Poly[tris­(μ3-2-amino­ethane­sulfonato)­cobalt(II)potassium]

Li, X.; Yu, J.; Ou, Y.-M.

doi:10.1107/S1600536811039390

metal-organic compounds

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Volume 67| Part 10| October 2011| Pages m1466-m1467

https://doi.org/10.1107/S1600536811039390

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Poly[tris(μ₃-2-aminoethanesulfonato)cobalt(II)potassium]

Xiao-lin Li,^a ^* Jing Yu ^a and Yang-Miao Ou ^b

^aPhysics and Chemistry Department, Jiangxi College of Traditional Chinese Medicine, Fuzhou, Jiangxi 344000, People's Republic of China, and ^bDepartment of Chemistry and Life Science, Hechi University, Yizhou, Guangxi 546300, People's Republic of China
^*Correspondence e-mail: caizhou2006@126.com

(Received 18 September 2011; accepted 26 September 2011; online 30 September 2011)

The title compound, [CoK(C₂H₆NO₃S)₃]_n, is isotypic with its Ni^II analogue. The Co^II atom is chelated by the three taurinate ligands in a distorted octahedral geometry and in a facial manner. Each taurinate ligand bridges two K⁺ ions via its sulfonate group, forming a three-dimensional framework. Weak N—H⋯O hydrogen bonding is observed in the crystal structure.

Related literature

For the isotypic Ni^II structure, see: Jiang et al. (2005 ). For the applications of taurine in medicine and biochemistry, see: Bottari & Festa (1998 ); Jiang et al. (2003 ). For general background to taurine complexes and their derivatives, see: Zhang & Jiang (2002 ); Zhong et al. (2003 ); Cai et al. (2004 , 2006 , 2011 ); Yang et al. (2010a ,b ). For S–O(–Co) bond lengths in bridging sulfonate groups, see: Zeng et al. (2009 ); Yang et al. (2010b).

Experimental

Crystal data

[CoK(C₂H₆NO₃S)₃]
M_r = 470.44
Orthorhombic, P n a 2₁
a = 10.6901 (19) Å
b = 15.669 (3) Å
c = 9.6094 (17) Å
V = 1609.6 (5) Å³
Z = 4
Mo Kα radiation
μ = 1.76 mm⁻¹
T = 296 K
0.26 × 0.22 × 0.14 mm

Data collection

Bruker SMART CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 1999 ) T_min = 0.657, T_max = 0.791
10792 measured reflections
3386 independent reflections
3146 reflections with I > 2σ(I)
R_int = 0.027

Refinement

R[F² > 2σ(F²)] = 0.024
wR(F²) = 0.058
S = 1.02
3386 reflections
208 parameters
1 restraint
H-atom parameters constrained
Δρ_max = 0.22 e Å⁻³
Δρ_min = −0.33 e Å⁻³
Absolute structure: Flack (1983 ), 1528 Friedel pairs
Flack parameter: 0.020 (13)

Table 1
Selected bond lengths (Å)

Co1—O1	2.1316 (18)
Co1—O7	2.1411 (18)
Co1—O4	2.142 (2)
Co1—N2	2.143 (2)
Co1—N3	2.146 (2)
Co1—N1	2.149 (2)
K1—O6ⁱ	2.687 (2)
K1—O3ⁱⁱ	2.7140 (19)
K1—O5ⁱⁱⁱ	2.8361 (19)
K1—O2^iv	2.8522 (19)
K1—O8^v	2.8893 (19)
K1—O9	2.816 (2)
Symmetry codes: (i) x, y, z-1; (ii) $[-x-{\script{1\over 2}}, y-{\script{1\over 2}}, z-{\script{1\over 2}}]$ ; (iii) $[x-{\script{1\over 2}}, -y+{\script{3\over 2}}, z-1]$ ; (iv) $[x-{\script{1\over 2}}, -y+{\script{3\over 2}}, z]$ ; (v) $[-x, -y+1, z-{\script{1\over 2}}]$ .

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N3—H3B⋯O7^vi	0.90	2.22	3.097 (3)	163
N2—H2B⋯O4^vi	0.90	2.40	3.166 (3)	143
N2—H2B⋯O1^vi	0.90	2.47	3.255 (3)	146
N1—H1D⋯O4^vi	0.90	2.55	3.423 (3)	165
N3—H3A⋯O2	0.90	2.28	3.113 (3)	153
N2—H2A⋯O8	0.90	2.39	3.219 (3)	152
N1—H1C⋯O5	0.90	2.49	3.229 (3)	140
Symmetry code: (vi) $[x+{\script{1\over 2}}, -y+{\script{3\over 2}}, z]$ .

Data collection: SMART (Bruker, 1999); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT; 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: SHELXTL.

Supporting information

Crystal structure: contains datablocks I, global. DOI: https://doi.org/10.1107/S1600536811039390/bx2374sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536811039390/bx2374Isup2.hkl

checkCIF report

Comment top

Taurine, an amino acid containing sulfur, is indispensable to human beings Because of its applications in medicine and biochemistry (Bottari & Festa,1998; Jiang et al.,2003). Several taurine complexes and their derivatives have recently been prepared (Zhong et al. (2003); Cai et al. (2004, 2006, 2011); Yang et al. (2010a,b)). we found that the taurine has manifold coordination modes. For the much less well study of the coordination modes of the sulfonate group, The title polymeric Co^II complex,(I), has been prepared and its structure determined.

The coordinated modes of the title compound are similar to the previously reported Ni (II) structure (Jiang et al. (2005)). The molecular structure of (I) is shown in Fig. 1 and the important bond lengths are listed in Table 1. The asymmetric unit of (I) consists of one Co^II atom, three taurinate ligands and one K⁺ ion. The cobalt is six-coordinate with three nitrogen atoms [N(1), N(2), N(3)] and three oxygen atoms [O(1), O(4), O(7)], thus giving an octahedral configuration. The Co atom forms six membered chelate rings (NiNC₂SO) with each taurinate ligand. This is a facial isomer. Each sulfonate group of the taurinate ligand takes part in the formation of a hydrogen bond (Table 2) with the amino group of a neighbouring ligand in the complex. The most common coordination modes of the sulfonate group are monodentate and µ₂-bridging, while µ₃-bridging is very rare. The coordination mode of the sulfonate group in (I) is µ₃-bridging, which makes the S–O(–Co) bonds [1.475 (2)–1.479 (2) Å] much longer than those previously reported [S–O(–Co) 1.464 (2) and 1.456 (3) Å; Yang et al., 2010b; Zeng et al., 2009]. The S=O(···K) bonds [1.443 (2)–1.453 (2) Å] are slightly longer than the uncoordinated S=O bond in taurine [1.446 (12)–1.457 (13) Å; Zhang & Jiang, 2002]. The K atom is surrounded by six O atoms from different taurinate ligands, The title complex forms a three-dimensional structure through the K···O linkage. The K···O distances are in the range 2.678 (2)–2.889 (2) Å, suggesting weak electrostatic interactions.

Related literature top

For the isotypic Ni^II structure, see: Jiang et al. (2005). For the applications of taurine in medicine and biochemistry, see: Bottari & Festa (1998); Jiang et al. (2003). For general background to taurine complexes and their derivatives, see: Zhang & Jiang (2002); Zhong et al. (2003); Cai et al. (2004, 2006, 2011); Yang et al. (2010a,b). For S–O(–Co) bond lengths in bridging sulfonate groups, see: Zeng et al. (2009); Yang et al. (2010b).

Experimental top

A mixture of Co(CH₃COO)₂.7H₂O (0.5 mmol, 152 mg), taurine (1.5 mmol 187 mg), KOH (1.5 mmol, 84 mg) and anhydrous methanol (15.0 ml) was placed in a Teflon-lined stainless steel vessel, and heated directly to 120 °C. After keeping at 120 °C for 4 days, it was cooled to room temperature at a rate for 10 °C/h. block red crystals of the complex were obtained.

Structure description top

For the isotypic Ni^II structure, see: Jiang et al. (2005). For the applications of taurine in medicine and biochemistry, see: Bottari & Festa (1998); Jiang et al. (2003). For general background to taurine complexes and their derivatives, see: Zhang & Jiang (2002); Zhong et al. (2003); Cai et al. (2004, 2006, 2011); Yang et al. (2010a,b). For S–O(–Co) bond lengths in bridging sulfonate groups, see: Zeng et al. (2009); Yang et al. (2010b).

Computing details top

Data collection: SMART (Bruker, 1999); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT (Bruker, 1999); 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: SHELXTL (Sheldrick, 2008).

Figures top

	Fig. 1. Molecular structure of the title compound.H atoms have been omitted for clarity. [Symmetry code: (i) x, y, z - 1; (ii) -x - 1/2, y - 1/2, z - 1/2; (iii) x - 1/2, -y + 3/2, z - 1; (iv) x - 1/2, -y + 3/2, z; (v) -x, -y + 1, z - 1/2.]
	Fig. 2. View of a three-dimensional supramolecular structure.

Poly[tris(µ₃-2-aminoethanesulfonato)cobalt(II)potassium] top

Crystal data top

[CoK(C₂H₆NO₃S)₃]	F(000) = 964
M_r = 470.44	D_x = 1.941 Mg m⁻³
Orthorhombic, Pna2₁	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2c -2n	Cell parameters from 7233 reflections
a = 10.6901 (19) Å	θ = 2.5–28.1°
b = 15.669 (3) Å	µ = 1.76 mm⁻¹
c = 9.6094 (17) Å	T = 296 K
V = 1609.6 (5) Å³	Block, red
Z = 4	0.26 × 0.22 × 0.14 mm

Data collection top

Bruker SMART CCD area-detector diffractometer	3386 independent reflections
Radiation source: fine-focus sealed tube	3146 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.027
φ and ω scans	θ_max = 27.0°, θ_min = 2.3°
Absorption correction: multi-scan (SADABS; Bruker, 1999)	h = −13→13
T_min = 0.657, T_max = 0.791	k = −20→20
10792 measured reflections	l = −11→12

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)] = 0.024	H-atom parameters constrained
wR(F²) = 0.058	w = 1/[σ²(F_o²) + (0.0303P)²] where P = (F_o² + 2F_c²)/3
S = 1.02	(Δ/σ)_max = 0.001
3386 reflections	Δρ_max = 0.22 e Å⁻³
208 parameters	Δρ_min = −0.33 e Å⁻³
1 restraint	Absolute structure: Flack (1983), 1528 Friedel pairs
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.020 (13)

Crystal data top

[CoK(C₂H₆NO₃S)₃]	V = 1609.6 (5) Å³
M_r = 470.44	Z = 4
Orthorhombic, Pna2₁	Mo Kα radiation
a = 10.6901 (19) Å	µ = 1.76 mm⁻¹
b = 15.669 (3) Å	T = 296 K
c = 9.6094 (17) Å	0.26 × 0.22 × 0.14 mm

Data collection top

Bruker SMART CCD area-detector diffractometer	3386 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 1999)	3146 reflections with I > 2σ(I)
T_min = 0.657, T_max = 0.791	R_int = 0.027
10792 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.024	H-atom parameters constrained
wR(F²) = 0.058	Δρ_max = 0.22 e Å⁻³
S = 1.02	Δρ_min = −0.33 e Å⁻³
3386 reflections	Absolute structure: Flack (1983), 1528 Friedel pairs
208 parameters	Absolute structure parameter: 0.020 (13)
1 restraint

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
Co1	0.11671 (3)	0.758726 (19)	0.15941 (5)	0.02649 (9)
S1	0.02451 (5)	0.93821 (4)	0.02671 (7)	0.02606 (14)
S2	0.01351 (6)	0.72499 (4)	0.46938 (7)	0.02860 (14)
S3	0.02648 (6)	0.60549 (4)	−0.04504 (7)	0.02819 (14)
O1	−0.00760 (15)	0.85153 (11)	0.0747 (2)	0.0323 (4)
O4	−0.01485 (17)	0.75606 (12)	0.3275 (2)	0.0354 (5)
C1	0.1093 (2)	0.98601 (17)	0.1650 (4)	0.0370 (6)
H1A	0.1248	1.0453	0.1416	0.044*
H1B	0.0575	0.9852	0.2479	0.044*
O7	−0.00597 (15)	0.66745 (11)	0.0653 (2)	0.0341 (4)
N3	0.2342 (2)	0.76329 (15)	−0.0215 (3)	0.0352 (5)
H3A	0.2121	0.8104	−0.0691	0.042*
H3B	0.3127	0.7721	0.0091	0.042*
O9	−0.08429 (17)	0.57634 (13)	−0.1176 (2)	0.0405 (5)
O6	−0.10014 (17)	0.70601 (14)	0.5464 (2)	0.0435 (5)
O5	0.09764 (18)	0.78116 (13)	0.5428 (2)	0.0410 (5)
N2	0.2285 (2)	0.65745 (15)	0.2430 (3)	0.0353 (5)
H2A	0.2123	0.6108	0.1915	0.042*
H2B	0.3089	0.6714	0.2269	0.042*
N1	0.2190 (2)	0.85854 (15)	0.2622 (3)	0.0406 (6)
H1C	0.1828	0.8664	0.3458	0.049*
H1D	0.2964	0.8383	0.2785	0.049*
O2	0.10597 (16)	0.93593 (13)	−0.0947 (2)	0.0335 (4)
O3	−0.08694 (16)	0.98967 (12)	0.0079 (2)	0.0372 (5)
O8	0.10532 (17)	0.53775 (12)	0.0077 (2)	0.0400 (5)
C2	0.2341 (2)	0.94364 (17)	0.1992 (3)	0.0358 (7)
H2C	0.2828	0.9383	0.1144	0.043*
H2D	0.2803	0.9799	0.2628	0.043*
C4	0.2203 (3)	0.6309 (2)	0.3918 (3)	0.0405 (7)
H4A	0.2601	0.5756	0.4027	0.049*
H4B	0.2658	0.6716	0.4486	0.049*
C5	0.2410 (2)	0.69305 (19)	−0.1240 (3)	0.0388 (7)
H5A	0.2858	0.6455	−0.0830	0.047*
H5B	0.2882	0.7122	−0.2044	0.047*
C6	0.1144 (3)	0.6630 (2)	−0.1711 (3)	0.0400 (7)
H6A	0.1253	0.6269	−0.2522	0.048*
H6B	0.0660	0.7123	−0.1998	0.048*
C3	0.0887 (3)	0.62542 (17)	0.4424 (3)	0.0391 (7)
H3C	0.0881	0.5940	0.5294	0.047*
H3D	0.0403	0.5929	0.3755	0.047*
K1	−0.25179 (5)	0.58729 (4)	−0.34300 (7)	0.03377 (13)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Co1	0.02482 (16)	0.02763 (16)	0.02701 (17)	−0.00158 (13)	−0.00214 (15)	0.00258 (18)
S1	0.0264 (3)	0.0271 (3)	0.0247 (3)	0.0020 (2)	0.0012 (3)	0.0002 (3)
S2	0.0305 (3)	0.0299 (3)	0.0255 (3)	−0.0029 (3)	−0.0005 (3)	0.0035 (3)
S3	0.0263 (3)	0.0273 (3)	0.0310 (3)	−0.0002 (2)	−0.0040 (3)	−0.0012 (3)
O1	0.0275 (9)	0.0322 (9)	0.0373 (11)	−0.0025 (8)	−0.0026 (8)	0.0060 (9)
O4	0.0347 (10)	0.0446 (12)	0.0269 (10)	0.0049 (9)	−0.0010 (8)	0.0091 (9)
C1	0.0433 (14)	0.0354 (13)	0.0324 (15)	0.0022 (12)	−0.0045 (13)	−0.0100 (16)
O7	0.0277 (9)	0.0327 (10)	0.0419 (12)	−0.0020 (8)	0.0015 (8)	−0.0095 (9)
N3	0.0294 (11)	0.0359 (12)	0.0403 (14)	−0.0045 (9)	0.0053 (10)	0.0031 (11)
O9	0.0356 (11)	0.0411 (11)	0.0448 (13)	−0.0029 (9)	−0.0125 (9)	−0.0060 (10)
O6	0.0357 (10)	0.0525 (13)	0.0424 (12)	−0.0065 (9)	0.0102 (9)	0.0090 (11)
O5	0.0464 (11)	0.0388 (11)	0.0378 (12)	−0.0084 (9)	−0.0056 (9)	−0.0048 (10)
N2	0.0315 (12)	0.0382 (13)	0.0362 (15)	0.0055 (10)	−0.0006 (10)	0.0017 (11)
N1	0.0420 (13)	0.0383 (13)	0.0416 (14)	−0.0097 (11)	−0.0125 (11)	0.0057 (12)
O2	0.0372 (10)	0.0369 (11)	0.0262 (10)	0.0008 (8)	0.0059 (8)	0.0018 (8)
O3	0.0343 (10)	0.0384 (11)	0.0388 (12)	0.0092 (8)	0.0005 (8)	0.0011 (9)
O8	0.0388 (11)	0.0319 (10)	0.0492 (14)	0.0076 (8)	−0.0064 (9)	0.0028 (10)
C2	0.0349 (15)	0.0383 (15)	0.0343 (16)	−0.0077 (12)	−0.0045 (11)	−0.0006 (12)
C4	0.0419 (16)	0.0382 (16)	0.0414 (18)	0.0080 (13)	−0.0072 (13)	0.0039 (13)
C5	0.0349 (15)	0.0422 (17)	0.0395 (17)	0.0007 (13)	0.0072 (12)	0.0031 (14)
C6	0.0484 (17)	0.0439 (17)	0.0277 (16)	−0.0019 (14)	−0.0015 (12)	−0.0001 (13)
C3	0.0534 (18)	0.0281 (14)	0.0357 (17)	0.0001 (12)	−0.0019 (14)	0.0061 (13)
K1	0.0351 (3)	0.0354 (3)	0.0309 (3)	−0.0048 (2)	−0.0014 (3)	0.0009 (3)

Geometric parameters (Å, º) top

Co1—O1	2.1316 (18)	N2—C4	1.492 (4)
Co1—O7	2.1411 (18)	N2—H2A	0.9000
Co1—O4	2.142 (2)	N2—H2B	0.9000
Co1—N2	2.143 (2)	N1—C2	1.473 (4)
Co1—N3	2.146 (2)	N1—H1C	0.9000
Co1—N1	2.149 (2)	N1—H1D	0.9000
S1—O3	1.4500 (18)	O2—K1ⁱⁱⁱ	2.8522 (19)
S1—O2	1.4567 (19)	O3—K1^iv	2.7140 (19)
S1—O1	1.4748 (18)	O8—K1^v	2.8893 (19)
S1—C1	1.775 (3)	C2—H2C	0.9700
S2—O5	1.443 (2)	C2—H2D	0.9700
S2—O6	1.4533 (19)	C4—C3	1.491 (4)
S2—O4	1.479 (2)	C4—H4A	0.9700
S2—C3	1.774 (3)	C4—H4B	0.9700
S3—O8	1.4472 (19)	C5—C6	1.503 (4)
S3—O9	1.4482 (19)	C5—H5A	0.9700
S3—O7	1.479 (2)	C5—H5B	0.9700
S3—C6	1.778 (3)	C6—H6A	0.9700
C1—C2	1.525 (4)	C6—H6B	0.9700
C1—H1A	0.9700	C3—H3C	0.9700
C1—H1B	0.9700	C3—H3D	0.9700
N3—C5	1.479 (4)	K1—O6^vi	2.687 (2)
N3—H3A	0.9000	K1—O3^vii	2.7140 (19)
N3—H3B	0.9000	K1—O5^viii	2.8361 (19)
O9—K1	2.816 (2)	K1—O2^ix	2.8522 (19)
O6—K1ⁱ	2.687 (2)	K1—O8^x	2.8893 (19)
O5—K1ⁱⁱ	2.8361 (19)	K1—O9	2.816 (2)

O1—Co1—O7	84.97 (7)	H2A—N2—H2B	106.6
O1—Co1—O4	83.80 (7)	C2—N1—Co1	121.71 (18)
O7—Co1—O4	84.46 (7)	C2—N1—H1C	106.9
O1—Co1—N2	174.95 (8)	Co1—N1—H1C	106.9
O7—Co1—N2	90.31 (8)	C2—N1—H1D	106.9
O4—Co1—N2	93.97 (8)	Co1—N1—H1D	106.9
O1—Co1—N3	91.86 (9)	H1C—N1—H1D	106.7
O7—Co1—N3	92.19 (8)	S1—O2—K1ⁱⁱⁱ	172.74 (12)
O4—Co1—N3	174.73 (8)	S1—O3—K1^iv	140.30 (12)
N2—Co1—N3	90.11 (9)	S3—O8—K1^v	170.75 (13)
O1—Co1—N1	89.78 (8)	N1—C2—C1	112.7 (2)
O7—Co1—N1	172.81 (8)	N1—C2—H2C	109.0
O4—Co1—N1	90.10 (9)	C1—C2—H2C	109.0
N2—Co1—N1	94.76 (10)	N1—C2—H2D	109.0
N3—Co1—N1	92.89 (9)	C1—C2—H2D	109.0
O3—S1—O2	113.88 (12)	H2C—C2—H2D	107.8
O3—S1—O1	111.10 (11)	C3—C4—N2	112.6 (2)
O2—S1—O1	111.52 (12)	C3—C4—H4A	109.1
O3—S1—C1	106.18 (12)	N2—C4—H4A	109.1
O2—S1—C1	107.75 (13)	C3—C4—H4B	109.1
O1—S1—C1	105.88 (13)	N2—C4—H4B	109.1
O5—S2—O6	113.38 (13)	H4A—C4—H4B	107.8
O5—S2—O4	112.20 (13)	N3—C5—C6	112.9 (2)
O6—S2—O4	111.44 (12)	N3—C5—H5A	109.0
O5—S2—C3	108.98 (13)	C6—C5—H5A	109.0
O6—S2—C3	105.87 (13)	N3—C5—H5B	109.0
O4—S2—C3	104.34 (14)	C6—C5—H5B	109.0
O8—S3—O9	114.43 (12)	H5A—C5—H5B	107.8
O8—S3—O7	111.54 (13)	C5—C6—S3	115.5 (2)
O9—S3—O7	111.12 (12)	C5—C6—H6A	108.4
O8—S3—C6	107.61 (13)	S3—C6—H6A	108.4
O9—S3—C6	105.31 (14)	C5—C6—H6B	108.4
O7—S3—C6	106.24 (13)	S3—C6—H6B	108.4
S1—O1—Co1	127.05 (10)	H6A—C6—H6B	107.5
S2—O4—Co1	124.53 (11)	C4—C3—S2	115.1 (2)
C2—C1—S1	115.1 (2)	C4—C3—H3C	108.5
C2—C1—H1A	108.5	S2—C3—H3C	108.5
S1—C1—H1A	108.5	C4—C3—H3D	108.5
C2—C1—H1B	108.5	S2—C3—H3D	108.5
S1—C1—H1B	108.5	H3C—C3—H3D	107.5
H1A—C1—H1B	107.5	O6^vi—K1—O3^vii	124.38 (7)
S3—O7—Co1	126.71 (10)	O6^vi—K1—O9	87.87 (6)
C5—N3—Co1	122.94 (17)	O3^vii—K1—O9	140.88 (6)
C5—N3—H3A	106.6	O6^vi—K1—O5^viii	71.71 (6)
Co1—N3—H3A	106.6	O3^vii—K1—O5^viii	81.07 (6)
C5—N3—H3B	106.6	O9—K1—O5^viii	134.66 (7)
Co1—N3—H3B	106.6	O6^vi—K1—O2^ix	137.80 (7)
H3A—N3—H3B	106.6	O3^vii—K1—O2^ix	91.78 (6)
S3—O9—K1	150.60 (13)	O9—K1—O2^ix	71.81 (6)
S2—O6—K1ⁱ	147.95 (13)	O5^viii—K1—O2^ix	96.53 (6)
S2—O5—K1ⁱⁱ	170.53 (14)	O6^vi—K1—O8^x	86.91 (7)
C4—N2—Co1	122.22 (18)	O3^vii—K1—O8^x	72.54 (6)
C4—N2—H2A	106.8	O9—K1—O8^x	89.77 (6)
Co1—N2—H2A	106.8	O5^viii—K1—O8^x	127.47 (7)
C4—N2—H2B	106.8	O2^ix—K1—O8^x	128.14 (6)
Co1—N2—H2B	106.8

O3—S1—O1—Co1	−165.99 (13)	O4—S2—O5—K1ⁱⁱ	24.0 (8)
O2—S1—O1—Co1	65.79 (17)	C3—S2—O5—K1ⁱⁱ	139.1 (8)
C1—S1—O1—Co1	−51.14 (17)	O1—Co1—N2—C4	−81.5 (11)
O7—Co1—O1—S1	−148.59 (16)	O7—Co1—N2—C4	−102.3 (2)
O4—Co1—O1—S1	126.45 (16)	O4—Co1—N2—C4	−17.8 (2)
N2—Co1—O1—S1	−169.5 (9)	N3—Co1—N2—C4	165.5 (2)
N3—Co1—O1—S1	−56.56 (16)	N1—Co1—N2—C4	72.6 (2)
N1—Co1—O1—S1	36.33 (17)	O1—Co1—N1—C2	−34.1 (2)
O5—S2—O4—Co1	69.55 (17)	O7—Co1—N1—C2	−77.2 (8)
O6—S2—O4—Co1	−162.09 (13)	O4—Co1—N1—C2	−117.9 (2)
C3—S2—O4—Co1	−48.29 (17)	N2—Co1—N1—C2	148.1 (2)
O1—Co1—O4—S2	−159.21 (15)	N3—Co1—N1—C2	57.7 (2)
O7—Co1—O4—S2	115.26 (15)	O3—S1—O2—K1ⁱⁱⁱ	−91.5 (9)
N2—Co1—O4—S2	25.34 (16)	O1—S1—O2—K1ⁱⁱⁱ	35.3 (9)
N3—Co1—O4—S2	166.0 (8)	C1—S1—O2—K1ⁱⁱⁱ	151.0 (9)
N1—Co1—O4—S2	−69.44 (15)	O2—S1—O3—K1^iv	−149.88 (15)
O3—S1—C1—C2	−177.7 (2)	O1—S1—O3—K1^iv	83.18 (19)
O2—S1—C1—C2	−55.3 (3)	C1—S1—O3—K1^iv	−31.5 (2)
O1—S1—C1—C2	64.1 (2)	O9—S3—O8—K1^v	−114.2 (7)
O8—S3—O7—Co1	71.69 (17)	O7—S3—O8—K1^v	13.0 (8)
O9—S3—O7—Co1	−159.33 (13)	C6—S3—O8—K1^v	129.1 (7)
C6—S3—O7—Co1	−45.30 (17)	Co1—N1—C2—C1	56.8 (3)
O1—Co1—O7—S3	117.83 (15)	S1—C1—C2—N1	−69.4 (3)
O4—Co1—O7—S3	−157.93 (15)	Co1—N2—C4—C3	43.5 (3)
N2—Co1—O7—S3	−63.97 (16)	Co1—N3—C5—C6	49.2 (3)
N3—Co1—O7—S3	26.15 (16)	N3—C5—C6—S3	−71.0 (3)
N1—Co1—O7—S3	161.1 (7)	O8—S3—C6—C5	−52.0 (3)
O1—Co1—N3—C5	−108.5 (2)	O9—S3—C6—C5	−174.4 (2)
O7—Co1—N3—C5	−23.5 (2)	O7—S3—C6—C5	67.6 (2)
O4—Co1—N3—C5	−73.9 (9)	N2—C4—C3—S2	−73.2 (3)
N2—Co1—N3—C5	66.8 (2)	O5—S2—C3—C4	−45.3 (3)
N1—Co1—N3—C5	161.6 (2)	O6—S2—C3—C4	−167.6 (2)
O8—S3—O9—K1	−136.5 (2)	O4—S2—C3—C4	74.7 (2)
O7—S3—O9—K1	96.0 (3)	S3—O9—K1—O6^vi	4.6 (3)
C6—S3—O9—K1	−18.6 (3)	S3—O9—K1—O3^vii	152.8 (2)
O5—S2—O6—K1ⁱ	−123.5 (2)	S3—O9—K1—O5^viii	−56.8 (3)
O4—S2—O6—K1ⁱ	108.8 (2)	S3—O9—K1—O2^ix	−137.8 (3)
C3—S2—O6—K1ⁱ	−4.1 (3)	S3—O9—K1—O8^x	91.6 (3)
O6—S2—O5—K1ⁱⁱ	−103.3 (8)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N3—H3B···O7ⁱⁱⁱ	0.90	2.22	3.097 (3)	163
N2—H2B···O4ⁱⁱⁱ	0.90	2.40	3.166 (3)	143
N2—H2B···O1ⁱⁱⁱ	0.90	2.47	3.255 (3)	146
N1—H1D···O4ⁱⁱⁱ	0.90	2.55	3.423 (3)	165
N3—H3A···O2	0.90	2.28	3.113 (3)	153
N2—H2A···O8	0.90	2.39	3.219 (3)	152
N1—H1C···O5	0.90	2.49	3.229 (3)	140

Symmetry code: (iii) x+1/2, −y+3/2, z.

Experimental details

Crystal data
Chemical formula	[CoK(C₂H₆NO₃S)₃]
M_r	470.44
Crystal system, space group	Orthorhombic, Pna2₁
Temperature (K)	296
a, b, c (Å)	10.6901 (19), 15.669 (3), 9.6094 (17)
V (Å³)	1609.6 (5)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	1.76
Crystal size (mm)	0.26 × 0.22 × 0.14

Data collection
Diffractometer	Bruker SMART CCD area-detector
Absorption correction	Multi-scan (SADABS; Bruker, 1999)
T_min, T_max	0.657, 0.791
No. of measured, independent and observed [I > 2σ(I)] reflections	10792, 3386, 3146
R_int	0.027
(sin θ/λ)_max (Å⁻¹)	0.639

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.024, 0.058, 1.02
No. of reflections	3386
No. of parameters	208
No. of restraints	1
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.22, −0.33
Absolute structure	Flack (1983), 1528 Friedel pairs
Absolute structure parameter	0.020 (13)

Computer programs: SMART (Bruker, 1999), SAINT (Bruker, 1999), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Selected bond lengths (Å) top

Co1—O1	2.1316 (18)	K1—O6ⁱ	2.687 (2)
Co1—O7	2.1411 (18)	K1—O3ⁱⁱ	2.7140 (19)
Co1—O4	2.142 (2)	K1—O5ⁱⁱⁱ	2.8361 (19)
Co1—N2	2.143 (2)	K1—O2^iv	2.8522 (19)
Co1—N3	2.146 (2)	K1—O8^v	2.8893 (19)
Co1—N1	2.149 (2)	K1—O9	2.816 (2)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
N3—H3B···O7^vi	0.90	2.22	3.097 (3)	163.2
N2—H2B···O4^vi	0.90	2.40	3.166 (3)	142.5
N2—H2B···O1^vi	0.90	2.47	3.255 (3)	145.5
N1—H1D···O4^vi	0.90	2.55	3.423 (3)	165.0
N3—H3A···O2	0.90	2.28	3.113 (3)	153.1
N2—H2A···O8	0.90	2.39	3.219 (3)	152.3
N1—H1C···O5	0.90	2.49	3.229 (3)	139.7

Symmetry code: (vi) x+1/2, −y+3/2, z.

Acknowledgements

We are grateful to the Education Department Foundation of the Guangxi Zhuang Autonomous Region of the People's Republic of China (201012MS203) and the Start-up Foundation for Advanced Talents of Hechi University (No. 2008QS-N019)

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