Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807026189/hb2435sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807026189/hb2435Isup2.hkl |
CCDC reference: 657598
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.003 Å
- R factor = 0.028
- wR factor = 0.078
- Data-to-parameter ratio = 14.6
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.98 PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.81 Ratio PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.12 Ratio
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K PLAT794_ALERT_5_G Check Predicted Bond Valency for Cu1 (2) 2.10
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
Thiophenol (630 mg, 5.7 mmol) was added to a stirred solution of KOH (320 mg, 5.7 mmol) in ethanol (30 ml). The mixture was refluxed for 30 min and a solution of 2-bromomethylpyridine (986 mg, 5.7 mmol) in ethanol (25 ml) was slowly added to it. The mixture was refluxed for 4 h more. The KBr precipitate was filtered off, and the filtrate was washed by water and evaporated to obtain ligand L as a brown oil in 40% yield. A solution (5.0 ml) of Cu(OAc)2 (0.1 mmol) and L (0.2 mmol) in methanol/chloroform (1:1 v/v) was stirred for 30 min at room temperature, and then filtered. Green single crystals of (I) were obtained from the filtrate.
The H atoms were positioned geometrically (C—H = 0.93–0.97 Å) and refined as riding with Uiso(H) = 1.2Ueq(C).
In the preparation of CuII complex with the ligand, 2-(phenylsulfanyl)methylpyridine (L), we obtained the title compound, (I), (Fig. 1).
The complex consists of a centrosymmetric dicopper(II) core with four acetate anions bridging the two copper atoms and two monodentate L ligands. The intradimer Cu···Cui (i = -x, 1 - y, -z) distance is 2.6309 (6) Å, which is similar to that (2.63 Å) in [Cu(O2CPh)2(DMF)]2 (Del Sesto et al., 2000). The copper ion in (I) presents a nearly square pyramidal geometry with four oxygen atoms in a plane, at a mean distance of 1.971 (2) Å. The axial site is occupied by the pyridine N atom of a ligand molecule at 2.232 (2) Å. The CuII ion is displaced from the basal plane towards the apical N atom by 0.199 (2) A. The L ligand takes a gauche conformation with a C6—S1—C7—C8 torsion angle of 76.8 (2)° between the two aryl groups.
For a related structure and background, see: Del Sesto et al. (2000).
Data collection: RAPID-AUTO (Rigaku, 2004); cell refinement: RAPID-AUTO; data reduction: RAPID-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: CrystalStructure (Rigaku, 2004).
Fig. 1. View of (I) with 30% probability displacement ellipsoids (arbitrary spheres of H atoms). Symmetry code: (i) -x, 1 - y, -z. |
[Cu2(C2H3O2)4(C12H11NS)2] | Z = 1 |
Mr = 765.85 | F(000) = 394 |
Triclinic, P1 | Dx = 1.551 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 7.7587 (16) Å | Cell parameters from 7557 reflections |
b = 7.9690 (16) Å | θ = 3.1–27.5° |
c = 13.986 (3) Å | µ = 1.48 mm−1 |
α = 102.51 (3)° | T = 293 K |
β = 101.86 (2)° | Block, green |
γ = 94.29 (3)° | 0.34 × 0.33 × 0.30 mm |
V = 819.7 (3) Å3 |
Rigaku R-AXIS RAPID IP area-detector diffractometer | 3029 independent reflections |
Radiation source: rotating anode | 2859 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.029 |
ω scans | θmax = 25.5°, θmin = 3.1° |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | h = −9→9 |
Tmin = 0.622, Tmax = 0.652 | k = −9→8 |
6775 measured reflections | l = −16→16 |
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)] = 0.028 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.078 | H-atom parameters constrained |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0382P)2 + 0.5716P] where P = (Fo2 + 2Fc2)/3 |
3029 reflections | (Δ/σ)max = 0.001 |
208 parameters | Δρmax = 0.41 e Å−3 |
0 restraints | Δρmin = −0.37 e Å−3 |
[Cu2(C2H3O2)4(C12H11NS)2] | γ = 94.29 (3)° |
Mr = 765.85 | V = 819.7 (3) Å3 |
Triclinic, P1 | Z = 1 |
a = 7.7587 (16) Å | Mo Kα radiation |
b = 7.9690 (16) Å | µ = 1.48 mm−1 |
c = 13.986 (3) Å | T = 293 K |
α = 102.51 (3)° | 0.34 × 0.33 × 0.30 mm |
β = 101.86 (2)° |
Rigaku R-AXIS RAPID IP area-detector diffractometer | 3029 independent reflections |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | 2859 reflections with I > 2σ(I) |
Tmin = 0.622, Tmax = 0.652 | Rint = 0.029 |
6775 measured reflections |
R[F2 > 2σ(F2)] = 0.028 | 0 restraints |
wR(F2) = 0.078 | H-atom parameters constrained |
S = 1.05 | Δρmax = 0.41 e Å−3 |
3029 reflections | Δρmin = −0.37 e Å−3 |
208 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
S1 | 0.15681 (7) | 1.02827 (7) | 0.41049 (4) | 0.02382 (14) | |
N1 | 0.3502 (2) | 0.7760 (2) | 0.18067 (12) | 0.0167 (3) | |
Cu1 | 0.12181 (3) | 0.60867 (3) | 0.069933 (16) | 0.01511 (10) | |
O1 | −0.0394 (2) | 0.78294 (19) | 0.04802 (11) | 0.0230 (3) | |
O2 | −0.2453 (2) | 0.59886 (19) | −0.07185 (12) | 0.0271 (4) | |
O3 | −0.0150 (2) | 0.5378 (2) | 0.16144 (11) | 0.0245 (3) | |
O4 | −0.2209 (2) | 0.3513 (2) | 0.04359 (11) | 0.0259 (3) | |
C1 | 0.2586 (3) | 1.3074 (3) | 0.33349 (17) | 0.0296 (5) | |
H1A | 0.2590 | 1.2289 | 0.2737 | 0.036* | |
C2 | 0.3046 (4) | 1.4820 (3) | 0.34379 (19) | 0.0377 (6) | |
H2A | 0.3354 | 1.5205 | 0.2906 | 0.045* | |
C3 | 0.3055 (4) | 1.5996 (3) | 0.4319 (2) | 0.0416 (6) | |
H3A | 0.3386 | 1.7170 | 0.4388 | 0.050* | |
C4 | 0.2570 (5) | 1.5422 (4) | 0.5097 (2) | 0.0471 (7) | |
H4A | 0.2558 | 1.6216 | 0.5690 | 0.057* | |
C5 | 0.2101 (4) | 1.3675 (3) | 0.50064 (19) | 0.0375 (6) | |
H5A | 0.1776 | 1.3298 | 0.5536 | 0.045* | |
C6 | 0.2118 (3) | 1.2487 (3) | 0.41206 (16) | 0.0236 (5) | |
C7 | 0.1672 (3) | 0.9108 (3) | 0.28692 (15) | 0.0213 (4) | |
H7A | 0.1012 | 0.7968 | 0.2738 | 0.026* | |
H7B | 0.1066 | 0.9697 | 0.2385 | 0.026* | |
C8 | 0.3503 (3) | 0.8875 (3) | 0.26746 (15) | 0.0168 (4) | |
C9 | 0.5058 (3) | 0.9744 (3) | 0.33319 (16) | 0.0236 (5) | |
H9A | 0.5022 | 1.0513 | 0.3929 | 0.028* | |
C10 | 0.6667 (3) | 0.9446 (3) | 0.30849 (17) | 0.0275 (5) | |
H10A | 0.7727 | 1.0007 | 0.3517 | 0.033* | |
C11 | 0.6675 (3) | 0.8307 (3) | 0.21884 (18) | 0.0268 (5) | |
H11A | 0.7737 | 0.8097 | 0.2002 | 0.032* | |
C12 | 0.5073 (3) | 0.7486 (3) | 0.15746 (16) | 0.0224 (4) | |
H12A | 0.5080 | 0.6710 | 0.0974 | 0.027* | |
C13 | −0.1833 (3) | 0.7472 (3) | −0.01779 (15) | 0.0185 (4) | |
C14 | −0.2888 (3) | 0.8945 (3) | −0.03217 (19) | 0.0287 (5) | |
H14A | −0.2322 | 0.9983 | 0.0167 | 0.043* | |
H14B | −0.4067 | 0.8675 | −0.0238 | 0.043* | |
H14C | −0.2948 | 0.9117 | −0.0986 | 0.043* | |
C15 | −0.1492 (3) | 0.4248 (3) | 0.13311 (15) | 0.0201 (4) | |
C16 | −0.2312 (4) | 0.3755 (3) | 0.21380 (18) | 0.0355 (6) | |
H16A | −0.3240 | 0.2808 | 0.1837 | 0.053* | |
H16B | −0.2796 | 0.4730 | 0.2471 | 0.053* | |
H16C | −0.1419 | 0.3412 | 0.2618 | 0.053* |
U11 | U22 | U33 | U12 | U13 | U23 | |
S1 | 0.0221 (3) | 0.0269 (3) | 0.0200 (3) | −0.0009 (2) | 0.0070 (2) | −0.0002 (2) |
N1 | 0.0151 (8) | 0.0168 (8) | 0.0174 (8) | 0.0000 (6) | 0.0027 (6) | 0.0037 (7) |
Cu1 | 0.01397 (14) | 0.01466 (15) | 0.01485 (14) | −0.00007 (9) | 0.00168 (9) | 0.00172 (10) |
O1 | 0.0225 (8) | 0.0181 (7) | 0.0248 (8) | 0.0029 (6) | 0.0003 (6) | 0.0020 (6) |
O2 | 0.0206 (8) | 0.0187 (8) | 0.0350 (9) | 0.0029 (6) | −0.0038 (6) | 0.0006 (7) |
O3 | 0.0280 (8) | 0.0255 (8) | 0.0175 (7) | −0.0063 (6) | 0.0046 (6) | 0.0036 (6) |
O4 | 0.0232 (8) | 0.0316 (9) | 0.0193 (7) | −0.0075 (6) | 0.0058 (6) | 0.0011 (6) |
C1 | 0.0370 (13) | 0.0312 (13) | 0.0189 (10) | 0.0094 (10) | 0.0038 (9) | 0.0031 (9) |
C2 | 0.0503 (16) | 0.0350 (14) | 0.0304 (13) | 0.0098 (12) | 0.0052 (11) | 0.0156 (11) |
C3 | 0.0603 (18) | 0.0260 (13) | 0.0348 (14) | 0.0091 (12) | 0.0001 (12) | 0.0083 (11) |
C4 | 0.081 (2) | 0.0278 (14) | 0.0295 (13) | 0.0116 (13) | 0.0139 (14) | −0.0016 (11) |
C5 | 0.0564 (17) | 0.0329 (13) | 0.0252 (12) | 0.0099 (12) | 0.0141 (11) | 0.0049 (11) |
C6 | 0.0198 (10) | 0.0258 (11) | 0.0218 (10) | 0.0062 (8) | 0.0000 (8) | 0.0020 (9) |
C7 | 0.0146 (10) | 0.0241 (11) | 0.0201 (10) | −0.0004 (8) | 0.0025 (8) | −0.0037 (8) |
C8 | 0.0144 (9) | 0.0170 (10) | 0.0177 (9) | −0.0007 (7) | 0.0021 (7) | 0.0042 (8) |
C9 | 0.0191 (10) | 0.0262 (11) | 0.0196 (10) | 0.0005 (8) | 0.0005 (8) | −0.0026 (9) |
C10 | 0.0134 (10) | 0.0337 (13) | 0.0296 (12) | −0.0013 (9) | −0.0013 (8) | 0.0021 (10) |
C11 | 0.0147 (10) | 0.0329 (12) | 0.0315 (12) | 0.0028 (9) | 0.0060 (9) | 0.0040 (10) |
C12 | 0.0177 (10) | 0.0248 (11) | 0.0233 (10) | 0.0024 (8) | 0.0050 (8) | 0.0023 (9) |
C13 | 0.0186 (10) | 0.0187 (10) | 0.0214 (10) | 0.0041 (8) | 0.0091 (8) | 0.0067 (8) |
C14 | 0.0270 (12) | 0.0231 (11) | 0.0358 (12) | 0.0074 (9) | 0.0037 (10) | 0.0088 (10) |
C15 | 0.0235 (11) | 0.0178 (10) | 0.0209 (10) | 0.0040 (8) | 0.0081 (8) | 0.0054 (8) |
C16 | 0.0446 (15) | 0.0380 (14) | 0.0252 (12) | −0.0083 (11) | 0.0165 (11) | 0.0065 (10) |
S1—C6 | 1.771 (2) | C4—C5 | 1.384 (4) |
S1—C7 | 1.799 (2) | C4—H4A | 0.9300 |
N1—C8 | 1.340 (3) | C5—C6 | 1.390 (3) |
N1—C12 | 1.345 (3) | C5—H5A | 0.9300 |
Cu1—O3 | 1.9663 (15) | C7—C8 | 1.517 (3) |
Cu1—O1 | 1.9680 (16) | C7—H7A | 0.9700 |
Cu1—N1 | 2.2227 (19) | C7—H7B | 0.9700 |
Cu1—O4i | 1.9743 (16) | C8—C9 | 1.387 (3) |
Cu1—O2i | 1.9746 (16) | C9—C10 | 1.385 (3) |
Cu1—Cu1i | 2.6309 (13) | C9—H9A | 0.9300 |
O1—C13 | 1.262 (3) | C10—C11 | 1.381 (3) |
O2—C13 | 1.257 (3) | C10—H10A | 0.9300 |
O2—Cu1i | 1.9746 (16) | C11—C12 | 1.381 (3) |
O3—C15 | 1.260 (3) | C11—H11A | 0.9300 |
O4—C15 | 1.252 (3) | C12—H12A | 0.9300 |
O4—Cu1i | 1.9743 (16) | C13—C14 | 1.505 (3) |
C1—C2 | 1.379 (4) | C14—H14A | 0.9600 |
C1—C6 | 1.385 (3) | C14—H14B | 0.9600 |
C1—H1A | 0.9300 | C14—H14C | 0.9600 |
C2—C3 | 1.376 (4) | C15—C16 | 1.511 (3) |
C2—H2A | 0.9300 | C16—H16A | 0.9600 |
C3—C4 | 1.376 (4) | C16—H16B | 0.9600 |
C3—H3A | 0.9300 | C16—H16C | 0.9600 |
C6—S1—C7 | 104.84 (11) | C1—C6—S1 | 124.78 (17) |
C8—N1—C12 | 118.22 (17) | C8—C7—S1 | 117.10 (14) |
C8—N1—Cu1 | 128.57 (13) | C8—C7—H7A | 108.0 |
C12—N1—Cu1 | 113.04 (13) | S1—C7—H7A | 108.0 |
O3—Cu1—O1 | 89.29 (7) | C8—C7—H7B | 108.0 |
O3—Cu1—O4i | 168.33 (6) | S1—C7—H7B | 108.0 |
O1—Cu1—O4i | 89.15 (7) | H7A—C7—H7B | 107.3 |
O3—Cu1—O2i | 88.87 (7) | N1—C8—C9 | 122.23 (18) |
O1—Cu1—O2i | 168.47 (6) | N1—C8—C7 | 114.47 (17) |
O4i—Cu1—O2i | 90.36 (8) | C9—C8—C7 | 123.30 (18) |
O3—Cu1—N1 | 100.28 (6) | C10—C9—C8 | 118.96 (19) |
O1—Cu1—N1 | 100.09 (7) | C10—C9—H9A | 120.5 |
O4i—Cu1—N1 | 91.38 (6) | C8—C9—H9A | 120.5 |
O2i—Cu1—N1 | 91.44 (7) | C11—C10—C9 | 119.1 (2) |
O3—Cu1—Cu1i | 83.62 (5) | C11—C10—H10A | 120.4 |
O1—Cu1—Cu1i | 85.08 (5) | C9—C10—H10A | 120.4 |
O4i—Cu1—Cu1i | 84.73 (5) | C12—C11—C10 | 118.6 (2) |
O2i—Cu1—Cu1i | 83.41 (5) | C12—C11—H11A | 120.7 |
N1—Cu1—Cu1i | 173.51 (5) | C10—C11—H11A | 120.7 |
C13—O1—Cu1 | 122.22 (14) | N1—C12—C11 | 122.9 (2) |
C13—O2—Cu1i | 124.00 (14) | N1—C12—H12A | 118.6 |
C15—O3—Cu1 | 123.84 (14) | C11—C12—H12A | 118.6 |
C15—O4—Cu1i | 122.33 (14) | O2—C13—O1 | 125.2 (2) |
C2—C1—C6 | 120.1 (2) | O2—C13—C14 | 117.68 (19) |
C2—C1—H1A | 120.0 | O1—C13—C14 | 117.14 (19) |
C6—C1—H1A | 120.0 | C13—C14—H14A | 109.5 |
C1—C2—C3 | 120.7 (2) | C13—C14—H14B | 109.5 |
C1—C2—H2A | 119.7 | H14A—C14—H14B | 109.5 |
C3—C2—H2A | 119.7 | C13—C14—H14C | 109.5 |
C4—C3—C2 | 119.5 (3) | H14A—C14—H14C | 109.5 |
C4—C3—H3A | 120.3 | H14B—C14—H14C | 109.5 |
C2—C3—H3A | 120.3 | O4—C15—O3 | 125.3 (2) |
C3—C4—C5 | 120.7 (2) | O4—C15—C16 | 117.43 (19) |
C3—C4—H4A | 119.7 | O3—C15—C16 | 117.25 (19) |
C5—C4—H4A | 119.7 | C15—C16—H16A | 109.5 |
C4—C5—C6 | 119.7 (2) | C15—C16—H16B | 109.5 |
C4—C5—H5A | 120.1 | H16A—C16—H16B | 109.5 |
C6—C5—H5A | 120.1 | C15—C16—H16C | 109.5 |
C5—C6—C1 | 119.4 (2) | H16A—C16—H16C | 109.5 |
C5—C6—S1 | 115.81 (19) | H16B—C16—H16C | 109.5 |
C8—N1—Cu1—O3 | −38.69 (18) | C2—C1—C6—S1 | −177.9 (2) |
C12—N1—Cu1—O3 | 136.51 (15) | C7—S1—C6—C5 | 179.03 (18) |
C8—N1—Cu1—O1 | 52.42 (18) | C7—S1—C6—C1 | −2.4 (2) |
C12—N1—Cu1—O1 | −132.38 (15) | C6—S1—C7—C8 | 76.80 (19) |
C8—N1—Cu1—O4i | 141.80 (18) | C12—N1—C8—C9 | 0.0 (3) |
C12—N1—Cu1—O4i | −43.00 (16) | Cu1—N1—C8—C9 | 175.01 (15) |
C8—N1—Cu1—O2i | −127.81 (18) | C12—N1—C8—C7 | 179.67 (19) |
C12—N1—Cu1—O2i | 47.39 (16) | Cu1—N1—C8—C7 | −5.3 (3) |
O3—Cu1—O1—C13 | −86.13 (16) | S1—C7—C8—N1 | 169.58 (15) |
O4i—Cu1—O1—C13 | 82.31 (16) | S1—C7—C8—C9 | −10.8 (3) |
O2i—Cu1—O1—C13 | −5.3 (4) | N1—C8—C9—C10 | −0.2 (3) |
N1—Cu1—O1—C13 | 173.56 (15) | C7—C8—C9—C10 | −179.8 (2) |
Cu1i—Cu1—O1—C13 | −2.47 (15) | C8—C9—C10—C11 | 0.6 (4) |
O1—Cu1—O3—C15 | 88.00 (18) | C9—C10—C11—C12 | −0.8 (4) |
O4i—Cu1—O3—C15 | 5.7 (4) | C8—N1—C12—C11 | −0.3 (3) |
O2i—Cu1—O3—C15 | −80.62 (18) | Cu1—N1—C12—C11 | −176.01 (18) |
N1—Cu1—O3—C15 | −171.88 (17) | C10—C11—C12—N1 | 0.7 (4) |
Cu1i—Cu1—O3—C15 | 2.87 (17) | Cu1i—O2—C13—O1 | −3.6 (3) |
C6—C1—C2—C3 | 0.3 (4) | Cu1i—O2—C13—C14 | 176.56 (15) |
C1—C2—C3—C4 | −1.1 (4) | Cu1—O1—C13—O2 | 4.3 (3) |
C2—C3—C4—C5 | 0.9 (5) | Cu1—O1—C13—C14 | −175.83 (14) |
C3—C4—C5—C6 | 0.0 (5) | Cu1i—O4—C15—O3 | 4.3 (3) |
C4—C5—C6—C1 | −0.7 (4) | Cu1i—O4—C15—C16 | −176.35 (16) |
C4—C5—C6—S1 | 177.9 (2) | Cu1—O3—C15—O4 | −5.1 (3) |
C2—C1—C6—C5 | 0.6 (4) | Cu1—O3—C15—C16 | 175.48 (16) |
Symmetry code: (i) −x, −y+1, −z. |
Experimental details
Crystal data | |
Chemical formula | [Cu2(C2H3O2)4(C12H11NS)2] |
Mr | 765.85 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 293 |
a, b, c (Å) | 7.7587 (16), 7.9690 (16), 13.986 (3) |
α, β, γ (°) | 102.51 (3), 101.86 (2), 94.29 (3) |
V (Å3) | 819.7 (3) |
Z | 1 |
Radiation type | Mo Kα |
µ (mm−1) | 1.48 |
Crystal size (mm) | 0.34 × 0.33 × 0.30 |
Data collection | |
Diffractometer | Rigaku R-AXIS RAPID IP area-detector |
Absorption correction | Multi-scan (ABSCOR; Higashi, 1995) |
Tmin, Tmax | 0.622, 0.652 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 6775, 3029, 2859 |
Rint | 0.029 |
(sin θ/λ)max (Å−1) | 0.606 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.028, 0.078, 1.05 |
No. of reflections | 3029 |
No. of parameters | 208 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.41, −0.37 |
Computer programs: RAPID-AUTO (Rigaku, 2004), RAPID-AUTO, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEPII (Johnson, 1976), CrystalStructure (Rigaku, 2004).
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In the preparation of CuII complex with the ligand, 2-(phenylsulfanyl)methylpyridine (L), we obtained the title compound, (I), (Fig. 1).
The complex consists of a centrosymmetric dicopper(II) core with four acetate anions bridging the two copper atoms and two monodentate L ligands. The intradimer Cu···Cui (i = -x, 1 - y, -z) distance is 2.6309 (6) Å, which is similar to that (2.63 Å) in [Cu(O2CPh)2(DMF)]2 (Del Sesto et al., 2000). The copper ion in (I) presents a nearly square pyramidal geometry with four oxygen atoms in a plane, at a mean distance of 1.971 (2) Å. The axial site is occupied by the pyridine N atom of a ligand molecule at 2.232 (2) Å. The CuII ion is displaced from the basal plane towards the apical N atom by 0.199 (2) A. The L ligand takes a gauche conformation with a C6—S1—C7—C8 torsion angle of 76.8 (2)° between the two aryl groups.