The title complex, [Co(pyet)2(H2O)2](sac)2 (sac− is the saccharinate anion, C7H4NO3S−, and pyet is 2-pyridylethanol, C7H9NO) contains sac− ions and [Co(H2O)2(pyet)2]2+ cations, in which the Co2+ ion lies on a centre of symmetry and is octahedrally coordinated by two water and two neutral pyet molecules, which act as N- and O-donor bidentate ligands forming two symmetrically-related six-membered chelate rings. The crystal packing is determined by hydrogen bonding, as well as weak sac−–sac− π–π-stacking interactions, resulting in a three-dimensional network.
Supporting information
CCDC reference: 202279
Key indicators
- Single-crystal X-ray study
- T = 133 K
- Mean (C-C) = 0.002 Å
- R factor = 0.026
- wR factor = 0.074
- Data-to-parameter ratio = 19.7
checkCIF results
No syntax errors found
ADDSYM reports no extra symmetry
General Notes
ABSTM_02 When printed, the submitted absorption T values will be replaced
by the scaled T values. Since the ratio of scaled T's is
identical to the ratio of reported T values, the scaling does
not imply a change to the absorption corrections used in the
study.
Ratio of Tmax expected/reported 0.949
Tmax scaled 0.880 Tmin scaled 0.790
Previously prepared [Co(sac)2(H2O)4]·2H2O (1.0 mmol, 0.53 g) was dissolved in methanol (30 ml) at 303 K with stirring. Pyet (0.25 g, 2.0 mmol) was then added to the solution dropwise. The resulting solution was left to stand at room temperature and allowed to evaporate slowly for crystallization. Yellow single crystals, obtained within a week, were collected by suction filtration, washed with acetone and dried in air.
The H atoms of the hydroxyl group and water molecules were refined freely, while H atoms bonded to carbon were included using a riding model, starting from calculated positions.
Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP (Siemens, 1994); software used to prepare material for publication: SHELXL97.
trans-Diaquabis(2-pyridylethanol-N,
O)cobalt(II) disaccharinate
top
Crystal data top
[Co(C7H9NO)2(H2O)2]·(C7H4NO3S)2 | F(000) = 730 |
Mr = 705.61 | Dx = 1.603 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 8.8391 (6) Å | Cell parameters from 7972 reflections |
b = 8.7910 (6) Å | θ = 2.2–30.5° |
c = 19.1564 (12) Å | µ = 0.80 mm−1 |
β = 100.876 (3)° | T = 133 K |
V = 1461.80 (17) Å3 | Prism, yellow |
Z = 2 | 0.24 × 0.21 × 0.16 mm |
Data collection top
Bruker SMART 1000CCD diffractometer | 4281 independent reflections |
Radiation source: fine-focus sealed tube | 3827 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.024 |
Detector resolution: 8.192 pixels mm-1 | θmax = 30.0°, θmin = 2.2° |
ω and ψ scans | h = −12→12 |
Absorption correction: multi-scan (SADABS; Bruker, 1998) | k = −12→12 |
Tmin = 0.833, Tmax = 0.928 | l = −26→26 |
27599 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)] = 0.026 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.074 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0486P)2 + 0.2616P] where P = (Fo2 + 2Fc2)/3 |
4281 reflections | (Δ/σ)max = 0.001 |
217 parameters | Δρmax = 0.48 e Å−3 |
0 restraints | Δρmin = −0.26 e Å−3 |
Crystal data top
[Co(C7H9NO)2(H2O)2]·(C7H4NO3S)2 | V = 1461.80 (17) Å3 |
Mr = 705.61 | Z = 2 |
Monoclinic, P21/n | Mo Kα radiation |
a = 8.8391 (6) Å | µ = 0.80 mm−1 |
b = 8.7910 (6) Å | T = 133 K |
c = 19.1564 (12) Å | 0.24 × 0.21 × 0.16 mm |
β = 100.876 (3)° | |
Data collection top
Bruker SMART 1000CCD diffractometer | 4281 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 1998) | 3827 reflections with I > 2σ(I) |
Tmin = 0.833, Tmax = 0.928 | Rint = 0.024 |
27599 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.026 | 0 restraints |
wR(F2) = 0.074 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.04 | Δρmax = 0.48 e Å−3 |
4281 reflections | Δρmin = −0.26 e Å−3 |
217 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 | Uiso*/Ueq | |
Co | 0.0000 | 0.0000 | 0.0000 | 0.01265 (6) | |
N2 | 0.02941 (10) | 0.15987 (10) | 0.08506 (5) | 0.01490 (17) | |
C31 | −0.01232 (13) | 0.30566 (12) | 0.07006 (6) | 0.0175 (2) | |
H31 | −0.0532 | 0.3318 | 0.0221 | 0.021* | |
C32 | 0.00145 (14) | 0.41910 (13) | 0.12106 (6) | 0.0222 (2) | |
H32 | −0.0299 | 0.5203 | 0.1084 | 0.027* | |
C33 | 0.06199 (14) | 0.38164 (14) | 0.19102 (7) | 0.0241 (2) | |
H33 | 0.0748 | 0.4571 | 0.2271 | 0.029* | |
C34 | 0.10366 (13) | 0.23149 (14) | 0.20731 (6) | 0.0206 (2) | |
H34 | 0.1455 | 0.2034 | 0.2549 | 0.025* | |
C35 | 0.08391 (12) | 0.12232 (12) | 0.15362 (5) | 0.01612 (19) | |
C36 | 0.11448 (13) | −0.04329 (13) | 0.17096 (6) | 0.0191 (2) | |
H36A | 0.1455 | −0.0547 | 0.2231 | 0.023* | |
H36B | 0.2015 | −0.0779 | 0.1491 | 0.023* | |
C37 | −0.02479 (14) | −0.14470 (13) | 0.14480 (6) | 0.0198 (2) | |
H37A | −0.0130 | −0.2425 | 0.1709 | 0.024* | |
H37B | −0.1197 | −0.0944 | 0.1536 | 0.024* | |
O3 | −0.03640 (10) | −0.17190 (9) | 0.07002 (4) | 0.01774 (16) | |
H3 | −0.112 (2) | −0.226 (2) | 0.0539 (9) | 0.032 (4)* | |
O4 | 0.23746 (9) | −0.04935 (9) | 0.01561 (4) | 0.01771 (15) | |
H4A | 0.2684 (19) | −0.077 (2) | −0.0203 (9) | 0.031 (4)* | |
H4B | 0.294 (2) | 0.026 (2) | 0.0285 (10) | 0.036 (5)* | |
C11 | 0.41880 (13) | 0.62431 (13) | 0.07653 (6) | 0.0213 (2) | |
H11 | 0.3390 | 0.6637 | 0.0408 | 0.026* | |
C12 | 0.51630 (14) | 0.72119 (13) | 0.12240 (7) | 0.0233 (2) | |
H12 | 0.5032 | 0.8282 | 0.1177 | 0.028* | |
C13 | 0.63265 (14) | 0.66257 (13) | 0.17506 (6) | 0.0220 (2) | |
H13 | 0.6973 | 0.7307 | 0.2057 | 0.026* | |
C14 | 0.65615 (13) | 0.50620 (12) | 0.18372 (6) | 0.0189 (2) | |
H14 | 0.7354 | 0.4661 | 0.2195 | 0.023* | |
C15 | 0.55799 (12) | 0.41189 (12) | 0.13750 (5) | 0.01575 (19) | |
C16 | 0.44227 (12) | 0.46856 (12) | 0.08480 (6) | 0.0166 (2) | |
C21 | 0.35517 (12) | 0.34171 (12) | 0.04223 (6) | 0.0168 (2) | |
O21 | 0.24834 (9) | 0.36658 (10) | −0.00873 (4) | 0.02187 (17) | |
N1 | 0.40596 (11) | 0.20193 (11) | 0.06525 (5) | 0.01859 (18) | |
S1 | 0.54759 (3) | 0.21147 (3) | 0.132127 (13) | 0.01590 (7) | |
O1 | 0.50754 (11) | 0.14871 (10) | 0.19589 (5) | 0.02510 (18) | |
O2 | 0.68657 (10) | 0.14789 (10) | 0.11397 (5) | 0.02422 (18) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co | 0.01476 (10) | 0.01067 (10) | 0.01197 (10) | −0.00001 (6) | 0.00116 (7) | −0.00045 (6) |
N2 | 0.0152 (4) | 0.0141 (4) | 0.0150 (4) | −0.0006 (3) | 0.0017 (3) | −0.0011 (3) |
C31 | 0.0178 (5) | 0.0147 (5) | 0.0195 (5) | −0.0001 (4) | 0.0022 (4) | −0.0017 (4) |
C32 | 0.0236 (5) | 0.0153 (5) | 0.0268 (6) | 0.0022 (4) | 0.0023 (4) | −0.0053 (4) |
C33 | 0.0245 (6) | 0.0220 (5) | 0.0247 (6) | 0.0007 (4) | 0.0014 (4) | −0.0102 (4) |
C34 | 0.0208 (5) | 0.0241 (5) | 0.0160 (5) | 0.0001 (4) | 0.0010 (4) | −0.0048 (4) |
C35 | 0.0144 (4) | 0.0177 (5) | 0.0158 (5) | −0.0005 (4) | 0.0014 (4) | −0.0018 (4) |
C36 | 0.0226 (5) | 0.0184 (5) | 0.0146 (5) | 0.0020 (4) | −0.0013 (4) | 0.0002 (4) |
C37 | 0.0275 (5) | 0.0165 (5) | 0.0152 (5) | −0.0036 (4) | 0.0036 (4) | 0.0011 (4) |
O3 | 0.0220 (4) | 0.0161 (4) | 0.0141 (3) | −0.0044 (3) | 0.0007 (3) | −0.0001 (3) |
O4 | 0.0169 (4) | 0.0155 (4) | 0.0202 (4) | −0.0012 (3) | 0.0022 (3) | −0.0030 (3) |
C11 | 0.0219 (5) | 0.0170 (5) | 0.0242 (5) | −0.0004 (4) | 0.0019 (4) | 0.0021 (4) |
C12 | 0.0270 (6) | 0.0145 (5) | 0.0287 (6) | −0.0013 (4) | 0.0057 (5) | −0.0006 (4) |
C13 | 0.0233 (5) | 0.0196 (5) | 0.0234 (5) | −0.0052 (4) | 0.0048 (4) | −0.0058 (4) |
C14 | 0.0181 (5) | 0.0203 (5) | 0.0176 (5) | −0.0021 (4) | 0.0018 (4) | −0.0026 (4) |
C15 | 0.0172 (5) | 0.0140 (5) | 0.0164 (5) | −0.0016 (3) | 0.0039 (4) | −0.0011 (3) |
C16 | 0.0165 (5) | 0.0156 (5) | 0.0177 (5) | −0.0023 (4) | 0.0030 (4) | −0.0005 (4) |
C21 | 0.0166 (5) | 0.0178 (5) | 0.0159 (5) | −0.0036 (4) | 0.0028 (4) | −0.0001 (4) |
O21 | 0.0200 (4) | 0.0230 (4) | 0.0202 (4) | −0.0044 (3) | −0.0021 (3) | 0.0017 (3) |
N1 | 0.0197 (4) | 0.0157 (4) | 0.0189 (4) | −0.0035 (3) | −0.0001 (3) | −0.0017 (3) |
S1 | 0.01744 (12) | 0.01355 (12) | 0.01630 (12) | −0.00060 (8) | 0.00215 (9) | −0.00014 (8) |
O1 | 0.0318 (4) | 0.0233 (4) | 0.0201 (4) | −0.0033 (3) | 0.0050 (3) | 0.0057 (3) |
O2 | 0.0207 (4) | 0.0230 (4) | 0.0286 (4) | 0.0040 (3) | 0.0037 (3) | −0.0057 (3) |
Geometric parameters (Å, º) top
Co—O3 | 2.0855 (8) | O3—H3 | 0.827 (18) |
Co—O4 | 2.1087 (8) | O4—H4A | 0.823 (17) |
Co—N2 | 2.1303 (9) | O4—H4B | 0.839 (19) |
N2—C31 | 1.3495 (13) | C11—C16 | 1.3894 (15) |
N2—C35 | 1.3517 (13) | C11—C12 | 1.3980 (16) |
C31—C32 | 1.3853 (15) | C11—H11 | 0.9500 |
C31—H31 | 0.9500 | C12—C13 | 1.3963 (17) |
C32—C33 | 1.3857 (17) | C12—H12 | 0.9500 |
C32—H32 | 0.9500 | C13—C14 | 1.3955 (16) |
C33—C34 | 1.3899 (17) | C13—H13 | 0.9500 |
C33—H33 | 0.9500 | C14—C15 | 1.3908 (14) |
C34—C35 | 1.3934 (15) | C14—H14 | 0.9500 |
C34—H34 | 0.9500 | C15—C16 | 1.3871 (15) |
C35—C36 | 1.5064 (15) | C15—S1 | 1.7663 (11) |
C36—C37 | 1.5260 (16) | C16—C21 | 1.5047 (15) |
C36—H36A | 0.9900 | C21—O21 | 1.2429 (13) |
C36—H36B | 0.9900 | C21—N1 | 1.3533 (14) |
C37—O3 | 1.4368 (13) | N1—S1 | 1.6156 (10) |
C37—H37A | 0.9900 | S1—O1 | 1.4439 (9) |
C37—H37B | 0.9900 | S1—O2 | 1.4505 (9) |
| | | |
O3i—Co—O3 | 180.00 | C36—C37—H37B | 109.9 |
O3i—Co—O4 | 88.28 (3) | H37A—C37—H37B | 108.3 |
O3—Co—O4 | 91.72 (3) | C37—O3—Co | 122.01 (6) |
O4i—Co—O4 | 180.00 | C37—O3—H3 | 111.6 (11) |
O3i—Co—N2 | 90.15 (3) | Co—O3—H3 | 112.6 (12) |
O3—Co—N2 | 89.85 (3) | Co—O4—H4A | 114.9 (12) |
O4i—Co—N2 | 86.98 (3) | Co—O4—H4B | 113.5 (13) |
O4—Co—N2 | 93.02 (3) | H4A—O4—H4B | 102.0 (17) |
N2i—Co—N2 | 180.00 | C16—C11—C12 | 117.88 (11) |
C31—N2—C35 | 118.16 (9) | C16—C11—H11 | 121.1 |
C31—N2—Co | 118.33 (7) | C12—C11—H11 | 121.1 |
C35—N2—Co | 123.49 (7) | C13—C12—C11 | 120.79 (11) |
N2—C31—C32 | 123.32 (10) | C13—C12—H12 | 119.6 |
N2—C31—H31 | 118.3 | C11—C12—H12 | 119.6 |
C32—C31—H31 | 118.3 | C14—C13—C12 | 121.48 (11) |
C31—C32—C33 | 118.52 (11) | C14—C13—H13 | 119.3 |
C31—C32—H32 | 120.7 | C12—C13—H13 | 119.3 |
C33—C32—H32 | 120.7 | C15—C14—C13 | 116.78 (10) |
C32—C33—C34 | 118.71 (10) | C15—C14—H14 | 121.6 |
C32—C33—H33 | 120.6 | C13—C14—H14 | 121.6 |
C34—C33—H33 | 120.6 | C16—C15—C14 | 122.35 (10) |
C33—C34—C35 | 119.82 (10) | C16—C15—S1 | 107.02 (8) |
C33—C34—H34 | 120.1 | C14—C15—S1 | 130.62 (9) |
C35—C34—H34 | 120.1 | C15—C16—C11 | 120.71 (10) |
N2—C35—C34 | 121.40 (10) | C15—C16—C21 | 111.09 (9) |
N2—C35—C36 | 117.81 (9) | C11—C16—C21 | 128.20 (10) |
C34—C35—C36 | 120.70 (10) | O21—C21—N1 | 124.88 (10) |
C35—C36—C37 | 113.09 (9) | O21—C21—C16 | 122.04 (10) |
C35—C36—H36A | 109.0 | N1—C21—C16 | 113.08 (9) |
C37—C36—H36A | 109.0 | C21—N1—S1 | 111.78 (7) |
C35—C36—H36B | 109.0 | O1—S1—O2 | 114.18 (5) |
C37—C36—H36B | 109.0 | O1—S1—N1 | 111.96 (5) |
H36A—C36—H36B | 107.8 | O2—S1—N1 | 110.76 (5) |
O3—C37—C36 | 109.03 (9) | O1—S1—C15 | 110.51 (5) |
O3—C37—H37A | 109.9 | O2—S1—C15 | 111.17 (5) |
C36—C37—H37A | 109.9 | N1—S1—C15 | 97.01 (5) |
O3—C37—H37B | 109.9 | | |
| | | |
O3i—Co—N2—C31 | 30.65 (8) | C16—C11—C12—C13 | −0.45 (18) |
O3—Co—N2—C31 | −149.35 (8) | C11—C12—C13—C14 | 0.19 (19) |
O4i—Co—N2—C31 | −61.06 (8) | C12—C13—C14—C15 | −0.12 (18) |
O4—Co—N2—C31 | 118.94 (8) | C13—C14—C15—C16 | 0.34 (16) |
O3i—Co—N2—C35 | −151.16 (8) | C13—C14—C15—S1 | −178.67 (9) |
O3—Co—N2—C35 | 28.84 (8) | C14—C15—C16—C11 | −0.62 (17) |
O4i—Co—N2—C35 | 117.13 (8) | S1—C15—C16—C11 | 178.59 (9) |
O4—Co—N2—C35 | −62.87 (8) | C14—C15—C16—C21 | 179.35 (10) |
C35—N2—C31—C32 | 1.63 (16) | S1—C15—C16—C21 | −1.44 (11) |
Co—N2—C31—C32 | 179.93 (9) | C12—C11—C16—C15 | 0.66 (17) |
N2—C31—C32—C33 | 0.42 (18) | C12—C11—C16—C21 | −179.30 (11) |
C31—C32—C33—C34 | −1.18 (18) | C15—C16—C21—O21 | −178.52 (10) |
C32—C33—C34—C35 | −0.07 (18) | C11—C16—C21—O21 | 1.44 (18) |
C31—N2—C35—C34 | −2.93 (15) | C15—C16—C21—N1 | 1.26 (13) |
Co—N2—C35—C34 | 178.88 (8) | C11—C16—C21—N1 | −178.77 (11) |
C31—N2—C35—C36 | 173.71 (10) | O21—C21—N1—S1 | 179.40 (9) |
Co—N2—C35—C36 | −4.49 (13) | C16—C21—N1—S1 | −0.38 (12) |
C33—C34—C35—N2 | 2.19 (17) | C21—N1—S1—O1 | 115.05 (8) |
C33—C34—C35—C36 | −174.34 (10) | C21—N1—S1—O2 | −116.26 (8) |
N2—C35—C36—C37 | −54.12 (13) | C21—N1—S1—C15 | −0.42 (9) |
C34—C35—C36—C37 | 122.54 (11) | C16—C15—S1—O1 | −115.50 (8) |
C35—C36—C37—O3 | 79.19 (11) | C14—C15—S1—O1 | 63.62 (12) |
C36—C37—O3—Co | −41.79 (12) | C16—C15—S1—O2 | 116.64 (8) |
O4i—Co—O3—C37 | −90.33 (8) | C14—C15—S1—O2 | −64.24 (12) |
O4—Co—O3—C37 | 89.67 (8) | C16—C15—S1—N1 | 1.13 (8) |
N2i—Co—O3—C37 | 176.65 (8) | C14—C15—S1—N1 | −179.74 (11) |
N2—Co—O3—C37 | −3.35 (8) | | |
Symmetry code: (i) −x, −y, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
C32—H32···O21ii | 0.95 | 2.64 | 3.3559 (15) | 133 |
C33—H33···O1iii | 0.95 | 2.44 | 3.3295 (14) | 156 |
O4—H4A···O2iv | 0.823 (17) | 2.010 (18) | 2.8270 (12) | 172 (1) |
O3—H3···O21i | 0.827 (18) | 1.830 (18) | 2.6433 (11) | 168 (1) |
Symmetry codes: (i) −x, −y, −z; (ii) −x, −y+1, −z; (iii) −x+1/2, y+1/2, −z+1/2; (iv) −x+1, −y, −z. |
Experimental details
Crystal data |
Chemical formula | [Co(C7H9NO)2(H2O)2]·(C7H4NO3S)2 |
Mr | 705.61 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 133 |
a, b, c (Å) | 8.8391 (6), 8.7910 (6), 19.1564 (12) |
β (°) | 100.876 (3) |
V (Å3) | 1461.80 (17) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 0.80 |
Crystal size (mm) | 0.24 × 0.21 × 0.16 |
|
Data collection |
Diffractometer | Bruker SMART 1000CCD diffractometer |
Absorption correction | Multi-scan (SADABS; Bruker, 1998) |
Tmin, Tmax | 0.833, 0.928 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 27599, 4281, 3827 |
Rint | 0.024 |
(sin θ/λ)max (Å−1) | 0.704 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.026, 0.074, 1.04 |
No. of reflections | 4281 |
No. of parameters | 217 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.48, −0.26 |
Selected geometric parameters (Å, º) topCo—O3 | 2.0855 (8) | Co—N2 | 2.1303 (9) |
Co—O4 | 2.1087 (8) | | |
| | | |
O3i—Co—O4 | 88.28 (3) | O3—Co—N2 | 89.85 (3) |
O3—Co—O4 | 91.72 (3) | O4i—Co—N2 | 86.98 (3) |
O3i—Co—N2 | 90.15 (3) | O4—Co—N2 | 93.02 (3) |
Symmetry code: (i) −x, −y, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
C32—H32···O21ii | 0.95 | 2.64 | 3.3559 (15) | 133 |
C33—H33···O1iii | 0.95 | 2.44 | 3.3295 (14) | 156 |
O4—H4A···O2iv | 0.823 (17) | 2.010 (18) | 2.8270 (12) | 172 (1) |
O3—H3···O21i | 0.827 (18) | 1.830 (18) | 2.6433 (11) | 168 (1) |
Symmetry codes: (i) −x, −y, −z; (ii) −x, −y+1, −z; (iii) −x+1/2, y+1/2, −z+1/2; (iv) −x+1, −y, −z. |
Saccharin, chemically known o-sulfobenzimide, is the most widely used artificial sweetener. Its deprotonated form, the saccharinate anion (C7H4NO3S)− (sac), readily coordinates to metal ions, forming stable metal complexes in the solid state. This study is a continuation of our research on the synthesis and structural characterization of complexes of metal saccharinates with other ligands containing hydroxymethyl and hydroxyethyl groups, such as monoethanolamine (Andac et al., 2000, Yilmaz, Andac et al., 2001; Yilmaz, Topcu et al., 2001), monoethanolethylenediamine (Yilmaz et al., 2002), diethanolamine (Yilmaz, Topcu et al., 2001), triethanolamine (Topcu et al., 2001), dimethanolpyridine (Andac et al., 2002) and 2-pyridylethanol (Hamamci et al., 2002a). In this paper, we report the crystal structure of 2-pyridylethanol (pyet) complex of cobalt(II) saccharinate, viz. [Co(H2O)2(pyet)2](sac)2, (I).
The structure of (I) is shown in Fig. 1, and consists of a complex cation, [Co(H2O)2(pyet)2]2+, and two sac anions. In the complex cation, the CoII ion lies on an inversion centre and is octahedrally coordinated by a pair of neutral pyet ligands and two water molecules, forming a CoN2O4 core. The sac ions are not in the primary coordination sphere, being as a counter-ion. Each pyet ligand behaves as a bidentate ligand through the N and hydroxyl O atoms, forming a six-membered chelate ring around the CoII ions. The two pyet ligands form the equatorial plane of the coordination octahedron, while two water molecules occupy the axial positions with a trans configuration. Some distortion of the metal coordination sphere from regular octahedral geometry is apparent, especially at the Owater—Co—Npyet angles (Table 1).
Both sac (C11–C16/C21/O21/N1/S1) and pyet (C31–C36/N2) are essentially planar, with an r.m.s. deviation of ca 0.01 and 0.04 Å, respectively, but the OH group deviates significantly from the pyet plane by ca 1.00 Å. Furthermore, the Co2+ ion is coplanar with the pyet plane. The crystal packing of the title compound is shown in Fig. 2. The crystal packing exhibits parallel stacking of pairs of the sac ions and therefore, results in weak π–π interactions (Cg···Cg > 4.0 Å). The H atoms of the water molecules (O4) and hydroxyl group (O3) of pyet form O—H···O hydrogen bonds with the sulfonyl O (O1) and carbonyl (O21) O atom of neighbouring sac anions. Additionally, two weak C—H···O interactions between H atoms of the pyridine ring and the carbonyl and sulfonyl O atoms of the adjacent sac ions occur. The hydrogen bonds and weak π-π interactions stabilize the crystal structure, forming a three-dimensional network.
The title compound is isostructural with the corresponding cobalt(II) complex (Hamamci et al., 2002b).