Poly[[triaqua­(μ3-pyridine-2,4,6-tricarboxyl­ato)terbium(III)] monohydrate]

Zhu, H.

doi:10.1107/S1600536812028929

metal-organic compounds

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ISSN: 2056-9890

Volume 68| Part 7| July 2012| Page m1017

https://doi.org/10.1107/S1600536812028929

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Poly[[triaqua(μ₃-pyridine-2,4,6-tricarboxylato)terbium(III)] monohydrate]

Hong-lin Zhu ^a ^*

^aCrystal Engineering Division, Center of Applied Solid State Chemistry Research, Ningbo University, Ningbo, Zhejiang 315211, People's Republic of China
^*Correspondence e-mail: Zhuhonglin1@nbu.edu.cn

(Received 16 June 2012; accepted 26 June 2012; online 30 June 2012)

The asymmetric unit of the title compound, {[Tb(C₈H₂NO₆)(H₂O)₃]·H₂O}_n, contains one Tb^III ion, one pyridine-2,4,6-tricarboxylate (ptc) anion, three aqua ligands and one lattice water molecule. The Tb^III ion is nine coordinated by one N and five O atoms from three ptc ligands and by three O atoms from the three aqua ligands in a distorted bicapped trigonal–prismatic geometry. The ptc ligands bridge the Tb^III ions into a two-dimensional polymeric framework parallel to (100). An extensive O—H⋯O hydrogen-bonding network consolidates the crystal packing.

Related literature

For the crystal structures of related complexes, see: Das et al. (2009 ); Wang & Zhang (2009 ); Wang et al. (2010 ); Lin et al. (2011 ); Jin et al. (2012 ).

Experimental

Crystal data

[Tb(C₈H₂NO₆)(H₂O)₃]·H₂O
M_r = 439.09
Monoclinic, P 2₁ /c
a = 11.936 (2) Å
b = 7.3343 (15) Å
c = 13.516 (3) Å
β = 96.43 (3)°
V = 1175.8 (4) Å³
Z = 4
Mo Kα radiation
μ = 6.07 mm⁻¹
T = 293 K
0.32 × 0.30 × 0.28 mm

Data collection

Rigaku R-AXIS RAPID diffractometer
Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ) T_min = 0.164, T_max = 0.183
10998 measured reflections
2664 independent reflections
2528 reflections with I > 2σ(I)
R_int = 0.066

Refinement

R[F² > 2σ(F²)] = 0.028
wR(F²) = 0.067
S = 1.06
2664 reflections
182 parameters
H-atom parameters constrained
Δρ_max = 2.18 e Å⁻³
Δρ_min = −1.11 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O7—H7A⋯O5ⁱ	0.83	1.98	2.642 (4)	136
O7—H7B⋯O4ⁱⁱ	0.84	2.45	2.966 (4)	120
O8—H8A⋯O5ⁱ	0.85	2.04	2.822 (4)	152
O8—H8B⋯O10ⁱⁱⁱ	0.81	1.95	2.760 (5)	174
O9—H9A⋯O1^iv	0.81	2.00	2.808 (4)	179
O9—H9B⋯O3^v	0.81	2.00	2.805 (4)	179
O10—H10A⋯O6^vi	0.84	2.33	2.977 (5)	134
O10—H10B⋯O7^vi	0.85	2.55	3.169 (5)	130
Symmetry codes: (i) $[-x, y+{\script{1\over 2}}, -z+{\script{3\over 2}}]$ ; (ii) $[x, -y+{\script{5\over 2}}, z-{\script{1\over 2}}]$ ; (iii) $[x, -y+{\script{3\over 2}}, z-{\script{1\over 2}}]$ ; (iv) $[-x+1, y+{\script{1\over 2}}, -z+{\script{3\over 2}}]$ ; (v) x, y+1, z; (vi) x, y-1, z.

Data collection: RAPID-AUTO (Rigaku, 1998 ); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2004 ); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXL97.

Supporting information

Crystal structure: contains datablocks global, I. DOI: https://doi.org/10.1107/S1600536812028929/cv5315sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536812028929/cv5315Isup2.hkl

checkCIF report

Comment top

As an ongoing part of our investigations of the lanthanide complexes with pyridine-2,4,6-tricarboxylate (Jin et al., 2012; Lin et al., 2011), we report here the title compound with Tb (I).

In (I) (Fig.1), all bond lengths and angles are normal and correspond to those observed in isostructural polymeric compounds with Gd (Wang & Zhang, 2009), Sm (Wang et al., 2010) and Dy (Wang et al., 2010; Das et al., 2009). Each Tb center is coordinated by three aqua ligands and three ptc ligands (H₃ptc = pyridine-2,4,6-tricarboxylate) to form 4,4'-bicapped trigonal prismatic TbNO₈ chromophore with a 4,4'-bicapped trigonal prismatic environment. The pyridyl N atom, 2-position and 6-position carboxylate group coordinated two Tb atoms, and the 4-position carboxylate group chelated one Tb atom.

The TbNO₈ chromophores are bridged by the ptc anions to form two-dimensional corrugated herringbone-like layers, which extend infinitely parallel to (100) (Fig. 2). The aqua ligands (O7, O8 and O9) donate hydrogen atom to carboxylate oxygen atoms (O4, O3 and O1) to form intralayer hydrogen bonds, and simultaneously O8 and O9 donate hydrogen atom to the carboxylate O5 to form interlayer hydrogen bonds (Table 1). Obviously, the former intralayer hydrogen bonding interactions contribute to stabilization of the two-dimensional layer, and the latter are found to be responsible for supramolecular assembly of the two-dimensional layers into a three-dimensional supramolecular architecture.

Related literature top

For the crystal structures of related complexes, see: Das et al. (2009); Wang & Zhang (2009); Wang et al. (2010); Lin et al. (2011); Jin et al. (2012).

Experimental top

A mixture of Tb₄O₇ (0.0556 g, 0.075 mmol), pyridine-2,4,6-tricarboxylic acid (0.0649 g, 0.3 mmol) and H₂O (10 ml) was sealed into a 23 ml Teflon-lined stainless autoclave, which was heated up to 180°C for 4 days, and then cooled to room temperature. A small amount of colourless needle-shaped crystals were obtained.

Structure description top

As an ongoing part of our investigations of the lanthanide complexes with pyridine-2,4,6-tricarboxylate (Jin et al., 2012; Lin et al., 2011), we report here the title compound with Tb (I).

For the crystal structures of related complexes, see: Das et al. (2009); Wang & Zhang (2009); Wang et al. (2010); Lin et al. (2011); Jin et al. (2012).

Computing details top

Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO (Rigaku, 1998); data reduction: CrystalStructure (Rigaku/MSC, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top

	Fig. 1. A portion of the crystal structure of (I) showing the atomic numbering and 45% probability dispalcement ellipsoids [symmetry codes: (#1) -x + 1, y + 1/2, -z + 3/2; (#2) x, -y + 3/2, z - 1/2; (#3) -x + 1, y - 1/2, -z + 3/2; (#4) x, -y + 3/2, z + 1/2]. H atoms omitted for clarity.
	Fig. 2. A portion of the two-dimensional polymeric framework in (I) viewed down the a axis. H atoms omitted for clarity

Poly[[triaqua(µ₃-pyridine-2,4,6-tricarboxylato)terbium(III)] monohydrate] top

Crystal data top

[Tb(C₈H₂NO₆)(H₂O)₃]·H₂O	F(000) = 840
M_r = 439.09	D_x = 2.480 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 9883 reflections
a = 11.936 (2) Å	θ = 3.0–27.4°
b = 7.3343 (15) Å	µ = 6.07 mm⁻¹
c = 13.516 (3) Å	T = 293 K
β = 96.43 (3)°	Block, colorless
V = 1175.8 (4) Å³	0.32 × 0.30 × 0.28 mm
Z = 4

Data collection top

Rigaku R-AXIS RAPID diffractometer	2664 independent reflections
Radiation source: fine-focus sealed tube	2528 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.066
Detector resolution: 0 pixels mm^-1	θ_max = 27.4°, θ_min = 3.0°
ω scan	h = −15→15
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	k = −9→9
T_min = 0.164, T_max = 0.183	l = −17→15
10998 measured reflections

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.028	H-atom parameters constrained
wR(F²) = 0.067	w = 1/[σ²(F_o²) + (0.0172P)² + 1.9544P] where P = (F_o² + 2F_c²)/3
S = 1.06	(Δ/σ)_max = 0.001
2664 reflections	Δρ_max = 2.18 e Å⁻³
182 parameters	Δρ_min = −1.11 e Å⁻³
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0031 (4)

Crystal data top

[Tb(C₈H₂NO₆)(H₂O)₃]·H₂O	V = 1175.8 (4) Å³
M_r = 439.09	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 11.936 (2) Å	µ = 6.07 mm⁻¹
b = 7.3343 (15) Å	T = 293 K
c = 13.516 (3) Å	0.32 × 0.30 × 0.28 mm
β = 96.43 (3)°

Data collection top

Rigaku R-AXIS RAPID diffractometer	2664 independent reflections
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	2528 reflections with I > 2σ(I)
T_min = 0.164, T_max = 0.183	R_int = 0.066
10998 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.028	0 restraints
wR(F²) = 0.067	H-atom parameters constrained
S = 1.06	Δρ_max = 2.18 e Å⁻³
2664 reflections	Δρ_min = −1.11 e Å⁻³
182 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

	x	y	z	U_iso*/U_eq
Tb	0.285028 (12)	1.21386 (2)	0.704284 (11)	0.01088 (9)
N	0.2959 (2)	1.0044 (4)	0.8499 (2)	0.0132 (5)
C1	0.3926 (3)	0.9190 (5)	0.8812 (2)	0.0140 (6)
C2	0.3992 (3)	0.7853 (5)	0.9547 (3)	0.0165 (7)
H2A	0.4669	0.7266	0.9750	0.020*
C3	0.3023 (3)	0.7424 (5)	0.9978 (3)	0.0167 (7)
C4	0.2025 (3)	0.8380 (5)	0.9689 (3)	0.0160 (7)
H4A	0.1382	0.8183	1.0000	0.019*
C5	0.2033 (3)	0.9641 (5)	0.8917 (2)	0.0141 (7)
C6	0.4904 (3)	0.9703 (4)	0.8255 (2)	0.0137 (6)
O1	0.4681 (2)	1.0675 (4)	0.74843 (18)	0.0186 (5)
O2	0.58643 (19)	0.9109 (3)	0.85646 (18)	0.0168 (5)
C7	0.2986 (3)	0.5894 (5)	1.0710 (2)	0.0162 (7)
O3	0.3445 (2)	0.4402 (4)	1.05122 (18)	0.0209 (5)
O4	0.2479 (2)	0.6092 (4)	1.14653 (19)	0.0238 (6)
C8	0.0984 (3)	1.0619 (5)	0.8451 (3)	0.0163 (7)
O5	0.0075 (2)	1.0267 (4)	0.8774 (2)	0.0250 (6)
O6	0.1127 (2)	1.1688 (4)	0.7744 (2)	0.0228 (6)
O7	0.1990 (2)	1.5188 (4)	0.7163 (2)	0.0262 (6)
H7A	0.1317	1.5476	0.7166	0.031*
H7B	0.2563	1.5872	0.7231	0.031*
O8	0.1356 (3)	1.2471 (4)	0.5676 (2)	0.0296 (7)
H8A	0.0844	1.3275	0.5632	0.050*
H8B	0.1167	1.1746	0.5237	0.050*
O9	0.3781 (2)	1.3706 (4)	0.85261 (19)	0.0243 (6)
H9A	0.4225	1.4272	0.8240	0.029*
H9B	0.3690	1.3909	0.9095	0.029*
O10	0.0703 (4)	0.4780 (5)	0.9079 (3)	0.0481 (9)
H10A	0.0413	0.4022	0.8662	0.058*
H10B	0.1358	0.4736	0.8891	0.058*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Tb	0.00838 (12)	0.01147 (13)	0.01279 (13)	−0.00008 (5)	0.00110 (8)	0.00033 (5)
N	0.0100 (13)	0.0133 (13)	0.0162 (13)	−0.0010 (11)	0.0007 (11)	0.0008 (11)
C1	0.0118 (15)	0.0129 (16)	0.0164 (15)	0.0003 (12)	−0.0022 (13)	−0.0011 (12)
C2	0.0119 (17)	0.0182 (19)	0.0188 (18)	0.0026 (12)	−0.0008 (15)	0.0034 (12)
C3	0.0205 (18)	0.0126 (15)	0.0168 (18)	0.0009 (14)	0.0015 (16)	0.0023 (13)
C4	0.0133 (16)	0.0159 (17)	0.0200 (17)	0.0012 (13)	0.0073 (14)	0.0029 (14)
C5	0.0141 (15)	0.0150 (17)	0.0127 (15)	0.0000 (12)	0.0000 (13)	0.0005 (12)
C6	0.0140 (15)	0.0084 (15)	0.0185 (16)	0.0013 (12)	0.0015 (13)	−0.0025 (12)
O1	0.0135 (11)	0.0220 (13)	0.0209 (12)	0.0040 (10)	0.0048 (10)	0.0084 (10)
O2	0.0109 (11)	0.0172 (13)	0.0215 (12)	0.0043 (9)	−0.0015 (10)	−0.0011 (10)
C7	0.0151 (16)	0.0159 (17)	0.0173 (16)	−0.0001 (13)	0.0001 (14)	0.0042 (13)
O3	0.0251 (13)	0.0172 (13)	0.0209 (12)	0.0047 (10)	0.0049 (11)	0.0059 (10)
O4	0.0320 (15)	0.0197 (14)	0.0214 (13)	0.0071 (11)	0.0108 (12)	0.0069 (10)
C8	0.0132 (15)	0.0160 (16)	0.0200 (16)	0.0008 (13)	0.0027 (14)	0.0017 (13)
O5	0.0092 (11)	0.0335 (16)	0.0321 (14)	−0.0009 (10)	0.0022 (11)	0.0106 (12)
O6	0.0162 (12)	0.0288 (15)	0.0242 (14)	0.0063 (11)	0.0052 (11)	0.0133 (11)
O7	0.0150 (12)	0.0184 (14)	0.0441 (17)	0.0012 (10)	−0.0016 (12)	0.0001 (12)
O8	0.0257 (16)	0.0348 (16)	0.0257 (16)	0.0121 (12)	−0.0084 (14)	−0.0057 (12)
O9	0.0280 (14)	0.0269 (15)	0.0180 (12)	−0.0104 (12)	0.0029 (11)	−0.0044 (11)
O10	0.067 (2)	0.041 (2)	0.0368 (17)	0.0117 (18)	0.0046 (18)	−0.0032 (15)

Geometric parameters (Å, º) top

Tb—O2ⁱ	2.324 (2)	C5—C8	1.518 (4)
Tb—O6	2.382 (3)	C6—O2	1.253 (4)
Tb—O8	2.432 (3)	C6—O1	1.266 (4)
Tb—O1	2.448 (2)	O2—Tbⁱⁱⁱ	2.324 (2)
Tb—O9	2.465 (3)	C7—O4	1.253 (4)
Tb—O7	2.474 (3)	C7—O3	1.266 (4)
Tb—N	2.488 (3)	C7—Tb^iv	2.878 (3)
Tb—O4ⁱⁱ	2.518 (3)	O3—Tb^iv	2.528 (3)
Tb—O3ⁱⁱ	2.528 (3)	O4—Tb^iv	2.518 (3)
Tb—C7ⁱⁱ	2.878 (3)	C8—O5	1.241 (4)
N—C5	1.329 (4)	C8—O6	1.263 (4)
N—C1	1.340 (4)	O7—H7A	0.8302
C1—C2	1.392 (5)	O7—H7B	0.8454
C1—C6	1.506 (5)	O8—H8A	0.8470
C2—C3	1.387 (6)	O8—H8B	0.8095
C2—H2A	0.9293	O9—H9A	0.8057
C3—C4	1.400 (5)	O9—H9B	0.8018
C3—C7	1.500 (5)	O10—H10A	0.8390
C4—C5	1.396 (5)	O10—H10B	0.8498
C4—H4A	0.9271

O2ⁱ—Tb—O6	149.38 (9)	C5—N—C1	119.3 (3)
O2ⁱ—Tb—O8	97.26 (11)	C5—N—Tb	120.1 (2)
O6—Tb—O8	73.97 (11)	C1—N—Tb	120.3 (2)
O2ⁱ—Tb—O1	75.64 (9)	N—C1—C2	122.2 (3)
O6—Tb—O1	128.99 (8)	N—C1—C6	114.5 (3)
O8—Tb—O1	141.98 (10)	C2—C1—C6	123.2 (3)
O2ⁱ—Tb—O9	75.06 (9)	C3—C2—C1	118.5 (3)
O6—Tb—O9	94.10 (10)	C3—C2—H2A	120.6
O8—Tb—O9	142.78 (10)	C1—C2—H2A	120.9
O1—Tb—O9	72.40 (10)	C2—C3—C4	119.5 (3)
O2ⁱ—Tb—O7	75.90 (9)	C2—C3—C7	122.3 (3)
O6—Tb—O7	73.49 (10)	C4—C3—C7	118.2 (3)
O8—Tb—O7	71.63 (10)	C5—C4—C3	117.6 (3)
O1—Tb—O7	138.26 (9)	C5—C4—H4A	121.2
O9—Tb—O7	71.18 (9)	C3—C4—H4A	121.2
O2ⁱ—Tb—N	133.27 (9)	N—C5—C4	122.7 (3)
O6—Tb—N	64.57 (9)	N—C5—C8	113.9 (3)
O8—Tb—N	129.16 (11)	C4—C5—C8	123.3 (3)
O1—Tb—N	64.56 (9)	O2—C6—O1	124.9 (3)
O9—Tb—N	70.47 (9)	O2—C6—C1	118.5 (3)
O7—Tb—N	119.42 (10)	O1—C6—C1	116.6 (3)
O2ⁱ—Tb—O4ⁱⁱ	125.16 (9)	C6—O1—Tb	123.2 (2)
O6—Tb—O4ⁱⁱ	82.13 (10)	C6—O2—Tbⁱⁱⁱ	135.5 (2)
O8—Tb—O4ⁱⁱ	76.72 (10)	O4—C7—O3	122.2 (3)
O1—Tb—O4ⁱⁱ	77.54 (9)	O4—C7—C3	120.2 (3)
O9—Tb—O4ⁱⁱ	137.60 (9)	O3—C7—C3	117.6 (3)
O7—Tb—O4ⁱⁱ	144.19 (9)	O4—C7—Tb^iv	60.86 (18)
N—Tb—O4ⁱⁱ	69.89 (9)	O3—C7—Tb^iv	61.32 (18)
O2ⁱ—Tb—O3ⁱⁱ	74.43 (9)	C3—C7—Tb^iv	177.3 (2)
O6—Tb—O3ⁱⁱ	126.72 (10)	C7—O3—Tb^iv	92.6 (2)
O8—Tb—O3ⁱⁱ	70.88 (10)	C7—O4—Tb^iv	93.4 (2)
O1—Tb—O3ⁱⁱ	71.25 (9)	O5—C8—O6	126.4 (3)
O9—Tb—O3ⁱⁱ	137.04 (9)	O5—C8—C5	118.0 (3)
O7—Tb—O3ⁱⁱ	127.92 (9)	O6—C8—C5	115.6 (3)
N—Tb—O3ⁱⁱ	112.14 (9)	C8—O6—Tb	125.7 (2)
O4ⁱⁱ—Tb—O3ⁱⁱ	51.80 (9)	Tb—O7—H7A	129.7
O2ⁱ—Tb—C7ⁱⁱ	100.00 (10)	Tb—O7—H7B	101.9
O6—Tb—C7ⁱⁱ	104.70 (10)	H7A—O7—H7B	128.4
O8—Tb—C7ⁱⁱ	71.93 (10)	Tb—O8—H8A	125.8
O1—Tb—C7ⁱⁱ	72.68 (9)	Tb—O8—H8B	127.7
O9—Tb—C7ⁱⁱ	144.85 (10)	H8A—O8—H8B	105.4
O7—Tb—C7ⁱⁱ	142.43 (9)	Tb—O9—H9A	96.4
N—Tb—C7ⁱⁱ	90.95 (10)	Tb—O9—H9B	140.3
O4ⁱⁱ—Tb—C7ⁱⁱ	25.75 (10)	H9A—O9—H9B	122.1
O3ⁱⁱ—Tb—C7ⁱⁱ	26.05 (9)	H10A—O10—H10B	95.6

Symmetry codes: (i) −x+1, y+1/2, −z+3/2; (ii) x, −y+3/2, z−1/2; (iii) −x+1, y−1/2, −z+3/2; (iv) x, −y+3/2, z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O7—H7A···O5^v	0.83	1.98	2.642 (4)	136
O7—H7B···O4^vi	0.84	2.45	2.966 (4)	120
O8—H8A···O5^v	0.85	2.04	2.822 (4)	152
O8—H8B···O10ⁱⁱ	0.81	1.95	2.760 (5)	174
O9—H9A···O1ⁱ	0.81	2.00	2.808 (4)	179
O9—H9B···O3^vii	0.81	2.00	2.805 (4)	179
O10—H10A···O6^viii	0.84	2.33	2.977 (5)	134
O10—H10B···O7^viii	0.85	2.55	3.169 (5)	130

Symmetry codes: (i) −x+1, y+1/2, −z+3/2; (ii) x, −y+3/2, z−1/2; (v) −x, y+1/2, −z+3/2; (vi) x, −y+5/2, z−1/2; (vii) x, y+1, z; (viii) x, y−1, z.

Experimental details

Crystal data
Chemical formula	[Tb(C₈H₂NO₆)(H₂O)₃]·H₂O
M_r	439.09
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	293
a, b, c (Å)	11.936 (2), 7.3343 (15), 13.516 (3)
β (°)	96.43 (3)
V (Å³)	1175.8 (4)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	6.07
Crystal size (mm)	0.32 × 0.30 × 0.28

Data collection
Diffractometer	Rigaku R-AXIS RAPID
Absorption correction	Multi-scan (ABSCOR; Higashi, 1995)
T_min, T_max	0.164, 0.183
No. of measured, independent and observed [I > 2σ(I)] reflections	10998, 2664, 2528
R_int	0.066
(sin θ/λ)_max (Å⁻¹)	0.648

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.028, 0.067, 1.06
No. of reflections	2664
No. of parameters	182
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	2.18, −1.11

Computer programs: RAPID-AUTO (Rigaku, 1998), CrystalStructure (Rigaku/MSC, 2004), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O7—H7A···O5ⁱ	0.83	1.98	2.642 (4)	136
O7—H7B···O4ⁱⁱ	0.84	2.45	2.966 (4)	120
O8—H8A···O5ⁱ	0.85	2.04	2.822 (4)	152
O8—H8B···O10ⁱⁱⁱ	0.81	1.95	2.760 (5)	174
O9—H9A···O1^iv	0.81	2.00	2.808 (4)	179
O9—H9B···O3^v	0.81	2.00	2.805 (4)	179
O10—H10A···O6^vi	0.84	2.33	2.977 (5)	134
O10—H10B···O7^vi	0.85	2.55	3.169 (5)	130

Symmetry codes: (i) −x, y+1/2, −z+3/2; (ii) x, −y+5/2, z−1/2; (iii) x, −y+3/2, z−1/2; (iv) −x+1, y+1/2, −z+3/2; (v) x, y+1, z; (vi) x, y−1, z.

Acknowledgements

This project was supported by the K. C. Wong Magna Fund of Ningbo University.

References

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