catena-Poly[[diaqua­bis­(3-methyl­pyridine-κN)cobalt(II)]-μ-sulfato-κ2O:O′]

Alam, N.; Zeller, M.; Ahmad Tajidi, N.S.; Arifin, Z.; Mazhar, M.

doi:10.1107/S1600536811025815

metal-organic compounds

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ISSN: 2056-9890

Volume 67| Part 8| August 2011| Pages m1065-m1066

doi:10.1107/S1600536811025815

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catena-Poly[[diaquabis(3-methylpyridine-κN)cobalt(II)]-μ-sulfato-κ²O:O′]

Naveed Alam,^a Matthias Zeller,^b Nur Syamimi Ahmad Tajidi,^c Zainudin Arifin ^c ^* and Muhammad Mazhar ^c

^aDepartment of Chemistry, Quaid-I-Azam University, Islamabad 45320, Pakistan, ^bDepartment of Chemistry, Youngstown State University, 1 University Plaza, Youngstown, Ohio 44555, USA, and ^cDepartment of Chemistry, Faculty of Science, University of Malaya, Lembah Pantai, 50603 Kuala Lumpur, Malaysia
^*Correspondence e-mail: zainudin@um.edu.my

(Received 27 April 2011; accepted 30 June 2011; online 9 July 2011)

The environment of the Co^II ion in the title compound, [Co(SO₄)(C₆H₇N)₂(H₂O)₂]_n, exhibits an octahedral configuration with the two 3-methylpyridine ligands lying in cis positions with respect to each other and trans to the two coordinated water molecules. The axial positions are occupied by O atoms of the sulfate ions. Co and S atoms occupy special positions (twofold axis, Wyckoff position 4c). Neighboring Co^II ions are covalently connected with each other through the sulfate ions, thus creating infinite polymeric chains that run along the c axis. The water molecules are connected with neighboring sulfate ions through strong O—H⋯O hydrogen bonds. Intramolecular hydrogen bonds parallel to the propagation direction of the chains stabilize the polymeric chains, and intermolecular hydrogen bonds between chains connect neighboring chains with each other, thus leading to polymeric double chains.

Related literature

For the complexation of cobalt ions by sulfate, see: Das et al. (2009 ); Majumder et al. (2005 ); Masuhara et al. (2007 ); Zhong et al. (2006 ); Zhong et al. (2011 ); Dietz et al. (2009 ); Wu et al. (2008 ); Carlucci et al. (2003 ); Ali et al. (2005 ); Vreshch et al. (2003 ).

Experimental

Crystal data

[Co(SO₄)(C₆H₇N)₂(H₂O)₂]
M_r = 377.27
Orthorhombic, P b c n
a = 15.132 (2) Å
b = 16.687 (2) Å
c = 6.4503 (9) Å
V = 1628.7 (4) Å³
Z = 4
Mo Kα radiation
μ = 1.21 mm⁻¹
T = 100 K
0.60 × 0.12 × 0.12 mm

Data collection

Bruker SMART APEX CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2003 ) T_min = 0.786, T_max = 0.865
15656 measured reflections
2028 independent reflections
1892 reflections with I > 2σ(I)
R_int = 0.034

Refinement

R[F² > 2σ(F²)] = 0.027
wR(F²) = 0.075
S = 1.08
2028 reflections
108 parameters
2 restraints
H atoms treated by a mixture of independent and constrained refinement
Δρ_max = 0.57 e Å⁻³
Δρ_min = −0.32 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1—H1B⋯O3ⁱ	0.82 (2)	1.86 (2)	2.6652 (15)	166 (2)
O1—H1A⋯O3ⁱⁱ	0.84 (2)	1.92 (2)	2.7331 (14)	165 (2)
Symmetry codes: (i) $[-x+1, y, -z+{\script{1\over 2}}]$ ; (ii) -x+1, -y+1, -z+1.

Data collection: SMART (Bruker, 2002 ); cell refinement: SAINT-Plus (Bruker, 2003); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ); program(s) used to refine structure: SHELXTL; molecular graphics: Mercury (Macrae et al., 2008 ); software used to prepare material for publication: publCIF (Westrip, 2010 ).

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536811025815/fi2108sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536811025815/fi2108Isup2.hkl

checkCIF report

Comment top

Sulfate coordination to cobalt ions may be divided into three commonly reported modes: monodentate (Das et al.,2009, Majumder et al., 2005), bidentate (Masuhara et al.., 2007, Zhong et al.,2006, 2011) or bidentate-bridged metal to metal coordination (Dietz et al., 2009, Wu et al., 2008, Carlucci et al., 2003, Ali et al., 2005, Vreshch et al., 2003). The last mode of coordination is particularly common where the sulfate ion acts as a bridge that links two cobalt ions to form an extended polymeric structure. Further evidence for the different modes of sulfate coordination is reflected in the infra-red absorption spectrum due to the reduction in symmetry in sulfate coordination.

In the title compound, the cobalt(II) complex exhibits octahedral symmetry with the two 3-methylpyridine ligands lying in cis position with respect to each other, and trans to the two coordinated water molecules. The axial positions are occupied by oxygen atoms of the sulfate ions. Both Co and S occupy special positions (two-fold axis, Wyckoff position 4c). Neighboring cobalt ions are covalently connected with each other through the sulfate ions thus creating infinite polymeric chains that stretch parallel to the c axis direction. The water molecules are connected with neighboring sulfate ions through strong O—H···O hydrogen bonds. Intramolecular hydrogen bonds parallel to the propagation direction of the chains stabilize the polymeric chains, and intermolecular hydrogen bonds between chains connect neighboring strains with each other, thus leading to polymeric double chains.

Related literature top

For the complexation of cobalt ions by sulfate, see: Das et al. (2009); Majumder et al. (2005); Masuhara et al. (2007); Zhong et al. (2006); Zhong et al. (2011); Dietz et al. (2009); Wu et al. (2008); Carlucci et al. (2003); Ali et al. (2005); Vreshch et al. (2003).

Experimental top

Potassium O-n-butyl xanthate (1.00 g, 0.53 mmol) was dissolved in acetone (20 mL) and placed in a three-necked round bottom flask fitted with a reflux condenser, a magnetic stirrer and a vacuum line. Co(NO₃)₂.6H₂O (0.78 g, 2.70 mmol) was added directly into the reaction flask. The contents were stirred to dissolve the salt completely. About 30 ml of 3-methylpyridine was added and stirring was continued for another hour. Any insoluble matter was removed by filtration, and slow evaporation of the reaction mixture at room temperature yielded 60% of red needles of the title compound as the unexpected product. m.p. = 373 K. Elemental analysis: Found (Calc.) for C₁₂H₁₈N₂CoO₆S: C 38.64 (38.20); H 4.66 (4.80); N 7.51 (7.42).

Computing details top

Data collection: SMART (Bruker, 2002); cell refinement: SAINT-Plus (Bruker, 2003); data reduction: SAINT-Plus (Bruker, 2003); program(s) used to solve structure: SHELXTL (Sheldrick, 2008); program(s) used to refine structure: SHELXTL (Sheldrick, 2008); molecular graphics: Mercury (Macrae et al., 2008); software used to prepare material for publication: publCIF (Westrip, 2010).

Figures top

	Fig. 1. Thermal ellipsoid representation of the title compound with atom numbering scheme. Displacement elliposoids are at the 50% level, hydrogen atoms are shown as spheres of arbitrari radii. Symmetry operators: (i) -x + 1, y, -z + 1/2; (ii) -x + 1, y, -z + 3/2.
	Fig. 2. One of the infinite double chains formed by the title compound. View down the b-axis. O—H···O hydrogen bonds are symbolized as blue dashed lines.
	Fig. 3. Packing arrangement of the title compound. H atoms have been omitted for clarity.

catena-Poly[[diaquabis(3-methylpyridine-κN)cobalt(II)]- µ-sulfato-κ²O:O'] top

Crystal data top

[Co(SO₄)(C₆H₇N)₂(H₂O)₂]	D_x = 1.539 Mg m⁻³
M_r = 377.27	Melting point: 373 K
Orthorhombic, Pbcn	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2n 2ab	Cell parameters from 5623 reflections
a = 15.132 (2) Å	θ = 2.4–30.5°
b = 16.687 (2) Å	µ = 1.21 mm⁻¹
c = 6.4503 (9) Å	T = 100 K
V = 1628.7 (4) Å³	Needle, red
Z = 4	0.60 × 0.12 × 0.12 mm
F(000) = 780

Data collection top

Bruker SMART APEX CCD diffractometer	2028 independent reflections
Radiation source: fine-focus sealed tube	1892 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.034
ω scans	θ_max = 28.3°, θ_min = 1.8°
Absorption correction: multi-scan (SADABS in SAINT-Plus; Bruker, 2003)	h = −20→19
T_min = 0.786, T_max = 0.865	k = −22→22
15656 measured reflections	l = −8→8

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)] = 0.027	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.075	H atoms treated by a mixture of independent and constrained refinement
S = 1.08	w = 1/[σ²(F_o²) + (0.0404P)² + 0.7529P] where P = (F_o² + 2F_c²)/3
2028 reflections	(Δ/σ)_max = 0.001
108 parameters	Δρ_max = 0.57 e Å⁻³
2 restraints	Δρ_min = −0.32 e Å⁻³

Crystal data top

[Co(SO₄)(C₆H₇N)₂(H₂O)₂]	V = 1628.7 (4) Å³
M_r = 377.27	Z = 4
Orthorhombic, Pbcn	Mo Kα radiation
a = 15.132 (2) Å	µ = 1.21 mm⁻¹
b = 16.687 (2) Å	T = 100 K
c = 6.4503 (9) Å	0.60 × 0.12 × 0.12 mm

Data collection top

Bruker SMART APEX CCD diffractometer	2028 independent reflections
Absorption correction: multi-scan (SADABS in SAINT-Plus; Bruker, 2003)	1892 reflections with I > 2σ(I)
T_min = 0.786, T_max = 0.865	R_int = 0.034
15656 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.027	2 restraints
wR(F²) = 0.075	H atoms treated by a mixture of independent and constrained refinement
S = 1.08	Δρ_max = 0.57 e Å⁻³
2028 reflections	Δρ_min = −0.32 e Å⁻³
108 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
C1	0.59471 (10)	0.18494 (8)	0.0429 (2)	0.0210 (3)
H1	0.5466	0.1895	−0.0509	0.025*
C2	0.65854 (10)	0.12686 (8)	0.0035 (2)	0.0236 (3)
C3	0.72901 (10)	0.12145 (9)	0.1412 (3)	0.0250 (3)
H3	0.7745	0.0832	0.1193	0.030*
C4	0.73227 (10)	0.17218 (9)	0.3100 (3)	0.0268 (3)
H4	0.7800	0.1691	0.4054	0.032*
C5	0.66527 (9)	0.22760 (9)	0.3387 (2)	0.0224 (3)
H5	0.6675	0.2617	0.4564	0.027*
C6	0.65160 (13)	0.07315 (11)	−0.1835 (3)	0.0384 (4)
H6A	0.6325	0.0196	−0.1399	0.058*
H6B	0.7094	0.0694	−0.2513	0.058*
H6C	0.6084	0.0955	−0.2808	0.058*
Co1	0.5000	0.325574 (15)	0.2500	0.01344 (10)
N1	0.59730 (8)	0.23485 (7)	0.20607 (18)	0.0175 (2)
O1	0.59964 (7)	0.41307 (6)	0.21413 (16)	0.0177 (2)
H1A	0.5893 (14)	0.4584 (10)	0.263 (3)	0.027*
H1B	0.6013 (12)	0.4199 (11)	0.088 (2)	0.027*
O2	0.52369 (7)	0.32565 (5)	0.57274 (15)	0.0183 (2)
O3	0.42370 (6)	0.42849 (6)	0.69346 (15)	0.0181 (2)
S1	0.5000	0.37749 (3)	0.7500	0.01309 (12)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
C1	0.0248 (7)	0.0188 (6)	0.0192 (6)	0.0005 (5)	−0.0001 (5)	−0.0020 (5)
C2	0.0287 (7)	0.0185 (6)	0.0234 (7)	0.0004 (5)	0.0057 (6)	−0.0018 (5)
C3	0.0221 (7)	0.0199 (7)	0.0329 (8)	0.0042 (5)	0.0066 (6)	0.0021 (6)
C4	0.0212 (7)	0.0271 (8)	0.0320 (8)	0.0017 (6)	−0.0033 (6)	0.0009 (6)
C5	0.0222 (7)	0.0236 (7)	0.0215 (7)	−0.0002 (5)	−0.0025 (5)	−0.0027 (5)
C6	0.0487 (10)	0.0320 (9)	0.0346 (9)	0.0125 (8)	0.0008 (8)	−0.0145 (8)
Co1	0.01657 (15)	0.01387 (15)	0.00988 (14)	0.000	0.00000 (8)	0.000
N1	0.0185 (6)	0.0168 (5)	0.0173 (5)	0.0001 (4)	0.0008 (4)	−0.0007 (4)
O1	0.0224 (5)	0.0159 (5)	0.0148 (5)	−0.0010 (4)	−0.0002 (4)	−0.0017 (4)
O2	0.0258 (5)	0.0187 (5)	0.0105 (5)	0.0047 (4)	0.0004 (4)	−0.0012 (3)
O3	0.0200 (5)	0.0184 (5)	0.0159 (4)	0.0032 (4)	−0.0009 (4)	−0.0012 (4)
S1	0.0168 (2)	0.0135 (2)	0.0090 (2)	0.000	0.00065 (14)	0.000

Geometric parameters (Å, º) top

C1—N1	1.3427 (18)	C6—H6C	0.9800
C1—C2	1.392 (2)	Co1—O1	2.1115 (10)
C1—H1	0.9500	Co1—O1ⁱ	2.1115 (10)
C2—C3	1.391 (2)	Co1—O2ⁱ	2.1124 (10)
C2—C6	1.506 (2)	Co1—O2	2.1124 (10)
C3—C4	1.380 (2)	Co1—N1	2.1308 (12)
C3—H3	0.9500	Co1—N1ⁱ	2.1308 (12)
C4—C5	1.385 (2)	O1—H1A	0.835 (15)
C4—H4	0.9500	O1—H1B	0.820 (15)
C5—N1	1.3431 (19)	O2—S1	1.4779 (10)
C5—H5	0.9500	O3—S1	1.4799 (10)
C6—H6A	0.9800	S1—O2ⁱⁱ	1.4779 (10)
C6—H6B	0.9800	S1—O3ⁱⁱ	1.4799 (10)

N1—C1—C2	123.71 (14)	O1ⁱ—Co1—O2	90.73 (4)
N1—C1—H1	118.1	O2ⁱ—Co1—O2	179.93 (5)
C2—C1—H1	118.1	O1—Co1—N1	89.05 (5)
C3—C2—C1	117.41 (13)	O1ⁱ—Co1—N1	177.82 (4)
C3—C2—C6	121.76 (14)	O2ⁱ—Co1—N1	89.23 (4)
C1—C2—C6	120.82 (14)	O2—Co1—N1	90.82 (4)
C4—C3—C2	119.45 (13)	O1—Co1—N1ⁱ	177.82 (4)
C4—C3—H3	120.3	O1ⁱ—Co1—N1ⁱ	89.05 (5)
C2—C3—H3	120.3	O2ⁱ—Co1—N1ⁱ	90.82 (4)
C3—C4—C5	119.27 (15)	O2—Co1—N1ⁱ	89.23 (4)
C3—C4—H4	120.4	N1—Co1—N1ⁱ	89.44 (6)
C5—C4—H4	120.4	C1—N1—C5	117.75 (12)
N1—C5—C4	122.40 (14)	C1—N1—Co1	121.65 (10)
N1—C5—H5	118.8	C5—N1—Co1	120.56 (9)
C4—C5—H5	118.8	Co1—O1—H1A	116.7 (15)
C2—C6—H6A	109.5	Co1—O1—H1B	103.1 (13)
C2—C6—H6B	109.5	H1A—O1—H1B	104.9 (17)
H6A—C6—H6B	109.5	S1—O2—Co1	136.19 (6)
C2—C6—H6C	109.5	O2—S1—O2ⁱⁱ	108.35 (8)
H6A—C6—H6C	109.5	O2—S1—O3ⁱⁱ	109.76 (6)
H6B—C6—H6C	109.5	O2ⁱⁱ—S1—O3ⁱⁱ	109.58 (5)
O1—Co1—O1ⁱ	92.51 (6)	O2—S1—O3	109.58 (5)
O1—Co1—O2ⁱ	90.73 (4)	O2ⁱⁱ—S1—O3	109.76 (6)
O1ⁱ—Co1—O2ⁱ	89.22 (4)	O3ⁱⁱ—S1—O3	109.79 (8)
O1—Co1—O2	89.22 (4)

N1—C1—C2—C3	−0.6 (2)	N1ⁱ—Co1—N1—C1	65.61 (10)
N1—C1—C2—C6	−179.69 (15)	O1—Co1—N1—C5	61.84 (11)
C1—C2—C3—C4	0.8 (2)	O2ⁱ—Co1—N1—C5	152.59 (11)
C6—C2—C3—C4	179.90 (15)	O2—Co1—N1—C5	−27.36 (11)
C2—C3—C4—C5	−0.1 (2)	N1ⁱ—Co1—N1—C5	−116.59 (12)
C3—C4—C5—N1	−1.0 (2)	O1—Co1—O2—S1	78.59 (9)
C2—C1—N1—C5	−0.4 (2)	O1ⁱ—Co1—O2—S1	−13.91 (9)
C2—C1—N1—Co1	177.45 (11)	N1—Co1—O2—S1	167.62 (9)
C4—C5—N1—C1	1.2 (2)	N1ⁱ—Co1—O2—S1	−102.95 (10)
C4—C5—N1—Co1	−176.65 (11)	Co1—O2—S1—O2ⁱⁱ	138.72 (11)
O1—Co1—N1—C1	−115.96 (11)	Co1—O2—S1—O3ⁱⁱ	−101.66 (9)
O2ⁱ—Co1—N1—C1	−25.22 (11)	Co1—O2—S1—O3	18.98 (11)
O2—Co1—N1—C1	154.83 (11)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1B···O3ⁱ	0.82 (2)	1.86 (2)	2.6652 (15)	166 (2)
O1—H1A···O3ⁱⁱⁱ	0.84 (2)	1.92 (2)	2.7331 (14)	165 (2)

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

Experimental details

Crystal data
Chemical formula	[Co(SO₄)(C₆H₇N)₂(H₂O)₂]
M_r	377.27
Crystal system, space group	Orthorhombic, Pbcn
Temperature (K)	100
a, b, c (Å)	15.132 (2), 16.687 (2), 6.4503 (9)
V (Å³)	1628.7 (4)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	1.21
Crystal size (mm)	0.60 × 0.12 × 0.12

Data collection
Diffractometer	Bruker SMART APEX CCD diffractometer
Absorption correction	Multi-scan (SADABS in SAINT-Plus; Bruker, 2003)
T_min, T_max	0.786, 0.865
No. of measured, independent and observed [I > 2σ(I)] reflections	15656, 2028, 1892
R_int	0.034
(sin θ/λ)_max (Å⁻¹)	0.666

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.027, 0.075, 1.08
No. of reflections	2028
No. of parameters	108
No. of restraints	2
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.57, −0.32

Computer programs: SMART (Bruker, 2002), SAINT-Plus (Bruker, 2003), SHELXTL (Sheldrick, 2008), Mercury (Macrae et al., 2008), publCIF (Westrip, 2010).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1B···O3ⁱ	0.820 (15)	1.862 (15)	2.6652 (15)	166.0 (18)
O1—H1A···O3ⁱⁱ	0.835 (15)	1.918 (16)	2.7331 (14)	164.8 (18)

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

Acknowledgements

This project was financed by the University of Malaya, UMRG grant: RG097/10AET. The X-ray diffractometer was funded by NSF Grant 0087210, Ohio Board of Regents Grant CAP-491, and Youngstown State University.

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