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

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 68| Part 5| May 2012| Pages i33-i34
doi:10.1107/S1600536812016169

Redetermination of Ce[B5O8(OH)(H2O)]NO3·2H2O

Wei Sun,a Teng-Teng Zhu,a Biao-Chun Zhao,a Ya-Xi Huanga and Jin-Xiao Mia*‡

aFujian Provincial Key Laboratory of Advanced Materials, Department 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 25 March 2012; accepted 13 April 2012; online 21 April 2012)

The crystal structure of Ce[B5O8(OH)(H2O)]NO3·2H2O, cerium(III) aqua­hydroxidoocta­oxidopenta­borate nitrate dihydrate, has been redetermined from single-crystal X-ray diffraction data. In contrast to the previous determination [Li et al. (2003[Li, L. Y., Jin, X. L., Li, G. B., Wang, Y. X., Liao, F. H., Yao, G. Q. & Lin, J. H. (2003). Chem. Mater. 15, 2253-2260.]). Chem. Mater. 15, 2253–2260], the present study reveals the location of all H atoms, slightly different fundamental building blocks (FBBs) of the polyborate anions, more reasonable displacement ellipsoids for all non-H atoms, as well as a model without disorder of the nitrate anion. The crystal structure is built from corrugated polyborate layers parallel to (010). These layers, consisting of [B5O8(OH)(H2O)]2− anions as FBBs, stack along [010] and are linked by Ce3+ ions, which exhibit a distorted CeO10 coordination sphere. The layers are additionally stabilized via O—H⋯O hydrogen bonds between water mol­ecules and nitrate anions, located at the inter­layer space. The [BO3(H2O)]-group shows a [3 + 1] coordination and is considerably distorted from a tetra­hedral configuration. Bond-valence-sum calculation shows that the valence sum of boron is only 2.63 valence units (v.u.) when the contribution of the water mol­ecule (0.49 v.u.) is neglected.

Related literature

For a previous structural study of the title compound, see: Li et al. (2003[Li, L. Y., Jin, X. L., Li, G. B., Wang, Y. X., Liao, F. H., Yao, G. Q. & Lin, J. H. (2003). Chem. Mater. 15, 2253-2260.]). For the La analogue, see: Li et al. (2005[Li, L. Y., Li, G. B., Liao, F. H. & Lin, J. H. (2005). Acta Phys-Chim. Sin. 21, 769-773.]). For the bond-valence method, see: Brown (2002[Brown, I. D. (2002). The Chemical Bond in Inorganic Chemistry: The Bond Valence Model. Oxford University Press.]). For related structures, see: Sun et al. (2010[Sun, H.-Y., Zhou, Y., Huang, Y.-X., Sun, W. & Mi, J.-X. (2010). Chin. J. Struct. Chem. 29, 1387-1393.], 2012[Sun, W., Zhao, B.-C., Huang, Y.-X. & Mi, J.-X. (2012). Acta Cryst. E68, i17.]). For a review on geometrical parameters of borate groups, see: Zobetz (1982[Zobetz, E. (1982). Z. Kristallogr. 160, 81-92.], 1990[Zobetz, E. (1990). Z. Kristallogr. 191, 45-57.]). FBBs in borate crystal chemistry were reviewed by Burns et al. (1995[Burns, P. C., Grice, J. D. & Hawthorne, F. C. (1995). Can. Mineral. 33, 1131-1151.]).

Experimental

Crystal data

  • Ce[B5O8(OH)(H2O)]NO3·2H2O

  • Mr = 455.24

  • Monoclinic, P 21 /n

  • a = 6.4438 (12) Å

  • b = 15.572 (3) Å

  • c = 10.745 (2) Å

  • β = 90.395 (3)°

  • V = 1078.2 (3) Å3

  • Z = 4

  • Mo Kα radiation

  • μ = 4.32 mm−1

  • T = 173 K

  • 0.30 × 0.12 × 0.04 mm
Data collection

  • Bruker SMART CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2001[Bruker (2001). SAINT, SMART and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.357, Tmax = 0.846

  • 6327 measured reflections

  • 2484 independent reflections

  • 2390 reflections with I > 2σ(I)

  • Rint = 0.021
Refinement

  • R[F2 > 2σ(F2)] = 0.026

  • wR(F2) = 0.061

  • S = 1.12

  • 2484 reflections

  • 221 parameters

  • 4 restraints

  • All H-atom parameters refined

  • Δρmax = 1.40 e Å−3

  • Δρmin = −0.50 e Å−3

Table 1
Selected geometric parameters (Å, °)

B5—O9 1.406 (5)
B5—O5i 1.412 (5)
B5—O8 1.444 (4)
B5—O10 1.637 (5)
O9—B5—O5i 109.8 (3)
O9—B5—O8 114.3 (3)
O5i—B5—O8 116.2 (3)
O9—B5—O10 107.1 (3)
O5i—B5—O10 107.3 (3)
O8—B5—O10 101.1 (3)
Symmetry code: (i) x+1, y, z.

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A D—H H⋯A D⋯A D—H⋯A
O1—H1⋯O3ii 0.88 (6) 1.75 (6) 2.622 (3) 173 (6)
O10—H2⋯O13i 0.85 (2) 1.89 (3) 2.705 (4) 160 (6)
O10—H3⋯O12 0.85 (2) 1.85 (2) 2.700 (4) 173 (6)
O15—H4⋯O4 0.84 (7) 2.21 (7) 2.967 (4) 150 (6)
O15—H4⋯O10iii 0.84 (7) 2.50 (6) 3.041 (4) 123 (6)
O15—H5⋯O13iv 0.84 (7) 2.10 (7) 2.912 (4) 164 (6)
O15—H5⋯O12iv 0.84 (7) 2.48 (7) 3.093 (4) 131 (5)
O14—H6⋯O2iv 0.81 (2) 2.01 (3) 2.756 (4) 153 (6)
Symmetry codes: (i) x+1, y, z; (ii) -x+1, -y+1, -z+1; (iii) [x-{\script{1\over 2}}, -y+{\script{1\over 2}}, z+{\script{1\over 2}}]; (iv) [-x+{\script{1\over 2}}, y-{\script{1\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

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536812016169/wm2613sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536812016169/wm2613Isup2.hkl

checkCIF report


Comment top

Borate compounds have been extensively studied due to their diverse structural chemistry and successful industry applications. The title compound, Ce[B5O8(OH)(H2O)][NO3].2H2O, has already been prepared and reported by Li et al. (2003) with a structure model that describes disordered oxygen positions of the nitrate anion, and where the hydrogen positions could not be determined even in the ordered model of the La analogue (Li et al., 2005). Herein we report the redetermined crystal structure based on single-crystal X-ray diffraction data of Ce[B5O8(OH)(H2O)][NO3].2H2O with the location of all H atoms, slightly different fundamental building blocks (FBBs) of the polyborate anions, more reasonable displacement ellipsoids for all non-hydrogen atoms as well as a model without disorder of the nitrate anion.

The crystal structure of Ce[B5O8(OH)(H2O)][NO3].2H2O is built from corrugated polyborate layers parallel to (010) which stack along the [010] direction (Figs 1, 2). The polyborate layer is made up of zigzag borate branched chains running along the [100] direction, and consists of B5O8(OH)(H2O) as fundamental building blocks (FBBs) (Burns et al., 1995). Each FBB consists of two [BO4] tetrahedra, one [BO3(H2O)] tetrahedron, one [BO3] triangle, and a planar trigonal [BO2(OH)] group. The borate groups of the FBB, except for the [BO2(OH)] group, form the backbone of the single infinite chain, one side of which is decorated by flanking trigonal planar [B1O2(OH)] groups. These zigzag infinite chains are, via symmetry operations (i.e. with each rotated by 180° with respect to the adjacent chains), alternately arranged with the flanking [BO2(OH)] groups up and down, respectively, and fused via common O-vertices, resulting in a two-dimensional corrugated layer with 9-membered rings within the layer. The 9-membered ring has a nearly equilateral triangular motif with edge lengths of about 7.0 Å (Fig. 2) as that in [Ce(B4O6(OH)2)Cl] (Sun et al., 2012). The Ce3+ ion resides at the center of the 9-membered rings and adopt a distorted 10-coordination to the surrounding oxygen atoms to form a 1–6–3 crown-shaped polyhedron (Figs. 1, 3), six of them coming from the nearly planar 9-membered ring in the middle, one from a triangular [NO3] anion on the top, one from an OH group (originating from a triangular [BO2(OH)] group from the next layer) and two from water molecules at the botton. The water molecules and the nitrate [NO3] groups, located at the interlayer space, additionally stabilize the structural set-up of the title nitrate borate compound, via their O–H···O hydrogen bonds (Table 2). In the present model, H-atom H7 (attached to O14) has no acceptor atom, and none of alternative approximate positions found in difference Fourier maps for H7 were reliable because they were too close to the Ce3+ ion. All hydrogen atoms except for H7 point to the backbone of the polyborate layers, whereas H-atom H7 points to the [100] direction (i.e. O14–H7 parallel to the polyborate layers).

In contrast to the previous report (Li et al., 2003), one of the 3-coordinated boron atoms with B–O distances less than 1.38 Å (denoted as B5 in this paper) was altered to be '3 + 1' coordinated to three surrounding O-atoms and a water molecule forming a highly distorted tetrahedral [BO3(H2O)]-group in the present description. The highly distorted tetrahedral [BO3(H2O)] group has quite a long B—O bond distance (d(B–OH2) = 1.637 (5) Å) and three normal distances (d(B–O) = 1.406 (5) to 1.444 (5) Å; Table 1), as observed in its La counterpart (Li et al., 2005) and previous reviews on the crystal chemistry of borates (Zobetz, 1982, 1990). This may be attributed to the fact that the water molecule strongly attracts the boron atom to offset from the trigonal plane. Additionally, bond valence sum calculations (Brown, 2002) also support this assumption because the valence sum of boron is only 2.63 v.u. if not considering the contribution of water molecule (0.49 v.u.).

Related literature top

For a previous structural study of the title compound, see: Li et al. (2003). For the La analogue, see: Li et al. (2005). For the bond-valence method, see: Brown (2002). For related structures, see: Sun et al. (2010, 2012). For a review on geometrical parameters of borate groups, see: Zobetz (1982, 1990). FBBs in borate crystal chemistry were reviewed by Burns et al. (1995).

Experimental top

During our systematically investigation on rare earth borates (Sun et al., 2010; Sun et al., 2012), the title compound, Ce[B5O8(OH)(H2O)][NO3].2H2O, was synthesized by using molten boric acid as flux which has been firstly described by Li et al. (2003). Typically, a mixture of Ce(NO3)3.6H2O (1.00 g) and H3BO3 (3.00 g) with molar ratio of Ce:B = 1:21 was prepared by thoroughly homogeneous grinding and transferred into a Teflon-lined stainless-steel autoclave (30 ml in volume), then heated to and kept at 513 K for three days. Transparent, colorless crystals of the title compound were obtained by filtration, rinsed with deionized water for several times, and dried in a desiccators. The phases of the as-prepared solid products were identified by powder X-ray diffraction (PXRD) analyses. Optical microscopy was used to check the selected crystals proper for single-crystal X-ray diffraction while their chemical compositions were examined by use of an Energy Dispersive X-ray Spectrometer (EDX) (Oxford Instruments). Scanning electron microscopy (SEM) was used to document the crystal morphologies.

Refinement top

Initially, all hydrogen positions were located from difference Fourier maps and refined freely. Then a common variable was used for the isotropic atomic displacement parameters (Uiso) of all hydrogen atoms while their atomic coordinates were refined. After refinement the O–H bond lengths of 2 water molecules (i.e. H3–O10–H2 and H7–O14–H6) became improper, soft restraints on Uiso and on bond lengths (d(O–H) = 0.82 (2) Å) were applied.

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. The crystal structure of Ce[B5O8(OH)(H2O)][NO3].2H2O projected onto (100). [BO4] groups are drawn as red tetrahedra; [BO3] as blue triangular groups; [NO3] as green triangular groups; Ce as black spheres; O as red spheres; H as small black spheres). The inset on the right represents the coordination environment of the Ce atom in a 1–6–3 crown-shaped polyhedron.
[Figure 2] Fig. 2. The Crystal structure of Ce[B5O8(OH)(H2O)][NO3].2H2O projected onto (010). Top right: the fundamental building block (FBB) of [B5O8(OH)(H2O)]; Bottom right: the 9-membered ring with a nearly equilateral triangular motif.
[Figure 3] Fig. 3. Coordination environment of the cerium atom with displacement ellipsoids drawn at the 50% probability level. [Symmetry codes: (i) x–1, y, z; (ii) –x + 1/2, y–1/2, –z + 1/2; (iii) x–1/2, –y + 1/2, z–1/2; (iv) x + 1/2, –y + 1/2, z–1/2; (v) x–1/2, –y + 1/2, z + 1/2; (vi) x + 1, y, z.]
cerium aquahydroxidooctaoxidopentaborate nitrate dihydrate top
Crystal data top
Ce[B5O8(OH)(H2O)]NO3·2H2OF(000) = 868
Mr = 455.24Dx = 2.805 Mg m−3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 6327 reflections
a = 6.4438 (12) Åθ = 2.3–28.2°
b = 15.572 (3) ŵ = 4.32 mm−1
c = 10.745 (2) ÅT = 173 K
β = 90.395 (3)°Prism, colorless
V = 1078.2 (3) Å30.30 × 0.12 × 0.04 mm
Z = 4
Data collection top
Bruker SMART CCD
diffractometer		2484 independent reflections
Radiation source: fine-focus sealed tube2390 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.021
1800 images,ϕ=0, 90, 180 degree, and Δω=0.3 degree, χ= 54.74 degree scansθmax = 28.2°, θmin = 2.3°
Absorption correction: multi-scan
(SADABS; Bruker, 2001)		h = −8→6
Tmin = 0.357, Tmax = 0.846k = −20→20
6327 measured reflectionsl = −13→14
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)] = 0.026Hydrogen site location: difference Fourier map
wR(F2) = 0.061All H-atom parameters refined
S = 1.12 w = 1/[σ2(Fo2) + (0.0269P)2 + 2.2495P]
where P = (Fo2 + 2Fc2)/3
2484 reflections(Δ/σ)max < 0.001
221 parametersΔρmax = 1.40 e Å−3
4 restraintsΔρmin = −0.50 e Å−3
Crystal data top
Ce[B5O8(OH)(H2O)]NO3·2H2OV = 1078.2 (3) Å3
Mr = 455.24Z = 4
Monoclinic, P21/nMo Kα radiation
a = 6.4438 (12) ŵ = 4.32 mm−1
b = 15.572 (3) ÅT = 173 K
c = 10.745 (2) Å0.30 × 0.12 × 0.04 mm
β = 90.395 (3)°
Data collection top
Bruker SMART CCD
diffractometer		2484 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2001)		2390 reflections with I > 2σ(I)
Tmin = 0.357, Tmax = 0.846Rint = 0.021
6327 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0264 restraints
wR(F2) = 0.061All H-atom parameters refined
S = 1.12Δρmax = 1.40 e Å−3
2484 reflectionsΔρmin = −0.50 e Å−3
221 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
Ce10.35178 (3)0.201751 (12)0.139251 (16)0.00786 (7)
B10.2409 (6)0.4622 (3)0.4100 (3)0.0094 (7)
B20.0226 (6)0.3373 (2)0.3613 (3)0.0083 (7)
B30.3600 (6)0.3163 (2)0.4625 (3)0.0081 (7)
B40.6568 (6)0.2918 (2)0.3206 (4)0.0088 (7)
B50.9081 (6)0.2807 (3)0.1513 (4)0.0125 (7)
N10.3614 (5)0.4247 (2)0.0851 (3)0.0166 (6)
O10.2738 (4)0.54996 (15)0.4121 (2)0.0116 (5)
O20.0638 (4)0.43136 (15)0.3587 (2)0.0095 (5)
O30.3906 (3)0.41051 (15)0.4608 (2)0.0096 (5)
O40.1407 (4)0.29595 (14)0.4617 (2)0.0074 (5)
O50.0654 (4)0.29975 (15)0.2391 (2)0.0088 (5)
O60.4540 (4)0.27987 (15)0.3470 (2)0.0094 (5)
O70.8026 (3)0.32384 (15)0.3991 (2)0.0086 (4)
O80.7032 (4)0.26620 (16)0.2007 (2)0.0106 (5)
O90.9770 (4)0.21643 (15)0.0695 (2)0.0088 (5)
O100.8694 (4)0.36739 (18)0.0682 (3)0.0182 (6)
O110.3550 (4)0.35075 (17)0.0378 (2)0.0180 (5)
O120.5235 (4)0.4534 (2)0.1344 (3)0.0285 (7)
O130.2040 (4)0.47208 (17)0.0797 (3)0.0226 (6)
O140.6030 (4)0.08603 (18)0.2165 (3)0.0195 (6)
O150.1547 (5)0.13445 (19)0.3154 (3)0.0190 (6)
H10.388 (9)0.559 (4)0.455 (5)0.056 (7)*
H20.967 (7)0.402 (3)0.054 (5)0.056 (7)*
H30.767 (6)0.398 (3)0.090 (5)0.056 (7)*
H40.160 (9)0.167 (5)0.378 (6)0.056 (7)*
H50.189 (9)0.084 (4)0.331 (6)0.056 (7)*
H60.582 (9)0.0349 (15)0.211 (6)0.056 (7)*
H70.729 (3)0.088 (4)0.223 (6)0.056 (7)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ce10.00734 (11)0.00863 (11)0.00758 (11)−0.00024 (6)−0.00198 (7)−0.00037 (6)
B10.0099 (17)0.0114 (18)0.0070 (16)−0.0001 (14)0.0018 (13)−0.0007 (13)
B20.0058 (16)0.0100 (18)0.0090 (16)−0.0002 (13)−0.0010 (13)−0.0007 (13)
B30.0069 (17)0.0116 (18)0.0057 (16)0.0008 (13)−0.0009 (13)0.0009 (13)
B40.0102 (18)0.0058 (17)0.0105 (17)0.0010 (13)−0.0005 (13)0.0031 (13)
B50.0089 (18)0.0160 (19)0.0125 (18)−0.0001 (15)0.0008 (14)−0.0024 (15)
N10.0140 (15)0.0147 (16)0.0213 (16)0.0002 (12)0.0054 (12)0.0013 (12)
O10.0118 (12)0.0092 (12)0.0138 (12)0.0005 (9)−0.0059 (9)−0.0001 (9)
O20.0092 (11)0.0083 (12)0.0111 (11)−0.0004 (9)−0.0030 (9)0.0009 (9)
O30.0079 (11)0.0079 (12)0.0128 (11)−0.0003 (9)−0.0029 (9)0.0005 (9)
O40.0068 (11)0.0094 (12)0.0061 (10)−0.0006 (8)−0.0021 (8)0.0008 (8)
O50.0054 (11)0.0121 (12)0.0089 (11)0.0002 (8)−0.0005 (9)−0.0012 (8)
O60.0079 (11)0.0143 (12)0.0058 (10)−0.0018 (9)−0.0024 (9)−0.0018 (9)
O70.0065 (11)0.0118 (12)0.0074 (10)−0.0010 (9)−0.0011 (8)−0.0011 (9)
O80.0088 (11)0.0156 (13)0.0074 (11)−0.0018 (9)−0.0022 (9)−0.0028 (9)
O90.0075 (11)0.0108 (12)0.0081 (11)0.0011 (9)−0.0020 (9)−0.0005 (9)
O100.0170 (14)0.0185 (14)0.0192 (13)0.0014 (10)−0.0022 (11)0.0025 (11)
O110.0237 (14)0.0128 (13)0.0176 (12)0.0006 (10)0.0057 (11)−0.0008 (10)
O120.0180 (15)0.0232 (16)0.0441 (19)0.0012 (12)−0.0086 (13)−0.0089 (13)
O130.0182 (14)0.0142 (14)0.0354 (16)0.0035 (11)0.0036 (12)0.0019 (12)
O140.0150 (13)0.0127 (13)0.0307 (15)0.0004 (10)−0.0074 (11)−0.0003 (11)
O150.0287 (16)0.0122 (13)0.0160 (13)−0.0008 (11)0.0068 (11)−0.0002 (11)
Geometric parameters (Å, º) top
Ce1—O152.515 (3)B3—O31.481 (4)
Ce1—O9i2.534 (2)B3—O61.496 (4)
Ce1—O142.557 (3)B4—O61.352 (4)
Ce1—O1ii2.558 (2)B4—O71.353 (4)
Ce1—O82.559 (2)B4—O81.383 (4)
Ce1—O112.564 (3)B5—O91.406 (5)
Ce1—O62.622 (2)B5—O5vi1.412 (5)
Ce1—O7iii2.628 (2)B5—O81.444 (4)
Ce1—O52.629 (2)B5—O101.637 (5)
Ce1—O4iv2.675 (2)N1—O121.250 (4)
B1—O21.352 (4)N1—O131.255 (4)
B1—O31.367 (4)N1—O111.260 (4)
B1—O11.383 (5)O1—H10.88 (6)
B2—O41.465 (4)O10—H20.85 (2)
B2—O51.466 (4)O10—H30.85 (2)
B2—O21.489 (4)O15—H40.84 (7)
B2—O7i1.492 (4)O15—H50.84 (7)
B3—O41.448 (4)O14—H60.81 (2)
B3—O9v1.462 (4)O14—H70.81 (2)
O15—Ce1—O9i77.00 (9)O2—B1—O1119.1 (3)
O15—Ce1—O1477.52 (10)O3—B1—O1117.9 (3)
O9i—Ce1—O14139.43 (8)O4—B2—O5112.6 (3)
O15—Ce1—O1ii67.46 (9)O4—B2—O2110.8 (3)
O9i—Ce1—O1ii73.74 (8)O5—B2—O2109.9 (3)
O14—Ce1—O1ii67.52 (8)O4—B2—O7i103.2 (3)
O15—Ce1—O8114.82 (9)O5—B2—O7i111.9 (3)
O9i—Ce1—O8151.72 (7)O2—B2—O7i108.3 (3)
O14—Ce1—O868.62 (8)O4—B3—O9v115.2 (3)
O1ii—Ce1—O8134.13 (8)O4—B3—O3110.3 (3)
O15—Ce1—O11134.64 (9)O9v—B3—O3106.7 (3)
O9i—Ce1—O1178.63 (8)O4—B3—O6108.2 (3)
O14—Ce1—O11140.26 (9)O9v—B3—O6108.1 (3)
O1ii—Ce1—O11138.42 (8)O3—B3—O6108.1 (3)
O8—Ce1—O1175.24 (8)O6—B4—O7126.0 (3)
O15—Ce1—O671.22 (9)O6—B4—O8111.8 (3)
O9i—Ce1—O6116.31 (7)O7—B4—O8122.2 (3)
O14—Ce1—O684.02 (8)O9—B5—O5vi109.8 (3)
O1ii—Ce1—O6133.62 (7)O9—B5—O8114.3 (3)
O8—Ce1—O651.82 (7)O5vi—B5—O8116.2 (3)
O11—Ce1—O686.53 (8)O9—B5—O10107.1 (3)
O15—Ce1—O7iii128.13 (9)O5vi—B5—O10107.3 (3)
O9i—Ce1—O7iii67.35 (7)O8—B5—O10101.1 (3)
O14—Ce1—O7iii106.49 (8)O12—N1—O13118.8 (3)
O1ii—Ce1—O7iii67.17 (7)O12—N1—O11121.5 (3)
O8—Ce1—O7iii114.42 (7)O13—N1—O11119.6 (3)
O11—Ce1—O7iii73.79 (8)Ce1vii—O1—H1103 (4)
O6—Ce1—O7iii159.08 (8)B1—O1—H1107 (4)
O15—Ce1—O564.87 (9)B1—O2—B2119.4 (3)
O9i—Ce1—O553.01 (7)B1—O3—B3119.6 (3)
O14—Ce1—O5136.14 (8)B3—O4—B2114.2 (3)
O1ii—Ce1—O5113.74 (8)B5i—O5—B2122.9 (3)
O8—Ce1—O5106.81 (7)B4—O6—B3121.3 (3)
O11—Ce1—O569.88 (8)B4—O7—B2vi122.6 (3)
O6—Ce1—O563.65 (7)B4—O8—B5120.1 (3)
O7iii—Ce1—O5114.11 (7)B5—O9—B3iv125.2 (3)
O15—Ce1—O4iv154.12 (8)B5—O10—H2121 (4)
O9i—Ce1—O4iv117.02 (7)B5—O10—H3115 (4)
O14—Ce1—O4iv78.40 (8)H2—O10—H3106 (6)
O1ii—Ce1—O4iv94.54 (7)N1—O11—Ce1131.0 (2)
O8—Ce1—O4iv63.89 (7)Ce1—O14—H6124 (4)
O11—Ce1—O4iv71.15 (7)Ce1—O14—H7129 (5)
O6—Ce1—O4iv115.40 (7)H6—O14—H7102 (6)
O7iii—Ce1—O4iv51.80 (7)Ce1—O15—H4110 (4)
O5—Ce1—O4iv141.00 (7)Ce1—O15—H5114 (4)
O2—B1—O3123.0 (3)H4—O15—H5113 (6)
Symmetry codes: (i) x−1, y, z; (ii) −x+1/2, y−1/2, −z+1/2; (iii) x−1/2, −y+1/2, z−1/2; (iv) x+1/2, −y+1/2, z−1/2; (v) x−1/2, −y+1/2, z+1/2; (vi) x+1, y, z; (vii) −x+1/2, y+1/2, −z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1···O3viii0.88 (6)1.75 (6)2.622 (3)173 (6)
O10—H2···O13vi0.85 (2)1.89 (3)2.705 (4)160 (6)
O10—H3···O120.85 (2)1.85 (2)2.700 (4)173 (6)
O15—H4···O40.84 (7)2.21 (7)2.967 (4)150 (6)
O15—H4···O10v0.84 (7)2.50 (6)3.041 (4)123 (6)
O15—H5···O13ii0.84 (7)2.10 (7)2.912 (4)164 (6)
O15—H5···O12ii0.84 (7)2.48 (7)3.093 (4)131 (5)
O14—H6···O2ii0.81 (2)2.01 (3)2.756 (4)153 (6)
Symmetry codes: (ii) −x+1/2, y−1/2, −z+1/2; (v) x−1/2, −y+1/2, z+1/2; (vi) x+1, y, z; (viii) −x+1, −y+1, −z+1.

Experimental details

Crystal data
Chemical formulaCe[B5O8(OH)(H2O)]NO3·2H2O
Mr455.24
Crystal system, space groupMonoclinic, P21/n
Temperature (K)173
a, b, c (Å)6.4438 (12), 15.572 (3), 10.745 (2)
β (°) 90.395 (3)
V (Å3)1078.2 (3)
Z4
Radiation typeMo Kα
µ (mm−1)4.32
Crystal size (mm)0.30 × 0.12 × 0.04
Data collection
DiffractometerBruker SMART CCD
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2001)
Tmin, Tmax0.357, 0.846
No. of measured, independent and
observed [I > 2σ(I)] reflections		6327, 2484, 2390
Rint0.021
(sin θ/λ)max (Å−1)0.664
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.026, 0.061, 1.12
No. of reflections2484
No. of parameters221
No. of restraints4
H-atom treatmentAll H-atom parameters refined
Δρmax, Δρmin (e Å−3)1.40, −0.50

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

Selected geometric parameters (Å, º) top
B5—O91.406 (5)B5—O81.444 (4)
B5—O5i1.412 (5)B5—O101.637 (5)
O9—B5—O5i109.8 (3)O9—B5—O10107.1 (3)
O9—B5—O8114.3 (3)O5i—B5—O10107.3 (3)
O5i—B5—O8116.2 (3)O8—B5—O10101.1 (3)
Symmetry code: (i) x+1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1···O3ii0.88 (6)1.75 (6)2.622 (3)173 (6)
O10—H2···O13i0.85 (2)1.89 (3)2.705 (4)160 (6)
O10—H3···O120.85 (2)1.85 (2)2.700 (4)173 (6)
O15—H4···O40.84 (7)2.21 (7)2.967 (4)150 (6)
O15—H4···O10iii0.84 (7)2.50 (6)3.041 (4)123 (6)
O15—H5···O13iv0.84 (7)2.10 (7)2.912 (4)164 (6)
O15—H5···O12iv0.84 (7)2.48 (7)3.093 (4)131 (5)
O14—H6···O2iv0.81 (2)2.01 (3)2.756 (4)153 (6)
Symmetry codes: (i) x+1, y, z; (ii) −x+1, −y+1, −z+1; (iii) x−1/2, −y+1/2, z+1/2; (iv) −x+1/2, y−1/2, −z+1/2.
 

Footnotes

‡Fax: 0086-592-2183937.

Acknowledgements

This work was supported by the National Natural Science Foundation of China (No. 40972035), the Natural Science Foundation of Fujian Province of China (No. 2010 J01308) and the Scientific and Technological Innovation Platform of Fujian Province (No. 2006 L2003).

References

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ISSN: 2056-9890
Volume 68| Part 5| May 2012| Pages i33-i34
doi:10.1107/S1600536812016169
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