Bis(tetra­butyl­ammonium) bis­(3,4,5-trioxocyclo­pent-1-ene-1,2-dithiol­ato-κ2S,S′)cadmate(II) 0.25-hydrate

Chen, H.-Y.; Xia, G.-M.; Zhang, Z.-W.; Li, P.

doi:10.1107/S1600536810049913

metal-organic compounds

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ISSN: 2056-9890

Volume 67| Part 1| January 2011| Pages m12-m13

https://doi.org/10.1107/S1600536810049913

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Bis(tetrabutylammonium) bis(3,4,5-trioxocyclopent-1-ene-1,2-dithiolato-κ²S,S′)cadmate(II) 0.25-hydrate

Hong-Yu Chen,^a Guang-Ming Xia,^b ^* Zhen-Wei Zhang ^b and Ping Li ^a

^aSchool of Chemistry and Chemical Engineering, TaiShan Medical University, Tai'an 271016, People's Republic of China, and ^bShandong Provincial Key Laboratory of Fluorine Chemistry and Chemical Materials, School of Chemistry and Chemical Engineering, University of Jinan, Ji'nan 250022, People's Republic of China
^*Correspondence e-mail: Binboll@126.com

(Received 1 October 2010; accepted 29 November 2010; online 4 December 2010)

The title compound, (C₁₆H₃₆N)₂[Cd(C₅O₃S₂)₂]·0.25H₂O, contains two disordered tetrabutylammonium cations, a complex [Cd(C₅O₃S₂)₂]²⁻ anion and a 0.25-hydrate water. The anion is composed of a bidentate coordinated 3,4,5-trioxocyclopent-1-ene-1,2-dithiolate (dtcroc) group forming a distorted tetrahedral configuration around the Cd^II ion. The dihedral angle between the least-squares planes of the ten-atom sulfur-substituted croconate groups in the anion is 84.10 (8)°. The crystal packing is stabilized by weak C—H⋯O and C—H⋯S cation–anion hydrogen-bond interactions. In each of the two cations one butyl group is disordered over two positions in the ratios 0.589 (11):0.411 (11) and 0.796 (12):0.204 (12).

Related literature

For the delocalized electronic structures, redox chemistry and range of coordination geometries of metal complexes of chelating ethylene-1,2-dithiolato ligands, see: Eisenberg (1970 ); Kato (2004 ). For the coordination behavior of the dtcroc dianion, see: Deplano et al. (2005 , 2006 ). For related structures, see: Dunitz et al. (2001 ); Castro et al. (2002 ); Maji et al. (2004 ).

Experimental

Crystal data

(C₁₆H₃₆N)₂[Cd(C₅O₃S₂)₂]·0.25H₂O
M_r = 946.16
Triclinic, $[P \overline 1]$
a = 9.820 (5) Å
b = 15.002 (5) Å
c = 17.406 (5) Å
α = 74.853 (5)°
β = 86.898 (5)°
γ = 87.705 (5)°
V = 2470.6 (17) Å³
Z = 2
Mo Kα radiation
μ = 0.65 mm⁻¹
T = 293 K
0.24 × 0.18 × 0.15 mm

Data collection

Oxford Diffraction CCD area-detector diffractometer
Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2007 $[Oxford Diffraction (2007). CrysAlis PRO and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England]$ ) T_min = 0.775, T_max = 0.858
30150 measured reflections
10069 independent reflections
6510 reflections with I > 2σ(I)
R_int = 0.032

Refinement

R[F² > 2σ(F²)] = 0.050
wR(F²) = 0.144
S = 1.04
10069 reflections
534 parameters
54 restraints
H-atom parameters constrained
Δρ_max = 0.72 e Å⁻³
Δρ_min = −0.42 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C12—H12A⋯O6ⁱ	0.97	2.48	3.412 (6)	161
C14—H14C⋯S2ⁱⁱ	0.97	2.70	3.472 (10)	137
C16—H16B⋯O2ⁱⁱⁱ	0.97	2.54	3.483 (7)	163
Symmetry codes: (i) -x, -y+1, -z+2; (ii) -x+1, -y+1, -z+2; (iii) x-1, y+1, z.

Data collection: CrysAlis PRO (Oxford Diffraction, 2007 $[Oxford Diffraction (2007). CrysAlis PRO and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England]$ ); cell refinement: CrysAlis PRO; data reduction: CrysAlis RED (Oxford Diffraction, 2007 $[Oxford Diffraction (2007). CrysAlis PRO and CrysAlis RED. Oxford Diffraction Ltd, Abingdon, England]$ ); program(s) used to solve structure: SIR97 (Altomare et al., 1999 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: WinGX (Farrugia, 1999 ).

Supporting information

Crystal structure: contains datablocks global, I. DOI: https://doi.org/10.1107/S1600536810049913/jj2066sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S1600536810049913/jj2066Isup2.hkl

checkCIF report

Comment top

Metal complexes of chelating ethylene-1,2-dithiolato ligands (metal dithiolene)are of continuing interest owing to their delocalized electronic structures, rich redox chemistry and range of coordination geometries (Eisenberg,1970; Kato, 2004). They have also proven useful as precursors for the preparation ofnovel molecular conductors, non-linear optical materials and magnetic charge-transfer salts. Accordingly, we have interests in investigating the solid chemistry based on the 3,4,5-trioxo-cyclopent-1 ene-ene-1, 2-dithiolate ion (C₅O₃S₂^2-), also abbreviated as dtcroc (alternative name sulfur-substituted croconate). The coordination behavior of the dtcroc dianion (C₅O₃S₂^2-) towards d⁸ transition metal ions, such as Pt²⁺(Deplano, et al. 2005) and Ni²⁺(Deplano, et al. 2006), have been investigated and all show a planar configuration. We present here the synthesis and characterization of a new Cd(II) coordination compound of dtcroc, which shows a distorted tetrahedral coordination conformation.

The asymmetric unit of title compound, (C₁₆H₃₆N)₂, [C₁₀CdO₆S₄], 0.25(H₂O) contains two disordered tetrabutylammonium cations, a coordinated [Cd(C₅O₃S₂)₂]^2- anion, and a 0.25 hydrate water (Fig. 1). The [Cd(C₅O₃S₂)₂]^2- anion is composed of a bidentate coordinated dtcroc group forming a distorted tetrahedral configuration around a Cd (II) ion with Cd—S bonds between 2.5254 (13)–2.5413 (12)Å and six S—Cd—S angles between adjacent sulfur atoms in the coordination sphere close to 109.5°. The dihedral angle between the least-square-planes of the ten atom sulfur-substituted croconate group in the (C₅O₃S₂^2-) anion is 84.10 (8)°.

Deviations of oxygen atoms, sulfur atoms and the cyclic five-membered ring in C₅O₃S₂^2- are less than 0.09 Å, indicating a planar molecular geometry for both ligands. The C≐O bonds in the title compound, vary by 1.209 (5)–1.224 (5)Å and show typical Csp² double bond character, while the C≐S bonds are in the range of 1.683 (4)–1.699 (4) Å, which are intermediate between the lengths of typical single C—S and double C≐S bonds. The difference among C—C distances within the ligands are in the range of 1.402 (5)–1.505 (6) Å, establishing a π-electron localized C_2v molecular symmetry which compares well with similar structure croconate anions (Dunitz, et al., 2001; Castro, et al., 2002; Maji, et al.2004).

The tetrabutlyammionium cations are disordered in the title crystal and a few solvent water molecules were cocrystalized to stabilize the structure. The [Cd(C₅O₃S₂)₂]^2- units form stacks along [1 0 0], surrounded by tetrabutylamonium cations (Fig.2). Crystal packing is stabilized by weak C—H···O, C—H···S cation–anion hydrogen bond interactions (Table 1).

Related literature top

For the delocalized electronic structures, redox chemistry and range of coordination geometries of metal complexes of chelating ethylene-1,2-dithiolato ligands, see: Eisenberg (1970); Kato (2004). For the coordination behavior of the dtcroc dianion, see: Deplano et al. (2005, 2006). For related structures, see: Dunitz et al. (2001); Castro et al. (2002); Maji et al. (2004).

Experimental top

To a solution containing K₂dtcroc (0.2 g, 0.8 mmol) in H₂O (20 mL) was addedto a solution containing Cd(NO₃).4H₂O (0.12 g, 0.4 mmol) in H₂O (5 mL). The resulting mixture was heated to 70 °C for 1 h, then filtered into a solution of NBu₄Br (0.40 g, 0.95 mmol) in ethanol (5 mL). Solid product was collected by suction filtration, washed with water and dried in air. Red block crystals were obtained by recrystallization from acetone.

Structure description top

For the delocalized electronic structures, redox chemistry and range of coordination geometries of metal complexes of chelating ethylene-1,2-dithiolato ligands, see: Eisenberg (1970); Kato (2004). For the coordination behavior of the dtcroc dianion, see: Deplano et al. (2005, 2006). For related structures, see: Dunitz et al. (2001); Castro et al. (2002); Maji et al. (2004).

Computing details top

Data collection: CrysAlis PRO (Oxford Diffraction, 2007); cell refinement: CrysAlis PRO (Oxford Diffraction, 2007); data reduction: CrysAlis RED (Oxford Diffraction, 2007); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: WinGX (Farrugia, 1999).

Figures top

	Fig. 1. Coordination configuration of the title compound with thermal ellipsoids at 30% probability levels. Hydrogen atoms have been omiitted for clarity. Dashed lines indicate disordered butyl groups.
	Fig. 2. A packing diagram viewed down the b axis. symmetry code: a(-x, 1-y, 2-z); b(1-x, 1-y, 2-z); c(-1+x, 1+y, z);

Bis(tetrabutylammonium) bis(3,4,5-trioxocyclopent-1-ene-1,2-dithiolato- κ²S,S')cadmate(II) 0.25-hydrate top

Crystal data top

(C₁₆H₃₆N)₂[Cd(C₅O₃S₂)₂]·0.25H₂O	Z = 2
M_r = 946.16	F(000) = 1001
Triclinic, P1	D_x = 1.272 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71069 Å
a = 9.820 (5) Å	Cell parameters from 6268 reflections
b = 15.002 (5) Å	θ = 2.5–27.5°
c = 17.406 (5) Å	µ = 0.65 mm⁻¹
α = 74.853 (5)°	T = 293 K
β = 86.898 (5)°	Prism, red
γ = 87.705 (5)°	0.24 × 0.18 × 0.15 mm
V = 2470.6 (17) Å³

Data collection top

Oxford Diffraction CCD area-detector diffractometer	10069 independent reflections
Radiation source: fine-focus sealed tube	6510 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.032
φ and ω scans	θ_max = 26.4°, θ_min = 3.1°
Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2007)	h = −12→12
T_min = 0.775, T_max = 0.858	k = −18→18
30150 measured reflections	l = −21→21

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)] = 0.050	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.144	H-atom parameters constrained
S = 1.04	w = 1/[σ²(F_o²) + (0.0756P)² + 0.4766P] where P = (F_o² + 2F_c²)/3
10069 reflections	(Δ/σ)_max = 0.001
534 parameters	Δρ_max = 0.72 e Å⁻³
54 restraints	Δρ_min = −0.42 e Å⁻³

Crystal data top

(C₁₆H₃₆N)₂[Cd(C₅O₃S₂)₂]·0.25H₂O	γ = 87.705 (5)°
M_r = 946.16	V = 2470.6 (17) Å³
Triclinic, P1	Z = 2
a = 9.820 (5) Å	Mo Kα radiation
b = 15.002 (5) Å	µ = 0.65 mm⁻¹
c = 17.406 (5) Å	T = 293 K
α = 74.853 (5)°	0.24 × 0.18 × 0.15 mm
β = 86.898 (5)°

Data collection top

Oxford Diffraction CCD area-detector diffractometer	10069 independent reflections
Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2007)	6510 reflections with I > 2σ(I)
T_min = 0.775, T_max = 0.858	R_int = 0.032
30150 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.050	54 restraints
wR(F²) = 0.144	H-atom parameters constrained
S = 1.04	Δρ_max = 0.72 e Å⁻³
10069 reflections	Δρ_min = −0.42 e Å⁻³
534 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	Occ. (<1)
C1	0.5036 (3)	0.0335 (2)	0.73690 (19)	0.0507 (8)
C2	0.6118 (4)	0.0659 (2)	0.7719 (2)	0.0542 (8)
C3	0.7159 (4)	−0.0061 (3)	0.7956 (2)	0.0673 (10)
C4	0.6686 (4)	−0.0890 (3)	0.7720 (3)	0.0670 (10)
C5	0.5340 (4)	−0.0624 (3)	0.7358 (2)	0.0607 (9)
C6	0.1825 (4)	0.3965 (2)	0.7705 (2)	0.0564 (9)
C7	0.2513 (4)	0.4415 (2)	0.6991 (2)	0.0537 (8)
C8	0.1950 (5)	0.5367 (3)	0.6716 (3)	0.0703 (11)
C9	0.0873 (4)	0.5494 (3)	0.7309 (3)	0.0723 (11)
C10	0.0816 (4)	0.4599 (3)	0.7949 (3)	0.0733 (11)
C11	0.2345 (4)	0.7393 (3)	0.9656 (2)	0.0725 (11)
H11A	0.2322	0.6810	0.9515	0.087*
H11B	0.3240	0.7645	0.9489	0.087*
C12	0.2188 (5)	0.7200 (3)	1.0553 (2)	0.0859 (13)	0.589 (11)
H12A	0.1385	0.6838	1.0749	0.103*	0.589 (11)
H12B	0.2086	0.7776	1.0709	0.103*	0.589 (11)
C13	0.3488 (11)	0.6657 (10)	1.0910 (6)	0.090 (5)	0.589 (11)
H13A	0.3774	0.6218	1.0608	0.108*	0.589 (11)
H13B	0.4222	0.7082	1.0872	0.108*	0.589 (11)
C14	0.3200 (11)	0.6145 (6)	1.1781 (5)	0.111 (4)	0.589 (11)
H14A	0.4001	0.5796	1.1988	0.167*	0.589 (11)
H14B	0.2461	0.5734	1.1818	0.167*	0.589 (11)
H14C	0.2958	0.6584	1.2083	0.167*	0.589 (11)
C12'	0.2188 (5)	0.7200 (3)	1.0553 (2)	0.0859 (13)	0.411 (11)
H12C	0.1266	0.7004	1.0723	0.103*	0.411 (11)
H12D	0.2320	0.7767	1.0706	0.103*	0.411 (11)
C13'	0.3202 (16)	0.6453 (13)	1.0989 (11)	0.098 (8)	0.411 (11)
H13C	0.3060	0.6354	1.1560	0.117*	0.411 (11)
H13D	0.3058	0.5874	1.0858	0.117*	0.411 (11)
C14'	0.4663 (15)	0.6772 (11)	1.0729 (10)	0.133 (6)	0.411 (11)
H14D	0.5301	0.6342	1.1039	0.199*	0.411 (11)
H14E	0.4770	0.7373	1.0812	0.199*	0.411 (11)
H14F	0.4829	0.6801	1.0175	0.199*	0.411 (11)
C15	0.1684 (4)	0.8095 (3)	0.8315 (2)	0.0765 (11)
H15A	0.2604	0.8322	0.8200	0.092*
H15B	0.1699	0.7474	0.8247	0.092*
C16	0.0772 (5)	0.8692 (4)	0.7713 (2)	0.0898 (13)
H16A	0.0837	0.9331	0.7727	0.108*
H16B	−0.0166	0.8512	0.7849	0.108*
C17	0.1165 (5)	0.8606 (4)	0.6879 (2)	0.0952 (15)
H17A	0.2069	0.8846	0.6723	0.114*
H17B	0.1194	0.7959	0.6879	0.114*
C18	0.0166 (6)	0.9124 (5)	0.6283 (3)	0.130 (2)
H18A	0.0422	0.9037	0.5767	0.195*
H18B	0.0172	0.9771	0.6260	0.195*
H18C	−0.0733	0.8896	0.6442	0.195*
C19	0.1267 (4)	0.8979 (3)	0.9364 (3)	0.0771 (11)
H19A	0.0885	0.8906	0.9902	0.093*
H19B	0.0650	0.9387	0.9006	0.093*
C20	0.2627 (5)	0.9453 (3)	0.9295 (3)	0.1104 (18)
H20A	0.3012	0.9576	0.8754	0.133*
H20B	0.3270	0.9067	0.9650	0.133*
C21	0.2321 (7)	1.0370 (3)	0.9532 (4)	0.144 (2)
H21A	0.1911	1.0807	0.9086	0.173*
H21B	0.1646	1.0253	0.9972	0.173*
C22	0.3502 (7)	1.0818 (5)	0.9768 (5)	0.164 (3)
H22A	0.3189	1.1364	0.9921	0.246*
H22B	0.4154	1.0982	0.9326	0.246*
H22C	0.3925	1.0396	1.0209	0.246*
C23	−0.0140 (4)	0.7709 (3)	0.9402 (2)	0.0715 (11)
H23A	−0.0360	0.7720	0.9949	0.086*
H23B	−0.0763	0.8141	0.9069	0.086*
C24	−0.0399 (5)	0.6756 (3)	0.9323 (3)	0.0910 (13)
H24A	0.0177	0.6302	0.9671	0.109*
H24B	−0.0201	0.6724	0.8778	0.109*
C25	−0.1950 (5)	0.6563 (4)	0.9565 (3)	0.1045 (16)
H25A	−0.2175	0.6711	1.0068	0.125*
H25B	−0.2514	0.6955	0.9164	0.125*
C26	−0.2239 (7)	0.5585 (4)	0.9642 (4)	0.138 (2)
H26A	−0.3190	0.5482	0.9780	0.206*
H26B	−0.1702	0.5199	1.0051	0.206*
H26C	−0.2013	0.5439	0.9145	0.206*
C27	0.3573 (4)	0.3164 (3)	0.3344 (2)	0.0645 (10)
H27A	0.3649	0.2527	0.3315	0.077*
H27B	0.2766	0.3438	0.3068	0.077*
C28	0.4794 (5)	0.3661 (3)	0.2909 (2)	0.0745 (11)
H28A	0.5618	0.3351	0.3140	0.089*
H28B	0.4772	0.4287	0.2967	0.089*
C29	0.4815 (6)	0.3686 (3)	0.2038 (2)	0.0891 (14)
H29A	0.3959	0.3956	0.1821	0.107*
H29B	0.4886	0.3058	0.1984	0.107*
C30	0.5983 (6)	0.4233 (4)	0.1554 (3)	0.1052 (17)
H30A	0.5935	0.4233	0.1005	0.158*
H30B	0.6836	0.3956	0.1751	0.158*
H30C	0.5916	0.4858	0.1600	0.158*
C31	0.4608 (4)	0.2796 (2)	0.4680 (2)	0.0594 (9)
H31A	0.5369	0.3184	0.4447	0.071*
H31B	0.4437	0.2856	0.5219	0.071*
C32	0.5039 (4)	0.1803 (3)	0.4729 (2)	0.0671 (10)
H32A	0.4328	0.1397	0.5011	0.081*
H32B	0.5161	0.1719	0.4195	0.081*
C33	0.6347 (4)	0.1550 (3)	0.5153 (3)	0.0787 (12)
H33A	0.6239	0.1678	0.5671	0.094*
H33B	0.7066	0.1934	0.4851	0.094*
C34	0.6773 (5)	0.0538 (3)	0.5263 (3)	0.1035 (16)
H34A	0.7608	0.0412	0.5539	0.155*
H34B	0.6908	0.0410	0.4751	0.155*
H34C	0.6072	0.0153	0.5569	0.155*
C35	0.2118 (4)	0.2592 (3)	0.4525 (2)	0.0656 (10)
H35A	0.1366	0.2846	0.4188	0.079*
H35B	0.2311	0.1971	0.4474	0.079*
C36	0.1655 (4)	0.2532 (3)	0.5383 (2)	0.0748 (11)
H36A	0.2396	0.2284	0.5730	0.090*
H36B	0.1415	0.3146	0.5440	0.090*
C37	0.0430 (5)	0.1918 (4)	0.5630 (3)	0.0986 (15)
H37A	−0.0319	0.2189	0.5297	0.118*
H37B	0.0659	0.1320	0.5534	0.118*
C38	−0.0033 (5)	0.1781 (4)	0.6488 (3)	0.1113 (18)
H38A	−0.0798	0.1380	0.6607	0.167*
H38B	−0.0297	0.2367	0.6584	0.167*
H38C	0.0699	0.1507	0.6823	0.167*
C39	0.3117 (4)	0.4152 (2)	0.4294 (2)	0.0673 (10)
H39A	0.3000	0.4123	0.4857	0.081*
H39B	0.3931	0.4500	0.4092	0.081*
C40	0.1907 (5)	0.4686 (3)	0.3877 (3)	0.0908 (14)	0.796 (12)
H40A	0.1140	0.4280	0.3948	0.109*	0.796 (12)
H40B	0.2134	0.4899	0.3311	0.109*	0.796 (12)
C41	0.1492 (7)	0.5537 (4)	0.4212 (5)	0.109 (3)	0.796 (12)
H41A	0.0721	0.5861	0.3926	0.131*	0.796 (12)
H41B	0.1196	0.5314	0.4768	0.131*	0.796 (12)
C42	0.2576 (7)	0.6183 (4)	0.4149 (5)	0.146 (2)	0.796 (12)
H42A	0.2252	0.6683	0.4366	0.219*	0.796 (12)
H42B	0.2859	0.6422	0.3600	0.219*	0.796 (12)
H42C	0.3336	0.5873	0.4441	0.219*	0.796 (12)
C40'	0.1907 (5)	0.4686 (3)	0.3877 (3)	0.0908 (14)	0.204 (12)
H40C	0.1125	0.4603	0.4251	0.109*	0.204 (12)
H40D	0.1693	0.4426	0.3445	0.109*	0.204 (12)
C41'	0.213 (3)	0.5728 (7)	0.3538 (9)	0.091 (9)	0.204 (12)
H41C	0.2811	0.5819	0.3103	0.110*	0.204 (12)
H41D	0.1283	0.6024	0.3324	0.110*	0.204 (12)
C42'	0.2576 (7)	0.6183 (4)	0.4149 (5)	0.146 (2)	0.204 (12)
H42D	0.2677	0.6832	0.3912	0.219*	0.204 (12)
H42E	0.3434	0.5913	0.4346	0.219*	0.204 (12)
H42F	0.1905	0.6095	0.4583	0.219*	0.204 (12)
Cd1	0.39579 (3)	0.238778 (19)	0.740476 (17)	0.06795 (13)
N1	0.1294 (3)	0.8046 (2)	0.91830 (17)	0.0630 (8)
N2	0.3363 (3)	0.31687 (19)	0.42099 (16)	0.0562 (7)
O1	0.8225 (3)	−0.0030 (2)	0.8281 (2)	0.0990 (10)
O2	0.7269 (4)	−0.1637 (2)	0.7821 (3)	0.1111 (12)
O3	0.4656 (3)	−0.11311 (19)	0.7096 (2)	0.0877 (9)
O4	0.2312 (4)	0.5948 (2)	0.6119 (2)	0.1084 (11)
O5	0.0145 (4)	0.6179 (2)	0.7289 (2)	0.1106 (11)
O6	0.0088 (4)	0.4455 (3)	0.8549 (2)	0.1246 (14)
S1	0.35964 (11)	0.09033 (7)	0.70076 (7)	0.0724 (3)
S2	0.62646 (11)	0.17189 (7)	0.78798 (7)	0.0771 (3)
S3	0.20701 (14)	0.28767 (7)	0.82643 (7)	0.0834 (3)
S4	0.38097 (11)	0.40010 (7)	0.64893 (6)	0.0682 (3)
O7	0.9700 (12)	0.1218 (8)	0.8742 (7)	0.086 (3)	0.25
H1O7	0.9367	0.1126	0.8330	0.128*	0.25
H2O7	1.0153	0.1710	0.8597	0.128*	0.25

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
C1	0.0465 (19)	0.0484 (19)	0.0585 (19)	0.0012 (15)	0.0009 (15)	−0.0173 (15)
C2	0.052 (2)	0.054 (2)	0.058 (2)	0.0052 (17)	−0.0039 (16)	−0.0180 (16)
C3	0.052 (2)	0.063 (2)	0.086 (3)	0.0056 (19)	−0.005 (2)	−0.020 (2)
C4	0.057 (2)	0.048 (2)	0.094 (3)	0.0105 (18)	−0.002 (2)	−0.0159 (19)
C5	0.060 (2)	0.051 (2)	0.073 (2)	0.0023 (18)	0.0017 (18)	−0.0209 (18)
C6	0.059 (2)	0.052 (2)	0.061 (2)	−0.0002 (17)	−0.0034 (17)	−0.0198 (17)
C7	0.060 (2)	0.050 (2)	0.054 (2)	−0.0004 (17)	−0.0085 (16)	−0.0176 (16)
C8	0.081 (3)	0.054 (2)	0.075 (3)	−0.004 (2)	−0.019 (2)	−0.013 (2)
C9	0.073 (3)	0.057 (2)	0.094 (3)	0.013 (2)	−0.017 (2)	−0.031 (2)
C10	0.067 (3)	0.068 (3)	0.087 (3)	0.008 (2)	0.004 (2)	−0.029 (2)
C11	0.069 (3)	0.066 (2)	0.084 (3)	0.015 (2)	−0.020 (2)	−0.020 (2)
C12	0.099 (4)	0.072 (3)	0.079 (3)	0.001 (3)	−0.028 (3)	−0.001 (2)
C13	0.132 (13)	0.042 (6)	0.102 (9)	0.000 (7)	−0.036 (8)	−0.023 (5)
C14	0.166 (9)	0.072 (5)	0.095 (7)	0.012 (5)	−0.066 (6)	−0.010 (4)
C12'	0.099 (4)	0.072 (3)	0.079 (3)	0.001 (3)	−0.028 (3)	−0.001 (2)
C13'	0.114 (13)	0.055 (11)	0.111 (14)	−0.006 (10)	−0.054 (10)	0.012 (8)
C14'	0.112 (11)	0.130 (12)	0.166 (13)	0.038 (9)	−0.047 (10)	−0.053 (10)
C15	0.069 (3)	0.089 (3)	0.069 (3)	0.011 (2)	−0.004 (2)	−0.017 (2)
C16	0.084 (3)	0.102 (4)	0.076 (3)	0.016 (3)	−0.013 (2)	−0.010 (2)
C17	0.098 (4)	0.116 (4)	0.068 (3)	−0.003 (3)	−0.009 (2)	−0.017 (3)
C18	0.142 (6)	0.160 (6)	0.083 (3)	−0.009 (5)	−0.032 (4)	−0.016 (4)
C19	0.087 (3)	0.062 (3)	0.079 (3)	0.014 (2)	−0.018 (2)	−0.011 (2)
C20	0.118 (4)	0.062 (3)	0.139 (5)	−0.003 (3)	−0.039 (4)	0.002 (3)
C21	0.143 (5)	0.068 (3)	0.210 (6)	0.001 (3)	−0.044 (5)	−0.008 (4)
C22	0.184 (7)	0.128 (6)	0.191 (7)	0.034 (5)	−0.057 (6)	−0.058 (5)
C23	0.063 (2)	0.080 (3)	0.068 (2)	0.006 (2)	−0.0034 (19)	−0.012 (2)
C24	0.082 (3)	0.088 (3)	0.100 (3)	−0.005 (3)	−0.013 (3)	−0.015 (3)
C25	0.109 (4)	0.103 (4)	0.101 (4)	−0.004 (3)	−0.015 (3)	−0.023 (3)
C26	0.134 (6)	0.118 (5)	0.156 (6)	−0.018 (4)	−0.019 (4)	−0.021 (4)
C27	0.081 (3)	0.055 (2)	0.061 (2)	−0.001 (2)	−0.0143 (19)	−0.0174 (17)
C28	0.095 (3)	0.065 (3)	0.065 (2)	−0.006 (2)	−0.008 (2)	−0.019 (2)
C29	0.120 (4)	0.081 (3)	0.068 (3)	−0.008 (3)	−0.007 (3)	−0.020 (2)
C30	0.138 (5)	0.094 (4)	0.082 (3)	−0.002 (3)	0.013 (3)	−0.024 (3)
C31	0.064 (2)	0.056 (2)	0.059 (2)	−0.0021 (18)	−0.0103 (17)	−0.0147 (17)
C32	0.074 (3)	0.056 (2)	0.071 (2)	0.003 (2)	−0.010 (2)	−0.0138 (18)
C33	0.062 (3)	0.070 (3)	0.097 (3)	0.007 (2)	−0.010 (2)	−0.008 (2)
C34	0.091 (4)	0.084 (3)	0.122 (4)	0.025 (3)	−0.005 (3)	−0.008 (3)
C35	0.065 (2)	0.056 (2)	0.077 (3)	−0.0050 (19)	−0.0149 (19)	−0.0164 (19)
C36	0.070 (3)	0.076 (3)	0.077 (3)	0.001 (2)	−0.009 (2)	−0.016 (2)
C37	0.074 (3)	0.103 (4)	0.117 (4)	−0.012 (3)	0.006 (3)	−0.026 (3)
C38	0.085 (4)	0.127 (5)	0.106 (4)	0.004 (3)	0.015 (3)	−0.007 (3)
C39	0.083 (3)	0.047 (2)	0.078 (2)	0.000 (2)	−0.014 (2)	−0.0242 (18)
C40	0.106 (4)	0.062 (3)	0.112 (4)	0.021 (3)	−0.038 (3)	−0.031 (2)
C41	0.105 (5)	0.066 (4)	0.159 (8)	0.018 (3)	−0.028 (5)	−0.035 (4)
C42	0.136 (6)	0.108 (5)	0.197 (7)	0.012 (4)	−0.011 (5)	−0.046 (5)
C40'	0.106 (4)	0.062 (3)	0.112 (4)	0.021 (3)	−0.038 (3)	−0.031 (2)
C41'	0.095 (19)	0.083 (17)	0.11 (2)	0.002 (14)	−0.006 (15)	−0.047 (15)
C42'	0.136 (6)	0.108 (5)	0.197 (7)	0.012 (4)	−0.011 (5)	−0.046 (5)
Cd1	0.0753 (2)	0.05395 (19)	0.0784 (2)	0.01462 (14)	−0.00680 (15)	−0.02569 (14)
N1	0.0611 (19)	0.065 (2)	0.0605 (18)	0.0078 (16)	−0.0078 (14)	−0.0123 (15)
N2	0.0654 (19)	0.0466 (16)	0.0599 (17)	0.0005 (14)	−0.0146 (14)	−0.0176 (13)
O1	0.067 (2)	0.091 (2)	0.150 (3)	0.0213 (17)	−0.0410 (19)	−0.047 (2)
O2	0.090 (2)	0.0582 (19)	0.186 (4)	0.0213 (17)	−0.031 (2)	−0.030 (2)
O3	0.078 (2)	0.0613 (17)	0.138 (3)	0.0057 (15)	−0.0235 (18)	−0.0479 (18)
O4	0.142 (3)	0.068 (2)	0.098 (2)	0.007 (2)	0.000 (2)	0.0061 (18)
O5	0.115 (3)	0.075 (2)	0.148 (3)	0.037 (2)	−0.024 (2)	−0.041 (2)
O6	0.124 (3)	0.103 (3)	0.136 (3)	0.025 (2)	0.056 (3)	−0.028 (2)
S1	0.0659 (6)	0.0606 (6)	0.0998 (7)	0.0167 (5)	−0.0315 (5)	−0.0341 (5)
S2	0.0676 (7)	0.0607 (6)	0.1173 (9)	0.0053 (5)	−0.0214 (6)	−0.0461 (6)
S3	0.1071 (9)	0.0572 (6)	0.0749 (7)	0.0133 (6)	0.0228 (6)	−0.0051 (5)
S4	0.0782 (7)	0.0620 (6)	0.0644 (6)	−0.0001 (5)	0.0105 (5)	−0.0193 (5)
O7	0.080 (8)	0.082 (8)	0.097 (8)	−0.018 (7)	−0.012 (6)	−0.023 (7)

Geometric parameters (Å, º) top

C1—C2	1.415 (5)	C24—C25	1.577 (6)
C1—C5	1.463 (5)	C24—H24A	0.9700
C1—S1	1.685 (4)	C24—H24B	0.9700
C2—C3	1.451 (5)	C25—C26	1.475 (6)
C2—S2	1.699 (4)	C25—H25A	0.9700
C3—O1	1.224 (5)	C25—H25B	0.9700
C3—C4	1.504 (6)	C26—H26A	0.9600
C4—O2	1.214 (4)	C26—H26B	0.9600
C4—C5	1.490 (5)	C26—H26C	0.9600
C5—O3	1.222 (4)	C27—C28	1.498 (6)
C6—C7	1.402 (5)	C27—N2	1.512 (4)
C6—C10	1.468 (5)	C27—H27A	0.9700
C6—S3	1.683 (4)	C27—H27B	0.9700
C7—C8	1.478 (5)	C28—C29	1.506 (5)
C7—S4	1.693 (4)	C28—H28A	0.9700
C8—O4	1.215 (5)	C28—H28B	0.9700
C8—C9	1.480 (6)	C29—C30	1.520 (6)
C9—O5	1.222 (5)	C29—H29A	0.9700
C9—C10	1.505 (6)	C29—H29B	0.9700
C10—O6	1.209 (5)	C30—H30A	0.9600
C11—C12	1.513 (5)	C30—H30B	0.9600
C11—N1	1.514 (5)	C30—H30C	0.9600
C11—H11A	0.9700	C31—C32	1.513 (5)
C11—H11B	0.9700	C31—N2	1.514 (5)
C12—C13	1.554 (8)	C31—H31A	0.9700
C12—H12A	0.9700	C31—H31B	0.9700
C12—H12B	0.9700	C32—C33	1.501 (5)
C13—C14	1.526 (9)	C32—H32A	0.9700
C13—H13A	0.9700	C32—H32B	0.9700
C13—H13B	0.9700	C33—C34	1.524 (6)
C14—H14A	0.9600	C33—H33A	0.9700
C14—H14B	0.9600	C33—H33B	0.9700
C14—H14C	0.9600	C34—H34A	0.9600
C13'—C14'	1.538 (10)	C34—H34B	0.9600
C13'—H13C	0.9700	C34—H34C	0.9600
C13'—H13D	0.9700	C35—C36	1.518 (5)
C14'—H14D	0.9600	C35—N2	1.519 (5)
C14'—H14E	0.9600	C35—H35A	0.9700
C14'—H14F	0.9600	C35—H35B	0.9700
C15—C16	1.499 (5)	C36—C37	1.518 (6)
C15—N1	1.522 (5)	C36—H36A	0.9700
C15—H15A	0.9700	C36—H36B	0.9700
C15—H15B	0.9700	C37—C38	1.502 (7)
C16—C17	1.520 (5)	C37—H37A	0.9700
C16—H16A	0.9700	C37—H37B	0.9700
C16—H16B	0.9700	C38—H38A	0.9600
C17—C18	1.507 (6)	C38—H38B	0.9600
C17—H17A	0.9700	C38—H38C	0.9600
C17—H17B	0.9700	C39—C40	1.514 (5)
C18—H18A	0.9600	C39—N2	1.529 (4)
C18—H18B	0.9600	C39—H39A	0.9700
C18—H18C	0.9600	C39—H39B	0.9700
C19—N1	1.511 (5)	C40—C41	1.568 (6)
C19—C20	1.524 (4)	C40—H40A	0.9700
C19—H19A	0.9700	C40—H40B	0.9700
C19—H19B	0.9700	C41—C42	1.450 (7)
C20—C21	1.550 (4)	C41—H41A	0.9700
C20—H20A	0.9700	C41—H41B	0.9700
C20—H20B	0.9700	C42—H42A	0.9600
C21—C22	1.492 (5)	C42—H42B	0.9600
C21—H21A	0.9700	C42—H42C	0.9600
C21—H21B	0.9700	C41'—H41C	0.9700
C22—H22A	0.9600	C41'—H41D	0.9700
C22—H22B	0.9600	Cd1—S3	2.5254 (13)
C22—H22C	0.9600	Cd1—S4	2.5296 (13)
C23—C24	1.503 (5)	Cd1—S2	2.5315 (15)
C23—N1	1.511 (5)	Cd1—S1	2.5413 (12)
C23—H23A	0.9700	O7—H1O7	0.8499
C23—H23B	0.9700	O7—H2O7	0.8500

C2—C1—C5	108.9 (3)	H25A—C25—H25B	108.1
C2—C1—S1	128.7 (3)	C25—C26—H26A	109.5
C5—C1—S1	122.4 (3)	C25—C26—H26B	109.5
C1—C2—C3	110.7 (3)	H26A—C26—H26B	109.5
C1—C2—S2	127.9 (3)	C25—C26—H26C	109.5
C3—C2—S2	121.4 (3)	H26A—C26—H26C	109.5
O1—C3—C2	128.6 (4)	H26B—C26—H26C	109.5
O1—C3—C4	125.0 (4)	C28—C27—N2	115.9 (3)
C2—C3—C4	106.4 (3)	C28—C27—H27A	108.3
O2—C4—C5	126.5 (4)	N2—C27—H27A	108.3
O2—C4—C3	126.8 (4)	C28—C27—H27B	108.3
C5—C4—C3	106.7 (3)	N2—C27—H27B	108.3
O3—C5—C1	128.0 (4)	H27A—C27—H27B	107.4
O3—C5—C4	124.7 (3)	C27—C28—C29	110.8 (3)
C1—C5—C4	107.3 (3)	C27—C28—H28A	109.5
C7—C6—C10	110.1 (3)	C29—C28—H28A	109.5
C7—C6—S3	128.4 (3)	C27—C28—H28B	109.5
C10—C6—S3	121.5 (3)	C29—C28—H28B	109.5
C6—C7—C8	109.2 (3)	H28A—C28—H28B	108.1
C6—C7—S4	128.4 (3)	C28—C29—C30	113.3 (4)
C8—C7—S4	122.4 (3)	C28—C29—H29A	108.9
O4—C8—C7	126.6 (4)	C30—C29—H29A	108.9
O4—C8—C9	125.9 (4)	C28—C29—H29B	108.9
C7—C8—C9	107.4 (3)	C30—C29—H29B	108.9
O5—C9—C8	127.6 (4)	H29A—C29—H29B	107.7
O5—C9—C10	125.7 (4)	C29—C30—H30A	109.5
C8—C9—C10	106.6 (3)	C29—C30—H30B	109.5
O6—C10—C6	127.9 (4)	H30A—C30—H30B	109.5
O6—C10—C9	125.5 (4)	C29—C30—H30C	109.5
C6—C10—C9	106.6 (3)	H30A—C30—H30C	109.5
C12—C11—N1	116.5 (3)	H30B—C30—H30C	109.5
C12—C11—H11A	108.2	C32—C31—N2	116.8 (3)
N1—C11—H11A	108.2	C32—C31—H31A	108.1
C12—C11—H11B	108.2	N2—C31—H31A	108.1
N1—C11—H11B	108.2	C32—C31—H31B	108.1
H11A—C11—H11B	107.3	N2—C31—H31B	108.1
C11—C12—C13	107.9 (5)	H31A—C31—H31B	107.3
C11—C12—H12A	110.1	C33—C32—C31	111.1 (3)
C13—C12—H12A	110.1	C33—C32—H32A	109.4
C11—C12—H12B	110.1	C31—C32—H32A	109.4
C13—C12—H12B	110.1	C33—C32—H32B	109.4
H12A—C12—H12B	108.4	C31—C32—H32B	109.4
C14—C13—C12	110.3 (8)	H32A—C32—H32B	108.0
C14—C13—H13A	109.6	C32—C33—C34	112.9 (4)
C12—C13—H13A	109.6	C32—C33—H33A	109.0
C14—C13—H13B	109.6	C34—C33—H33A	109.0
C12—C13—H13B	109.6	C32—C33—H33B	109.0
H13A—C13—H13B	108.1	C34—C33—H33B	109.0
C13—C14—H14A	109.5	H33A—C33—H33B	107.8
C13—C14—H14B	109.5	C33—C34—H34A	109.5
H14A—C14—H14B	109.5	C33—C34—H34B	109.5
C13—C14—H14C	109.5	H34A—C34—H34B	109.5
H14A—C14—H14C	109.5	C33—C34—H34C	109.5
H14B—C14—H14C	109.5	H34A—C34—H34C	109.5
C14'—C13'—H13C	109.9	H34B—C34—H34C	109.5
C14'—C13'—H13D	109.9	C36—C35—N2	116.0 (3)
H13C—C13'—H13D	108.3	C36—C35—H35A	108.3
C13'—C14'—H14D	109.5	N2—C35—H35A	108.3
C13'—C14'—H14E	109.5	C36—C35—H35B	108.3
H14D—C14'—H14E	109.5	N2—C35—H35B	108.3
C13'—C14'—H14F	109.5	H35A—C35—H35B	107.4
H14D—C14'—H14F	109.5	C37—C36—C35	110.7 (4)
H14E—C14'—H14F	109.5	C37—C36—H36A	109.5
C16—C15—N1	115.8 (3)	C35—C36—H36A	109.5
C16—C15—H15A	108.3	C37—C36—H36B	109.5
N1—C15—H15A	108.3	C35—C36—H36B	109.5
C16—C15—H15B	108.3	H36A—C36—H36B	108.1
N1—C15—H15B	108.3	C38—C37—C36	113.7 (4)
H15A—C15—H15B	107.4	C38—C37—H37A	108.8
C15—C16—C17	111.2 (4)	C36—C37—H37A	108.8
C15—C16—H16A	109.4	C38—C37—H37B	108.8
C17—C16—H16A	109.4	C36—C37—H37B	108.8
C15—C16—H16B	109.4	H37A—C37—H37B	107.7
C17—C16—H16B	109.4	C37—C38—H38A	109.5
H16A—C16—H16B	108.0	C37—C38—H38B	109.5
C18—C17—C16	111.5 (4)	H38A—C38—H38B	109.5
C18—C17—H17A	109.3	C37—C38—H38C	109.5
C16—C17—H17A	109.3	H38A—C38—H38C	109.5
C18—C17—H17B	109.3	H38B—C38—H38C	109.5
C16—C17—H17B	109.3	C40—C39—N2	116.5 (3)
H17A—C17—H17B	108.0	C40—C39—H39A	108.2
C17—C18—H18A	109.5	N2—C39—H39A	108.2
C17—C18—H18B	109.5	C40—C39—H39B	108.2
H18A—C18—H18B	109.5	N2—C39—H39B	108.2
C17—C18—H18C	109.5	H39A—C39—H39B	107.3
H18A—C18—H18C	109.5	C39—C40—C41	111.5 (4)
H18B—C18—H18C	109.5	C39—C40—H40A	109.3
N1—C19—C20	116.7 (3)	C41—C40—H40A	109.3
N1—C19—H19A	108.1	C39—C40—H40B	109.3
C20—C19—H19A	108.1	C41—C40—H40B	109.3
N1—C19—H19B	108.1	H40A—C40—H40B	108.0
C20—C19—H19B	108.1	C42—C41—C40	114.0 (6)
H19A—C19—H19B	107.3	C42—C41—H41A	108.7
C19—C20—C21	106.2 (4)	C40—C41—H41A	108.7
C19—C20—H20A	110.5	C42—C41—H41B	108.7
C21—C20—H20A	110.5	C40—C41—H41B	108.7
C19—C20—H20B	110.5	H41A—C41—H41B	107.6
C21—C20—H20B	110.5	C41—C42—H42A	109.5
H20A—C20—H20B	108.7	C41—C42—H42B	109.5
C22—C21—C20	116.7 (5)	H42A—C42—H42B	109.5
C22—C21—H21A	108.1	C41—C42—H42C	109.5
C20—C21—H21A	108.1	H42A—C42—H42C	109.5
C22—C21—H21B	108.1	H42B—C42—H42C	109.5
C20—C21—H21B	108.1	H41C—C41'—H41D	107.8
H21A—C21—H21B	107.3	S3—Cd1—S4	87.62 (4)
C21—C22—H22A	109.5	S3—Cd1—S2	125.26 (5)
C21—C22—H22B	109.5	S4—Cd1—S2	119.07 (4)
H22A—C22—H22B	109.5	S3—Cd1—S1	116.04 (4)
C21—C22—H22C	109.5	S4—Cd1—S1	125.49 (4)
H22A—C22—H22C	109.5	S2—Cd1—S1	87.59 (3)
H22B—C22—H22C	109.5	C19—N1—C23	104.1 (3)
C24—C23—N1	116.0 (3)	C19—N1—C11	111.6 (3)
C24—C23—H23A	108.3	C23—N1—C11	112.0 (3)
N1—C23—H23A	108.3	C19—N1—C15	113.0 (3)
C24—C23—H23B	108.3	C23—N1—C15	111.3 (3)
N1—C23—H23B	108.3	C11—N1—C15	105.0 (3)
H23A—C23—H23B	107.4	C27—N2—C31	111.9 (3)
C23—C24—C25	107.0 (4)	C27—N2—C35	106.0 (3)
C23—C24—H24A	110.3	C31—N2—C35	112.0 (3)
C25—C24—H24A	110.3	C27—N2—C39	111.0 (3)
C23—C24—H24B	110.3	C31—N2—C39	105.8 (3)
C25—C24—H24B	110.3	C35—N2—C39	110.2 (3)
H24A—C24—H24B	108.6	C1—S1—Cd1	97.67 (12)
C26—C25—C24	110.6 (5)	C2—S2—Cd1	97.87 (13)
C26—C25—H25A	109.5	C6—S3—Cd1	97.98 (13)
C24—C25—H25A	109.5	C7—S4—Cd1	97.59 (12)
C26—C25—H25B	109.5	H1O7—O7—H2O7	107.7
C24—C25—H25B	109.5

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C12—H12A···O6ⁱ	0.97	2.48	3.412 (6)	161
C14—H14C···S2ⁱⁱ	0.97	2.70	3.472 (10)	137
C16—H16B···O2ⁱⁱⁱ	0.97	2.54	3.483 (7)	163

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

Experimental details

Crystal data
Chemical formula	(C₁₆H₃₆N)₂[Cd(C₅O₃S₂)₂]·0.25H₂O
M_r	946.16
Crystal system, space group	Triclinic, P1
Temperature (K)	293
a, b, c (Å)	9.820 (5), 15.002 (5), 17.406 (5)
α, β, γ (°)	74.853 (5), 86.898 (5), 87.705 (5)
V (Å³)	2470.6 (17)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	0.65
Crystal size (mm)	0.24 × 0.18 × 0.15

Data collection
Diffractometer	Oxford Diffraction CCD area-detector
Absorption correction	Multi-scan (CrysAlis RED; Oxford Diffraction, 2007)
T_min, T_max	0.775, 0.858
No. of measured, independent and observed [I > 2σ(I)] reflections	30150, 10069, 6510
R_int	0.032
(sin θ/λ)_max (Å⁻¹)	0.625

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.050, 0.144, 1.04
No. of reflections	10069
No. of parameters	534
No. of restraints	54
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.72, −0.42

Computer programs: CrysAlis PRO (Oxford Diffraction, 2007), CrysAlis RED (Oxford Diffraction, 2007), SIR97 (Altomare et al., 1999), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008), WinGX (Farrugia, 1999).

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C12—H12A···O6ⁱ	0.97	2.48	3.412 (6)	161
C14—H14C···S2ⁱⁱ	0.97	2.70	3.472 (10)	137
C16—H16B···O2ⁱⁱⁱ	0.97	2.54	3.483 (7)	163

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

Acknowledgements

This work was supported by the Shandong Key Scientific and Technological Project (2008 GG30002014), the Project of the Key Laboratory of Photochemical Conversion and Optoelectronic Materials, the TIPC and the Chinese Academy of Sciences

References

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