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The centrosymmetric title compound, [Cu(C7H8O3S)2(H2O)4], forms a pillared hydrogen-bonded layered network. The coordination geometry of the CuII ion is distorted octahedral, involving four aqua ligands and two N-atom donors of two 2-(4-pyridyl)ethanesulfonate (PES) ligands. The sulfonate group of PES is not involved in coordination to the metal, but participates in hydrogen bonds with the aqua ligands.
Supporting information
CCDC reference: 298538
Key indicators
- Single-crystal X-ray study
- T = 130 K
- Mean (C-C) = 0.007 Å
- R factor = 0.055
- wR factor = 0.141
- Data-to-parameter ratio = 12.8
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.96
PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ?
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.32
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 7
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 4
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
5 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
1 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
2 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens,1994); data reduction: XPREP in SHELXTL (Siemens, 1994); program(s) used to solve structure: SHELXTL; program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
Tetraaquabis[2-(4-pyridyl)ethanesulfonato-
κN]copper(II)
top
Crystal data top
[Cu(C7H8O3S)2(H2O)4] | F(000) = 526 |
Mr = 508.04 | Dx = 1.670 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 2454 reflections |
a = 9.0089 (11) Å | θ = 2.3–25.0° |
b = 8.7859 (11) Å | µ = 1.34 mm−1 |
c = 12.7866 (16) Å | T = 130 K |
β = 93.402 (2)° | Prism, blue |
V = 1010.3 (2) Å3 | 0.30 × 0.20 × 0.10 mm |
Z = 2 | |
Data collection top
Bruker SMART CCD area-detector diffractometer | 1713 independent reflections |
Radiation source: fine-focus sealed tube | 1683 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.031 |
φ and ω scans | θmax = 25.0°, θmin = 2.3° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −10→10 |
Tmin = 0.732, Tmax = 0.874 | k = −7→10 |
2781 measured reflections | l = −7→15 |
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)] = 0.055 | H-atom parameters constrained |
wR(F2) = 0.141 | w = 1/[σ2(Fo2) + (0.0629P)2 + 4.7962P] where P = (Fo2 + 2Fc2)/3 |
S = 1.06 | (Δ/σ)max < 0.001 |
1713 reflections | Δρmax = 0.61 e Å−3 |
134 parameters | Δρmin = −0.69 e Å−3 |
0 restraints | Extinction correction: SHELXTL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.054 (4) |
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 | Uiso*/Ueq | |
Cu1 | 0.5000 | 0.5000 | 0.0000 | 0.0224 (3) | |
S1 | −0.25125 (13) | 0.44924 (14) | 0.40869 (9) | 0.0292 (4) | |
O1 | −0.3247 (5) | 0.5909 (5) | 0.4324 (4) | 0.0658 (14) | |
O1W | 0.6756 (4) | 0.3647 (4) | 0.1164 (3) | 0.0389 (9) | |
H1WA | 0.7151 | 0.2969 | 0.0838 | 0.047* | |
H1WB | 0.6738 | 0.3353 | 0.1768 | 0.047* | |
O2 | −0.1917 (4) | 0.3678 (5) | 0.5009 (3) | 0.0457 (10) | |
O2W | 0.4388 (3) | 0.3003 (4) | −0.0648 (3) | 0.0301 (8) | |
H2WA | 0.4013 | 0.2396 | −0.0272 | 0.036* | |
H2WB | 0.5079 | 0.2574 | −0.0907 | 0.036* | |
O3 | −0.3447 (4) | 0.3516 (4) | 0.3397 (3) | 0.0334 (8) | |
N1 | 0.3374 (4) | 0.4778 (4) | 0.0987 (3) | 0.0226 (8) | |
C1 | 0.3619 (5) | 0.4902 (5) | 0.2025 (4) | 0.0256 (10) | |
H1 | 0.4547 | 0.5237 | 0.2288 | 0.031* | |
C2 | 0.2563 (5) | 0.4558 (6) | 0.2726 (4) | 0.0300 (11) | |
H2 | 0.2784 | 0.4646 | 0.3443 | 0.036* | |
C3 | 0.1150 (5) | 0.4073 (5) | 0.2344 (4) | 0.0281 (10) | |
C4 | 0.0874 (5) | 0.4013 (6) | 0.1267 (4) | 0.0289 (10) | |
H4 | −0.0065 | 0.3748 | 0.0983 | 0.035* | |
C5 | 0.2002 (5) | 0.4351 (5) | 0.0617 (4) | 0.0271 (10) | |
H5 | 0.1808 | 0.4280 | −0.0104 | 0.032* | |
C6 | −0.0038 (5) | 0.3635 (6) | 0.3089 (4) | 0.0336 (12) | |
H6A | −0.0672 | 0.2850 | 0.2768 | 0.040* | |
H6B | 0.0433 | 0.3224 | 0.3730 | 0.040* | |
C7 | −0.0977 (5) | 0.5005 (5) | 0.3346 (4) | 0.0293 (11) | |
H7A | −0.1343 | 0.5490 | 0.2700 | 0.035* | |
H7B | −0.0361 | 0.5735 | 0.3741 | 0.035* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cu1 | 0.0202 (4) | 0.0233 (5) | 0.0250 (5) | −0.0027 (3) | 0.0111 (3) | −0.0020 (3) |
S1 | 0.0293 (6) | 0.0296 (7) | 0.0307 (6) | −0.0061 (5) | 0.0173 (5) | −0.0052 (5) |
O1 | 0.070 (3) | 0.036 (2) | 0.098 (4) | 0.004 (2) | 0.058 (3) | −0.015 (2) |
O1W | 0.048 (2) | 0.042 (2) | 0.0273 (18) | 0.0101 (17) | 0.0081 (15) | 0.0049 (16) |
O2 | 0.043 (2) | 0.069 (3) | 0.0261 (18) | −0.020 (2) | 0.0082 (15) | 0.0087 (18) |
O2W | 0.0287 (16) | 0.0265 (17) | 0.0368 (18) | −0.0013 (14) | 0.0173 (14) | −0.0016 (14) |
O3 | 0.0278 (17) | 0.044 (2) | 0.0292 (17) | −0.0105 (15) | 0.0093 (13) | 0.0007 (15) |
N1 | 0.0173 (17) | 0.024 (2) | 0.027 (2) | 0.0001 (14) | 0.0076 (15) | 0.0021 (15) |
C1 | 0.019 (2) | 0.030 (3) | 0.029 (2) | 0.0008 (18) | 0.0050 (18) | −0.0042 (19) |
C2 | 0.033 (2) | 0.034 (3) | 0.024 (2) | 0.001 (2) | 0.0094 (19) | 0.001 (2) |
C3 | 0.026 (2) | 0.021 (2) | 0.039 (3) | 0.0057 (19) | 0.0181 (19) | 0.006 (2) |
C4 | 0.018 (2) | 0.031 (3) | 0.038 (3) | 0.0010 (19) | 0.0080 (18) | 0.004 (2) |
C5 | 0.029 (2) | 0.025 (2) | 0.027 (2) | 0.0027 (19) | 0.0050 (19) | 0.0023 (19) |
C6 | 0.031 (2) | 0.030 (3) | 0.042 (3) | 0.004 (2) | 0.019 (2) | 0.011 (2) |
C7 | 0.029 (2) | 0.023 (2) | 0.038 (3) | −0.0069 (19) | 0.018 (2) | 0.0010 (19) |
Geometric parameters (Å, º) top
Cu1—N1 | 1.999 (4) | N1—C5 | 1.351 (6) |
Cu1—N1i | 1.999 (4) | C1—C2 | 1.379 (6) |
Cu1—O2Wi | 2.004 (3) | C1—H1 | 0.9300 |
Cu1—O2W | 2.004 (3) | C2—C3 | 1.402 (7) |
Cu1—O1Wi | 2.419 (3) | C2—H2 | 0.9300 |
Cu1—O1W | 2.419 (3) | C3—C4 | 1.387 (7) |
S1—O1 | 1.450 (4) | C3—C6 | 1.524 (6) |
S1—O2 | 1.455 (4) | C4—C5 | 1.382 (6) |
S1—O3 | 1.460 (4) | C4—H4 | 0.9300 |
S1—C7 | 1.780 (4) | C5—H5 | 0.9300 |
O1W—H1WA | 0.8200 | C6—C7 | 1.518 (7) |
O1W—H1WB | 0.8152 | C6—H6A | 0.9700 |
O2W—H2WA | 0.8058 | C6—H6B | 0.9700 |
O2W—H2WB | 0.8143 | C7—H7A | 0.9700 |
N1—C1 | 1.338 (6) | C7—H7B | 0.9700 |
| | | |
N1—Cu1—N1i | 180.0 (2) | C5—N1—Cu1 | 119.7 (3) |
N1—Cu1—O2Wi | 91.04 (14) | N1—C1—C2 | 123.2 (4) |
N1i—Cu1—O2Wi | 88.96 (14) | N1—C1—H1 | 118.4 |
N1—Cu1—O2W | 88.96 (14) | C2—C1—H1 | 118.4 |
N1i—Cu1—O2W | 91.04 (14) | C1—C2—C3 | 119.2 (4) |
O2Wi—Cu1—O2W | 180.00 (17) | C1—C2—H2 | 120.4 |
N1—Cu1—O1Wi | 87.67 (14) | C3—C2—H2 | 120.4 |
N1i—Cu1—O1Wi | 92.33 (14) | C4—C3—C2 | 117.6 (4) |
O2Wi—Cu1—O1Wi | 88.74 (13) | C4—C3—C6 | 121.3 (4) |
O2W—Cu1—O1Wi | 91.26 (13) | C2—C3—C6 | 121.1 (4) |
N1—Cu1—O1W | 92.33 (14) | C5—C4—C3 | 119.6 (4) |
N1i—Cu1—O1W | 87.67 (14) | C5—C4—H4 | 120.2 |
O2Wi—Cu1—O1W | 91.26 (13) | C3—C4—H4 | 120.2 |
O2W—Cu1—O1W | 88.74 (13) | N1—C5—C4 | 122.7 (4) |
O1Wi—Cu1—O1W | 180.00 (16) | N1—C5—H5 | 118.7 |
O1—S1—O2 | 113.8 (3) | C4—C5—H5 | 118.7 |
O1—S1—O3 | 112.1 (3) | C7—C6—C3 | 110.8 (4) |
O2—S1—O3 | 111.8 (2) | C7—C6—H6A | 109.5 |
O1—S1—C7 | 105.8 (2) | C3—C6—H6A | 109.5 |
O2—S1—C7 | 107.2 (2) | C7—C6—H6B | 109.5 |
O3—S1—C7 | 105.4 (2) | C3—C6—H6B | 109.5 |
Cu1—O1W—H1WA | 109.4 | H6A—C6—H6B | 108.1 |
Cu1—O1W—H1WB | 133.6 | C6—C7—S1 | 112.0 (3) |
H1WA—O1W—H1WB | 106.5 | C6—C7—H7A | 109.2 |
Cu1—O2W—H2WA | 116.6 | S1—C7—H7A | 109.2 |
Cu1—O2W—H2WB | 112.1 | C6—C7—H7B | 109.2 |
H2WA—O2W—H2WB | 107.1 | S1—C7—H7B | 109.2 |
C1—N1—C5 | 117.6 (4) | H7A—C7—H7B | 107.9 |
C1—N1—Cu1 | 122.3 (3) | | |
Symmetry code: (i) −x+1, −y+1, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1WA···O2ii | 0.82 | 2.01 | 2.827 (5) | 179 |
O1W—H1WB···O3iii | 0.82 | 2.11 | 2.875 (5) | 157 |
O2W—H2WA···O1iv | 0.81 | 1.94 | 2.742 (5) | 176 |
O2W—H2WB···O3ii | 0.81 | 1.90 | 2.713 (4) | 175 |
Symmetry codes: (ii) x+1, −y+1/2, z−1/2; (iii) x+1, y, z; (iv) −x, y−1/2, −z+1/2. |
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