inorganic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

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ISSN: 2056-9890

Cerium(III) di­hydroxidohexa­oxido­tetra­borate chloride

aDepartment of Materials Science and Engineering, College of Materials, Xiamen University, Xiamen 361005, Fujian Province, People's Republic of China
*Correspondence e-mail: jxmi@xmu.edu.cn

(Received 6 December 2011; accepted 23 January 2012; online 31 January 2012)

The crystal structure of the title compound, Ce[B4O6(OH)2]Cl, is built from polyborate sheets parallel to the (001) plane. These sheets stack along the [001] direction and are linked by Ce atoms exhibiting an CeO8Cl2 coordination sphere. O—H⋯O and O—H⋯Cl hydrogen bonds additionally stabilize the structural set-up. The polyborate sheet is made up of zigzag borate chains running along the [[\overline{1}]10] direction. These zigzag chains are inter­connected by shared O-vertices, resulting in a two-dimensional layer with nine-membered rings. All B and O atoms (except for the terminal OH atoms) lie in the nearly planar sheets of polyborates, leading to their isotropic atomic displacement parameters being significantly smaller than usual. This may be attributed to the fact that the atomic displacement parameters correlate not only with their atomic masses but with their coordination environments also.

Related literature

For background to borate compounds and their applications, see: Burns et al. (1995[Burns, P. C., Grice, J. D. & Hawthorne, F. C. (1995). Can. Mineral. 33, 1131-1151.]); Chen et al. (1985[Chen, C. T., Wu, B. C., Jiang, A. D. & You, G. M. (1985). Sci. Sin. B, 15, 235-243.]); Zhao et al. (1990[Zhao, S. Q., Huang, C. E. & Zhang, H. W. (1990). J. Cryst. Growth, 99, 805-810.]); Sun, Sun et al. (2010[Sun, H. Y., Sun, W., Huang, Y. X. & Mi, J. X. (2010). Z. Anorg. Allg. Chem. 636, 977-981.]); Sun, Zhou et al. (2010[Sun, H. Y., Zhou, Y., Huang, Y. X., Sun, W. & Mi, J. X. (2010). Chin. J. Struct. Chem. 29, 1387-1393.]). For isotypic structures, see: Belokoneva et al. (2002[Belokoneva, E. L., Stefanovich, S. Yu., Dimitrova, O. V. & Ivanova, A. G. (2002). Zh. Neorg. Khim. 47, 370-377.]) for Ln[B4O6(OH)2]Cl (Ln = Pr, Nd).

Experimental

Crystal data
  • Ce[B4O6(OH)2]Cl

  • Mr = 348.83

  • Monoclinic, C c

  • a = 6.5169 (11) Å

  • b = 11.245 (2) Å

  • c = 9.7575 (17) Å

  • β = 105.284 (3)°

  • V = 689.8 (2) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 7.00 mm−1

  • T = 295 K

  • 0.16 × 0.07 × 0.03 mm

Data collection
  • Bruker SMART APEX CCD area-detector diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2001[Bruker (2001). SAINT, SMART and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.401, Tmax = 0.818

  • 2825 measured reflections

  • 1532 independent reflections

  • 1523 reflections with I > 2σ(I)

  • Rint = 0.022

Refinement
  • R[F2 > 2σ(F2)] = 0.020

  • wR(F2) = 0.051

  • S = 1.00

  • 1532 reflections

  • 134 parameters

  • 10 restraints

  • All H-atom parameters refined

  • Δρmax = 0.53 e Å−3

  • Δρmin = −1.64 e Å−3

  • Absolute structure: Flack (1983[Flack, H. D. (1983). Acta Cryst. A39, 876-881.]), 716 Friedel pairs

  • Flack parameter: 0.034 (19)

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A DA D—H⋯A
O8—H1⋯O1i 0.82 (2) 2.43 (7) 2.859 (5) 114 (6)
O8—H1⋯Cl1ii 0.82 (2) 2.52 (5) 3.219 (4) 145 (7)
O7—H2⋯O4ii 0.83 (2) 2.13 (6) 2.860 (6) 148 (10)
O7—H2⋯Cl1ii 0.83 (2) 2.81 (11) 3.220 (4) 112 (9)
Symmetry codes: (i) [x, -y+1, z+{\script{1\over 2}}]; (ii) [x+{\script{1\over 2}}, -y+{\script{3\over 2}}, z+{\script{1\over 2}}].

Data collection: SMART (Bruker, 2001[Bruker (2001). SAINT, SMART and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2001[Bruker (2001). SAINT, SMART and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: DIAMOND (Brandenburg, 2011[Brandenburg, K. (2011). DIAMOND. Crystal Impact GbR, Bonn, Germany.]) and ATOMS (Dowty, 2004[Dowty, E. (2004). ATOMS. Shape Software, Kingsport, Tennessee, USA.]); software used to prepare material for publication: SHELXL97.

Supporting information


Comment top

Borate compounds have been extensively studied due to their variety of fundamental building blocks and crystal structure types (Burns et al., 1995), as well as their successful industry applications as nonlinear optical materials, e.g. β-Ba(B2O4) (BBO) (Chen et al., 1985) and LiB3O5 (LBO) (Zhao et al., 1990). Besides alkali metals and alkaline-earth metals (Sun, Sun et al., 2010), rare-earth elements become highlighted with being introduced into the borate system in order to obtain multifunctional materials with the distinctive luminescence properties of rare-earth elements. Belokoneva et al. (2002) claimed that Ln(B4O6(OH)2)Cl (Ln = Pr, Nd) exhibits excellent nonlinear optical properties. But the atomic coordinates of its cerium analogue have not been reported until now. Herein, we report the crystal structure of Ce(B4O6(OH)2)Cl determined from single-crystal X-ray diffraction data, including the sites of hydrogen atoms.

The crystal structure of Ce(B4O6(OH)2)Cl is characterized as a layered strcuture of polyborate sheets parallel to (001)(Fig. 1 & 2). In the structure boron atoms have two types of polyhedral coordinations. One is 3-coordinated by oxygen atoms, forming a triangular planar [BO3] group. The other is 4-coordinated to three O-atoms and one hydroxyl group to form a [BO3(OH)] tetrahedron (Fig. 3). Both [BO3] group and [BO3(OH)] polyhedron link to three neighbouring borate groups via their common O-corners except for OH terminals. Two [BO3(OH)] tetrahedra and two triangular planar [BO3] groups compose a borate tetramer as a fundamental building block (FBB) (Fig. 2) (Burns et al., 1995). The FBBs share their common oxygen vertices to form a zigzag borate chain running along the [110] direction. The zigzag chains are further interconnected with each other by sharing their common O-corners, resulting in a two-dimensional layer with 9-membered rings within the layer. The 9-membered ring has a nearly equilateral (about 7.00 Å) triangular motif (Fig. 2). The Ce atoms just reside at the center of 9-membered rings and adopt a 10-coordination with the surrounding eight oxygen and two chlorine atoms, forming a 1-6-3 crown-shaped polyhedron (Fig. 2). The two-dimensional layers stack along the [001] direction and are linked by Ce and Cl atoms as well as hydrogen bonds to form the three-dimensional crystal structure (Fig. 1). It is interesting that all boron and oxygen atoms (except for OH terminals) lying in the nearly planar sheets of polyborates lead to their isotropic atomic parameters significantly smaller than as-expected usually. For example, the isotropic atomic parameters of boron atoms are distributed in the range of 0.0062 (10) to 0.0085 (10) Å2, significantly smaller than that of chlorine atom (0.0130 (2) Å2). This may give a hint that the atomic displacement parameters correlate not only with their atomic masses but with their coordination environments also. However the standard uncertainties of atomic displacement parameters do have close correlation with their atomic masses of individual elements. As-observed in the title compound, standard uncertainties of atomic displacement parameters of all atoms distribute as-expected in the sequence of Ce, Cl, O, B and H, increasing while their atomic masses decrease.

Related literature top

For background to borate compounds and their applications, see: Burns et al. (1995); Chen et al. (1985); Zhao et al. (1990); Sun, Sun et al. (2010); Sun, Zhou et al. (2010). For related structures, see: Belokoneva et al. (2002) for Ln(B4O6(OH)2)Cl (Ln = Pr, Nd).

Experimental top

The title compound, Ce(B4O6(OH)2)Cl was synthesized by using a hydrothermal method during our systematically exploiting rare earth borates (Sun, Zhou et al., 2010). Typically, a mixture of Ce2O3 (0.33 g), CrCl3.6H2O (0.80 g), H3BO3 (2.00 g) and 2 ml distilled water with molar ratio of Ce: Cl: B = 1: 9: 32 was prepared, and transferred into a Teflon-lined stainless-steel autoclave (30 ml in volume), then heated to and kept at 468 K for three days. Transparent, colorless crystals of the title compound were obtained by filtration, rinsed with distilled water several times, and dried in desiccators. Optical examination and powder X-ray diffraction (PXRD) analyses were used to identify the phases of the solid products.

Refinement top

The hydrogen positions were obtained from the difference Fourier map and refined via fixing the bond distance of d(OH) = 0.82 (2)Å with the donator of coordinated oxygen atoms. Moreover a common variable was set for the isotropic atomic displacement parameters of all hydrogen atoms during the refinement.

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2011) and ATOMS (Dowty, 2004); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. Crystal structure of Ce(B4O6(OH)2)Cl. ([BO4] drawn in red tetrahedra; [BO3] in blue triangular groups; Ce in black spheres; Cl in green spheres; H in small black balls).
[Figure 2] Fig. 2. Left: a two-dimensional sheet with 9-membered rings, the fundamental building block (FBB) marked by a dash-line ellipse; Right upper: a 9-membered ring with a nearly equilateral triangular motif; Right down: coordination environment of Ce in a 1-6-3 crown-shaped polyhedron.
[Figure 3] Fig. 3. Coordination environment of metal atoms, with displacement ellipsoids drawn at the 50% probability level (symmetry codes: (vi) x–1/2, y–1/2, z; (vii) x–1, y, z; (viii) x + 1/2, y–1/2, z)
Cerium(III) dihydroxidohexaoxidotetraborate chloride top
Crystal data top
Ce[B4O6(OH)2]ClF(000) = 644
Mr = 348.83Dx = 3.359 Mg m3
Monoclinic, CcMo Kα radiation, λ = 0.71073 Å
Hall symbol: C -2ycCell parameters from 2825 reflections
a = 6.5169 (11) Åθ = 3.6–28.0°
b = 11.245 (2) ŵ = 7.00 mm1
c = 9.7575 (17) ÅT = 295 K
β = 105.284 (3)°Prism, colorless
V = 689.8 (2) Å30.16 × 0.07 × 0.03 mm
Z = 4
Data collection top
Bruker SMART APEX CCD area-detector
diffractometer
1532 independent reflections
Radiation source: fine-focus sealed tube1523 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.022
1800 images,ϕ = 0, 90, 180°, χ = 54.74°, Δω=0.3°, Exp time: 15 s. scansθmax = 28.0°, θmin = 3.6°
Absorption correction: multi-scan
(SADABS; Bruker, 2001)
h = 88
Tmin = 0.401, Tmax = 0.818k = 1414
2825 measured reflectionsl = 1212
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.020All H-atom parameters refined
wR(F2) = 0.051 w = 1/[σ2(Fo2) + (0.0285P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.00(Δ/σ)max = 0.001
1532 reflectionsΔρmax = 0.53 e Å3
134 parametersΔρmin = 1.64 e Å3
10 restraintsAbsolute structure: Flack (1983), 716 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.034 (19)
Crystal data top
Ce[B4O6(OH)2]ClV = 689.8 (2) Å3
Mr = 348.83Z = 4
Monoclinic, CcMo Kα radiation
a = 6.5169 (11) ŵ = 7.00 mm1
b = 11.245 (2) ÅT = 295 K
c = 9.7575 (17) Å0.16 × 0.07 × 0.03 mm
β = 105.284 (3)°
Data collection top
Bruker SMART APEX CCD area-detector
diffractometer
1532 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2001)
1523 reflections with I > 2σ(I)
Tmin = 0.401, Tmax = 0.818Rint = 0.022
2825 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.020All H-atom parameters refined
wR(F2) = 0.051Δρmax = 0.53 e Å3
S = 1.00Δρmin = 1.64 e Å3
1532 reflectionsAbsolute structure: Flack (1983), 716 Friedel pairs
134 parametersAbsolute structure parameter: 0.034 (19)
10 restraints
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
Ce10.98063 (4)0.706775 (17)0.56430 (4)0.00585 (8)
Cl10.6202 (2)0.82445 (12)0.37031 (14)0.0130 (2)
B10.1685 (9)0.4466 (5)0.6439 (6)0.0073 (10)
B20.8287 (9)0.4064 (5)0.6939 (6)0.0085 (10)
B30.5112 (9)0.5338 (5)0.6256 (6)0.0068 (10)
B40.5809 (9)0.7447 (5)0.7169 (6)0.0062 (10)
O10.9639 (5)0.4852 (3)0.6324 (3)0.0076 (7)
O20.7362 (6)0.8358 (3)0.6858 (4)0.0086 (7)
O30.6294 (6)0.6361 (3)0.6426 (4)0.0093 (7)
O40.3652 (6)0.7819 (3)0.6635 (4)0.0068 (7)
O50.2933 (6)0.5383 (3)0.6124 (4)0.0087 (7)
O60.6027 (6)0.4259 (3)0.6207 (4)0.0086 (7)
O70.6335 (7)0.7247 (3)0.8706 (4)0.0116 (7)
O80.8688 (6)0.4269 (3)0.8477 (4)0.0101 (7)
H10.894 (13)0.495 (3)0.876 (7)0.04 (2)*
H20.731 (13)0.706 (6)0.940 (7)0.04 (2)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ce10.00577 (12)0.00558 (12)0.00601 (12)0.00003 (13)0.00121 (8)0.00002 (14)
Cl10.0132 (6)0.0155 (6)0.0094 (6)0.0047 (5)0.0012 (5)0.0001 (5)
B10.004 (2)0.009 (2)0.009 (3)0.0008 (19)0.001 (2)0.002 (2)
B20.009 (3)0.006 (2)0.009 (3)0.001 (2)0.002 (2)0.001 (2)
B30.011 (3)0.005 (2)0.005 (2)0.001 (2)0.0029 (19)0.0021 (19)
B40.009 (3)0.003 (2)0.006 (2)0.003 (2)0.002 (2)0.0001 (19)
O10.0040 (16)0.0072 (16)0.0124 (17)0.0020 (13)0.0036 (14)0.0006 (13)
O20.0079 (18)0.0045 (16)0.0131 (19)0.0007 (14)0.0025 (14)0.0005 (14)
O30.0083 (18)0.0063 (15)0.0145 (18)0.0011 (14)0.0055 (14)0.0014 (14)
O40.0061 (17)0.0036 (16)0.0105 (19)0.0009 (12)0.0015 (14)0.0010 (12)
O50.0046 (16)0.0042 (15)0.0180 (18)0.0009 (13)0.0041 (14)0.0023 (14)
O60.0027 (15)0.0077 (14)0.0138 (17)0.0020 (13)0.0004 (13)0.0019 (13)
O70.0091 (19)0.0155 (17)0.0097 (19)0.0059 (15)0.0017 (15)0.0023 (15)
O80.0161 (18)0.0084 (17)0.0048 (17)0.0029 (14)0.0007 (14)0.0010 (13)
Geometric parameters (Å, º) top
Ce1—O7i2.480 (4)B1—O51.396 (6)
Ce1—O8ii2.539 (4)B2—O4viii1.464 (6)
Ce1—O4iii2.579 (4)B2—O81.472 (6)
Ce1—O12.589 (3)B2—O61.474 (6)
Ce1—O6iv2.603 (3)B2—O11.483 (7)
Ce1—O22.654 (4)B3—O61.359 (6)
Ce1—O32.716 (4)B3—O31.370 (6)
Ce1—O5iii2.731 (3)B3—O51.392 (7)
Ce1—Cl1v2.9041 (14)B4—O41.427 (6)
Ce1—Cl12.9168 (14)B4—O71.465 (6)
B1—O2vi1.349 (6)B4—O31.496 (6)
B1—O1vii1.378 (6)B4—O21.526 (7)
O7i—Ce1—O8ii68.55 (12)O8ii—Ce1—Cl173.91 (9)
O7i—Ce1—O4iii68.81 (13)O4iii—Ce1—Cl1129.17 (8)
O8ii—Ce1—O4iii122.93 (12)O1—Ce1—Cl1121.47 (8)
O7i—Ce1—O1123.18 (11)O6iv—Ce1—Cl181.76 (8)
O8ii—Ce1—O167.76 (11)O2—Ce1—Cl164.30 (8)
O4iii—Ce1—O1108.75 (10)O3—Ce1—Cl173.81 (8)
O7i—Ce1—O6iv72.87 (12)O5iii—Ce1—Cl1149.66 (8)
O8ii—Ce1—O6iv137.83 (11)Cl1v—Ce1—Cl1134.62 (5)
O4iii—Ce1—O6iv53.00 (10)Ce1ix—Cl1—Ce1126.35 (5)
O1—Ce1—O6iv152.63 (11)O2vi—B1—O1vii123.2 (5)
O7i—Ce1—O2125.41 (12)O2vi—B1—O5125.8 (5)
O8ii—Ce1—O2128.40 (12)O1vii—B1—O5110.9 (4)
O4iii—Ce1—O2106.95 (11)O4viii—B2—O8111.2 (4)
O1—Ce1—O2109.92 (11)O4viii—B2—O6103.8 (4)
O6iv—Ce1—O264.77 (11)O8—B2—O6110.9 (4)
O7i—Ce1—O3147.45 (13)O4viii—B2—O1110.1 (4)
O8ii—Ce1—O389.01 (12)O8—B2—O1110.8 (4)
O4iii—Ce1—O3142.92 (12)O6—B2—O1109.9 (4)
O1—Ce1—O363.28 (10)O6—B3—O3121.1 (5)
O6iv—Ce1—O3116.78 (11)O6—B3—O5118.4 (5)
O2—Ce1—O352.04 (11)O3—B3—O5120.6 (4)
O7i—Ce1—O5iii85.14 (13)O4—B4—O7111.1 (4)
O8ii—Ce1—O5iii76.69 (11)O4—B4—O3112.1 (4)
O4iii—Ce1—O5iii63.61 (10)O7—B4—O3110.4 (4)
O1—Ce1—O5iii50.80 (10)O4—B4—O2111.9 (4)
O6iv—Ce1—O5iii116.61 (11)O7—B4—O2108.6 (4)
O2—Ce1—O5iii144.19 (12)O3—B4—O2102.5 (4)
O3—Ce1—O5iii113.23 (11)B1iii—O1—B2116.4 (4)
O7i—Ce1—Cl1v137.84 (10)B1iv—O2—B4119.9 (4)
O8ii—Ce1—Cl1v136.70 (9)B3—O3—B4124.1 (4)
O4iii—Ce1—Cl1v69.13 (9)B4—O4—B2x113.8 (4)
O1—Ce1—Cl1v69.06 (8)B3—O5—B1126.3 (4)
O6iv—Ce1—Cl1v84.35 (8)B3—O6—B2120.5 (4)
O2—Ce1—Cl1v70.67 (8)B4—O7—H2143 (8)
O3—Ce1—Cl1v74.57 (8)Ce1xi—O7—H280 (8)
O5iii—Ce1—Cl1v73.87 (8)B2—O8—H1117 (5)
O7i—Ce1—Cl177.35 (10)Ce1xii—O8—H1107 (5)
Symmetry codes: (i) x+1/2, y+3/2, z1/2; (ii) x, y+1, z1/2; (iii) x+1, y, z; (iv) x+1/2, y+1/2, z; (v) x+1/2, y+3/2, z+1/2; (vi) x1/2, y1/2, z; (vii) x1, y, z; (viii) x+1/2, y1/2, z; (ix) x1/2, y+3/2, z1/2; (x) x1/2, y+1/2, z; (xi) x1/2, y+3/2, z+1/2; (xii) x, y+1, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O8—H1···O1xii0.82 (2)2.43 (7)2.859 (5)114 (6)
O8—H1···Cl1v0.82 (2)2.52 (5)3.219 (4)145 (7)
O7—H2···O4v0.83 (2)2.13 (6)2.860 (6)148 (10)
O7—H2···Cl1v0.83 (2)2.81 (11)3.220 (4)112 (9)
Symmetry codes: (v) x+1/2, y+3/2, z+1/2; (xii) x, y+1, z+1/2.

Experimental details

Crystal data
Chemical formulaCe[B4O6(OH)2]Cl
Mr348.83
Crystal system, space groupMonoclinic, Cc
Temperature (K)295
a, b, c (Å)6.5169 (11), 11.245 (2), 9.7575 (17)
β (°) 105.284 (3)
V3)689.8 (2)
Z4
Radiation typeMo Kα
µ (mm1)7.00
Crystal size (mm)0.16 × 0.07 × 0.03
Data collection
DiffractometerBruker SMART APEX CCD area-detector
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2001)
Tmin, Tmax0.401, 0.818
No. of measured, independent and
observed [I > 2σ(I)] reflections
2825, 1532, 1523
Rint0.022
(sin θ/λ)max1)0.661
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.020, 0.051, 1.00
No. of reflections1532
No. of parameters134
No. of restraints10
H-atom treatmentAll H-atom parameters refined
Δρmax, Δρmin (e Å3)0.53, 1.64
Absolute structureFlack (1983), 716 Friedel pairs
Absolute structure parameter0.034 (19)

Computer programs: SMART (Bruker, 2001), SAINT (Bruker, 2001), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 2011) and ATOMS (Dowty, 2004).

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O8—H1···O1i0.82 (2)2.43 (7)2.859 (5)114 (6)
O8—H1···Cl1ii0.82 (2)2.52 (5)3.219 (4)145 (7)
O7—H2···O4ii0.83 (2)2.13 (6)2.860 (6)148 (10)
O7—H2···Cl1ii0.83 (2)2.81 (11)3.220 (4)112 (9)
Symmetry codes: (i) x, y+1, z+1/2; (ii) x+1/2, y+3/2, z+1/2.
 

Acknowledgements

This work was supported by the National Natural Science Foundation of China (grant No. 40972035), the Natural Science Foundation of Fujian Province of China (grant No. 2010 J01308) and the Scientific and Technological Innovation Platform of Fujian Province (grant No. 2009 J1009).

References

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