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The structure of the title compound, {[Mg(C4H7O2)2(H2O)3]·H2O}n, features one-dimensional ...2-ib)Mg(μ2-ib)Mg... zigzag chains (ib is isobutyrate) parallel to the c axis. The octa­hedral Mg environment is completed by three fac-oriented terminal water ligands, as well as one further monodentate end-on coordinated ib ligand. In the crystal structure, the hydro­phobic ib groups are all oriented within one half of the coordination perimeter of each chain, whereas the water ligands, together with hydrogen-bonded non­coordinated solvent water mol­ecules, define the other half. Along the a axis, neighbouring strands are oriented so that both the hydro­philic and hydro­phobic sides are adjacent to each other. This results in an extensive hydrogen-bonding network within the hydro­philic areas, also involving an additional solvent water mol­ecule per formula unit. There are van der Waals contacts between the aliphatic isopropyl groups of the hydro­phobic areas.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270113025043/fg3307sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270113025043/fg3307Isup2.hkl
Contains datablock I

mol

MDL mol file https://doi.org/10.1107/S0108270113025043/fg3307Isup3.mol
Supplementary material

cml

Chemical Markup Language (CML) file https://doi.org/10.1107/S0108270113025043/fg3307Isup4.cml
Supplementary material

CCDC reference: 960018

Introduction top

Although metal isobutyrate salts are important precursors for the synthesis of a wide variety of polynuclear coordination complexes (Baca et al., 2011; Malaestean, Ellern et al., 2012 or Malaestean, Kutluca-Alici et al., 2012 ?) and coordination polymers (Malaestean, Ellern et al., 2012 or Malaestean, Kutluca-Alici et al., 2012 ?), only two single-crystal X-ray diffraction-derived structures of such salts have been published to date: [Mg6(µ-ib)12(Hib)6] [Hib is isobutyric acid; CSD (Allen, 2002) deposition No. 228263; Coker et al., 2004] and [MnII6(µ-ib)12(Hib)6] (CSD deposition No. 882829; Malaestean et al., 2013). Both compounds crystallize in the space group R3 and feature hexanuclear rings consisting of an M6(µ-ib)12 core in a regular chair conformation, while six Hib groups each coordinate to an M2+ site as terminal monodentate ligands. We now present details of a third such compound, the title complex, (I). [Please check added double bonds in ib carboxyl­ates in scheme]

Experimental top

Synthesis and crystallization top

{[Mg(ib)2(H2O)3].H2O}n, (I), was obtained by heating Mg(OH)2 (2.0 g, 34.28 mmol) in isobutyric acid (20 ml, 220.1 mmol) at 423 K until all excess of organic acid was evaporated. The colourless microcrystalline product obtained was washed with water and ethanol and dried in air (yield 3.25 g, 35%). Needle-like colourless single crystals of (I) were obtained by recrystallization of the crude product from aceto­nitrile. Elemental analysis, calculated for C8H22O8Mg: C 35.51, H 8.20%; found: C 36.19, H 8.08%. IR (4000–370 cm-1, KBr pellet, ν, cm-1): 3433 (br, s), 2966 (m), 2926 (sh), 2868 (w), 1564 (vs), 1475 (m), 1437 (m), 1416 (sh), 1358 (w), 1360 (sh), 1309 (m), 1282 (sh), 1167 (w), 1099 (m), 905 (w), 845 (w), 812 (w), 785 (w), 733 (sh), 644 (m), 534 (m), 409 (w).

Thermogravimetric and thermodifferential analysis was performed in the temperature range 298–873 K (5 K min-1) under N2 flow (60 ml min-1). Two well defined steps were observed. The first step, from 298 to 383 K, corresponds to the loss of the solvent and two of the coordinated H2O molecules (calculated 19.9%, found 23.7%). The second step, from 385 to 753 K, corresponds to the loss of the remaining ligands (calculated 71.7%, found 70.8%).

Refinement top

Crystal data, data collection and structure refinement details are summarized in Table 1. Crystal data, data collection and structure refinement details are summarized in Table 1. The systematic absences in the diffraction data were consistent for the stated space group. The positions of almost all non-H atoms were found by direct methods. The remaining atoms were located in an alternating series of least-squares cycles on difference Fourier maps. All non-H atoms were refined in full-matrix anisotropic approximation. The H atoms of the coordinated and solvent water molecules were found objectively in a difference Fourier map and refined isotropically. All other H atoms were placed in idealized positions, with C—H = 0.98 Å for methyl H or 1.0 Å otherwise, and allowed to ride on their parent atoms, with Uiso(H) = 1.5Ueq(C) for methyl H or 1.2Ueq(C) otherwise. [Please check added text]

Results and discussion top

The direct reaction of magnesium hydroxide with isobutyric acid yields a crude product that can be recrystallized from aceto­nitrile to yield crystals of magnesium isobutyrate tetra­hydrate, (I), suitable for single-crystal X-ray diffraction analysis. The monoclinic solid-state structure (space group P21/c) of (I) features an asymmetric unit consisting of an Mg2+ cation with three water and two ib ligands, along with one non-coordinated solvent water molecule (Fig. 1). The crystal structure is characterized by collinear zigzag chains of Mg2+ cations inter­linked by ib anions in a standard µ2-bridging fashion, propagating along c. The ···Mg···Mg···Mg··· zigzag planes are parallel to the bc plane [Mg···Mg = 4.9018 (12) Å] (Fig. 2). Each Mg2+ cation is six-coordinated, with three fac-arranged H2O ligands [Mg—OH2O = 2.0824 (19)–2.1671 (18) Å], two bidentate µ-ib groups [Mg—Ocarb = 2.0103 (17)–2.0399 (17) Å] and a further monodentate terminal ib ligand [Mg—Ocarb = 2.0485 (17) Å]. The deprotonated state of the monodentate ib ligand is evident from the short CO bond distance [1.244 (3) Å].

This binding situation leads to one half of the coordination perimeter of each polymer strand being hydro­philic, whereas the hydro­phobic iso­propyl groups of the ib ligands are arranged on the opposite side of the zigzag plane. Along the a axis, adjacent polymer strands are stacked in alternating orientations, leading to a pairing of both the hydro­philic and hydro­phobic environments of neighbouring polymer chains. This configuration appears to be strongly stabilized by an extensive network of intra- and inter­chain hydrogen bonds. The solvent water molecule forms two inter­chain hydrogen bonds, one with the uncoordinated carb­oxy group of the monodentate ib [O8(–H1W)···O1 = 2.777 (3) Å)] and one with one of the coordinated water molecules [O8(–H2W)···O5i = 2.845 (3) Å] (see Table 2 for full geometric parameters and symmetry codes).

Each of the three coordinated water molecules forms two hydrogen bonds. Atom O3 forms one inter­chain bond [O3(–H3W)···O2ii = 2.670 (2) Å] with the coordinated group of the monodentate ib ligand and one inter­chain bond [O3(–H4W)···O8iii = 2.807 (3) Å] with a solvent water molecule. Atom O4 forms one intra­chain bond [O4(–H5W)···O3iv = 2.894 (3) Å] with the uncoordinated CO group from an adjacent repeat unit and one inter­chain bond [O4(–H6W)···O1ii = 2.713 (3) Å] with the uncoordinated group of the monodentate ib. Atom O5 forms one inter­chain bond [O5(–H7W)···O8ii = 2.869 (3) Å] with a solvent water molecule and one intra­chain bond [O5(–H8W)···O6v = 2.720 (2) Å] with an O atom of the bidentate ib ligand.

On the other hand, the hydro­phobic parts of neighbouring polymer chains are oriented so as to maximize the van der Waals inter­actions between ib ligands. Overall, this stacking results in alternating hydro­phobic–hydro­philic slabs along a (Fig. 3), and we postulate that the stabilizing supra­molecular inter­actions that are possible within this arrangement are the primary reason for the successful growth of sufficiently sized single crystals of this compound.

Related literature top

For related literature, see: Allen (2002); Baca et al. (2011); Coker et al. (2004); Malaestean et al. (2013); Malaestean, Ellern, Baca & Kögerler (2012); Malaestean, Kutluca-Alici, Ellern, van Leusen, Schilder, Speldrich, Baca & Kögerler (2012).

Computing details top

Data collection: APEX2 (Bruker, 2009); cell refinement: SAINT (Bruker, 2009); data reduction: SAINT (Bruker, 2009); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XSHELL (Bruker, 2007); software used to prepare material for publication: APEX2 (Bruker, 2009).

Figures top
[Figure 1] Fig. 1. The asymmetric unit of (I), with the atom-numbering scheme. Displacement ellipsoids are drawn at the 50% probability level. C-bound H atoms have been omitted. [Added text OK?] [TONY: is this practice acceptable or should they all be included?]
[Figure 2] Fig. 2. Ball-and-stick representation of two [Mg(ib)2(H2O)3]n strands protruding from the unit cell parallel to c. Dashed lines indicate hydrogen bonds [Added text OK?]. Colour code in the electronic version of the journal: Mg blue, O (ib) red, O (H2O ligands) yellow, O (H2O solvent) purple, C (monodentate ib) green, C (bridging ib) light grey and H black.
[Figure 3] Fig. 3. Simplified representation of the crystal packing of (I), seen along the direction of the zigzag polymer strands, i.e. c. Shown are the two strands crossing the central unit cell and segments of neighbouring groups. In the electronic version of the journal, the light-yellow and light-grey shading indicates the sequence of hydrophilic and hydrophobic volume slabs that alternate along a. Colour codes: Mg blue, O red, C grey and H black. [Is revised orientation acceptable?]
catena-Poly[[[triaqua(isobutyrato-κO)magnesium(II)]-µ-isobutyrato-κ2O:O'] monohydrate] top
Crystal data top
[Mg(C4H7O2)2(H2O)3]·H2OZ = 4
Mr = 270.57F(000) = 584
Monoclinic, P21/cDx = 1.324 Mg m3
Hall symbol: -P 2ybcMo Kα radiation, λ = 0.71073 Å
a = 13.808 (4) ŵ = 0.16 mm1
b = 10.704 (3) ÅT = 173 K
c = 9.183 (2) ÅNeedle, colourless
β = 90.241 (4)°0.32 × 0.08 × 0.06 mm
V = 1357.2 (6) Å3
Data collection top
Bruker APEX2 CCD area-detector
diffractometer
1721 reflections with I > 2σ(I)
ω scansRint = 0.077
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
θmax = 25.0°, θmin = 2.4°
Tmin = 0.95, Tmax = 0.99h = 1616
10631 measured reflectionsk = 1212
2403 independent reflectionsl = 1010
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)] = 0.042Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.092H atoms treated by a mixture of independent and constrained refinement
S = 1.03 w = 1/[σ2(Fo2) + (0.0368P)2 + 0.1518P]
where P = (Fo2 + 2Fc2)/3
2403 reflections(Δ/σ)max < 0.001
190 parametersΔρmax = 0.21 e Å3
0 restraintsΔρmin = 0.26 e Å3
Crystal data top
[Mg(C4H7O2)2(H2O)3]·H2OV = 1357.2 (6) Å3
Mr = 270.57Z = 4
Monoclinic, P21/cMo Kα radiation
a = 13.808 (4) ŵ = 0.16 mm1
b = 10.704 (3) ÅT = 173 K
c = 9.183 (2) Å0.32 × 0.08 × 0.06 mm
β = 90.241 (4)°
Data collection top
Bruker APEX2 CCD area-detector
diffractometer
2403 independent reflections
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
1721 reflections with I > 2σ(I)
Tmin = 0.95, Tmax = 0.99Rint = 0.077
10631 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0420 restraints
wR(F2) = 0.092H atoms treated by a mixture of independent and constrained refinement
S = 1.03Δρmax = 0.21 e Å3
2403 reflectionsΔρmin = 0.26 e Å3
190 parameters
Special details top

Experimental. A X-ray quality crystal was selected under ambient conditions and covered with Paratone oil. The crystal was mounted and centered in the X-ray beam by using a video camera. The crystal evaluation and data collection were performed on APEX2 CCD diffractometer with the detector to crystal distance of 5 cm. The initial cell constants were obtained from three series of OMEGA scans at different starting angles. Each series consisted of 30 frames collected at intervals of 0.3 in a 10 range about OMEGA with the exposure time of 10 s per frame. The obtained reflections were successfully indexed by an automated indexing routine built to APEX2 program package. The final cell constants were calculated from a set of strong reflections from the actual data collection.

The data were collected using the full sphere routine by collecting four sets of frames with 0.3 scans in ω with an exposure time of 10 sec per frame until a resolution of 0.69 Å. Data were truncated to the resolution with statistically reasonable R.

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. Final results were tested with CHECKCIF routine and all A-warnings (if any) were addressed on the very top of this file.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Mg10.12438 (5)0.33018 (6)0.00388 (8)0.0143 (2)
C10.19482 (17)0.5987 (2)0.0682 (2)0.0177 (5)
C20.29819 (17)0.5696 (2)0.1128 (3)0.0220 (6)
H20.31560.48660.07050.026*
C30.3031 (2)0.5581 (3)0.2777 (3)0.0431 (8)
H3A0.28350.63740.32210.065*
H3B0.36960.53820.30740.065*
H3C0.25950.49140.30980.065*
C40.37052 (19)0.6644 (2)0.0576 (3)0.0347 (7)
H4A0.3630.67390.0480.052*
H4B0.43640.63580.07980.052*
H4C0.35910.7450.10520.052*
C50.24982 (16)0.1865 (2)0.2312 (3)0.0161 (5)
C60.33175 (18)0.1333 (2)0.1417 (3)0.0263 (6)
H60.30640.11880.04090.032*
C70.3687 (2)0.0102 (2)0.1985 (3)0.0425 (8)
H7A0.39820.02250.29460.064*
H7B0.41720.02330.13130.064*
H7C0.31470.04880.20640.064*
C80.4127 (2)0.2271 (3)0.1311 (4)0.0644 (11)
H8A0.4350.24940.22920.097*
H8B0.38930.30210.0810.097*
H8C0.46650.19070.07630.097*
O10.17124 (12)0.70709 (14)0.03443 (19)0.0284 (4)
O20.13337 (11)0.50954 (14)0.07277 (16)0.0189 (4)
O30.03266 (13)0.39687 (15)0.17316 (18)0.0167 (4)
O40.00138 (13)0.29858 (16)0.1149 (2)0.0192 (4)
O50.10061 (14)0.14380 (14)0.08897 (19)0.0175 (4)
O60.19584 (11)0.26861 (14)0.17328 (16)0.0185 (4)
O70.23989 (11)0.15100 (14)0.36010 (16)0.0182 (4)
O80.09656 (14)0.93926 (17)0.10880 (19)0.0245 (4)
H1W0.135 (3)0.878 (3)0.094 (4)0.075 (12)*
H2W0.117 (2)0.993 (3)0.042 (3)0.051 (9)*
H3W0.022 (2)0.428 (3)0.138 (3)0.042 (9)*
H4W0.055 (2)0.454 (3)0.228 (3)0.047 (9)*
H5W0.0019 (18)0.246 (2)0.169 (3)0.022 (8)*
H6W0.064 (2)0.297 (3)0.069 (3)0.066 (11)*
H7W0.037 (2)0.123 (2)0.108 (3)0.043 (9)*
H8W0.130 (2)0.155 (2)0.168 (3)0.038 (9)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mg10.0187 (4)0.0117 (4)0.0126 (4)0.0001 (3)0.0007 (3)0.0002 (3)
C10.0239 (14)0.0139 (12)0.0153 (13)0.0017 (11)0.0026 (11)0.0041 (10)
C20.0236 (14)0.0161 (13)0.0264 (15)0.0001 (11)0.0027 (12)0.0006 (10)
C30.0416 (19)0.055 (2)0.0324 (18)0.0159 (15)0.0132 (15)0.0109 (15)
C40.0266 (16)0.0324 (16)0.0449 (18)0.0046 (13)0.0037 (13)0.0040 (13)
C50.0154 (12)0.0143 (12)0.0185 (13)0.0036 (10)0.0007 (10)0.0018 (10)
C60.0268 (15)0.0372 (15)0.0148 (13)0.0106 (12)0.0057 (11)0.0011 (12)
C70.0389 (18)0.0261 (15)0.063 (2)0.0078 (14)0.0163 (16)0.0053 (15)
C80.0350 (18)0.0411 (19)0.117 (3)0.0128 (16)0.037 (2)0.038 (2)
O10.0269 (10)0.0122 (9)0.0462 (12)0.0003 (8)0.0071 (9)0.0025 (8)
O20.0195 (9)0.0136 (8)0.0235 (9)0.0019 (7)0.0015 (7)0.0040 (7)
O30.0208 (10)0.0141 (9)0.0152 (9)0.0031 (8)0.0022 (8)0.0022 (7)
O40.0231 (11)0.0170 (10)0.0174 (10)0.0009 (8)0.0009 (8)0.0054 (8)
O50.0226 (11)0.0148 (9)0.0150 (10)0.0008 (8)0.0023 (8)0.0015 (7)
O60.0221 (9)0.0212 (9)0.0121 (8)0.0046 (7)0.0001 (7)0.0021 (7)
O70.0211 (9)0.0213 (9)0.0122 (9)0.0038 (7)0.0032 (7)0.0034 (7)
O80.0347 (11)0.0156 (9)0.0232 (11)0.0014 (9)0.0050 (9)0.0037 (8)
Geometric parameters (Å, º) top
Mg1—O62.0103 (17)C5—O61.268 (3)
Mg1—O7i2.0399 (17)C5—C61.512 (3)
Mg1—O22.0485 (17)C6—C71.505 (3)
Mg1—O42.0824 (19)C6—C81.506 (4)
Mg1—O32.1245 (18)C6—H61.0
Mg1—O52.1671 (18)C7—H7A0.98
Mg1—H8W2.41 (3)C7—H7B0.98
C1—O11.244 (3)C7—H7C0.98
C1—O21.278 (3)C8—H8A0.98
C1—C21.516 (3)C8—H8B0.98
C2—C41.513 (3)C8—H8C0.98
C2—C31.520 (3)O3—H3W0.88 (3)
C2—H21.0O3—H4W0.85 (3)
C3—H3A0.98O4—H5W0.75 (3)
C3—H3B0.98O4—H6W0.96 (3)
C3—H3C0.98O5—H7W0.92 (3)
C4—H4A0.98O5—H8W0.84 (3)
C4—H4B0.98O7—Mg1ii2.0399 (17)
C4—H4C0.98O8—H1W0.85 (4)
C5—O71.252 (3)O8—H2W0.89 (3)
O6—Mg1—O7i98.37 (7)H4A—C4—H4B109.5
O6—Mg1—O290.02 (7)C2—C4—H4C109.5
O7i—Mg1—O294.10 (7)H4A—C4—H4C109.5
O6—Mg1—O486.00 (8)H4B—C4—H4C109.5
O7i—Mg1—O4173.09 (8)O7—C5—O6122.7 (2)
O2—Mg1—O491.24 (7)O7—C5—C6119.0 (2)
O6—Mg1—O3172.47 (8)O6—C5—C6118.2 (2)
O7i—Mg1—O389.08 (8)C7—C6—C8110.8 (2)
O2—Mg1—O388.37 (7)C7—C6—C5113.2 (2)
O4—Mg1—O386.68 (8)C8—C6—C5110.0 (2)
O6—Mg1—O593.61 (7)C7—C6—H6107.5
O7i—Mg1—O589.30 (7)C8—C6—H6107.5
O2—Mg1—O5174.62 (8)C5—C6—H6107.5
O4—Mg1—O585.06 (7)C6—C7—H7A109.5
O3—Mg1—O587.51 (7)C6—C7—H7B109.5
O6—Mg1—H8W103.5 (6)H7A—C7—H7B109.5
O7i—Mg1—H8W70.6 (7)C6—C7—H7C109.5
O2—Mg1—H8W160.6 (7)H7A—C7—H7C109.5
O4—Mg1—H8W103.3 (7)H7B—C7—H7C109.5
O3—Mg1—H8W79.9 (6)C6—C8—H8A109.5
O5—Mg1—H8W20.3 (6)C6—C8—H8B109.5
O1—C1—O2122.1 (2)H8A—C8—H8B109.5
O1—C1—C2120.3 (2)C6—C8—H8C109.5
O2—C1—C2117.5 (2)H8A—C8—H8C109.5
C4—C2—C1113.2 (2)H8B—C8—H8C109.5
C4—C2—C3111.2 (2)C1—O2—Mg1136.73 (15)
C1—C2—C3108.9 (2)Mg1—O3—H3W111.5 (18)
C4—C2—H2107.8Mg1—O3—H4W117 (2)
C1—C2—H2107.8H3W—O3—H4W105 (3)
C3—C2—H2107.8Mg1—O4—H5W119 (2)
C2—C3—H3A109.5Mg1—O4—H6W121.2 (18)
C2—C3—H3B109.5H5W—O4—H6W105 (3)
H3A—C3—H3B109.5Mg1—O5—H7W115.9 (17)
C2—C3—H3C109.5Mg1—O5—H8W96.3 (18)
H3A—C3—H3C109.5H7W—O5—H8W109 (3)
H3B—C3—H3C109.5C5—O6—Mg1148.47 (15)
C2—C4—H4A109.5C5—O7—Mg1ii129.67 (15)
C2—C4—H4B109.5H1W—O8—H2W101 (3)
Symmetry codes: (i) x, y+1/2, z1/2; (ii) x, y+1/2, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O8—H1W···O10.85 (4)1.97 (4)2.777 (3)155 (3)
O8—H2W···O5iii0.89 (3)2.02 (3)2.845 (3)153 (3)
O3—H3W···O2iv0.88 (3)1.79 (3)2.670 (2)178 (3)
O3—H4W···O8v0.85 (3)1.97 (3)2.807 (3)166 (3)
O4—H5W···O3ii0.75 (2)2.16 (3)2.894 (3)166 (3)
O4—H6W···O1iv0.97 (4)1.76 (3)2.713 (3)173 (3)
O5—H7W···O8iv0.92 (3)1.96 (3)2.869 (3)168 (2)
O5—H8W···O6i0.84 (3)1.90 (3)2.720 (2)162 (2)
Symmetry codes: (i) x, y+1/2, z1/2; (ii) x, y+1/2, z+1/2; (iii) x, y+1, z; (iv) x, y+1, z; (v) x, y+3/2, z1/2.

Experimental details

Crystal data
Chemical formula[Mg(C4H7O2)2(H2O)3]·H2O
Mr270.57
Crystal system, space groupMonoclinic, P21/c
Temperature (K)173
a, b, c (Å)13.808 (4), 10.704 (3), 9.183 (2)
β (°) 90.241 (4)
V3)1357.2 (6)
Z4
Radiation typeMo Kα
µ (mm1)0.16
Crystal size (mm)0.32 × 0.08 × 0.06
Data collection
DiffractometerBruker APEX2 CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Sheldrick, 1996)
Tmin, Tmax0.95, 0.99
No. of measured, independent and
observed [I > 2σ(I)] reflections
10631, 2403, 1721
Rint0.077
(sin θ/λ)max1)0.596
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.042, 0.092, 1.03
No. of reflections2403
No. of parameters190
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.21, 0.26

Computer programs: APEX2 (Bruker, 2009), SAINT (Bruker, 2009), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), XSHELL (Bruker, 2007).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O8—H1W···O10.85 (4)1.97 (4)2.777 (3)155 (3)
O8—H2W···O5i0.89 (3)2.02 (3)2.845 (3)153 (3)
O3—H3W···O2ii0.88 (3)1.79 (3)2.670 (2)178 (3)
O3—H4W···O8iii0.85 (3)1.97 (3)2.807 (3)166 (3)
O4—H5W···O3iv0.75 (2)2.16 (3)2.894 (3)166 (3)
O4—H6W···O1ii0.97 (4)1.76 (3)2.713 (3)173 (3)
O5—H7W···O8ii0.92 (3)1.96 (3)2.869 (3)168 (2)
O5—H8W···O6v0.84 (3)1.90 (3)2.720 (2)162 (2)
Symmetry codes: (i) x, y+1, z; (ii) x, y+1, z; (iii) x, y+3/2, z1/2; (iv) x, y+1/2, z+1/2; (v) x, y+1/2, z1/2.
 

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