Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270113025043/fg3307sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270113025043/fg3307Isup2.hkl | |
MDL mol file https://doi.org/10.1107/S0108270113025043/fg3307Isup3.mol | |
Chemical Markup Language (CML) file https://doi.org/10.1107/S0108270113025043/fg3307Isup4.cml |
CCDC reference: 960018
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]
{[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%).
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]
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 C═O 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 C═O 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.
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).
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).
[Mg(C4H7O2)2(H2O)3]·H2O | Z = 4 |
Mr = 270.57 | F(000) = 584 |
Monoclinic, P21/c | Dx = 1.324 Mg m−3 |
Hall symbol: -P 2ybc | Mo Kα radiation, λ = 0.71073 Å |
a = 13.808 (4) Å | µ = 0.16 mm−1 |
b = 10.704 (3) Å | T = 173 K |
c = 9.183 (2) Å | Needle, colourless |
β = 90.241 (4)° | 0.32 × 0.08 × 0.06 mm |
V = 1357.2 (6) Å3 |
Bruker APEX2 CCD area-detector diffractometer | 1721 reflections with I > 2σ(I) |
ω scans | Rint = 0.077 |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | θmax = 25.0°, θmin = 2.4° |
Tmin = 0.95, Tmax = 0.99 | h = −16→16 |
10631 measured reflections | k = −12→12 |
2403 independent reflections | l = −10→10 |
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)] = 0.042 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.092 | H 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 parameters | Δρmax = 0.21 e Å−3 |
0 restraints | Δρmin = −0.26 e Å−3 |
[Mg(C4H7O2)2(H2O)3]·H2O | V = 1357.2 (6) Å3 |
Mr = 270.57 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 13.808 (4) Å | µ = 0.16 mm−1 |
b = 10.704 (3) Å | T = 173 K |
c = 9.183 (2) Å | 0.32 × 0.08 × 0.06 mm |
β = 90.241 (4)° |
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 = 0.99 | Rint = 0.077 |
10631 measured reflections |
R[F2 > 2σ(F2)] = 0.042 | 0 restraints |
wR(F2) = 0.092 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.03 | Δρmax = 0.21 e Å−3 |
2403 reflections | Δρmin = −0.26 e Å−3 |
190 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
Mg1 | 0.12438 (5) | 0.33018 (6) | −0.00388 (8) | 0.0143 (2) | |
C1 | 0.19482 (17) | 0.5987 (2) | 0.0682 (2) | 0.0177 (5) | |
C2 | 0.29819 (17) | 0.5696 (2) | 0.1128 (3) | 0.0220 (6) | |
H2 | 0.3156 | 0.4866 | 0.0705 | 0.026* | |
C3 | 0.3031 (2) | 0.5581 (3) | 0.2777 (3) | 0.0431 (8) | |
H3A | 0.2835 | 0.6374 | 0.3221 | 0.065* | |
H3B | 0.3696 | 0.5382 | 0.3074 | 0.065* | |
H3C | 0.2595 | 0.4914 | 0.3098 | 0.065* | |
C4 | 0.37052 (19) | 0.6644 (2) | 0.0576 (3) | 0.0347 (7) | |
H4A | 0.363 | 0.6739 | −0.048 | 0.052* | |
H4B | 0.4364 | 0.6358 | 0.0798 | 0.052* | |
H4C | 0.3591 | 0.745 | 0.1052 | 0.052* | |
C5 | 0.24982 (16) | 0.1865 (2) | 0.2312 (3) | 0.0161 (5) | |
C6 | 0.33175 (18) | 0.1333 (2) | 0.1417 (3) | 0.0263 (6) | |
H6 | 0.3064 | 0.1188 | 0.0409 | 0.032* | |
C7 | 0.3687 (2) | 0.0102 (2) | 0.1985 (3) | 0.0425 (8) | |
H7A | 0.3982 | 0.0225 | 0.2946 | 0.064* | |
H7B | 0.4172 | −0.0233 | 0.1313 | 0.064* | |
H7C | 0.3147 | −0.0488 | 0.2064 | 0.064* | |
C8 | 0.4127 (2) | 0.2271 (3) | 0.1311 (4) | 0.0644 (11) | |
H8A | 0.435 | 0.2494 | 0.2292 | 0.097* | |
H8B | 0.3893 | 0.3021 | 0.081 | 0.097* | |
H8C | 0.4665 | 0.1907 | 0.0763 | 0.097* | |
O1 | 0.17124 (12) | 0.70709 (14) | 0.03443 (19) | 0.0284 (4) | |
O2 | 0.13337 (11) | 0.50954 (14) | 0.07277 (16) | 0.0189 (4) | |
O3 | 0.03266 (13) | 0.39687 (15) | −0.17316 (18) | 0.0167 (4) | |
O4 | −0.00138 (13) | 0.29858 (16) | 0.1149 (2) | 0.0192 (4) | |
O5 | 0.10061 (14) | 0.14380 (14) | −0.08897 (19) | 0.0175 (4) | |
O6 | 0.19584 (11) | 0.26861 (14) | 0.17328 (16) | 0.0185 (4) | |
O7 | 0.23989 (11) | 0.15100 (14) | 0.36010 (16) | 0.0182 (4) | |
O8 | 0.09656 (14) | 0.93926 (17) | 0.10880 (19) | 0.0245 (4) | |
H1W | 0.135 (3) | 0.878 (3) | 0.094 (4) | 0.075 (12)* | |
H2W | 0.117 (2) | 0.993 (3) | 0.042 (3) | 0.051 (9)* | |
H3W | −0.022 (2) | 0.428 (3) | −0.138 (3) | 0.042 (9)* | |
H4W | 0.055 (2) | 0.454 (3) | −0.228 (3) | 0.047 (9)* | |
H5W | −0.0019 (18) | 0.246 (2) | 0.169 (3) | 0.022 (8)* | |
H6W | −0.064 (2) | 0.297 (3) | 0.069 (3) | 0.066 (11)* | |
H7W | 0.037 (2) | 0.123 (2) | −0.108 (3) | 0.043 (9)* | |
H8W | 0.130 (2) | 0.155 (2) | −0.168 (3) | 0.038 (9)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mg1 | 0.0187 (4) | 0.0117 (4) | 0.0126 (4) | 0.0001 (3) | 0.0007 (3) | −0.0002 (3) |
C1 | 0.0239 (14) | 0.0139 (12) | 0.0153 (13) | −0.0017 (11) | 0.0026 (11) | −0.0041 (10) |
C2 | 0.0236 (14) | 0.0161 (13) | 0.0264 (15) | 0.0001 (11) | −0.0027 (12) | −0.0006 (10) |
C3 | 0.0416 (19) | 0.055 (2) | 0.0324 (18) | −0.0159 (15) | −0.0132 (15) | 0.0109 (15) |
C4 | 0.0266 (16) | 0.0324 (16) | 0.0449 (18) | −0.0046 (13) | −0.0037 (13) | 0.0040 (13) |
C5 | 0.0154 (12) | 0.0143 (12) | 0.0185 (13) | −0.0036 (10) | −0.0007 (10) | −0.0018 (10) |
C6 | 0.0268 (15) | 0.0372 (15) | 0.0148 (13) | 0.0106 (12) | 0.0057 (11) | −0.0011 (12) |
C7 | 0.0389 (18) | 0.0261 (15) | 0.063 (2) | 0.0078 (14) | 0.0163 (16) | −0.0053 (15) |
C8 | 0.0350 (18) | 0.0411 (19) | 0.117 (3) | 0.0128 (16) | 0.037 (2) | 0.038 (2) |
O1 | 0.0269 (10) | 0.0122 (9) | 0.0462 (12) | 0.0003 (8) | −0.0071 (9) | 0.0025 (8) |
O2 | 0.0195 (9) | 0.0136 (8) | 0.0235 (9) | −0.0019 (7) | 0.0015 (7) | −0.0040 (7) |
O3 | 0.0208 (10) | 0.0141 (9) | 0.0152 (9) | 0.0031 (8) | 0.0022 (8) | 0.0022 (7) |
O4 | 0.0231 (11) | 0.0170 (10) | 0.0174 (10) | −0.0009 (8) | 0.0009 (8) | 0.0054 (8) |
O5 | 0.0226 (11) | 0.0148 (9) | 0.0150 (10) | −0.0008 (8) | 0.0023 (8) | 0.0015 (7) |
O6 | 0.0221 (9) | 0.0212 (9) | 0.0121 (8) | 0.0046 (7) | −0.0001 (7) | 0.0021 (7) |
O7 | 0.0211 (9) | 0.0213 (9) | 0.0122 (9) | 0.0038 (7) | 0.0032 (7) | 0.0034 (7) |
O8 | 0.0347 (11) | 0.0156 (9) | 0.0232 (11) | 0.0014 (9) | 0.0050 (9) | 0.0037 (8) |
Mg1—O6 | 2.0103 (17) | C5—O6 | 1.268 (3) |
Mg1—O7i | 2.0399 (17) | C5—C6 | 1.512 (3) |
Mg1—O2 | 2.0485 (17) | C6—C7 | 1.505 (3) |
Mg1—O4 | 2.0824 (19) | C6—C8 | 1.506 (4) |
Mg1—O3 | 2.1245 (18) | C6—H6 | 1.0 |
Mg1—O5 | 2.1671 (18) | C7—H7A | 0.98 |
Mg1—H8W | 2.41 (3) | C7—H7B | 0.98 |
C1—O1 | 1.244 (3) | C7—H7C | 0.98 |
C1—O2 | 1.278 (3) | C8—H8A | 0.98 |
C1—C2 | 1.516 (3) | C8—H8B | 0.98 |
C2—C4 | 1.513 (3) | C8—H8C | 0.98 |
C2—C3 | 1.520 (3) | O3—H3W | 0.88 (3) |
C2—H2 | 1.0 | O3—H4W | 0.85 (3) |
C3—H3A | 0.98 | O4—H5W | 0.75 (3) |
C3—H3B | 0.98 | O4—H6W | 0.96 (3) |
C3—H3C | 0.98 | O5—H7W | 0.92 (3) |
C4—H4A | 0.98 | O5—H8W | 0.84 (3) |
C4—H4B | 0.98 | O7—Mg1ii | 2.0399 (17) |
C4—H4C | 0.98 | O8—H1W | 0.85 (4) |
C5—O7 | 1.252 (3) | O8—H2W | 0.89 (3) |
O6—Mg1—O7i | 98.37 (7) | H4A—C4—H4B | 109.5 |
O6—Mg1—O2 | 90.02 (7) | C2—C4—H4C | 109.5 |
O7i—Mg1—O2 | 94.10 (7) | H4A—C4—H4C | 109.5 |
O6—Mg1—O4 | 86.00 (8) | H4B—C4—H4C | 109.5 |
O7i—Mg1—O4 | 173.09 (8) | O7—C5—O6 | 122.7 (2) |
O2—Mg1—O4 | 91.24 (7) | O7—C5—C6 | 119.0 (2) |
O6—Mg1—O3 | 172.47 (8) | O6—C5—C6 | 118.2 (2) |
O7i—Mg1—O3 | 89.08 (8) | C7—C6—C8 | 110.8 (2) |
O2—Mg1—O3 | 88.37 (7) | C7—C6—C5 | 113.2 (2) |
O4—Mg1—O3 | 86.68 (8) | C8—C6—C5 | 110.0 (2) |
O6—Mg1—O5 | 93.61 (7) | C7—C6—H6 | 107.5 |
O7i—Mg1—O5 | 89.30 (7) | C8—C6—H6 | 107.5 |
O2—Mg1—O5 | 174.62 (8) | C5—C6—H6 | 107.5 |
O4—Mg1—O5 | 85.06 (7) | C6—C7—H7A | 109.5 |
O3—Mg1—O5 | 87.51 (7) | C6—C7—H7B | 109.5 |
O6—Mg1—H8W | 103.5 (6) | H7A—C7—H7B | 109.5 |
O7i—Mg1—H8W | 70.6 (7) | C6—C7—H7C | 109.5 |
O2—Mg1—H8W | 160.6 (7) | H7A—C7—H7C | 109.5 |
O4—Mg1—H8W | 103.3 (7) | H7B—C7—H7C | 109.5 |
O3—Mg1—H8W | 79.9 (6) | C6—C8—H8A | 109.5 |
O5—Mg1—H8W | 20.3 (6) | C6—C8—H8B | 109.5 |
O1—C1—O2 | 122.1 (2) | H8A—C8—H8B | 109.5 |
O1—C1—C2 | 120.3 (2) | C6—C8—H8C | 109.5 |
O2—C1—C2 | 117.5 (2) | H8A—C8—H8C | 109.5 |
C4—C2—C1 | 113.2 (2) | H8B—C8—H8C | 109.5 |
C4—C2—C3 | 111.2 (2) | C1—O2—Mg1 | 136.73 (15) |
C1—C2—C3 | 108.9 (2) | Mg1—O3—H3W | 111.5 (18) |
C4—C2—H2 | 107.8 | Mg1—O3—H4W | 117 (2) |
C1—C2—H2 | 107.8 | H3W—O3—H4W | 105 (3) |
C3—C2—H2 | 107.8 | Mg1—O4—H5W | 119 (2) |
C2—C3—H3A | 109.5 | Mg1—O4—H6W | 121.2 (18) |
C2—C3—H3B | 109.5 | H5W—O4—H6W | 105 (3) |
H3A—C3—H3B | 109.5 | Mg1—O5—H7W | 115.9 (17) |
C2—C3—H3C | 109.5 | Mg1—O5—H8W | 96.3 (18) |
H3A—C3—H3C | 109.5 | H7W—O5—H8W | 109 (3) |
H3B—C3—H3C | 109.5 | C5—O6—Mg1 | 148.47 (15) |
C2—C4—H4A | 109.5 | C5—O7—Mg1ii | 129.67 (15) |
C2—C4—H4B | 109.5 | H1W—O8—H2W | 101 (3) |
Symmetry codes: (i) x, −y+1/2, z−1/2; (ii) x, −y+1/2, z+1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O8—H1W···O1 | 0.85 (4) | 1.97 (4) | 2.777 (3) | 155 (3) |
O8—H2W···O5iii | 0.89 (3) | 2.02 (3) | 2.845 (3) | 153 (3) |
O3—H3W···O2iv | 0.88 (3) | 1.79 (3) | 2.670 (2) | 178 (3) |
O3—H4W···O8v | 0.85 (3) | 1.97 (3) | 2.807 (3) | 166 (3) |
O4—H5W···O3ii | 0.75 (2) | 2.16 (3) | 2.894 (3) | 166 (3) |
O4—H6W···O1iv | 0.97 (4) | 1.76 (3) | 2.713 (3) | 173 (3) |
O5—H7W···O8iv | 0.92 (3) | 1.96 (3) | 2.869 (3) | 168 (2) |
O5—H8W···O6i | 0.84 (3) | 1.90 (3) | 2.720 (2) | 162 (2) |
Symmetry codes: (i) x, −y+1/2, z−1/2; (ii) x, −y+1/2, z+1/2; (iii) x, y+1, z; (iv) −x, −y+1, −z; (v) x, −y+3/2, z−1/2. |
Experimental details
Crystal data | |
Chemical formula | [Mg(C4H7O2)2(H2O)3]·H2O |
Mr | 270.57 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 173 |
a, b, c (Å) | 13.808 (4), 10.704 (3), 9.183 (2) |
β (°) | 90.241 (4) |
V (Å3) | 1357.2 (6) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.16 |
Crystal size (mm) | 0.32 × 0.08 × 0.06 |
Data collection | |
Diffractometer | Bruker APEX2 CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.95, 0.99 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 10631, 2403, 1721 |
Rint | 0.077 |
(sin θ/λ)max (Å−1) | 0.596 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.042, 0.092, 1.03 |
No. of reflections | 2403 |
No. of parameters | 190 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.21, −0.26 |
Computer programs: APEX2 (Bruker, 2009), SAINT (Bruker, 2009), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), XSHELL (Bruker, 2007).
D—H···A | D—H | H···A | D···A | D—H···A |
O8—H1W···O1 | 0.85 (4) | 1.97 (4) | 2.777 (3) | 155 (3) |
O8—H2W···O5i | 0.89 (3) | 2.02 (3) | 2.845 (3) | 153 (3) |
O3—H3W···O2ii | 0.88 (3) | 1.79 (3) | 2.670 (2) | 178 (3) |
O3—H4W···O8iii | 0.85 (3) | 1.97 (3) | 2.807 (3) | 166 (3) |
O4—H5W···O3iv | 0.75 (2) | 2.16 (3) | 2.894 (3) | 166 (3) |
O4—H6W···O1ii | 0.97 (4) | 1.76 (3) | 2.713 (3) | 173 (3) |
O5—H7W···O8ii | 0.92 (3) | 1.96 (3) | 2.869 (3) | 168 (2) |
O5—H8W···O6v | 0.84 (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, z−1/2; (iv) x, −y+1/2, z+1/2; (v) x, −y+1/2, z−1/2. |
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