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The crystal structure of the title compound, [Mg(H2O)6]0.5[Mg2(C16H14ClN2O9)(H2O)4]·10H2O, shows that this bi­nuclear complex consists of two Mg centres in distorted octahedral geometry, joined by an oxo bridge which is a derivative of the deprotoned hydroxy group of the phenolate in the ligand mol­ecule. In the anion, the coordination sphere of each MgII ion is completed by two carboxyl­ates, a tertiary N atom and two water mol­ecules. The inner coordination spheres for the MgII ions are very similar, both in ligand sets and in geometry. Each unit of the binuclear complex has one negative charge neutralized by a neighbouring hydrated cation, [Mg(H2O)6]2+, in which the Mg atom lies on an inversion centre. In each cell, there are 34 water mol­ecules and most of them participate in the formation of hydrogen bonds, which contribute greatly to the stability of the whole structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270104012867/na1658sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270104012867/na1658Isup2.hkl
Contains datablock I

CCDC reference: 245872

Comment top

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.

Experimental top

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.

Refinement top

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).

Computing details top

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.

Figures top
[Figure 1] Fig. 1. The structure of (I), with the atom-numbering scheme. Displacement ellipsoids are drawn at the 35% probability level and H atoms are shown as small spheres of arbitrary radii [symmetry code: (A) −x, 1 − y, 1 − z].
[Figure 2] Fig. 2. The crystal packing of (I), viewed along a favourable direction Please specify axis. The hydrogen bonds are shown as dashed lines.
Hexaaquamagnesium(II) (µ-2,6-bis{[bis(carboxylatomethyl)amino]methyl}-4- chlorophenolato)bis[diaquamagnesium(II)] decahydrate top
Crystal data top
[Mg(H2O)6]0.5[Mg2(C16H14ClN2O9)(H2O)4]·10H2OZ = 2
Mr = 780.79F(000) = 826
Triclinic, P1Dx = 1.507 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.871 (2) ÅCell parameters from 3324 reflections
b = 13.119 (3) Åθ = 2.2–26.4°
c = 13.438 (3) ŵ = 0.25 mm1
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
Data collection top
Bruker SMART 1K CCD area-detector
diffractometer
5921 independent reflections
Radiation source: fine-focus sealed tube4743 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.016
ϕ and ω scansθmax = 25.0°, θmin = 1.5°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2000)
h = 1111
Tmin = 0.928, Tmax = 0.951k = 1514
7116 measured reflectionsl = 1515
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.050Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.137H-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 parametersΔρmax = 1.22 e Å3
0 restraintsΔρmin = 1.12 e Å3
Crystal data top
[Mg(H2O)6]0.5[Mg2(C16H14ClN2O9)(H2O)4]·10H2Oγ = 84.050 (3)°
Mr = 780.79V = 1721.2 (6) Å3
Triclinic, P1Z = 2
a = 9.871 (2) ÅMo Kα radiation
b = 13.119 (3) ŵ = 0.25 mm1
c = 13.438 (3) ÅT = 183 K
α = 88.421 (3)°0.30 × 0.20 × 0.20 mm
β = 84.029 (2)°
Data collection top
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 = 0.951Rint = 0.016
7116 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0500 restraints
wR(F2) = 0.137H-atom parameters constrained
S = 1.05Δρmax = 1.22 e Å3
5921 reflectionsΔρmin = 1.12 e Å3
430 parameters
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
xyzUiso*/Ueq
Mg10.25058 (9)0.28947 (7)0.12477 (6)0.0208 (2)
N10.0853 (2)0.28325 (17)0.02677 (15)0.0208 (5)
O10.23642 (18)0.13804 (13)0.16583 (13)0.0215 (4)
O30.36293 (18)0.27078 (15)0.01291 (13)0.0259 (4)
O40.07700 (18)0.34135 (14)0.21915 (13)0.0240 (4)
O100.3892 (2)0.28969 (16)0.22468 (15)0.0339 (5)
H10C0.40840.23520.26420.041*
H10D0.45520.32120.21840.041*
O110.2600 (2)0.44749 (15)0.09321 (15)0.0331 (5)
H11A0.32570.47100.06130.040*
H11B0.22230.49210.13280.040*
Mg20.20534 (9)0.06441 (7)0.30351 (6)0.0212 (2)
N20.3662 (2)0.05934 (17)0.25833 (16)0.0211 (5)
O60.09101 (18)0.04285 (14)0.25160 (14)0.0266 (5)
O80.38225 (18)0.11556 (14)0.35318 (13)0.0254 (4)
O120.0679 (2)0.17992 (16)0.34937 (15)0.0405 (6)
H12C0.02370.18550.40330.049*
H12D0.04680.23170.30860.049*
O130.1598 (2)0.00291 (15)0.44291 (14)0.0328 (5)
H13C0.12360.05640.45160.039*
H13D0.15960.02430.50110.039*
C10.2575 (3)0.0548 (2)0.0725 (2)0.0240 (6)
C20.3467 (3)0.0766 (2)0.0005 (2)0.0239 (6)
H20.41010.13420.00610.029*
C30.3412 (3)0.0117 (2)0.08065 (19)0.0215 (6)
C40.2432 (3)0.0748 (2)0.08794 (19)0.0199 (6)
C50.1515 (3)0.0932 (2)0.01519 (19)0.0211 (6)
C60.1596 (3)0.0283 (2)0.0659 (2)0.0251 (6)
H60.09970.04080.11490.030*
C70.0381 (3)0.1787 (2)0.0323 (2)0.0234 (6)
H7A0.02590.17460.01720.028*
H7B0.01070.16880.09770.028*
C80.0287 (3)0.3570 (2)0.0667 (2)0.0255 (6)
H8A0.11440.33530.04980.031*
H8B0.01820.42380.03560.031*
C90.0337 (3)0.3658 (2)0.1802 (2)0.0267 (6)
C100.1442 (3)0.3070 (2)0.07600 (19)0.0256 (6)
H10A0.12110.37910.09080.031*
H10B0.10350.26770.12310.031*
C110.2994 (3)0.2828 (2)0.0902 (2)0.0238 (6)
C120.4376 (3)0.0312 (2)0.15924 (19)0.0228 (6)
H12A0.48330.02970.16640.027*
H12B0.50690.08640.13810.027*
C130.2991 (3)0.1535 (2)0.2522 (2)0.0244 (6)
H13A0.30250.19150.31500.029*
H13B0.34870.19600.19980.029*
C140.1497 (3)0.1308 (2)0.2303 (2)0.0263 (6)
C150.4633 (3)0.0623 (2)0.3341 (2)0.0255 (6)
H15A0.55090.09640.30750.031*
H15B0.42950.10080.39250.031*
C160.4810 (3)0.0469 (2)0.36380 (19)0.0243 (6)
Cl10.27111 (8)0.13582 (6)0.17551 (5)0.0364 (2)
Mg30.00000.50000.50000.0260 (3)
O240.1462 (2)0.41896 (16)0.40522 (15)0.0362 (5)
H24A0.13280.39770.34610.043*
H24B0.20830.38290.42860.043*
O250.0093 (2)0.62042 (15)0.39533 (14)0.0321 (5)
H25A0.06230.60880.34370.039*
H25B0.06740.65300.37340.039*
O260.1566 (2)0.55080 (17)0.56955 (15)0.0386 (5)
H26A0.14980.56490.63120.046*
H26B0.23150.56150.53940.046*
O20.3547 (2)0.28069 (17)0.17779 (14)0.0334 (5)
O50.1428 (2)0.3975 (2)0.22821 (16)0.0484 (7)
O70.0927 (2)0.20135 (16)0.19791 (18)0.0420 (6)
O90.58955 (19)0.06212 (16)0.39794 (15)0.0328 (5)
O140.5885 (5)0.3831 (5)0.9885 (3)0.265 (5)
H14A0.56750.32740.96850.318*
H14B0.52250.42460.99750.318*
O150.5924 (2)0.41402 (19)0.1864 (2)0.0590 (7)
H15C0.55680.46700.22330.071*
H15D0.67560.40530.19810.071*
O160.3590 (2)0.29611 (17)0.47508 (16)0.0425 (6)
H16A0.36110.24370.44690.051*
H16B0.32340.28630.53280.051*
O170.6855 (3)0.2471 (2)0.3979 (2)0.0598 (7)
H17A0.64300.18800.39000.072*
H17B0.69230.27620.34400.072*
O180.8911 (2)0.20793 (17)0.51810 (16)0.0404 (5)
H18A0.82410.23140.48190.049*
H18B0.92070.25840.54250.049*
O190.2159 (2)0.26359 (16)0.65840 (15)0.0353 (5)
H19A0.25680.26850.70790.042*
H19B0.19060.20580.66250.042*
O200.5854 (3)0.4155 (2)0.5270 (2)0.0601 (7)
H20A0.52180.45860.51660.072*
H20B0.55730.35530.50790.072*
O210.5410 (2)0.40710 (18)0.73326 (18)0.0472 (6)
H21A0.49340.36440.75850.057*
H21B0.53820.40790.67310.057*
O220.1886 (2)0.60382 (16)0.22587 (16)0.0387 (5)
H22A0.27660.60610.23890.046*
H22B0.16410.66230.21240.046*
O230.8368 (2)0.93689 (16)0.36189 (15)0.0355 (5)
H23A0.89950.95150.32260.043*
H23B0.76960.97670.35070.043*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mg10.0205 (5)0.0215 (5)0.0209 (5)0.0039 (4)0.0019 (4)0.0016 (4)
N10.0184 (11)0.0235 (12)0.0199 (11)0.0016 (9)0.0000 (9)0.0009 (9)
O10.0253 (10)0.0206 (10)0.0194 (9)0.0038 (8)0.0040 (8)0.0026 (8)
O30.0229 (10)0.0329 (11)0.0222 (10)0.0059 (8)0.0002 (8)0.0022 (8)
O40.0222 (10)0.0259 (11)0.0238 (10)0.0012 (8)0.0022 (8)0.0024 (8)
O100.0330 (12)0.0328 (12)0.0399 (12)0.0133 (9)0.0145 (9)0.0069 (10)
O110.0359 (12)0.0261 (11)0.0366 (12)0.0084 (9)0.0059 (9)0.0032 (9)
Mg20.0210 (5)0.0220 (5)0.0206 (5)0.0031 (4)0.0013 (4)0.0016 (4)
N20.0205 (12)0.0223 (12)0.0215 (12)0.0039 (9)0.0044 (9)0.0001 (10)
O60.0232 (10)0.0268 (11)0.0306 (11)0.0047 (8)0.0045 (8)0.0002 (9)
O80.0256 (10)0.0273 (11)0.0247 (10)0.0048 (9)0.0061 (8)0.0036 (8)
O120.0478 (13)0.0332 (12)0.0329 (12)0.0109 (10)0.0158 (10)0.0047 (10)
O130.0449 (13)0.0322 (12)0.0228 (10)0.0137 (10)0.0001 (9)0.0007 (9)
C10.0249 (15)0.0274 (16)0.0203 (14)0.0107 (12)0.0046 (12)0.0080 (12)
C20.0245 (15)0.0199 (15)0.0266 (15)0.0055 (11)0.0043 (12)0.0046 (12)
C30.0210 (14)0.0237 (15)0.0200 (14)0.0070 (11)0.0013 (11)0.0012 (11)
C40.0221 (14)0.0199 (14)0.0182 (13)0.0086 (11)0.0031 (11)0.0028 (11)
C50.0219 (14)0.0199 (14)0.0222 (14)0.0074 (11)0.0001 (11)0.0001 (11)
C60.0257 (15)0.0307 (16)0.0208 (14)0.0122 (13)0.0020 (12)0.0012 (12)
C70.0208 (14)0.0275 (16)0.0234 (14)0.0082 (12)0.0037 (11)0.0009 (12)
C80.0242 (15)0.0240 (15)0.0280 (15)0.0006 (12)0.0039 (12)0.0004 (12)
C90.0266 (16)0.0248 (16)0.0288 (15)0.0023 (12)0.0036 (13)0.0032 (12)
C100.0263 (15)0.0311 (16)0.0202 (14)0.0051 (12)0.0046 (12)0.0021 (12)
C110.0265 (15)0.0214 (15)0.0246 (15)0.0075 (12)0.0018 (12)0.0026 (12)
C120.0181 (14)0.0243 (15)0.0253 (15)0.0022 (11)0.0019 (11)0.0039 (12)
C130.0267 (15)0.0208 (15)0.0260 (15)0.0034 (12)0.0029 (12)0.0012 (12)
C140.0308 (16)0.0270 (17)0.0229 (14)0.0079 (13)0.0067 (12)0.0028 (12)
C150.0228 (14)0.0264 (16)0.0277 (15)0.0004 (12)0.0066 (12)0.0001 (12)
C160.0230 (15)0.0314 (16)0.0193 (14)0.0070 (13)0.0018 (12)0.0014 (12)
Cl10.0364 (4)0.0441 (5)0.0292 (4)0.0091 (3)0.0035 (3)0.0181 (3)
Mg30.0292 (7)0.0247 (7)0.0248 (7)0.0048 (6)0.0035 (6)0.0035 (6)
O240.0405 (13)0.0383 (13)0.0288 (11)0.0059 (10)0.0059 (10)0.0110 (10)
O250.0312 (11)0.0325 (12)0.0311 (11)0.0006 (9)0.0009 (9)0.0027 (9)
O260.0332 (12)0.0548 (15)0.0301 (11)0.0144 (10)0.0013 (9)0.0101 (10)
O20.0297 (11)0.0488 (14)0.0215 (11)0.0086 (10)0.0037 (9)0.0036 (9)
O50.0253 (12)0.0821 (19)0.0354 (13)0.0128 (11)0.0026 (10)0.0255 (12)
O70.0431 (13)0.0286 (12)0.0603 (15)0.0110 (10)0.0253 (11)0.0041 (11)
O90.0267 (11)0.0382 (13)0.0358 (12)0.0064 (9)0.0096 (9)0.0054 (10)
O140.244 (6)0.523 (11)0.097 (3)0.330 (7)0.098 (3)0.154 (5)
O150.0315 (13)0.0387 (14)0.109 (2)0.0071 (11)0.0109 (14)0.0128 (15)
O160.0497 (14)0.0402 (14)0.0360 (12)0.0015 (11)0.0031 (10)0.0092 (10)
O170.0662 (17)0.0529 (17)0.0643 (17)0.0187 (14)0.0097 (14)0.0141 (14)
O180.0484 (14)0.0352 (13)0.0376 (12)0.0103 (10)0.0034 (10)0.0042 (10)
O190.0367 (12)0.0385 (13)0.0319 (11)0.0053 (10)0.0084 (9)0.0003 (10)
O200.0565 (16)0.0558 (17)0.0675 (18)0.0140 (13)0.0081 (14)0.0147 (14)
O210.0398 (13)0.0446 (15)0.0569 (15)0.0101 (11)0.0008 (11)0.0037 (12)
O220.0381 (12)0.0279 (12)0.0498 (14)0.0047 (10)0.0017 (10)0.0047 (10)
O230.0264 (11)0.0411 (13)0.0382 (12)0.0021 (9)0.0004 (9)0.0023 (10)
Geometric parameters (Å, º) top
Mg1—O102.015 (2)C9—O51.236 (3)
Mg1—O12.062 (2)C10—C111.525 (4)
Mg1—O32.063 (2)C10—H10A0.9700
Mg1—O42.088 (2)C10—H10B0.9700
Mg1—O112.114 (2)C11—O21.245 (3)
Mg1—N12.210 (2)C12—H12A0.9700
N1—C81.472 (3)C12—H12B0.9700
N1—C101.480 (3)C13—C141.531 (4)
N1—C71.490 (3)C13—H13A0.9700
O1—C41.345 (3)C13—H13B0.9700
O1—Mg22.072 (2)C14—O71.242 (3)
O3—C111.266 (3)C15—C161.530 (4)
O4—C91.268 (3)C15—H15A0.9700
O10—H10C0.8944C15—H15B0.9700
O10—H10D0.8031C16—O91.245 (3)
O11—H11A0.8216Mg3—O24i2.051 (2)
O11—H11B0.8336Mg3—O242.051 (2)
Mg2—O121.992 (2)Mg3—O262.0634 (19)
Mg2—O62.071 (2)Mg3—O26i2.0634 (19)
Mg2—O132.075 (2)Mg3—O25i2.089 (2)
Mg2—O82.111 (2)Mg3—O252.089 (2)
Mg2—N22.201 (2)O24—H24A0.8757
N2—C151.466 (3)O24—H24B0.8186
N2—C131.469 (3)O25—H25A0.8314
N2—C121.496 (3)O25—H25B0.9034
O6—C141.262 (3)O26—H26A0.8482
O8—C161.274 (3)O26—H26B0.8288
O12—H12C0.8066O14—H14A0.8379
O12—H12D0.8822O14—H14B0.8060
O13—H13C0.8207O15—H15C0.8852
O13—H13D0.8687O15—H15D0.8483
C1—C61.378 (4)O16—H16A0.7910
C1—C21.379 (4)O16—H16B0.8295
C1—Cl11.754 (3)O17—H17A0.9329
C2—C31.395 (4)O17—H17B0.8096
C2—H20.9300O18—H18A0.8861
C3—C41.412 (4)O18—H18B0.8392
C3—C121.493 (4)O19—H19A0.8201
C4—C51.400 (4)O19—H19B0.8215
C5—C61.393 (4)O20—H20A0.8198
C5—C71.505 (4)O20—H20B0.9162
C6—H60.9300O21—H21A0.8124
C7—H7A0.9700O21—H21B0.8120
C7—H7B0.9700O22—H22A0.9081
C8—C91.528 (4)O22—H22B0.8010
C8—H8A0.9700O23—H23A0.8055
C8—H8B0.9700O23—H23B0.8245
O10—Mg1—O186.59 (8)C5—C7—H7A108.7
O10—Mg1—O3105.62 (9)N1—C7—H7B108.7
O1—Mg1—O399.82 (8)C5—C7—H7B108.7
O10—Mg1—O497.90 (9)H7A—C7—H7B107.6
O1—Mg1—O493.27 (8)N1—C8—C9111.6 (2)
O3—Mg1—O4153.61 (9)N1—C8—H8A109.3
O10—Mg1—O1191.51 (9)C9—C8—H8A109.3
O1—Mg1—O11175.96 (9)N1—C8—H8B109.3
O3—Mg1—O1184.13 (8)C9—C8—H8B109.3
O4—Mg1—O1183.45 (8)H8A—C8—H8B108.0
O10—Mg1—N1174.52 (9)O5—C9—O4123.9 (3)
O1—Mg1—N190.04 (8)O5—C9—C8119.0 (3)
O3—Mg1—N179.20 (8)O4—C9—C8117.1 (2)
O4—Mg1—N177.97 (8)N1—C10—C11112.5 (2)
O11—Mg1—N191.58 (9)N1—C10—H10A109.1
C8—N1—C10114.7 (2)C11—C10—H10A109.1
C8—N1—C7108.7 (2)N1—C10—H10B109.1
C10—N1—C7110.6 (2)C11—C10—H10B109.1
C8—N1—Mg1106.48 (16)H10A—C10—H10B107.8
C10—N1—Mg1106.59 (15)O2—C11—O3124.8 (3)
C7—N1—Mg1109.68 (16)O2—C11—C10116.9 (2)
C4—O1—Mg1113.87 (15)O3—C11—C10118.2 (2)
C4—O1—Mg2113.35 (15)C3—C12—N2112.3 (2)
Mg1—O1—Mg2132.72 (9)C3—C12—H12A109.1
C11—O3—Mg1117.88 (17)N2—C12—H12A109.1
C9—O4—Mg1118.00 (17)C3—C12—H12B109.1
Mg1—O10—H10C121.6N2—C12—H12B109.1
Mg1—O10—H10D125.2H12A—C12—H12B107.9
H10C—O10—H10D107.4N2—C13—C14112.0 (2)
Mg1—O11—H11A123.7N2—C13—H13A109.2
Mg1—O11—H11B121.6C14—C13—H13A109.2
H11A—O11—H11B108.0N2—C13—H13B109.2
O12—Mg2—O6104.57 (9)C14—C13—H13B109.2
O12—Mg2—O189.45 (8)H13A—C13—H13B107.9
O6—Mg2—O194.33 (8)O7—C14—O6124.6 (3)
O12—Mg2—O1386.54 (9)O7—C14—C13118.0 (3)
O6—Mg2—O1385.07 (8)O6—C14—C13117.3 (2)
O1—Mg2—O13175.66 (9)N2—C15—C16109.8 (2)
O12—Mg2—O899.64 (9)N2—C15—H15A109.7
O6—Mg2—O8154.89 (9)C16—C15—H15A109.7
O1—Mg2—O892.44 (8)N2—C15—H15B109.7
O13—Mg2—O889.88 (8)C16—C15—H15B109.7
O12—Mg2—N2176.46 (10)H15A—C15—H15B108.2
O6—Mg2—N278.81 (8)O9—C16—O8124.7 (3)
O1—Mg2—N291.36 (8)O9—C16—C15118.0 (2)
O13—Mg2—N292.74 (9)O8—C16—C15117.3 (2)
O8—Mg2—N276.89 (8)O24i—Mg3—O24180.0
C15—N2—C13114.8 (2)O24i—Mg3—O2691.98 (8)
C15—N2—C12108.8 (2)O24—Mg3—O2688.02 (8)
C13—N2—C12111.3 (2)O24i—Mg3—O26i88.02 (8)
C15—N2—Mg2105.48 (16)O24—Mg3—O26i91.98 (8)
C13—N2—Mg2107.35 (15)O26—Mg3—O26i180.00 (12)
C12—N2—Mg2108.78 (16)O24i—Mg3—O25i86.88 (8)
C14—O6—Mg2118.44 (17)O24—Mg3—O25i93.12 (8)
C16—O8—Mg2116.01 (17)O26—Mg3—O25i89.18 (8)
Mg2—O12—H12C127.2O26i—Mg3—O25i90.82 (8)
Mg2—O12—H12D120.8O24i—Mg3—O2593.12 (8)
H12C—O12—H12D112.0O24—Mg3—O2586.88 (8)
Mg2—O13—H13C124.0O26—Mg3—O2590.82 (8)
Mg2—O13—H13D127.5O26i—Mg3—O2589.18 (8)
H13C—O13—H13D107.5O25i—Mg3—O25180.0
C6—C1—C2122.1 (2)Mg3—O24—H24A124.7
C6—C1—Cl1119.6 (2)Mg3—O24—H24B119.3
C2—C1—Cl1118.3 (2)H24A—O24—H24B111.0
C1—C2—C3119.7 (3)Mg3—O25—H25A115.9
C1—C2—H2120.2Mg3—O25—H25B121.2
C3—C2—H2120.2H25A—O25—H25B104.7
C2—C3—C4119.2 (2)Mg3—O26—H26A123.5
C2—C3—C12121.5 (2)Mg3—O26—H26B123.1
C4—C3—C12119.4 (2)H26A—O26—H26B113.4
O1—C4—C5120.2 (2)H14A—O14—H14B111.6
O1—C4—C3119.9 (2)H15C—O15—H15D104.5
C5—C4—C3119.8 (2)H16A—O16—H16B106.4
C6—C5—C4120.2 (2)H17A—O17—H17B107.2
C6—C5—C7121.6 (2)H18A—O18—H18B107.9
C4—C5—C7118.0 (2)H19A—O19—H19B105.1
C1—C6—C5119.1 (3)H20A—O20—H20B104.0
C1—C6—H6120.5H21A—O21—H21B109.0
C5—C6—H6120.5H22A—O22—H22B103.3
N1—C7—C5114.3 (2)H23A—O23—H23B106.8
N1—C7—H7A108.7
O10—Mg1—N1—C865.5 (10)N2—Mg2—O6—C148.5 (2)
O1—Mg1—N1—C8117.39 (16)O12—Mg2—O8—C16159.13 (18)
O3—Mg1—N1—C8142.62 (17)O6—Mg2—O8—C165.4 (3)
O4—Mg1—N1—C824.05 (16)O1—Mg2—O8—C16111.01 (18)
O11—Mg1—N1—C858.91 (16)O13—Mg2—O8—C1672.66 (19)
O10—Mg1—N1—C10171.7 (9)N2—Mg2—O8—C1620.18 (18)
O1—Mg1—N1—C10119.79 (17)C6—C1—C2—C31.8 (4)
O3—Mg1—N1—C1019.79 (16)Cl1—C1—C2—C3178.02 (19)
O4—Mg1—N1—C10146.88 (18)C1—C2—C3—C40.6 (4)
O11—Mg1—N1—C1063.92 (17)C1—C2—C3—C12178.7 (2)
O10—Mg1—N1—C752.0 (11)Mg1—O1—C4—C555.9 (3)
O1—Mg1—N1—C70.07 (16)Mg2—O1—C4—C5121.6 (2)
O3—Mg1—N1—C799.92 (16)Mg1—O1—C4—C3125.6 (2)
O4—Mg1—N1—C793.41 (16)Mg2—O1—C4—C356.9 (3)
O11—Mg1—N1—C7176.36 (16)C2—C3—C4—O1179.9 (2)
O10—Mg1—O1—C4132.42 (17)C12—C3—C4—O10.8 (4)
O3—Mg1—O1—C427.15 (17)C2—C3—C4—C51.3 (4)
O4—Mg1—O1—C4129.85 (16)C12—C3—C4—C5179.4 (2)
O11—Mg1—O1—C4165.5 (12)O1—C4—C5—C6179.4 (2)
N1—Mg1—O1—C451.90 (17)C3—C4—C5—C62.1 (4)
O10—Mg1—O1—Mg250.67 (13)O1—C4—C5—C75.8 (4)
O3—Mg1—O1—Mg2155.95 (12)C3—C4—C5—C7172.7 (2)
O4—Mg1—O1—Mg247.05 (13)C2—C1—C6—C51.0 (4)
O11—Mg1—O1—Mg211.4 (13)Cl1—C1—C6—C5178.77 (19)
N1—Mg1—O1—Mg2125.01 (13)C4—C5—C6—C10.9 (4)
O10—Mg1—O3—C11170.04 (19)C7—C5—C6—C1173.7 (2)
O1—Mg1—O3—C11100.78 (19)C8—N1—C7—C5167.4 (2)
O4—Mg1—O3—C1117.9 (3)C10—N1—C7—C565.9 (3)
O11—Mg1—O3—C1180.1 (2)Mg1—N1—C7—C551.3 (2)
N1—Mg1—O3—C1112.63 (19)C6—C5—C7—N1116.8 (3)
O10—Mg1—O4—C9170.34 (19)C4—C5—C7—N168.5 (3)
O1—Mg1—O4—C9102.66 (19)C10—N1—C8—C9149.1 (2)
O3—Mg1—O4—C917.3 (3)C7—N1—C8—C986.6 (3)
O11—Mg1—O4—C979.7 (2)Mg1—N1—C8—C931.5 (2)
N1—Mg1—O4—C913.32 (19)Mg1—O4—C9—O5180.0 (2)
C4—O1—Mg2—O12136.41 (17)Mg1—O4—C9—C81.2 (3)
Mg1—O1—Mg2—O1240.50 (14)N1—C8—C9—O5157.5 (3)
C4—O1—Mg2—O631.84 (17)N1—C8—C9—O423.7 (3)
Mg1—O1—Mg2—O6145.07 (12)C8—N1—C10—C11142.0 (2)
C4—O1—Mg2—O13113.8 (11)C7—N1—C10—C1194.7 (3)
Mg1—O1—Mg2—O1363.1 (12)Mg1—N1—C10—C1124.5 (3)
C4—O1—Mg2—O8123.96 (17)Mg1—O3—C11—O2175.0 (2)
Mg1—O1—Mg2—O859.12 (13)Mg1—O3—C11—C101.8 (3)
C4—O1—Mg2—N247.03 (17)N1—C10—C11—O2166.1 (2)
Mg1—O1—Mg2—N2136.05 (13)N1—C10—C11—O316.9 (4)
O12—Mg2—N2—C1520.7 (16)C2—C3—C12—N2112.7 (3)
O6—Mg2—N2—C15141.87 (17)C4—C3—C12—N268.0 (3)
O1—Mg2—N2—C15123.98 (16)C15—N2—C12—C3171.7 (2)
O13—Mg2—N2—C1557.45 (16)C13—N2—C12—C360.8 (3)
O8—Mg2—N2—C1531.80 (16)Mg2—N2—C12—C357.3 (2)
O12—Mg2—N2—C13143.6 (15)C15—N2—C13—C14143.2 (2)
O6—Mg2—N2—C1319.00 (16)C12—N2—C13—C1492.6 (3)
O1—Mg2—N2—C13113.15 (16)Mg2—N2—C13—C1426.3 (2)
O13—Mg2—N2—C1365.43 (16)Mg2—O6—C14—O7179.5 (2)
O8—Mg2—N2—C13154.67 (17)Mg2—O6—C14—C134.5 (3)
O12—Mg2—N2—C1295.9 (15)N2—C13—C14—O7161.7 (2)
O6—Mg2—N2—C12101.52 (16)N2—C13—C14—O622.1 (3)
O1—Mg2—N2—C127.37 (16)C13—N2—C15—C16156.9 (2)
O13—Mg2—N2—C12174.06 (15)C12—N2—C15—C1677.6 (3)
O8—Mg2—N2—C1284.82 (16)Mg2—N2—C15—C1639.0 (2)
O12—Mg2—O6—C14170.4 (2)Mg2—O8—C16—O9175.5 (2)
O1—Mg2—O6—C1499.0 (2)Mg2—O8—C16—C153.3 (3)
O13—Mg2—O6—C1485.3 (2)N2—C15—C16—O9155.1 (2)
O8—Mg2—O6—C146.2 (3)N2—C15—C16—O826.0 (3)
Symmetry code: (i) x, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O10—H10C···O80.891.972.828 (3)160
O10—H10D···O150.801.922.714 (3)169
O11—H11A···O14ii0.822.232.932 (4)143
O11—H11B···O220.831.932.743 (3)164
O12—H12C···O18iii0.811.932.723 (3)170
O12—H12D···O40.881.882.712 (3)157
O13—H13C···O18iv0.822.032.812 (3)158
O13—H13D···O23ii0.871.932.789 (3)171
O24—H24A···O40.882.032.897 (3)171
O24—H24B···O160.821.922.742 (3)176
O25—H25A···O220.831.912.734 (3)171
O25—H25B···O19i0.901.822.712 (3)170
O26—H26A···O5i0.851.962.805 (3)177
O26—H26B···O20ii0.831.982.807 (3)177
O14—H14A···O3v0.842.212.796 (4)127
O15—H15C···O21ii0.891.902.759 (3)163
O15—H15D···O5vi0.851.872.716 (3)175
O16—H16A···O80.792.112.893 (3)171
O16—H16B···O190.831.932.754 (3)172
O17—H17A···O90.931.782.695 (3)166
O18—H18A···O170.891.852.722 (4)166
O18—H18B···O25ii0.842.032.869 (3)179
O19—H19A···O2v0.821.922.737 (3)179
O19—H19B···O23ii0.821.962.760 (3)164
O20—H20A···O20ii0.821.982.770 (6)162
O20—H20B···O160.922.273.008 (3)138
O21—H21A···O2v0.811.962.762 (3)170
O21—H21B···O200.811.972.761 (4)164
O22—H22A···O21ii0.911.872.769 (3)173
O22—H22B···O7vii0.801.872.662 (3)173
O23—H23A···O6viii0.812.032.812 (3)162
O23—H23B···O9vii0.822.052.803 (3)151
Symmetry codes: (i) x, y+1, z+1; (ii) x+1, y+1, z+1; (iii) x1, 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
Mr780.79
Crystal system, space groupTriclinic, 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)
V3)1721.2 (6)
Z2
Radiation typeMo Kα
µ (mm1)0.25
Crystal size (mm)0.30 × 0.20 × 0.20
Data collection
DiffractometerBruker SMART 1K CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 2000)
Tmin, Tmax0.928, 0.951
No. of measured, independent and
observed [I > 2σ(I)] reflections
7116, 5921, 4743
Rint0.016
(sin θ/λ)max1)0.595
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.050, 0.137, 1.05
No. of reflections5921
No. of parameters430
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)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.

Selected geometric parameters (Å, º) top
Mg1—O102.015 (2)O1—Mg22.072 (2)
Mg1—O12.062 (2)Mg2—O121.992 (2)
Mg1—O32.063 (2)Mg2—O62.071 (2)
Mg1—O42.088 (2)Mg2—O132.075 (2)
Mg1—O112.114 (2)Mg2—O82.111 (2)
Mg1—N12.210 (2)Mg2—N22.201 (2)
O10—Mg1—O186.59 (8)O12—Mg2—O189.45 (8)
O10—Mg1—O3105.62 (9)O6—Mg2—O194.33 (8)
O1—Mg1—O399.82 (8)O12—Mg2—O1386.54 (9)
O10—Mg1—O497.90 (9)O6—Mg2—O1385.07 (8)
O1—Mg1—O493.27 (8)O1—Mg2—O13175.66 (9)
O3—Mg1—O4153.61 (9)O12—Mg2—O899.64 (9)
O10—Mg1—O1191.51 (9)O6—Mg2—O8154.89 (9)
O1—Mg1—O11175.96 (9)O1—Mg2—O892.44 (8)
O3—Mg1—O1184.13 (8)O13—Mg2—O889.88 (8)
O4—Mg1—O1183.45 (8)O12—Mg2—N2176.46 (10)
O10—Mg1—N1174.52 (9)O6—Mg2—N278.81 (8)
O1—Mg1—N190.04 (8)O1—Mg2—N291.36 (8)
O3—Mg1—N179.20 (8)O13—Mg2—N292.74 (9)
O4—Mg1—N177.97 (8)O8—Mg2—N276.89 (8)
O11—Mg1—N191.58 (9)O24—Mg3—O2688.02 (8)
Mg1—O1—Mg2132.72 (9)O24—Mg3—O2586.88 (8)
O12—Mg2—O6104.57 (9)O26—Mg3—O2590.82 (8)
O10—Mg1—O1—Mg250.67 (13)Mg1—O1—Mg2—O1240.50 (14)
O3—Mg1—O1—Mg2155.95 (12)Mg1—O1—Mg2—O6145.07 (12)
O4—Mg1—O1—Mg247.05 (13)Mg1—O1—Mg2—O1363.1 (12)
O11—Mg1—O1—Mg211.4 (13)Mg1—O1—Mg2—O859.12 (13)
N1—Mg1—O1—Mg2125.01 (13)Mg1—O1—Mg2—N2136.05 (13)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O10—H10C···O80.891.972.828 (3)160
O10—H10D···O150.801.922.714 (3)169
O11—H11A···O14i0.822.232.932 (4)143
O11—H11B···O220.831.932.743 (3)164
O12—H12C···O18ii0.811.932.723 (3)170
O12—H12D···O40.881.882.712 (3)157
O13—H13C···O18iii0.822.032.812 (3)158
O13—H13D···O23i0.871.932.789 (3)171
O24—H24A···O40.882.032.897 (3)171
O24—H24B···O160.821.922.742 (3)176
O25—H25A···O220.831.912.734 (3)171
O25—H25B···O19iv0.901.822.712 (3)170
O26—H26A···O5iv0.851.962.805 (3)177
O26—H26B···O20i0.831.982.807 (3)177
O14—H14A···O3v0.842.212.796 (4)127
O15—H15C···O21i0.891.902.759 (3)163
O15—H15D···O5vi0.851.872.716 (3)175
O16—H16A···O80.792.112.893 (3)171
O16—H16B···O190.831.932.754 (3)172
O17—H17A···O90.931.782.695 (3)166
O18—H18A···O170.891.852.722 (4)166
O18—H18B···O25i0.842.032.869 (3)179
O19—H19A···O2v0.821.922.737 (3)179
O19—H19B···O23i0.821.962.760 (3)164
O20—H20A···O20i0.821.982.770 (6)162
O20—H20B···O160.922.273.008 (3)138
O21—H21A···O2v0.811.962.762 (3)170
O21—H21B···O200.811.972.761 (4)164
O22—H22A···O21i0.911.872.769 (3)173
O22—H22B···O7vii0.801.872.662 (3)173
O23—H23A···O6viii0.812.032.812 (3)162
O23—H23B···O9vii0.822.052.803 (3)151
Symmetry codes: (i) x+1, y+1, z+1; (ii) x1, 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.
 

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