Poly[tetra­deca­aqua­tetra­kis­(μ3-imidazole-4,5-dicarboxyl­ato)hexa-μ3-sulfato-cobalt(II)hexa­samarium(III)]

Zhu, L.-C.; Zhu, S.-M.

doi:10.1107/S1600536811030169

metal-organic compounds

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 67| Part 8| August 2011| Pages m1166-m1167

doi:10.1107/S1600536811030169

Open

access

Poly[tetradecaaquatetrakis(μ₃-imidazole-4,5-dicarboxylato)hexa-μ₃-sulfato-cobalt(II)hexasamarium(III)]

Li-Cai Zhu ^a and Si-Ming Zhu ^b ^*

^aSchool of Chemistry and the Environment, South China Normal University, Guangzhou 510631, People's Republic of China, and ^bSchool of Light Industry and Food Science, South China University of Technology, Guangzhou 510641, People's Republic of China
^*Correspondence e-mail: simingzhu76@yahoo.com.cn

(Received 15 July 2011; accepted 26 July 2011; online 30 July 2011)

In the title three-dimensional compound, [CoSm₆(C₅H₂N₂O₄)₄(SO₄)₆(H₂O)₁₄]_n, the Co^II ion is six-coordinated with two O atoms and two N atoms from two imidazole-4,5-dicarboxylate ligands and two coordinated water molecules, giving a slightly distorted octahedral geometry. One Sm^III ion is eight-coordinated in a bicapped trigonal–prismatic coordination geometry by four O atoms from two imidazole-4,5-dicarboxylate ligands, two O atoms from two SO₄²⁻ anions and two coordinated water molecules. The other two Sm^III ions are nine-coordinated in a tricapped trigonal–prismatic coordination geometry; one of these Sm^III ions is bonded to four O atoms from two imidazole-4,5-dicarboxylate ligands, three O atoms from three SO₄²⁻ anions and two water O atoms, and the other Sm^III ion is coordinated by one O atom and one N atom from one imidazole-4,5-dicarboxylate ligand, five O atoms from three SO₄²⁻ anions, as well as two coordinated water molecules. The crystal structure is further stabilized by N—H⋯O, O—H⋯O, and C—H⋯O hydrogen-bonding interactions.

Related literature

For the application of lanthanide transition metal heterometallic complexes with bridging multifunctional organic ligands, see: Cheng et al. (2006 ); Kuang et al. (2007 ); Sun & Yang (2007 ); Zhu et al. (2010 ).

Experimental

Crystal data

[CoSm₆(C₅H₂N₂O₄)₄(SO₄)₆(H₂O)₁₄]
M_r = 2406.08
Triclinic, $[P \overline 1]$
a = 6.6395 (10) Å
b = 9.5090 (14) Å
c = 21.619 (3) Å
α = 97.068 (2)°
β = 94.391 (2)°
γ = 98.006 (2)°
V = 1335.2 (3) Å³
Z = 1
Mo Kα radiation
μ = 7.17 mm⁻¹
T = 296 K
0.20 × 0.18 × 0.15 mm

Data collection

Bruker APEXII area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ) T_min = 0.260, T_max = 0.341
6967 measured reflections
4716 independent reflections
3971 reflections with I > 2σ(I)
R_int = 0.024

Refinement

R[F² > 2σ(F²)] = 0.031
wR(F²) = 0.070
S = 1.02
4716 reflections
478 parameters
23 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 1.00 e Å⁻³
Δρ_min = −1.03 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N2—H1⋯O18ⁱ	0.87 (6)	2.06 (5)	2.916 (8)	170 (6)
O1W—H1W⋯O7	0.82 (5)	2.52 (8)	3.140 (8)	133 (7)
O1W—H1W⋯O16ⁱ	0.82 (5)	2.12 (6)	2.777 (6)	136 (8)
N4—H2⋯O7ⁱⁱ	0.87 (4)	1.94 (5)	2.803 (8)	171 (8)
O1W—H2W⋯O1ⁱⁱⁱ	0.82 (5)	2.51 (6)	3.247 (7)	150 (7)
O2W—H3W⋯O3W	0.83 (5)	2.02 (5)	2.809 (8)	160 (6)
O2W—H4W⋯O6^iv	0.83 (4)	2.55 (4)	3.303 (9)	152 (8)
O2W—H4W⋯O8^iv	0.83 (4)	2.53 (7)	3.204 (8)	140 (6)
O3W—H5W⋯O4^v	0.83 (4)	1.98 (5)	2.789 (7)	166 (8)
O3W—H6W⋯O1^iv	0.83 (5)	1.93 (5)	2.732 (7)	161 (5)
O4W—H7W⋯O17	0.81 (5)	2.59 (6)	3.270 (8)	142 (7)
O4W—H7W⋯O19	0.81 (5)	2.20 (6)	2.874 (7)	141 (5)
O4W—H8W⋯O6^vi	0.81 (7)	2.47 (7)	3.186 (8)	149 (6)
O5W—H10W⋯O7W^vii	0.82 (6)	2.10 (6)	2.794 (8)	142 (6)
O6W—H11W⋯O14^viii	0.81 (4)	1.99 (5)	2.751 (7)	157 (5)
O6W—H12W⋯O5W^viii	0.81 (6)	2.27 (7)	3.053 (8)	162 (7)
O7W—H13W⋯O11^vii	0.81 (5)	2.45 (5)	3.063 (6)	133 (7)
O7W—H13W⋯O12^vii	0.81 (5)	2.06 (6)	2.855 (7)	168 (7)
O7W—H14W⋯O12^ix	0.81 (5)	1.85 (5)	2.661 (7)	174 (7)
C5—H5⋯O3^x	0.93	2.52	3.388 (8)	155
C10—H11⋯O17^ix	0.93	2.54	3.430 (9)	161
Symmetry codes: (i) x, y+1, z; (ii) x, y-1, z; (iii) -x, -y+1, -z+1; (iv) -x, -y, -z+1; (v) -x+1, -y, -z+1; (vi) x+1, y, z; (vii) -x, -y, -z+2; (viii) -x+1, -y, -z+2; (ix) x-1, y-1, z; (x) -x+1, -y+1, -z+1.

Data collection: APEX2 (Bruker, 2004 ); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP in SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536811030169/om2450sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536811030169/om2450Isup2.hkl

checkCIF report

Comment top

In the past few years, lanthanide-transition metal heterometallic complexs with bridging multifunctionnal organic ligands gained increasing interest, not only because of their impressive topological structures, but also due to their versatile applications in ion exchange, magnetism, bimetallic catalysis and as luminescent probes (Cheng et al., 2006; Kuang et al., 2007; Sun & Yang, 2007; Zhu et al., 2010). As an extension of this research, the structure of the title compound, a new heterometallic coordination polymer has been determined which is presented in this artcle.

The asymmetric unit of the title compound (Fig. 1), contains a Co^II ion, three Sm^III ions, two imidazole-4, 5-dicarboxylate ligands, three SO₄^2- anions, and seven coordinated water molecules. The Co^II ion lie in the inversion center and is six-coordinated with two O atoms from two coordinated water molecules, two O atoms and two N atoms from two imidazole-4, 5-dicarboxylate ligands, giving a slightly distorted octahedral geometry. The Sm^III ions exhibit three types of coordination environment. One Sm^III ion is eight-coordinated in a bicapped trigonal prismatic coordination geometry by four O atoms from two imidazole-4,5-dicarboxylate ligands, two O atoms from two SO₄^2- anions and two coordinated water molecules. The other Sm^III ions are nine-coordinated in a tricapped trigonal prismatic coordination geometry; one of these Sm^III ions is bonded to four O atoms from two imidazole-4,5-dicarboxylate ligands, three O atoms from three SO₄^2- anions and two water O atoms and the other Sm^III ion is coordinated by one O atom and one N atom from one imidazole-4, 5-dicarboxylate ligand, five O atoms from three SO₄^2- anions as well as two coordinated water molecules. These metal coordination units are connected by bridging imidazole-4, 5-dicarboxylate and sulfate ligands, generating a three-dimensional network (Fig. 2). The crystal structure is further stabilized by N—H···O, O—H···O, and C—H···O hydrogen-bonding interactions between water molecules, SO₄^2- anions, and imidazole-4, 5-dicarboxylate ligands (Table 1).

Related literature top

For the application of lanthanide transition metal heterometallic complexes with bridging multifunctional organic ligands, see: Cheng et al. (2006); Kuang et al. (2007); Sun & Yang (2007); Zhu et al. (2010).

Experimental top

A mixture of CoSO₄.7H₂O(0.141 g, 0.5 mmol), Sm₂O₃(0.087 g, 0.25 mmol), imidazole-4,5-dicarboxylic acid (0.156 g, 1 mmol), and H₂O(10 ml) was sealed in a 20 ml Teflon-lined reaction vessel at 443 K for 5 days then slowly cooled to room temperature. The product was collected by filtration, washed with water and air-dried. Red block crystals suitable for X-ray analysis were obtained.

Computing details top

Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT (Bruker, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP in SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top

	Fig. 1. The molecular structure showing the atomic-numbering scheme and displacement ellipsoids drawn at the 30% probability level. Hydrogen atoms were omitted for clarity. Symmetry codes: (A) -x, -1 - y, 2 - z; (B) -1 + x, y, z; (C) - x, - y, 1 - z; (D) 1 + x, y, z; (E) 1 - x, 1 - y, 1 - z.
	Fig. 2. A view of the three-dimensional structure of the title compound. Hydrogen atoms were omitted for clarity.

Poly[tetradecaaquatetrakis(µ₃-imidazole-4,5-dicarboxylato)hexa-µ₃- sulfato-cobalt(II)hexasamarium(III)] top

Crystal data top

[CoSm₆(C₅H₂N₂O₄)₄(SO₄)₆(H₂O)₁₄]	Z = 1
M_r = 2406.08	F(000) = 1139
Triclinic, P1	D_x = 2.992 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 6.6395 (10) Å	Cell parameters from 2636 reflections
b = 9.5090 (14) Å	θ = 2.2–27.9°
c = 21.619 (3) Å	µ = 7.17 mm⁻¹
α = 97.068 (2)°	T = 296 K
β = 94.391 (2)°	Block, red
γ = 98.006 (2)°	0.20 × 0.18 × 0.15 mm
V = 1335.2 (3) Å³

Data collection top

Bruker APEXII area-detector diffractometer	4716 independent reflections
Radiation source: fine-focus sealed tube	3971 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.024
ϕ and ω scan	θ_max = 25.2°, θ_min = 1.9°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −7→5
T_min = 0.260, T_max = 0.341	k = −11→11
6967 measured reflections	l = −25→25

Refinement top

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)] = 0.031	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.070	H atoms treated by a mixture of independent and constrained refinement
S = 1.02	w = 1/[σ²(F_o²) + (0.0293P)² + 2.3668P] where P = (F_o² + 2F_c²)/3
4716 reflections	(Δ/σ)_max = 0.002
478 parameters	Δρ_max = 1.00 e Å⁻³
23 restraints	Δρ_min = −1.03 e Å⁻³

Crystal data top

[CoSm₆(C₅H₂N₂O₄)₄(SO₄)₆(H₂O)₁₄]	γ = 98.006 (2)°
M_r = 2406.08	V = 1335.2 (3) Å³
Triclinic, P1	Z = 1
a = 6.6395 (10) Å	Mo Kα radiation
b = 9.5090 (14) Å	µ = 7.17 mm⁻¹
c = 21.619 (3) Å	T = 296 K
α = 97.068 (2)°	0.20 × 0.18 × 0.15 mm
β = 94.391 (2)°

Data collection top

Bruker APEXII area-detector diffractometer	4716 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	3971 reflections with I > 2σ(I)
T_min = 0.260, T_max = 0.341	R_int = 0.024
6967 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.031	23 restraints
wR(F²) = 0.070	H atoms treated by a mixture of independent and constrained refinement
S = 1.02	Δρ_max = 1.00 e Å⁻³
4716 reflections	Δρ_min = −1.03 e Å⁻³
478 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
Sm3	0.33206 (6)	0.01643 (4)	0.860687 (16)	0.01396 (10)
Sm2	0.06536 (5)	−0.11526 (4)	0.677756 (16)	0.01039 (9)
Sm1	0.34787 (5)	0.29252 (4)	0.577813 (16)	0.01209 (10)
Co1	0.0000	−0.5000	1.0000	0.0144 (3)
S1	0.3305 (3)	0.35636 (18)	0.43568 (8)	0.0117 (3)
S2	−0.1527 (3)	0.18219 (18)	0.62306 (8)	0.0144 (4)
S3	0.7700 (3)	−0.05896 (19)	0.81404 (8)	0.0163 (4)
N1	0.4459 (9)	0.4015 (6)	0.6919 (3)	0.0158 (13)
N2	0.5267 (9)	0.5408 (6)	0.7811 (3)	0.0145 (13)
N3	−0.0134 (9)	−0.5242 (6)	0.8997 (3)	0.0139 (13)
N4	−0.0377 (9)	−0.5503 (6)	0.7965 (2)	0.0129 (12)
C1	0.3005 (10)	0.1744 (7)	0.7196 (3)	0.0110 (14)
C2	0.4007 (10)	0.3228 (7)	0.7395 (3)	0.0123 (14)
C3	0.4487 (10)	0.4087 (7)	0.7958 (3)	0.0113 (14)
C4	0.4360 (10)	0.3875 (7)	0.8624 (3)	0.0147 (15)
C5	0.5213 (11)	0.5311 (8)	0.7190 (3)	0.0176 (16)
H5	0.5655	0.6069	0.6975	0.021*
C6	0.1796 (11)	−0.2840 (7)	0.9305 (3)	0.0154 (15)
C7	0.0741 (10)	−0.3984 (7)	0.8801 (3)	0.0131 (15)
C8	0.0601 (10)	−0.4121 (7)	0.8155 (3)	0.0114 (14)
C9	0.1121 (11)	−0.3170 (7)	0.7687 (3)	0.0148 (15)
C10	−0.0769 (10)	−0.6128 (7)	0.8472 (3)	0.0144 (15)
H11	−0.1408	−0.7067	0.8459	0.017*
O1	0.1806 (7)	0.3703 (5)	0.4827 (2)	0.0177 (11)
O2	0.4117 (8)	0.4971 (5)	0.4209 (2)	0.0221 (12)
O3	0.2273 (7)	0.2689 (5)	0.3784 (2)	0.0198 (11)
O4	0.4904 (7)	0.2855 (5)	0.4640 (2)	0.0232 (12)
O5	−0.0086 (8)	0.2036 (6)	0.5754 (2)	0.0259 (12)
O6	−0.1534 (8)	0.0358 (5)	0.6398 (3)	0.0319 (14)
O7	−0.0966 (9)	0.2882 (6)	0.6773 (3)	0.0410 (16)
O8	−0.3591 (7)	0.1881 (5)	0.5942 (2)	0.0242 (12)
O9	0.2794 (7)	0.1296 (5)	0.6617 (2)	0.0152 (10)
O10	0.2340 (7)	0.0918 (5)	0.7580 (2)	0.0137 (10)
O11	0.3918 (8)	0.2647 (5)	0.8764 (2)	0.0231 (12)
O12	0.4709 (8)	0.4987 (5)	0.9016 (2)	0.0226 (12)
O13	0.2724 (8)	−0.1722 (5)	0.9173 (2)	0.0205 (12)
O14	0.1701 (8)	−0.3116 (5)	0.9862 (2)	0.0184 (11)
O15	0.2062 (7)	−0.1901 (5)	0.7844 (2)	0.0148 (11)
O16	0.0501 (8)	−0.3614 (5)	0.7124 (2)	0.0198 (11)
O17	0.6400 (8)	0.0535 (6)	0.8074 (3)	0.0347 (14)
O18	0.6559 (11)	−0.1679 (6)	0.8443 (3)	0.052 (2)
O19	0.8096 (7)	−0.1215 (5)	0.7507 (2)	0.0212 (12)
O20	0.9627 (7)	0.0049 (5)	0.8501 (2)	0.0243 (12)
H1	0.563 (12)	0.623 (5)	0.804 (3)	0.036*
H2	−0.042 (12)	−0.598 (7)	0.7595 (18)	0.036*
O1W	0.1566 (8)	0.5002 (6)	0.6016 (2)	0.0261 (13)
H1W	0.096 (10)	0.495 (9)	0.6332 (19)	0.039*
H2W	0.065 (8)	0.500 (9)	0.574 (2)	0.039*
O2W	0.2776 (10)	0.0581 (6)	0.5120 (3)	0.0341 (14)
H3W	0.218 (13)	−0.017 (5)	0.522 (3)	0.051*
H4W	0.292 (14)	0.032 (8)	0.4750 (16)	0.051*
O3W	0.1551 (8)	−0.1832 (5)	0.5707 (2)	0.0227 (12)
H5W	0.266 (5)	−0.213 (7)	0.567 (4)	0.034*
H6W	0.073 (7)	−0.249 (6)	0.550 (3)	0.034*
O4W	0.4309 (8)	−0.1323 (6)	0.6751 (2)	0.0259 (12)
H7W	0.496 (10)	−0.127 (9)	0.7089 (18)	0.039*
H8W	0.504 (10)	−0.087 (8)	0.654 (3)	0.039*
O5W	0.1776 (9)	0.0980 (6)	0.9654 (3)	0.0349 (14)
H9W	0.060 (6)	0.083 (9)	0.949 (4)	0.052*
H10W	0.184 (12)	0.170 (6)	0.991 (3)	0.052*
O6W	0.6080 (9)	0.0697 (5)	0.9447 (2)	0.0259 (13)
H11W	0.651 (12)	0.152 (3)	0.959 (3)	0.039*
H12W	0.639 (12)	0.021 (6)	0.971 (3)	0.039*
O7W	−0.2592 (8)	−0.3945 (6)	0.9992 (2)	0.0225 (12)
H13W	−0.311 (10)	−0.413 (8)	1.0306 (17)	0.034*
H14W	−0.348 (8)	−0.425 (8)	0.971 (2)	0.034*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Sm3	0.0175 (2)	0.01187 (19)	0.01055 (18)	−0.00508 (15)	−0.00139 (15)	0.00379 (14)
Sm2	0.01014 (19)	0.01094 (18)	0.00963 (18)	−0.00008 (14)	0.00035 (14)	0.00181 (13)
Sm1	0.0119 (2)	0.01235 (19)	0.01166 (18)	0.00027 (14)	0.00082 (14)	0.00227 (14)
Co1	0.0199 (8)	0.0113 (7)	0.0108 (7)	−0.0047 (6)	0.0021 (6)	0.0040 (5)
S1	0.0102 (9)	0.0135 (8)	0.0101 (8)	−0.0031 (7)	0.0000 (7)	0.0024 (6)
S2	0.0132 (9)	0.0142 (9)	0.0161 (9)	0.0018 (7)	0.0027 (7)	0.0034 (7)
S3	0.0127 (9)	0.0206 (9)	0.0133 (9)	−0.0015 (7)	0.0020 (7)	−0.0023 (7)
N1	0.022 (3)	0.015 (3)	0.011 (3)	−0.001 (3)	0.005 (3)	0.003 (2)
N2	0.018 (3)	0.011 (3)	0.013 (3)	−0.001 (3)	0.003 (3)	0.000 (2)
N3	0.015 (3)	0.011 (3)	0.014 (3)	−0.007 (2)	−0.001 (3)	0.004 (2)
N4	0.021 (3)	0.011 (3)	0.007 (3)	0.001 (2)	0.004 (3)	−0.002 (2)
C1	0.011 (4)	0.011 (3)	0.013 (3)	0.002 (3)	0.004 (3)	0.002 (3)
C2	0.008 (3)	0.016 (4)	0.013 (3)	0.003 (3)	0.002 (3)	0.001 (3)
C3	0.016 (4)	0.008 (3)	0.010 (3)	−0.003 (3)	0.006 (3)	−0.001 (3)
C4	0.011 (4)	0.015 (4)	0.017 (4)	0.006 (3)	−0.002 (3)	−0.004 (3)
C5	0.020 (4)	0.020 (4)	0.013 (4)	0.001 (3)	0.003 (3)	0.006 (3)
C6	0.015 (4)	0.018 (4)	0.011 (3)	0.001 (3)	0.001 (3)	−0.001 (3)
C7	0.015 (4)	0.009 (3)	0.016 (4)	0.000 (3)	0.003 (3)	0.009 (3)
C8	0.011 (4)	0.016 (4)	0.007 (3)	0.005 (3)	−0.002 (3)	0.003 (3)
C9	0.016 (4)	0.015 (4)	0.016 (4)	0.005 (3)	0.005 (3)	0.003 (3)
C10	0.009 (4)	0.013 (3)	0.021 (4)	−0.004 (3)	0.004 (3)	0.002 (3)
O1	0.015 (3)	0.022 (3)	0.013 (2)	−0.004 (2)	0.003 (2)	0.002 (2)
O2	0.030 (3)	0.016 (3)	0.020 (3)	−0.006 (2)	0.007 (2)	0.007 (2)
O3	0.019 (3)	0.024 (3)	0.013 (2)	−0.007 (2)	0.004 (2)	−0.004 (2)
O4	0.016 (3)	0.028 (3)	0.028 (3)	0.008 (2)	0.000 (2)	0.009 (2)
O5	0.015 (3)	0.040 (3)	0.023 (3)	−0.001 (2)	0.004 (2)	0.010 (2)
O6	0.015 (3)	0.018 (3)	0.066 (4)	0.000 (2)	0.002 (3)	0.025 (3)
O7	0.044 (4)	0.045 (4)	0.026 (3)	0.003 (3)	0.001 (3)	−0.021 (3)
O8	0.015 (3)	0.033 (3)	0.028 (3)	0.011 (2)	−0.001 (2)	0.010 (2)
O9	0.021 (3)	0.012 (2)	0.011 (2)	0.000 (2)	0.001 (2)	0.0008 (19)
O10	0.016 (3)	0.013 (2)	0.013 (2)	−0.002 (2)	0.005 (2)	0.0036 (19)
O11	0.041 (3)	0.012 (3)	0.016 (3)	−0.001 (2)	0.005 (2)	0.006 (2)
O12	0.031 (3)	0.017 (3)	0.017 (3)	−0.001 (2)	0.000 (2)	−0.003 (2)
O13	0.030 (3)	0.016 (3)	0.010 (2)	−0.011 (2)	−0.004 (2)	0.001 (2)
O14	0.028 (3)	0.013 (2)	0.010 (2)	−0.012 (2)	−0.001 (2)	0.0035 (19)
O15	0.021 (3)	0.010 (2)	0.012 (2)	−0.003 (2)	0.002 (2)	0.0015 (19)
O16	0.032 (3)	0.015 (3)	0.010 (3)	0.004 (2)	−0.004 (2)	−0.001 (2)
O17	0.022 (3)	0.059 (4)	0.026 (3)	0.022 (3)	0.003 (3)	−0.001 (3)
O18	0.079 (5)	0.042 (4)	0.022 (3)	−0.031 (4)	0.019 (3)	−0.008 (3)
O19	0.013 (3)	0.033 (3)	0.016 (3)	0.001 (2)	0.003 (2)	−0.005 (2)
O20	0.014 (3)	0.029 (3)	0.025 (3)	−0.002 (2)	0.000 (2)	−0.010 (2)
O1W	0.032 (3)	0.034 (3)	0.014 (3)	0.011 (3)	0.006 (2)	0.003 (3)
O2W	0.048 (4)	0.022 (3)	0.027 (3)	−0.006 (3)	0.005 (3)	−0.002 (2)
O3W	0.015 (3)	0.025 (3)	0.024 (3)	−0.004 (2)	0.004 (2)	−0.006 (2)
O4W	0.019 (3)	0.041 (4)	0.020 (3)	0.009 (3)	0.002 (2)	0.006 (3)
O5W	0.043 (4)	0.028 (3)	0.031 (4)	0.002 (3)	0.005 (3)	−0.005 (3)
O6W	0.041 (4)	0.016 (3)	0.016 (3)	−0.002 (3)	−0.012 (3)	0.003 (2)
O7W	0.024 (3)	0.030 (3)	0.013 (3)	0.003 (2)	0.003 (2)	0.001 (2)

Geometric parameters (Å, º) top

Sm3—O13	2.300 (5)	S3—O19	1.481 (5)
Sm3—O11	2.317 (5)	N1—C5	1.311 (9)
Sm3—O15	2.411 (4)	N1—C2	1.374 (8)
Sm3—O17	2.427 (5)	N2—C5	1.331 (8)
Sm3—O20ⁱ	2.431 (5)	N2—C3	1.375 (8)
Sm3—O6W	2.432 (5)	N2—H1	0.87 (2)
Sm3—O10	2.484 (4)	N3—C10	1.330 (8)
Sm3—O5W	2.631 (6)	N3—C7	1.384 (8)
Sm3—S3	3.2922 (19)	N4—C10	1.335 (8)
Sm2—O6	2.353 (5)	N4—C8	1.380 (8)
Sm2—O19ⁱ	2.404 (5)	N4—H2	0.86 (2)
Sm2—O3ⁱⁱ	2.408 (5)	C1—O9	1.262 (8)
Sm2—O4W	2.459 (5)	C1—O10	1.272 (7)
Sm2—O3W	2.465 (5)	C1—C2	1.471 (9)
Sm2—O10	2.527 (4)	C2—C3	1.368 (9)
Sm2—O16	2.535 (5)	C3—C4	1.486 (9)
Sm2—O9	2.630 (4)	C4—O11	1.243 (8)
Sm2—O15	2.636 (4)	C4—O12	1.252 (8)
Sm2—C9	2.939 (7)	C5—H5	0.9300
Sm2—C1	2.969 (6)	C6—O13	1.229 (8)
Sm1—O8ⁱⁱⁱ	2.327 (5)	C6—O14	1.268 (8)
Sm1—O2^iv	2.375 (5)	C6—C7	1.496 (9)
Sm1—O5	2.394 (5)	C7—C8	1.382 (9)
Sm1—O2W	2.457 (5)	C8—C9	1.467 (9)
Sm1—O1	2.502 (5)	C9—O16	1.255 (8)
Sm1—O1W	2.515 (5)	C9—O15	1.272 (8)
Sm1—N1	2.552 (6)	C10—H11	0.9300
Sm1—O9	2.553 (4)	O2—Sm1^iv	2.375 (5)
Sm1—O4	2.699 (5)	O3—Sm2ⁱⁱ	2.408 (5)
Sm1—S1	3.2011 (17)	O8—Sm1ⁱ	2.327 (5)
Co1—O14	2.048 (4)	O19—Sm2ⁱⁱⁱ	2.404 (5)
Co1—O14^v	2.048 (4)	O20—Sm3ⁱⁱⁱ	2.431 (5)
Co1—O7W	2.109 (5)	O1W—H1W	0.82 (2)
Co1—O7W^v	2.109 (5)	O1W—H2W	0.82 (2)
Co1—N3^v	2.146 (5)	O2W—H3W	0.83 (2)
Co1—N3	2.146 (5)	O2W—H4W	0.82 (2)
S1—O2	1.454 (5)	O3W—H5W	0.83 (2)
S1—O3	1.467 (5)	O3W—H6W	0.83 (2)
S1—O4	1.469 (5)	O4W—H7W	0.81 (2)
S1—O1	1.483 (5)	O4W—H8W	0.81 (2)
S2—O7	1.438 (5)	O5W—H9W	0.82 (2)
S2—O5	1.472 (5)	O5W—H10W	0.81 (2)
S2—O8	1.473 (5)	O6W—H11W	0.81 (2)
S2—O6	1.480 (5)	O6W—H12W	0.80 (2)
S3—O18	1.449 (6)	O7W—H13W	0.81 (2)
S3—O20	1.459 (5)	O7W—H14W	0.81 (2)
S3—O17	1.478 (6)

O13—Sm3—O11	139.58 (16)	O4—Sm1—S1	27.17 (11)
O13—Sm3—O15	74.54 (15)	O14—Co1—O14^v	180.000 (1)
O11—Sm3—O15	143.87 (16)	O14—Co1—O7W	88.2 (2)
O13—Sm3—O17	120.75 (19)	O14^v—Co1—O7W	91.8 (2)
O11—Sm3—O17	81.19 (19)	O14—Co1—O7W^v	91.8 (2)
O15—Sm3—O17	89.23 (17)	O14^v—Co1—O7W^v	88.2 (2)
O13—Sm3—O20ⁱ	85.31 (19)	O7W—Co1—O7W^v	180.000 (3)
O11—Sm3—O20ⁱ	93.60 (18)	O14—Co1—N3^v	101.16 (19)
O15—Sm3—O20ⁱ	74.62 (16)	O14^v—Co1—N3^v	78.84 (19)
O17—Sm3—O20ⁱ	144.84 (18)	O7W—Co1—N3^v	88.7 (2)
O13—Sm3—O6W	76.76 (17)	O7W^v—Co1—N3^v	91.3 (2)
O11—Sm3—O6W	77.13 (18)	O14—Co1—N3	78.84 (19)
O15—Sm3—O6W	133.98 (17)	O14^v—Co1—N3	101.16 (19)
O17—Sm3—O6W	75.58 (19)	O7W—Co1—N3	91.3 (2)
O20ⁱ—Sm3—O6W	137.37 (18)	O7W^v—Co1—N3	88.7 (2)
O13—Sm3—O10	141.54 (15)	N3^v—Co1—N3	180.000 (2)
O11—Sm3—O10	74.32 (16)	O2—S1—O3	109.0 (3)
O15—Sm3—O10	69.57 (15)	O2—S1—O4	111.9 (3)
O17—Sm3—O10	72.68 (17)	O3—S1—O4	111.1 (3)
O20ⁱ—Sm3—O10	72.44 (16)	O2—S1—O1	110.0 (3)
O6W—Sm3—O10	139.86 (17)	O3—S1—O1	108.9 (3)
O13—Sm3—O5W	69.51 (18)	O4—S1—O1	105.9 (3)
O11—Sm3—O5W	73.27 (18)	O2—S1—Sm1	120.5 (2)
O15—Sm3—O5W	127.62 (17)	O3—S1—Sm1	130.2 (2)
O17—Sm3—O5W	142.04 (19)	O4—S1—Sm1	57.0 (2)
O20ⁱ—Sm3—O5W	65.80 (18)	O1—S1—Sm1	49.36 (19)
O6W—Sm3—O5W	71.7 (2)	O7—S2—O5	110.8 (3)
O10—Sm3—O5W	124.27 (17)	O7—S2—O8	111.8 (3)
O13—Sm3—S3	96.29 (14)	O5—S2—O8	107.8 (3)
O11—Sm3—S3	101.50 (14)	O7—S2—O6	111.0 (4)
O15—Sm3—S3	80.81 (12)	O5—S2—O6	108.4 (3)
O17—Sm3—S3	24.47 (14)	O8—S2—O6	106.9 (3)
O20ⁱ—Sm3—S3	154.02 (12)	O18—S3—O20	112.5 (4)
O6W—Sm3—S3	67.43 (14)	O18—S3—O17	107.1 (4)
O10—Sm3—S3	91.30 (11)	O20—S3—O17	109.2 (3)
O5W—Sm3—S3	138.88 (14)	O18—S3—O19	109.7 (3)
O6—Sm2—O19ⁱ	77.78 (18)	O20—S3—O19	109.8 (3)
O6—Sm2—O3ⁱⁱ	73.35 (18)	O17—S3—O19	108.5 (3)
O19ⁱ—Sm2—O3ⁱⁱ	75.41 (16)	O18—S3—Sm3	64.5 (3)
O6—Sm2—O4W	134.97 (18)	O20—S3—Sm3	120.6 (2)
O19ⁱ—Sm2—O4W	139.39 (17)	O17—S3—Sm3	42.9 (2)
O3ⁱⁱ—Sm2—O4W	129.63 (17)	O19—S3—Sm3	127.5 (2)
O6—Sm2—O3W	90.2 (2)	C5—N1—C2	105.9 (6)
O19ⁱ—Sm2—O3W	148.19 (16)	C5—N1—Sm1	133.2 (4)
O3ⁱⁱ—Sm2—O3W	72.93 (16)	C2—N1—Sm1	120.6 (4)
O4W—Sm2—O3W	67.74 (17)	C5—N2—C3	107.9 (6)
O6—Sm2—O10	88.95 (18)	C5—N2—H1	120 (6)
O19ⁱ—Sm2—O10	81.35 (15)	C3—N2—H1	131 (6)
O3ⁱⁱ—Sm2—O10	153.19 (15)	C10—N3—C7	104.9 (6)
O4W—Sm2—O10	77.07 (17)	C10—N3—Co1	144.9 (5)
O3W—Sm2—O10	128.31 (15)	C7—N3—Co1	110.2 (4)
O6—Sm2—O16	140.10 (17)	C10—N4—C8	108.7 (5)
O19ⁱ—Sm2—O16	75.70 (17)	C10—N4—H2	123 (6)
O3ⁱⁱ—Sm2—O16	71.47 (17)	C8—N4—H2	126 (5)
O4W—Sm2—O16	83.19 (18)	O9—C1—O10	119.7 (6)
O3W—Sm2—O16	96.93 (16)	O9—C1—C2	117.5 (6)
O10—Sm2—O16	115.56 (14)	O10—C1—C2	122.9 (6)
O6—Sm2—O9	70.15 (16)	O9—C1—Sm2	62.2 (3)
O19ⁱ—Sm2—O9	120.47 (16)	O10—C1—Sm2	57.6 (3)
O3ⁱⁱ—Sm2—O9	134.74 (16)	C2—C1—Sm2	175.1 (5)
O4W—Sm2—O9	68.06 (17)	C3—C2—N1	109.4 (6)
O3W—Sm2—O9	81.28 (15)	C3—C2—C1	135.0 (6)
O10—Sm2—O9	50.23 (14)	N1—C2—C1	115.4 (6)
O16—Sm2—O9	149.71 (16)	C2—C3—N2	105.2 (6)
O6—Sm2—O15	140.23 (18)	C2—C3—C4	135.0 (6)
O19ⁱ—Sm2—O15	69.01 (16)	N2—C3—C4	119.8 (6)
O3ⁱⁱ—Sm2—O15	116.59 (15)	O11—C4—O12	124.0 (7)
O4W—Sm2—O15	70.80 (16)	O11—C4—C3	119.9 (6)
O3W—Sm2—O15	129.46 (16)	O12—C4—C3	116.1 (6)
O10—Sm2—O15	65.45 (14)	N1—C5—N2	111.6 (6)
O16—Sm2—O15	50.12 (14)	N1—C5—H5	124.2
O9—Sm2—O15	108.56 (14)	N2—C5—H5	124.2
O6—Sm2—C9	143.70 (19)	O13—C6—O14	123.2 (6)
O19ⁱ—Sm2—C9	66.30 (18)	O13—C6—C7	120.7 (6)
O3ⁱⁱ—Sm2—C9	92.08 (18)	O14—C6—C7	116.0 (6)
O4W—Sm2—C9	79.88 (19)	C8—C7—N3	110.4 (6)
O3W—Sm2—C9	117.63 (18)	C8—C7—C6	133.2 (6)
O10—Sm2—C9	90.65 (17)	N3—C7—C6	116.1 (6)
O16—Sm2—C9	25.15 (17)	N4—C8—C7	104.3 (5)
O9—Sm2—C9	133.08 (17)	N4—C8—C9	119.9 (6)
O15—Sm2—C9	25.64 (16)	C7—C8—C9	135.7 (6)
O6—Sm2—C1	77.54 (18)	O16—C9—O15	120.3 (6)
O19ⁱ—Sm2—C1	100.65 (17)	O16—C9—C8	117.9 (6)
O3ⁱⁱ—Sm2—C1	150.81 (18)	O15—C9—C8	121.6 (6)
O4W—Sm2—C1	71.87 (18)	O16—C9—Sm2	59.1 (3)
O3W—Sm2—C1	105.37 (17)	O15—C9—Sm2	63.8 (3)
O10—Sm2—C1	25.15 (15)	C8—C9—Sm2	159.8 (5)
O16—Sm2—C1	136.44 (17)	N3—C10—N4	111.7 (6)
O9—Sm2—C1	25.14 (15)	N3—C10—H11	124.2
O15—Sm2—C1	87.51 (16)	N4—C10—H11	124.2
C9—Sm2—C1	113.14 (19)	S1—O1—Sm1	103.9 (2)
O8ⁱⁱⁱ—Sm1—O2^iv	82.97 (18)	S1—O2—Sm1^iv	157.7 (3)
O8ⁱⁱⁱ—Sm1—O5	132.72 (18)	S1—O3—Sm2ⁱⁱ	151.1 (3)
O2^iv—Sm1—O5	143.93 (18)	S1—O4—Sm1	95.8 (2)
O8ⁱⁱⁱ—Sm1—O2W	74.9 (2)	S2—O5—Sm1	135.0 (3)
O2^iv—Sm1—O2W	134.42 (18)	S2—O6—Sm2	141.8 (3)
O5—Sm1—O2W	71.7 (2)	S2—O8—Sm1ⁱ	154.6 (3)
O8ⁱⁱⁱ—Sm1—O1	132.36 (16)	C1—O9—Sm1	123.4 (4)
O2^iv—Sm1—O1	84.65 (16)	C1—O9—Sm2	92.6 (4)
O5—Sm1—O1	74.15 (16)	Sm1—O9—Sm2	141.08 (19)
O2W—Sm1—O1	81.88 (18)	C1—O10—Sm3	141.3 (4)
O8ⁱⁱⁱ—Sm1—O1W	149.16 (18)	C1—O10—Sm2	97.2 (4)
O2^iv—Sm1—O1W	73.88 (18)	Sm3—O10—Sm2	112.87 (16)
O5—Sm1—O1W	70.95 (18)	C4—O11—Sm3	157.0 (5)
O2W—Sm1—O1W	135.9 (2)	C6—O13—Sm3	155.7 (5)
O1—Sm1—O1W	66.14 (16)	C6—O14—Co1	118.2 (4)
O8ⁱⁱⁱ—Sm1—N1	82.36 (18)	C9—O15—Sm3	152.2 (4)
O2^iv—Sm1—N1	72.20 (17)	C9—O15—Sm2	90.6 (4)
O5—Sm1—N1	103.37 (18)	Sm3—O15—Sm2	111.56 (17)
O2W—Sm1—N1	140.42 (19)	C9—O16—Sm2	95.7 (4)
O1—Sm1—N1	135.86 (17)	S3—O17—Sm3	112.7 (3)
O1W—Sm1—N1	71.45 (18)	S3—O19—Sm2ⁱⁱⁱ	142.2 (3)
O8ⁱⁱⁱ—Sm1—O9	73.54 (17)	S3—O20—Sm3ⁱⁱⁱ	146.5 (3)
O2^iv—Sm1—O9	130.86 (16)	Sm1—O1W—H1W	112 (6)
O5—Sm1—O9	68.57 (16)	Sm1—O1W—H2W	111 (6)
O2W—Sm1—O9	80.04 (17)	H1W—O1W—H2W	104 (3)
O1—Sm1—O9	142.05 (15)	Sm1—O2W—H3W	125 (5)
O1W—Sm1—O9	106.70 (16)	Sm1—O2W—H4W	133 (5)
N1—Sm1—O9	62.47 (16)	H3W—O2W—H4W	101 (7)
O8ⁱⁱⁱ—Sm1—O4	78.70 (16)	Sm2—O3W—H5W	118 (6)
O2^iv—Sm1—O4	72.14 (16)	Sm2—O3W—H6W	114 (5)
O5—Sm1—O4	114.36 (16)	H5W—O3W—H6W	102 (3)
O2W—Sm1—O4	64.80 (17)	Sm2—O4W—H7W	116 (6)
O1—Sm1—O4	53.73 (15)	Sm2—O4W—H8W	123 (6)
O1W—Sm1—O4	112.03 (16)	H7W—O4W—H8W	106 (7)
N1—Sm1—O4	141.24 (17)	Sm3—O5W—H9W	94 (6)
O9—Sm1—O4	139.76 (15)	Sm3—O5W—H10W	139 (7)
O8ⁱⁱⁱ—Sm1—S1	105.85 (13)	H9W—O5W—H10W	105 (8)
O2^iv—Sm1—S1	74.94 (12)	Sm3—O6W—H11W	120 (5)
O5—Sm1—S1	95.75 (12)	Sm3—O6W—H12W	129 (5)
O2W—Sm1—S1	73.64 (14)	H11W—O6W—H12W	107 (3)
O1—Sm1—S1	26.73 (11)	Co1—O7W—H13W	104 (6)
O1W—Sm1—S1	87.74 (12)	Co1—O7W—H14W	116 (6)
N1—Sm1—S1	144.82 (13)	H13W—O7W—H14W	105 (3)
O9—Sm1—S1	152.67 (11)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N2—H1···O18^vi	0.87 (6)	2.06 (5)	2.916 (8)	170 (6)
O1W—H1W···O7	0.82 (5)	2.52 (8)	3.140 (8)	133 (7)
O1W—H1W···O16^vi	0.82 (5)	2.12 (6)	2.777 (6)	136 (8)
N4—H2···O7^vii	0.87 (4)	1.94 (5)	2.803 (8)	171 (8)
O1W—H2W···O1^viii	0.82 (5)	2.51 (6)	3.247 (7)	150 (7)
O2W—H3W···O3W	0.83 (5)	2.02 (5)	2.809 (8)	160 (6)
O2W—H4W···O6ⁱⁱ	0.83 (4)	2.55 (4)	3.303 (9)	152 (8)
O2W—H4W···O8ⁱⁱ	0.83 (4)	2.53 (7)	3.204 (8)	140 (6)
O3W—H5W···O4^ix	0.83 (4)	1.98 (5)	2.789 (7)	166 (8)
O3W—H6W···O1ⁱⁱ	0.83 (5)	1.93 (5)	2.732 (7)	161 (5)
O4W—H7W···O17	0.81 (5)	2.59 (6)	3.270 (8)	142 (7)
O4W—H7W···O19	0.81 (5)	2.20 (6)	2.874 (7)	141 (5)
O4W—H8W···O6ⁱⁱⁱ	0.81 (7)	2.47 (7)	3.186 (8)	149 (6)
O5W—H10W···O7W^x	0.82 (6)	2.10 (6)	2.794 (8)	142 (6)
O6W—H11W···O14^xi	0.81 (4)	1.99 (5)	2.751 (7)	157 (5)
O6W—H12W···O5W^xi	0.81 (6)	2.27 (7)	3.053 (8)	162 (7)
O7W—H13W···O11^x	0.81 (5)	2.45 (5)	3.063 (6)	133 (7)
O7W—H13W···O12^x	0.81 (5)	2.06 (6)	2.855 (7)	168 (7)
O7W—H14W···O12^xii	0.81 (5)	1.85 (5)	2.661 (7)	174 (7)
C5—H5···O3^iv	0.93	2.52	3.388 (8)	155
C10—H11···O17^xii	0.93	2.54	3.430 (9)	161

Symmetry codes: (ii) −x, −y, −z+1; (iii) x+1, y, z; (iv) −x+1, −y+1, −z+1; (vi) x, y+1, z; (vii) x, y−1, z; (viii) −x, −y+1, −z+1; (ix) −x+1, −y, −z+1; (x) −x, −y, −z+2; (xi) −x+1, −y, −z+2; (xii) x−1, y−1, z.

Experimental details

Crystal data
Chemical formula	[CoSm₆(C₅H₂N₂O₄)₄(SO₄)₆(H₂O)₁₄]
M_r	2406.08
Crystal system, space group	Triclinic, P1
Temperature (K)	296
a, b, c (Å)	6.6395 (10), 9.5090 (14), 21.619 (3)
α, β, γ (°)	97.068 (2), 94.391 (2), 98.006 (2)
V (Å³)	1335.2 (3)
Z	1
Radiation type	Mo Kα
µ (mm⁻¹)	7.17
Crystal size (mm)	0.20 × 0.18 × 0.15

Data collection
Diffractometer	Bruker APEXII area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.260, 0.341
No. of measured, independent and observed [I > 2σ(I)] reflections	6967, 4716, 3971
R_int	0.024
(sin θ/λ)_max (Å⁻¹)	0.599

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.031, 0.070, 1.02
No. of reflections	4716
No. of parameters	478
No. of restraints	23
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	1.00, −1.03

Computer programs: APEX2 (Bruker, 2004), SAINT (Bruker, 2004), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), XP in SHELXTL (Sheldrick, 2008).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N2—H1···O18ⁱ	0.87 (6)	2.06 (5)	2.916 (8)	170 (6)
O1W—H1W···O7	0.82 (5)	2.52 (8)	3.140 (8)	133 (7)
O1W—H1W···O16ⁱ	0.82 (5)	2.12 (6)	2.777 (6)	136 (8)
N4—H2···O7ⁱⁱ	0.87 (4)	1.94 (5)	2.803 (8)	171 (8)
O1W—H2W···O1ⁱⁱⁱ	0.82 (5)	2.51 (6)	3.247 (7)	150 (7)
O2W—H3W···O3W	0.83 (5)	2.02 (5)	2.809 (8)	160 (6)
O2W—H4W···O6^iv	0.83 (4)	2.55 (4)	3.303 (9)	152 (8)
O2W—H4W···O8^iv	0.83 (4)	2.53 (7)	3.204 (8)	140 (6)
O3W—H5W···O4^v	0.83 (4)	1.98 (5)	2.789 (7)	166 (8)
O3W—H6W···O1^iv	0.83 (5)	1.93 (5)	2.732 (7)	161 (5)
O4W—H7W···O17	0.81 (5)	2.59 (6)	3.270 (8)	142 (7)
O4W—H7W···O19	0.81 (5)	2.20 (6)	2.874 (7)	141 (5)
O4W—H8W···O6^vi	0.81 (7)	2.47 (7)	3.186 (8)	149 (6)
O5W—H10W···O7W^vii	0.82 (6)	2.10 (6)	2.794 (8)	142 (6)
O6W—H11W···O14^viii	0.81 (4)	1.99 (5)	2.751 (7)	157 (5)
O6W—H12W···O5W^viii	0.81 (6)	2.27 (7)	3.053 (8)	162 (7)
O7W—H13W···O11^vii	0.81 (5)	2.45 (5)	3.063 (6)	133 (7)
O7W—H13W···O12^vii	0.81 (5)	2.06 (6)	2.855 (7)	168 (7)
O7W—H14W···O12^ix	0.81 (5)	1.85 (5)	2.661 (7)	174 (7)
C5—H5···O3^x	0.9300	2.5200	3.388 (8)	155.00
C10—H11···O17^ix	0.9300	2.5400	3.430 (9)	161.00

Symmetry codes: (i) x, y+1, z; (ii) x, y−1, z; (iii) −x, −y+1, −z+1; (iv) −x, −y, −z+1; (v) −x+1, −y, −z+1; (vi) x+1, y, z; (vii) −x, −y, −z+2; (viii) −x+1, −y, −z+2; (ix) x−1, y−1, z; (x) −x+1, −y+1, −z+1.

Acknowledgements

The authors acknowledge South China Normal University and South China University of Technology for supporting this work.

References

Bruker (2004). APEX2 and SAINT . Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Cheng, J.-W., Zhang, J., Zheng, S.-T., Zhang, M.-B. & Yang, G.-Y. (2006). Angew. Chem. Int. Ed. 45, 73–77. Web of Science CSD CrossRef CAS Google Scholar
Kuang, D.-Z., Feng, Y.-L., Peng, Y.-L. & Deng, Y.-F. (2007). Acta Cryst. E63, m2526–m2527. Web of Science CSD CrossRef IUCr Journals Google Scholar
Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Sun, Y.-Q. & Yang, G.-Y. (2007). Dalton Trans. pp. 3771–3781. Web of Science CSD CrossRef Google Scholar
Zhu, L.-C., Zhao, Y., Yu, S.-J. & Zhao, M.-M. (2010). Inorg. Chem. Commun. 13, 1299–1303. Web of Science CSD CrossRef CAS Google Scholar

This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.