cyclo-Tetrakis(μ2-3-sulfidopropyl-κ3C1,S:S)tetrakis[chloridocobalt(III)]

Awan, S.A.; Tahir, M.N.; Muhammad, I.K.; Ahmad, S.; Tariq, M.I.

doi:10.1107/S1600536811013067

metal-organic compounds

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ISSN: 2056-9890

Volume 67| Part 5| May 2011| Pages m576-m577

doi:10.1107/S1600536811013067

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RETRACTED ARTICLE

This article has been retracted. To view the retraction notice, click here.

Retracted: cyclo-Tetrakis(μ₂-3-sulfidopropyl-κ³C¹,S:S)tetrakis[chloridocobalt(III)]

Shafique Ahmad Awan,^a M. Nawaz Tahir,^b ^* Iram Khushi Muhammad,^c Saeed Ahmad ^c and Muhammad Ilyas Tariq ^d

^aPAEC, PO Box # 1114, Islamabad GPO 44000, Pakistan, ^bDepartment of Physics, University of Sargodha, Sargodha, Pakistan, ^cDepartment of Chemistry, University of Engineering and Technology, Lahore 54890, Pakistan, and ^dDepartment of Chemistry, University of Sargodha, Sargodha, Pakistan
^*Correspondence e-mail: dmntahir_uos@yahoo.com

(Received 2 April 2011; accepted 7 April 2011; online 13 April 2011)

In the centrosymmetric title compound, [Co₄Cl₄(C₃H₆S)]₄], the two independent Co^III ions are each coordinated in a distorted tetrahedral geometry by one C, one Cl and two S atoms. The molecules are stabilized by C—H⋯Cl hydrogen bonds. In the crystal, intermolecular C—H⋯Cl and C—H⋯S hydrogen bonds with R₂²(8), R₄²(8) and R₂²(6) ring motifs generate a polymeric network.

Related literature

For related background see: Shahid et al. (2009 ); Altaf et al. (2010 ). For related structures, see: Duan et al. (1997 ); Tremel et al. (1992 ). For graph-set notation, see: Bernstein et al. (1995 ).

Experimental

Crystal data

[Co₄Cl₄(C₃H₆S)]₄]
M_r = 674.07
Monoclinic, C 2/c
a = 23.6135 (12) Å
b = 7.8465 (3) Å
c = 16.8693 (9) Å
β = 130.440 (4)°
V = 2378.9 (2) Å³
Z = 4
Mo Kα radiation
μ = 3.54 mm⁻¹
T = 296 K
0.24 × 0.16 × 0.14 mm

Data collection

Bruker Kappa APEXII CCD diffractometer
Absorption correction: multi-scan (SADABS; Bruker, 2005 ) T_min = 0.675, T_max = 0.683
13736 measured reflections
2152 independent reflections
1782 reflections with I > 2σ(I)
R_int = 0.058

Refinement

R[F² > 2σ(F²)] = 0.041
wR(F²) = 0.125
S = 1.04
2152 reflections
109 parameters
H-atom parameters constrained
Δρ_max = 0.70 e Å⁻³
Δρ_min = −0.62 e Å⁻³

Table 1
Selected bond lengths (Å)

Co1—Cl1	2.228 (2)
Co1—S1	2.3570 (17)
Co1—S2	2.318 (2)
Co1—C3	2.038 (6)
Co2—Cl2	2.236 (3)
Co2—S1	2.305 (2)
Co2—S2ⁱ	2.3648 (16)
Co2—C6ⁱ	2.051 (6)
S1—C1	1.826 (7)
S2—C4	1.837 (8)
Symmetry code: (i) $[-x+{\script{1\over 2}}, -y-{\script{1\over 2}}, -z+1]$ .

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C3—H3A⋯S2ⁱⁱ	0.97	2.57	3.539 (8)	175
C3—H3B⋯Cl2ⁱⁱⁱ	0.97	2.74	3.512 (7)	138
C3—H3B⋯Cl2^iv	0.97	2.81	3.412 (6)	121
C6—H6A⋯Cl1ⁱ	0.97	2.62	3.379 (7)	135
C6—H6B⋯Cl1^v	0.97	2.48	3.343 (7)	148
Symmetry codes: (i) $[-x+{\script{1\over 2}}, -y-{\script{1\over 2}}, -z+1]$ ; (ii) $[-x+{\script{1\over 2}}, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (iii) $[-x, y, -z+{\script{1\over 2}}]$ ; (iv) $[x, -y, z-{\script{1\over 2}}]$ ; (v) $[x+{\script{1\over 2}}, -y-{\script{1\over 2}}, z+{\script{1\over 2}}]$ .

Data collection: APEX2 (Bruker, 2009 ); cell refinement: SAINT (Bruker, 2009); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEPIII (Burnett & Johnson, 1996 ), ORTEP-3 for Windows (Farrugia, 1997 ) and PLATON (Spek, 2009 ); software used to prepare material for publication: WinGX (Farrugia, 1999 ) and PLATON.

Supporting information

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536811013067/si2349sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536811013067/si2349Isup2.hkl

checkCIF report

Comment top

Recently, we have reported the crystal structure of zinc(II) and mercury(II) complexes of pyrrolidinedithiocarbamate (PDTC) (Shahid et al., 2009) & (Altaf, et al., 2010). In the present study, we attempted to prepare a cobalt(II) complex with PDTC, but surprisingly the title compound (I, Fig. 1) was isolated, the crystal structure of which is being presented.

The crystal structure of (II) i.e, tetranuclear molecular square[Co(HL)]₄⁴⁺ [H₂L = tetra(2-pyridyl)thiocarbazone] (Duan et al., 1997) and (III) i.e., bis(tetraethylammonium) hexakis(µ₂-phenylthiolato)-tetrachloro-tetra -cobalt acetonitrile solvate (Tremel et al., 1992) have been published which are related to the title compound (I).

The crystal structure of the title compound (I) is centrosymmetric. The coordination around two independent Coⁱⁱⁱ ions is distorted tetrahedral from one C, Cl and two S-atoms. The range of Co—C [2.038 (6)–2.051 (6) Å] is shorter compared to Co—S [2.305 (2)–2.3648 (16) Å]. The Co—Cl bonds have values of 2.228 (2) and 2.236 (2) Å. The important bond distances are given in Table 1. The molecules are stabilized in the form of a polymeric network due to C—H···Cl and C—H···S intermolecular H-bonds (Table 2) forming R₂²(8), R₄²(8) and R₂²(6) ring motifs (Bernstein et al., 1995).

Related literature top

For related background see: Shahid et al. (2009); Altaf et al. (2010). For related structures, see: Duan et al. (1997); Tremel et al. (1992). For graph-set notation, see: Bernstein et al. (1995).

Experimental top

The title compound was prepared by adding two equivalents of ammonium pyrrolidinedithiocarbamate (PDTC) in 15 ml methanol to a solution of CoCl₂.6H₂O in 10 ml methanol. The addition of PDTC in the pink colored metal ion solution resulted in the formation of green precipitates immediately. After stirring for half an hour, the precipitates were filtered off and dried. The blackish brown crystals of the title compound (I) were prepared by dissolving 0.03 g precipitates in 3 ml DMSO on heating in a vial and then cooling the resulting solution at room temperature.

Computing details top

Data collection: APEX2 (Bruker, 2009); cell refinement: SAINT (Bruker, 2009); data reduction: SAINT (Bruker, 2009); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEPIII (Burnett & Johnson, 1996), ORTEP-3 for Windows (Farrugia, 1997) and PLATON (Spek, 2009); software used to prepare material for publication: WinGX (Farrugia, 1999) and PLATON (Spek, 2009).

Figures top

	Fig. 1. View of the centrosymmetric title compound. Symmetry code i = -x + 1/2, -y - 1/2, -z + 1. The thermal ellipsoids are drawn at the 50% probability level. H-atoms are shown by small circles of arbitrary radii.
	Fig. 2. The partial packing (PLATON; Spek, 2009) which shows that molecules form a polymeric network with ring motifs. H-atoms not involved in H-bondings are omitted for clarity.

cyclo-Tetrakis(µ₂-3-sulfidopropyl- κ³C¹,S:S)tetrakis[chloridocobalt(III)] top

Crystal data top

[Co₄Cl₄(C₃H₆S)]₄]	F(000) = 1344
M_r = 674.07	D_x = 1.882 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 1782 reflections
a = 23.6135 (12) Å	θ = 2.3–25.2°
b = 7.8465 (3) Å	µ = 3.54 mm⁻¹
c = 16.8693 (9) Å	T = 296 K
β = 130.440 (4)°	Prisms, white
V = 2378.9 (2) Å³	0.24 × 0.16 × 0.14 mm
Z = 4

Data collection top

Bruker Kappa APEXII CCD diffractometer	2152 independent reflections
Radiation source: fine-focus sealed tube	1782 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.058
Detector resolution: 8.10 pixels mm^-1	θ_max = 25.2°, θ_min = 2.3°
ω scans	h = −28→28
Absorption correction: multi-scan (SADABS; Bruker, 2005)	k = −9→8
T_min = 0.675, T_max = 0.683	l = −20→20
13736 measured reflections

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)] = 0.041	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.125	H-atom parameters constrained
S = 1.04	w = 1/[σ²(F_o²) + (0.0653P)² + 15.5359P] where P = (F_o² + 2F_c²)/3
2152 reflections	(Δ/σ)_max < 0.001
109 parameters	Δρ_max = 0.70 e Å⁻³
0 restraints	Δρ_min = −0.62 e Å⁻³

Crystal data top

[Co₄Cl₄(C₃H₆S)]₄]	V = 2378.9 (2) Å³
M_r = 674.07	Z = 4
Monoclinic, C2/c	Mo Kα radiation
a = 23.6135 (12) Å	µ = 3.54 mm⁻¹
b = 7.8465 (3) Å	T = 296 K
c = 16.8693 (9) Å	0.24 × 0.16 × 0.14 mm
β = 130.440 (4)°

Data collection top

Bruker Kappa APEXII CCD diffractometer	2152 independent reflections
Absorption correction: multi-scan (SADABS; Bruker, 2005)	1782 reflections with I > 2σ(I)
T_min = 0.675, T_max = 0.683	R_int = 0.058
13736 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.041	0 restraints
wR(F²) = 0.125	H-atom parameters constrained
S = 1.04	w = 1/[σ²(F_o²) + (0.0653P)² + 15.5359P] where P = (F_o² + 2F_c²)/3
2152 reflections	Δρ_max = 0.70 e Å⁻³
109 parameters	Δρ_min = −0.62 e Å⁻³

Special details top

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

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	0.17597 (4)	−0.17781 (9)	0.30876 (5)	0.0323 (2)
Co2	0.14629 (4)	−0.12119 (9)	0.50575 (5)	0.0336 (2)
Cl1	0.09923 (9)	−0.3988 (2)	0.25283 (12)	0.0555 (5)
Cl2	0.07469 (11)	0.0860 (3)	0.49043 (15)	0.0694 (7)
S1	0.21157 (8)	−0.0272 (2)	0.45587 (11)	0.0460 (4)
S2	0.28224 (8)	−0.2358 (2)	0.33225 (11)	0.0481 (5)
C1	0.1631 (4)	0.1666 (8)	0.3814 (5)	0.066 (3)
C2	0.0959 (4)	0.1316 (9)	0.2708 (5)	0.061 (2)
C3	0.1163 (3)	0.0287 (7)	0.2182 (4)	0.0362 (17)
C4	0.3356 (4)	−0.0372 (9)	0.3904 (6)	0.064 (3)
C5	0.4140 (4)	−0.0689 (10)	0.4862 (6)	0.065 (3)
C6	0.4164 (3)	−0.1622 (7)	0.5638 (4)	0.0417 (17)
H1A	0.14799	0.22914	0.41469	0.0787*
H1B	0.19711	0.23811	0.38263	0.0787*
H2A	0.05934	0.07031	0.26878	0.0733*
H2B	0.07391	0.23855	0.23404	0.0733*
H3A	0.14572	0.09690	0.20863	0.0435*
H3B	0.07165	−0.00820	0.15024	0.0435*
H4A	0.33533	0.02242	0.33979	0.0769*
H4B	0.31166	0.03559	0.40757	0.0769*
H5A	0.43922	−0.13460	0.46849	0.0783*
H5B	0.43980	0.03894	0.51537	0.0783*
H6A	0.39644	−0.09200	0.58805	0.0502*
H6B	0.46733	−0.19168	0.62322	0.0502*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Co1	0.0275 (4)	0.0399 (4)	0.0300 (4)	−0.0012 (3)	0.0189 (3)	−0.0025 (3)
Co2	0.0338 (4)	0.0373 (4)	0.0312 (4)	−0.0014 (3)	0.0217 (3)	0.0004 (3)
Cl1	0.0496 (9)	0.0537 (9)	0.0545 (9)	−0.0089 (7)	0.0299 (8)	−0.0081 (7)
Cl2	0.0683 (11)	0.0733 (11)	0.0725 (12)	0.0219 (9)	0.0483 (10)	0.0114 (9)
S1	0.0485 (8)	0.0520 (8)	0.0377 (7)	−0.0099 (7)	0.0281 (7)	−0.0045 (6)
S2	0.0407 (8)	0.0667 (10)	0.0398 (8)	0.0055 (7)	0.0274 (7)	0.0030 (7)
C1	0.091 (5)	0.045 (4)	0.054 (4)	−0.010 (4)	0.044 (4)	−0.004 (3)
C2	0.066 (4)	0.047 (4)	0.056 (4)	0.003 (3)	0.033 (4)	0.008 (3)
C3	0.034 (3)	0.045 (3)	0.030 (3)	−0.003 (2)	0.021 (2)	0.005 (2)
C4	0.056 (4)	0.064 (4)	0.074 (5)	0.000 (3)	0.043 (4)	0.022 (4)
C5	0.056 (4)	0.067 (4)	0.074 (5)	−0.010 (3)	0.043 (4)	0.003 (4)
C6	0.038 (3)	0.047 (3)	0.037 (3)	−0.012 (2)	0.023 (3)	−0.005 (2)

Geometric parameters (Å, º) top

Co1—Cl1	2.228 (2)	C5—C6	1.469 (11)
Co1—S1	2.3570 (17)	C1—H1A	0.9700
Co1—S2	2.318 (2)	C1—H1B	0.9700
Co1—C3	2.038 (6)	C2—H2A	0.9700
Co2—Cl2	2.236 (3)	C2—H2B	0.9700
Co2—S1	2.305 (2)	C3—H3A	0.9700
Co2—S2ⁱ	2.3648 (16)	C3—H3B	0.9700
Co2—C6ⁱ	2.051 (6)	C4—H4A	0.9700
S1—C1	1.826 (7)	C4—H4B	0.9700
S2—C4	1.837 (8)	C5—H5A	0.9700
C1—C2	1.495 (10)	C5—H5B	0.9700
C2—C3	1.492 (11)	C6—H6A	0.9700
C4—C5	1.490 (13)	C6—H6B	0.9700

Co1···H4Aⁱⁱ	3.3200	S2···H4Aⁱⁱ	3.0500
Cl1···C3	3.473 (6)	C2···Cl2^iv	3.570 (7)
Cl1···C6ⁱⁱⁱ	3.343 (7)	C3···Cl1	3.473 (6)
Cl1···C6ⁱ	3.379 (7)	C3···S1	3.103 (5)
Cl2···C1	3.623 (11)	C3···S2	3.686 (7)
Cl2···C3^iv	3.512 (7)	C3···C1	2.455 (9)
Cl2···C6ⁱ	3.492 (6)	C3···Cl2^iv	3.512 (7)
Cl2···C3^v	3.412 (6)	C3···Cl2^viii	3.412 (6)
Cl2···S1	3.744 (4)	C3···S2^ix	3.539 (8)
Cl2···C2^iv	3.570 (7)	C6···Cl1ⁱ	3.379 (7)
Cl1···H4Aⁱⁱ	2.8900	C6···Cl2ⁱ	3.491 (6)
Cl1···H2B^vi	2.8800	C6···Cl1^x	3.343 (7)
Cl1···H6Aⁱ	2.6200	H1A···Cl2	2.9600
Cl1···H6Bⁱⁱⁱ	2.4800	H1B···H3A	2.5900
Cl2···H1A	2.9600	H1B···S1^vii	3.1000
Cl2···H3B^v	2.8100	H2A···H2A^iv	2.4400
Cl2···H3B^iv	2.7400	H2B···Cl1^xi	2.8800
Cl2···H5B^vii	2.9600	H3A···H1B	2.5900
S1···Cl2	3.744 (4)	H3A···S2^ix	2.5700
S1···S2	3.785 (3)	H3B···Cl2^iv	2.7400
S1···C2	2.774 (7)	H3B···Cl2^viii	2.8100
S1···C3	3.103 (5)	H4A···Co1^ix	3.3200
S1···Co1ⁱ	3.8074 (16)	H4A···Cl1^ix	2.8900
S1···S1ⁱ	3.773 (2)	H4A···S2^ix	3.0500
S2···C3ⁱⁱ	3.539 (8)	H4B···S1	3.0000
S2···S1	3.785 (3)	H4B···H6A	2.5200
S2···C3	3.686 (7)	H5B···Cl2^vii	2.9600
S1···H4B	3.0000	H6A···H4B	2.5200
S1···H1B^vii	3.1000	H6A···Cl1ⁱ	2.6200
S2···H3Aⁱⁱ	2.5700	H6B···Cl1^x	2.4800

Cl1—Co1—S1	118.22 (8)	C2—C1—H1B	109.00
Cl1—Co1—S2	114.37 (8)	H1A—C1—H1B	108.00
Cl1—Co1—C3	108.9 (2)	C1—C2—H2A	110.00
S1—Co1—S2	108.14 (7)	C1—C2—H2B	109.00
S1—Co1—C3	89.52 (17)	C3—C2—H2A	110.00
S2—Co1—C3	115.5 (2)	C3—C2—H2B	109.00
Cl2—Co2—S1	111.09 (9)	H2A—C2—H2B	108.00
Cl2—Co2—S2ⁱ	113.44 (8)	Co1—C3—H3A	110.00
Cl2—Co2—C6ⁱ	109.0 (2)	Co1—C3—H3B	110.00
S1—Co2—S2ⁱ	115.39 (8)	C2—C3—H3A	110.00
S1—Co2—C6ⁱ	117.5 (2)	C2—C3—H3B	110.00
S2ⁱ—Co2—C6ⁱ	88.68 (15)	H3A—C3—H3B	108.00
Co1—S1—Co2	110.96 (8)	S2—C4—H4A	109.00
Co1—S1—C1	93.3 (2)	S2—C4—H4B	109.00
Co2—S1—C1	104.4 (4)	C5—C4—H4A	109.00
Co1—S2—C4	102.5 (4)	C5—C4—H4B	109.00
Co1—S2—Co2ⁱ	99.94 (8)	H4A—C4—H4B	108.00
Co2ⁱ—S2—C4	93.3 (2)	C4—C5—H5A	110.00
S1—C1—C2	113.0 (5)	C4—C5—H5B	110.00
C1—C2—C3	110.6 (8)	C6—C5—H5A	109.00
Co1—C3—C2	108.5 (4)	C6—C5—H5B	110.00
S2—C4—C5	112.1 (5)	H5A—C5—H5B	108.00
C4—C5—C6	110.6 (9)	C5—C6—H6A	110.00
Co2ⁱ—C6—C5	107.9 (4)	C5—C6—H6B	110.00
S1—C1—H1A	109.00	H6A—C6—H6B	108.00
S1—C1—H1B	109.00	Co2ⁱ—C6—H6A	110.00
C2—C1—H1A	109.00	Co2ⁱ—C6—H6B	110.00

Cl1—Co1—S1—Co2	−7.06 (11)	S2ⁱ—Co2—S1—C1	−148.1 (2)
Cl1—Co1—S1—C1	−113.8 (3)	C6ⁱ—Co2—S1—Co1	10.1 (2)
S2—Co1—S1—Co2	−139.02 (7)	C6ⁱ—Co2—S1—C1	109.3 (3)
S2—Co1—S1—C1	114.2 (3)	Cl2—Co2—S2ⁱ—Co1ⁱ	−145.79 (9)
C3—Co1—S1—Co2	104.3 (2)	Cl2—Co2—S2ⁱ—C4ⁱ	110.9 (4)
C3—Co1—S1—C1	−2.5 (4)	S1—Co2—S2ⁱ—Co1ⁱ	−16.01 (8)
Cl1—Co1—S2—C4	−174.3 (3)	S1—Co2—S2ⁱ—C4ⁱ	−119.3 (4)
Cl1—Co1—S2—Co2ⁱ	−78.66 (7)	Cl2—Co2—C6ⁱ—C5ⁱ	−87.1 (6)
S1—Co1—S2—C4	−40.3 (3)	S1—Co2—C6ⁱ—C5ⁱ	145.4 (5)
S1—Co1—S2—Co2ⁱ	55.34 (7)	Co1—S1—C1—C2	30.3 (8)
C3—Co1—S2—C4	58.1 (3)	Co2—S1—C1—C2	−82.3 (7)
C3—Co1—S2—Co2ⁱ	153.74 (17)	Co1—S2—C4—C5	130.1 (7)
Cl1—Co1—C3—C2	95.3 (5)	Co2ⁱ—S2—C4—C5	29.2 (7)
S1—Co1—C3—C2	−24.5 (5)	S1—C1—C2—C3	−56.3 (9)
S2—Co1—C3—C2	−134.5 (5)	C1—C2—C3—Co1	51.0 (7)
Cl2—Co2—S1—Co1	−116.41 (8)	S2—C4—C5—C6	−57.7 (9)
Cl2—Co2—S1—C1	−17.1 (2)	C4—C5—C6—Co2ⁱ	54.4 (7)
S2ⁱ—Co2—S1—Co1	112.67 (7)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C3—H3A···S2^ix	0.97	2.57	3.539 (8)	175
C3—H3B···Cl2^iv	0.97	2.74	3.512 (7)	138
C3—H3B···Cl2^viii	0.97	2.81	3.412 (6)	121
C6—H6A···Cl1ⁱ	0.97	2.62	3.379 (7)	135
C6—H6B···Cl1^x	0.97	2.48	3.343 (7)	148

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

Experimental details

Crystal data
Chemical formula	[Co₄Cl₄(C₃H₆S)]₄]
M_r	674.07
Crystal system, space group	Monoclinic, C2/c
Temperature (K)	296
a, b, c (Å)	23.6135 (12), 7.8465 (3), 16.8693 (9)
β (°)	130.440 (4)
V (Å³)	2378.9 (2)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	3.54
Crystal size (mm)	0.24 × 0.16 × 0.14

Data collection
Diffractometer	Bruker Kappa APEXII CCD diffractometer
Absorption correction	Multi-scan (SADABS; Bruker, 2005)
T_min, T_max	0.675, 0.683
No. of measured, independent and observed [I > 2σ(I)] reflections	13736, 2152, 1782
R_int	0.058
(sin θ/λ)_max (Å⁻¹)	0.600

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.041, 0.125, 1.04
No. of reflections	2152
No. of parameters	109
H-atom treatment	H-atom parameters constrained
	w = 1/[σ²(F_o²) + (0.0653P)² + 15.5359P] where P = (F_o² + 2F_c²)/3
Δρ_max, Δρ_min (e Å⁻³)	0.70, −0.62

Computer programs: APEX2 (Bruker, 2009), SAINT (Bruker, 2009), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEPIII (Burnett & Johnson, 1996), ORTEP-3 for Windows (Farrugia, 1997) and PLATON (Spek, 2009), WinGX (Farrugia, 1999) and PLATON (Spek, 2009).

Selected bond lengths (Å) top

Co1—Cl1	2.228 (2)	Co2—S1	2.305 (2)
Co1—S1	2.3570 (17)	Co2—S2ⁱ	2.3648 (16)
Co1—S2	2.318 (2)	Co2—C6ⁱ	2.051 (6)
Co1—C3	2.038 (6)	S1—C1	1.826 (7)
Co2—Cl2	2.236 (3)	S2—C4	1.837 (8)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C3—H3A···S2ⁱⁱ	0.97	2.57	3.539 (8)	175
C3—H3B···Cl2ⁱⁱⁱ	0.97	2.74	3.512 (7)	138
C3—H3B···Cl2^iv	0.97	2.81	3.412 (6)	121
C6—H6A···Cl1ⁱ	0.97	2.62	3.379 (7)	135
C6—H6B···Cl1^v	0.97	2.48	3.343 (7)	148

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

Acknowledgements

The authors acknowledge the provision of funds for the purchase of the diffractometer and encouragement by Dr Muhammad Akram Chaudhary, Vice Chancellor, University of Sargodha, Pakistan.

References

Altaf, M., Stoeckli-Evans, H., Batool, S. S., Isab, A. A., Ahmad, S., Saleem, M., Awan, S. A. & Shaheen, M. A. (2010). J. Coord. Chem. 63, 1176–1185. CrossRef CAS Google Scholar
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ISSN: 2056-9890

Volume 67| Part 5| May 2011| Pages m576-m577

doi:10.1107/S1600536811013067

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

Retracted: cyclo-Tetra­kis­(μ2-3-sulfido­propyl-κ3C1,S:S)tetra­kis­[chloridocobalt(III)]

Related literature

Experimental

Crystal data

Data collection

Refinement

Supporting information

Acknowledgements

References

metal-organic compounds

Retracted: cyclo-Tetrakis(μ₂-3-sulfidopropyl-κ³C¹,S:S)tetrakis[chloridocobalt(III)]