—O26 | 88.02 (8) |
Mg1—O1—Mg2 | 132.72 (9) | O24—Mg3—O25 | 86.88 (8) |
O12—Mg2—O6 | 104.57 (9) | O26—Mg3—O25 | 90.82 (8) |
O10—Mg1—O1—Mg2 | 50.67 (13) | Mg1—O1—Mg2—O12 | 40.50 (14) |
O3—Mg1—O1—Mg2 | 155.95 (12) | Mg1—O1—Mg2—O6 | 145.07 (12) |
O4—Mg1—O1—Mg2 | −47.05 (13) | Mg1—O1—Mg2—O13 | 63.1 (12) |
O11—Mg1—O1—Mg2 | −11.4 (13) | Mg1—O1—Mg2—O8 | −59.12 (13) |
N1—Mg1—O1—Mg2 | −125.01 (13) | Mg1—O1—Mg2—N2 | −136.05 (13) |
D—H···A | D—H | H···A | D···A | D—H···A |
O10—H10C···O8 | 0.89 | 1.97 | 2.828 (3) | 160 |
O10—H10D···O15 | 0.80 | 1.92 | 2.714 (3) | 169 |
O11—H11A···O14i | 0.82 | 2.23 | 2.932 (4) | 143 |
O11—H11B···O22 | 0.83 | 1.93 | 2.743 (3) | 164 |
O12—H12C···O18ii | 0.81 | 1.93 | 2.723 (3) | 170 |
O12—H12D···O4 | 0.88 | 1.88 | 2.712 (3) | 157 |
O13—H13C···O18iii | 0.82 | 2.03 | 2.812 (3) | 158 |
O13—H13D···O23i | 0.87 | 1.93 | 2.789 (3) | 171 |
O24—H24A···O4 | 0.88 | 2.03 | 2.897 (3) | 171 |
O24—H24B···O16 | 0.82 | 1.92 | 2.742 (3) | 176 |
O25—H25A···O22 | 0.83 | 1.91 | 2.734 (3) | 171 |
O25—H25B···O19iv | 0.90 | 1.82 | 2.712 (3) | 170 |
O26—H26A···O5iv | 0.85 | 1.96 | 2.805 (3) | 177 |
O26—H26B···O20i | 0.83 | 1.98 | 2.807 (3) | 177 |
O14—H14A···O3v | 0.84 | 2.21 | 2.796 (4) | 127 |
O15—H15C···O21i | 0.89 | 1.90 | 2.759 (3) | 163 |
O15—H15D···O5vi | 0.85 | 1.87 | 2.716 (3) | 175 |
O16—H16A···O8 | 0.79 | 2.11 | 2.893 (3) | 171 |
O16—H16B···O19 | 0.83 | 1.93 | 2.754 (3) | 172 |
O17—H17A···O9 | 0.93 | 1.78 | 2.695 (3) | 166 |
O18—H18A···O17 | 0.89 | 1.85 | 2.722 (4) | 166 |
O18—H18B···O25i | 0.84 | 2.03 | 2.869 (3) | 179 |
O19—H19A···O2v | 0.82 | 1.92 | 2.737 (3) | 179 |
O19—H19B···O23i | 0.82 | 1.96 | 2.760 (3) | 164 |
O20—H20A···O20i | 0.82 | 1.98 | 2.770 (6) | 162 |
O20—H20B···O16 | 0.92 | 2.27 | 3.008 (3) | 138 |
O21—H21A···O2v | 0.81 | 1.96 | 2.762 (3) | 170 |
O21—H21B···O20 | 0.81 | 1.97 | 2.761 (4) | 164 |
O22—H22A···O21i | 0.91 | 1.87 | 2.769 (3) | 173 |
O22—H22B···O7vii | 0.80 | 1.87 | 2.662 (3) | 173 |
O23—H23A···O6viii | 0.81 | 2.03 | 2.812 (3) | 162 |
O23—H23B···O9vii | 0.82 | 2.05 | 2.803 (3) | 151 |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x−1, y, z; (iii) −x+1, −y, −z+1; (iv) −x, −y+1, −z+1; (v) x, y, z+1; (vi) x+1, y, z; (vii) x, y+1, z; (viii) x+1, y+1, z. |
It is well known that Mg arises out of the active centres in many nucleases (Wilcox, 1996; Sam & Perona, 1999). However, the usage has not been reported of simple complexes of Mg to mimic the nucleases to hydrolyse DNA. Recently, we synthesized the title novel complex, (I), of Mg with Cl-HXTA (Cl-HXTA is 5-chloro-2-hydroxy-1,3-xylene-α,α-diamine-N,N,N',N'-tetraacetic acid), and found that this complex is able to cleave DNA in a hydrolytic path. Cl-HXTA is one of the acyclic dinucleating ligands with a phenolate bridge (Murch et al., 1987). As a pentavalent anionic ligand, it has four methoxycarbonyl chelating arms with two sets of donor atoms, namely one N and three O atoms, as the coordination sites. One of the advantage of Cl-HXTA is that most of its dinuclear metal complexes are soluble in water and it is thus convenient to carry out experiments on biological activity. \sch
The main features of the molecular geometry of (I) are listed in Table 1, and the molecular configuration and crystal packing are illustrated in Figs. 1 and 2, respectively.
From Fig.1, it can readily be seen that the inner coordination spheres for the two MgII ions are similar in geometry and donor atoms. Each metal ion adopts a distorted octahedral coordination geometry comprised of two carboxylates, a tertiary N atom, two water molecules and the bridging phenolate (atom O1). The Mg1···Mg2 separation is 3.787 (1) Å, suggesting no obvious bonding. Here, there is only one oxo-bridge formed in (I), which is quite different from the structure of [Fe2(HXTA)(OH)(H2O)2] (Murch et al., 1987), where there are two oxo-bridges (one O stems from the phenolate and the other from a hydroxide group in a water molecule). For (I), the average Mg—O bond length in the phenolate bridge is 2.067 (5) Å, in accordance with that of the metal-phenolate bonds in other reported dinulear complexes, such as [Fe2(sal)3trien(OMe)]Cl2 (Chiari et al., 1982) and [Fe2(sal)3trien(OH)]Cl2 (Chiari et al., 1983). The coordination spheres of the two MgII ions possess evident similarity both in ligand sets and in geometry. More specifically, in each coordination sphere, the tertiary N, the bridging O and two O atoms from water molecules make up the equatorial plane, while two carboxylate O atoms occupy two polar positions and thus complete a distorted octahedral geometry. The complex anion as a whole has a pseudo-C2 axis along Cl1/C1/C4/O1, which has been reported previously by Sakiyama et al. (1999).
The Mg1—O1—Mg2 angle in (I) is 132.72 (9)°, which is obviously larger than the analogous Fe1—O—Fe2 angle in the [Fe2(HXTA)OH(H2O)2] complex (102.56°; Murch et al., 1987), perhaps due to the different numbers of oxo-bridges formed between the two metal ions. The axial coordination atoms perpendicular to the equatorial plane of the Mg core lean away from the core somewhat, as demonstrated by the two largest angles at each Mg, i.e. O10—Mg1—O3 [105.62 (9)°] and O6—Mg2—O12 [104.57 (9)°]. In addition, the four angles in the equatorial plane for each Mg core, taking the metal as the common apex, are close to right angles, being in the range 86.59 (8)–91.58 (9)° for atom Mg1 and 86.54 (9)–92.74 (9)° for Mg2. In addition, the least-squares plane of the aromatic ring of Cl-HXTA and the plane defined by atoms Mg1, Mg2 and O1 are twisted, with a dihedral angle of 56.23 (7)°.
Interestingly, each unit of this binuclear complex has one negative charge neutralized by a neighbouring hydrated cation, [Mg(H2O)6]2+, which is shared by another complexing unit. From another viewpoint, in the two faces of the cell in the c direction, there are two hydrated MgII ions, to achieve charge balance.
In each cell there are 34 water molecules, contributing greatly to the stability of the whole structure by forming hydrogen bonds. Some of these intra- and intermolecular hydrogen bonds are illustrated in Fig.2 and their numerical values are given in Table 2.